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BrAiNFeVeR
October 13th, 2002, 03:55 PM
Diphoronepentaperoxide(DPPP)

The compound currently being discussed at the madscience forum raises big interest: the starting materials acetone, conc. HCl and 30% H2O2 are (dirt-) cheap, and the substance performs an incredible vod of about 9000m/s.

Other favourable properties, like better stability than AP, are listed in the following german patent of the late 70`(translation by Hoffmann-LaRoche):

German patent DE 1951660.

1969

Diphoronepentaperoxide C18H26O2(O2)5

Field of invention: the invention refers to an explosive which has special properties that make it suitable especially for mining and as well for military purposes.

Task: The invention wants to make blasting operations cheaper and easier.

Solution: Following cheap substances are required for synthesis:

1 part conc. hydrochloric acid(HCl)
1 part acetone (CH3COCH3)
2 parts 30% hydrogen peroxide(H2O2)


Process of manufacture:

1 part of acetone are added to 1 part hydrochloric acid, through which acetone polymerizes to phoron; then 2 parts of hydrogen peroxide are added, through which two molecules of HCl bond with the two C-double-bonds of the phoron.

In the course of the reaction free chlorine
develops, which bonds with 3 hydrogen atoms of the phoron to give 3 HCl(see drawing) and bonds itself with phoron.
Hydrogen peroxide causes the chlorine atoms to split off the phoron and the peroxide itself bonds with the phoron.

Because of the fact, that one peroxy-bond stays half-opened, one also open phoronperoxide adds to give diphoronpentaperoxide, which precipitates from the solution in crystalline form.


Properties:

a) insoluble in water
b) still explosive when heavily contaminated
c) detonation velocity approx. 9000m/s
d) low detonation temperature approx. 200°C
e) does not develop smoke upon detonation, does not smell, no solid residues.
f) ignition by fire, blasting cap or electric
g) does not decompose at long storage
h) yield of manufacturing process approx. 90%

I have to mention that this was already discussed a bit in the medina-thread of high explosives, but stopped in the early stage and deserves an own thread.
The madscience thread shows a lot of progress, on the synthesis of phorone for instance.

<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=179" target="_blank">DPPP thread on mad sci</a>
<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=228" target="_blank">Phorone thread on mad sci</a>

I do not take the credit for this post, I just wanted to make sure this exiting new energetic substance is opened up to as wide as possible of an audience.
This message is posted on usenet too for exactly the same purpose.

Rat Bastard
October 13th, 2002, 04:33 PM
Is there more detail on the synth, because it does not state anything about temprature control, or how fast the H202 is added, ect. ect.

Call me paranoid, but I don't like vaugeness.

<small>[ October 13, 2002, 03:41 PM: Message edited by: Rat Bastard ]</small>

BrAiNFeVeR
October 13th, 2002, 04:52 PM
That's where the "research" comes into play ...

When the patent is followed stricly, you will get mostly AP, and very little DPPP, that's why the most common thought is to first prepare phorone, then dissolve that in HCl solution, and then add the peroxide.

The production of phorone is allready succesful, (and thus it is easy to produce DPPP from that) but still we need more data on the reaction and the required quantities/PH-values/...

And then we can compose a good production manual from this!

H2O2
October 13th, 2002, 11:11 PM
sounds interesting for sure!

Boob Raider
October 14th, 2002, 01:58 AM
Lets say I try making Diphoronepentaperoxide ...... How would I know that DPPP is formed and NOT AP. What differences does it have compared to AP. Color, crystaline structure, solubility, etc.....
Now that you mention it brainfever whenever I made AP I added H2SO4 first to the Acetone (I don't know if HCl is crucial for DPPP synth) but my AP never dissolved in acetone, a shit load of product per batch, it (~150g) didn't decompose on me even after 7 months in a glass jar with room temp of 40*C. It would detonate even when wet, and would detonate ~ 20*C beyond the product's melting pt. It had a peculiar smell but on ignition it was odorless and left no residue. I did mention this in my previous posts when I had the name Ezikiel.

IPN
October 14th, 2002, 08:42 AM
This is how I would do it
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">preparation:
To a 1000 ml erlenmeyer flask add 185 ml of 20% HCl (i don`t
have 35% HCl at this time). To a second flask add 100 ml of aceton.
To an third flask add 200 ml of 30% H2O2. Cool all to 5 C.
After cooling, slowly add the aceton to the HCl and stir the mixture
for 5 minutes.(very slight yellow colouring over a few minutes)
The patent don`t say heat at this time and the patent don`t say
some product (poron) should precipitate from the solution at this time.
If you heat or not, the content of AP are always present at end of the synthesis. On the contrary, if you heat to much or to long, the reaction fails.
Cool the mixture to 5 C for 2 hours and stir occasionally.
After standing, set the mixture to magnetic stirring at room
temperature and slowly (over 10 minutes) add the H2O2 to the
aceton/HCl mixture. The temperature can rise over 40 C and
the mixture become a sligth green colouring.
(second reaction-step, formation of pentachlorporon and free
Cl with H2O2 as catalyst)
The DPPP should precipitate on top of the mixture and some fumes bubble of.
You can distinguish this of AP crystalls, which formes in the reaction-mixture and which are a bit larger than crystals of DPPP.
After all H2O2 is added, continue stirring for 2 hours an more till the liquid on the bottom of the flask are clear and no fumes bubble of.
Filter out the crystals, wash them with 1 L of 10 % sodium bicarbonate solution, and again with water.
Dry crystals of DPPP at room temperature for 48 hours.
The next step are very important to remove all traces of acid and AP in the product, that you can handle safe with DPPP.
Dissolving the crystals in minimum amount of hot ethyl alcohol (60 C),
let cool to 5 C, filter, add a large volume of cold distilled water, let sit for 1-2 hours below 10 C and filter again.
Let dry DPPP at room temperature for 1-2 weeks to decompose and evaporate the rest of AP on the air.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">

BrAiNFeVeR
October 14th, 2002, 09:24 AM
I actually tried that sublimation method, but on a far smaller scale.

I had a beginning of 5 grams of product or something, it's been lying in a moderately warm area (15-20°C) for more then 3 weeks now, and it still smell alot like AP, and on detonation, still gives the characteristic AP-just-detonated-here smell ...

That plus the hazard of having a large amount of primary to start with on in a warm place !!

Conclusion: this is not the method to go, there's just too much AP that has to sublimate ...

Madog555
October 14th, 2002, 10:47 AM
what concentration H2O2 do you use? i used 12%, with adjusted ratios, and it gave a real shit yield.

ALENGOSVIG1
October 14th, 2002, 01:33 PM
Is it just me, or is this just another recipie for AP? I've read in federoff that the reactants (H202, (CH3)2CO, and HCl) for AP can be added in any order. I think this is just another AP synthesis.

IPN
October 14th, 2002, 01:42 PM
No this is not a recipie for AP. This is much better. If you don´t believe me try mixing some acetone and HCL. Notice the yellow color that is phorone

BrAiNFeVeR
October 14th, 2002, 01:53 PM
IPN is right, this is definately not just another AP synth.

When mixing 35% HCl with acetone a yellow liquid is obtained, wich darkens when you boil it.

Phorone specs:
<a href="http://users.pandora.be/l.s/phoron.jpg" target="_blank">http://users.pandora.be/l.s/phoron.jpg</a>

It's pretty insoluble in water, but the HCl seems to make it more soluble. When adding a base, you can ppt out some yellow crystals which are most likely phorone.
Also, some oily substance can be noticed, I don't know what this is ...

The crystals of DPPP are supposed to be smaller then AP.

Mic
October 14th, 2002, 04:00 PM
hello all,
today i tried DPPP: I mix 10mL HCl (31%) with 10mL Acetone (99%). I heat it until the solution turn yellow. I cool it in the freezer and had 60mL H2O2 (9%). Nothing happen ! :( . no precipitation! I put it in the freezer until now. maybe my H2O2 is not enaugh concentrate. I will buy 35% H2O2 and gonna try this method again later.

nbk2000
October 14th, 2002, 05:50 PM
(Back when dinosaurs roamed the earth... :D )

I tried making chloroacetone (tear gas) by bubbling gaseous HCl through acetone. The acetone turned yellow and seperated out a heavier layer.

Over time (weeks) the liquid turned orange, then red, then finally such a deep shade of purple as to resemble motor oil, and just as opaque.

So, try bubbling HCl gas through the acetone, then treating with baquacil H2O2.

dave
October 14th, 2002, 05:51 PM
HOLY SH*T so simple! I have to try this once my hand heals. Sounds like a good alternative to AP. Got all the chemicals in my garage ready

Mic
October 14th, 2002, 08:33 PM
Hello,
I just check the solution in my freezer and some very small cristals (much smaller than AP cristal) are laying on the botom of the beaker! :) there is not much but maybe there's going to have more later!
Could it be DPPP ? or just AP?

ALENGOSVIG1
October 15th, 2002, 02:00 AM
I dont think crystal size will help you determine anything. If AP crystals were formed in a freezer over a long period of time they'd be tiny too.

I agree with nbk about bubbling the HCl gas throughtr the acetone. Just make a HCl gas generator as described here: <a href="http://www.rhodium.ws/chemistry/hcl-gas.html" target="_blank">http://www.rhodium.ws/chemistry/hcl-gas.html</a>

If you want to make it anhydrous, bubble the HCl throught some H2SO4 or pass the HCl gas throught a tube containing a descicant.

<small>[ October 16, 2002, 12:06 AM: Message edited by: ALENGOSVIG1 ]</small>

cutefix
October 15th, 2002, 04:34 AM
One thing that is hard to believe is the detonation velocity is extremely high for a peroxide: 9000 m/s Wow! I was wondering if the data did come from from anarchy archives. <img border="0" title="" alt="[Wink]" src="wink.gif" />
Did somebody of you guys manage to detonate it the same density and compare its performance versus the common homemade acetone peroxide?
If its indeed is powerful, the conservative rough estimate of its power is in the vicinity of would be around 6000-7000 m/s.
:)

inferno
October 15th, 2002, 05:00 AM
My HCl forms a yellow solution with acetone instantly...It is Digger's brand, and all people I know who use it get the same yellow colour, that almost resembles urine...

I am quite doubtful of this synth, I believe that the chemists actually prepared AP, and made a rough estimate of 9,000m/s VoD, being quite out on their judgement. Any explosive with that kind of velocity would be quite well known, even if it wasn't used by the military.

My 2 cents.

xyz
October 15th, 2002, 07:58 AM
Whenever I make AP the solution is always yellow and turns clear again when I neutralize it at the end.

I am not sure what brand my HCL is but I get it from a pool shop and it has the pool shop logo on it (there is only one of this pool shop too, it's not a chain like bunnings), it is conc. HCL by the way.

IPN
October 15th, 2002, 09:06 AM
That seems to be a good idea NBK that way both (acetone and HCL) will be almost 100% when mixing :D

Anthony
October 15th, 2002, 03:18 PM
Anyone heard of a primary with a VoD even close to 9000m/sec?

If this explosive was so powerful, stable, easy and cheap to manufature, then it would have industrial or military usage.

Sounds too good to be true to me, I reckon it's just AP.

IPN
October 15th, 2002, 03:37 PM
Why do you judge it if you haven´t tried it out or don´t know much about it?
I also think that the VoD isn´t going to be over 9000m/sec but it will be more than what AP has!
Personally I´m not going to try it out because i am mostly interested in information not in preparation.

TheBear
October 15th, 2002, 03:47 PM
The only way to be sure if it's as good as stated would be to try out ourselves, right?
Perhaps someone with a detcord could make an estimation. I think that this explosive might very well exist but 9000 m/s sounds too good to be true. Could some one whos wellequiped try it's shocksensitivity. I think I will do a test on ironplates comparing regular AP's brisance with this potentionally new explosives and post the results here. I hope I will be able to carry out these test sometime during the next two weeks.

Anthony, exactly what I thought too: Why isn't it being used if it's as good as stated?

Polverone
October 15th, 2002, 09:24 PM
If you just follow the patent directions you won't get much to write home about. I'm not willing to dismiss this entirely as fiction - somebody did bother to pay the money to file a patent, after all - but I think the actual manufacturing process is more involved than the patent indicates. As for why it never achieved wide use - well, it does have a poor oxygen balance, which would limit its overall power, even if the patent's vdet claims aren't exagerrated. On alt.engr.explosives one of the knowledgeable regulars ("Boomer") claimed the actual vdet is about 6,600 m/s, though I don't know his source. In the same thread, Philou Zrealone posted a fairly long message about the chemistry involved in producing DPPP. Basically, it sounds unlikely that the reaction actually proceeds in the way that the patent author imagined it proceeding.

So there's certainly potential for experimentation here, but it is not at all clear that the patent lives up to its claims.

IPN
October 16th, 2002, 01:53 AM
The reason for the VoD not being so high is that DPPP´s density is small so when it is highly packed it´s VoD will increase giving almost 9000m/sec (if i´m correct).

Flake2m
October 16th, 2002, 07:04 AM
This I gather is the formula for Diphoronepentaperoxide:
C<sub>18</sub>H<sub>26</sub>O<sub>2</sub>(O<sub>2</sub>)<sub>5</sub>

I have all the chemicals needed to make DPPP,30% H<sub>2</sub>O<sub>2</sub>, HCL and acetone. When ever I make AP I the solution always turns a yellow colour, I had always though that this might be to do will an Fe compound contaminating the mixture, but now I know that it is phoron. I am very intrested in this DPPP, If it is as powerful as the patent says and is more stable the AP then we all might be on to something <img border="0" title="" alt="[Wink]" src="wink.gif" /> . I will try synthesising this compound this weekend.

Microtek
October 16th, 2002, 07:55 AM
I mentioned this in the MEDINA thread, but I'll just summarize my findings. I prepared a batch of some kind of peroxide using the guidelines in the patent. I used 40 vol % H2O2, 30% HCl and acetone. The product obtained had the following properties:
- Flashed when ignited in the open just like AP, HMTD or NC.
- Was about as sensitive to impact as HMTD ( using a better test than I did at first ).
- Flashed without explosion when ignited in a 2.5 mm tube ( contrary to AP ).
- Was quite volatile and had evaporated almost completely over the course of about one month.
- Detonated when initiated with Ag2C2*AgNO3, but only flashed when initiated with lead styphnate.
- Exhibited much lower brisance in 2.5 mm coloumns than PETN.

IPN
October 16th, 2002, 10:41 AM
I see you didn´t let the AP to evaporate meaning bad results. If you would have purified the product your tests would have been different (if i´m correct).
Next time first prepare the phorone, purify it, add HCL and continue whith the prosedure.

nbk2000
October 16th, 2002, 12:03 PM
Well phorone has an M.P. of 26-29*C, so that's easy enough to let melt down. Then oxidize with H2O2, filter off, and...evaporate off AP? How DO you seperate the AP from the DPPP? Crystal size isn't going to help none.

IPN
October 16th, 2002, 12:52 PM
You just said it
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> Then oxidize with H2O2, filter off, and...evaporate off AP </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">It will evaporate because DPPP won´t

BLASTER
November 2nd, 2002, 04:43 PM
maybe vod should be 9000ft/s and not 9000m/s

Anthony
November 3rd, 2002, 09:27 AM
That would be 2743m/s ( :D ) in which case I'd doubt it would be worth pursuing and then I'd bet that is was just the dicyclo or mono version of AP :p

THErAPIST
November 15th, 2002, 01:44 AM
ok not really on topic here but i didnt want to make a new topic for fear of being deleted since i dont post all that much. but this has to do with peroxide so i figured id put it here.
i had a thought a couple days ago. would it be possible to have a peroxide and a nitrate type explosive? let me explain... say someone who has little reguard for their own life decided to mix H<sub>2</sub>O<sub>2</sub> with some H<sub>2</sub>SO<sub>4</sub> and some sort of nitrate then tried to make some kind of compound with the resulting mixture? I dont even know if having a peroxide nitrate is possible. it might be too unstable to exist for even a short time but if it were possible, the extra oxygen plus the nitrogen and other items in a compound could be a good thing. ive never heard or seen anything about a peroxide nitrate of any kind so if you have heard of something of the sort please let me know. i was thinking about attempting to make an HMTD type compound but i would like to have someone elses ideas and opinions about the subject. i always add a small amount of NH<sub>4</sub>NO<sub>3</sub> to my hexamethylenetetramine, citric acid, and peroxide when i make HMTD anyways since it seems to give a more powerful product, so i just thought of using H<sub>2</sub>SO<sub>4</sub>as a catalyst instead of the citric acid along with a little more xNO<sub>3</sub> to maybe somewhat nitrate. i dunno. its 1 in the morning and im trying to type this up as best i can without confusing anyone and without looking extremely stupid. but theres my thought. any imput would be appreciated. :(

edit: put in UBB code instead of HTML code for the subs

<small>[ November 15, 2002, 04:53 AM: Message edited by: nbk2000 ]</small>

carbonated
November 15th, 2002, 10:39 PM
I'm pretty sure somewhere on the forum it says HMTD can be used to make RDX. Other than that, I have no idea, but since that is possible, maybe others are.

THErAPIST
December 2nd, 2002, 01:03 PM
oh... an update since i had the idea. i put 90 mL of 6% peroxide into a mason jar and then i added the 5 heaping teaspoons of hex along with 2 heaping teaspoons of NH4NO3 and another 45 mL of 30% H2SO4. when i added the sulfuric the whole thing turned yellow like orange juice and then got really really cloudy, so i let it set there for a few minutes. within about 10 minutes i had some yellow fluffy precipitate on the bottom and top of the liquid, so i let it sit there another 3 hours. then I went and filtered and washed the stuff. the stuff was yellow to start with but the more i ran water thrue it the more white it got. then when i added the 10% sodium bicarb it got pretty much pure white. so i dried it and all and then went and pressed 2 grams (i made 2 batches) into a plastic drinking straw. I fused it and then took it and an acorn squash out into the woods. i stabbed a hole in the squash with a pencil when i was on the way there. when i got there i put the extremely large blasting cap inside the hole, lit the fuse and trotted off about 100 feet. when it went off it didnt make much noise at all but ill be damned if the squash didnt get obliterated. the biggest piece i found was about as big as a marble, and not ona those big marbles either. not to mention the piece was some 70 feet away. the dirt where it had been sitting was pretty messed up too. in my opinion it was more powerful than HMTD but i dont know how to conduct many tests to prove this. im gonna make a gram charge of both and set them on the same thing to test bristance and such sometime soon though. the crystals seem to be slightly smaller than those of HMTD also. anyone care to give me some ideas on how to test the stuff? or maybe make a batch yourself and test it? whatever. just makin an update. ill get the pics up when i can. cant find my fire wire <img border="0" title="" alt="[Frown]" src="frown.gif" />

<small>[ December 02, 2002, 12:07 PM: Message edited by: THErAPIST ]</small>

NERV
December 2nd, 2002, 05:13 PM
It’s possible that the NH4NO3 is mixing with your finished HMTD forming a fuse sensitive AN/HMTD mix. That would explain the power increase. Although I would think that the AN would be washed away during the rinsing step. I might try to make this stuff and compare it to a normal batch of HMTD.

On the subject of DPPP, I attempted to make it about a month ago. I never got to posting my results though. I mixed about 10ml of Acetone with 10ml of HCl. I left that standing far about an hour, at that point it had turned a beautiful urine yellow. I then added about 20 ml of H2O2 to the mix in an ice bath. The solution turned cloudy and started to warm up. After about 2 hour’s I filtered the product out. I placed it on top of our central heating system for a week to evaporate impurities. About half of the original materiel was gone at the end of the week. I loaded what was left (about 10 grams) into a paper tube and set it off in the woods next to my house. When I went to the detonation site I found the AP just detonated here odor in the air. I think that all I got was AP I am planning on trying it again with all the new developments on the manufacture.

THErAPIST
December 2nd, 2002, 08:00 PM
yea im gonna try to make somee DPPP when i can get the time and cash. i went to madscientists forum ands someone there said they had some success with makin the stuff so i copied what the guy said he did. at the moment though im a little more supriseed that ona my ideas worked. so im gonna do a little more eexperimenting with whatever it is i made before i go to the DPPP. does anyone even know what the stuff i made would be called? i dont have the slightest clue.

ShockWave
December 2nd, 2002, 08:08 PM
I have done the same thing, After adding the H2o2 there was lot of with powder, after drying I found out that this stuff evaporated much Faster then AP, and it wasn't really crystalline, like AP, so I still don't know what it was.

Anthony
December 2nd, 2002, 08:59 PM
Congrats, you've all made HMTD! :D

ShockWave
December 3rd, 2002, 07:15 AM
well, I think you are right !!

Now that I am thinking about it, it was a bit yellow and it didn't burn very extreme like my AP, when I lighted a bit it was more WHOOM instead of Bhoem.

But... It evaporated much much faster then AP, and I thought that AP evaporated faster then HMTD.

Anyway, If this is really HMTD, than it is the most simple way to make it, and the fastest way, and a very good yield for HMTD !

THErAPIST
December 3rd, 2002, 12:33 PM
correct me if im wrong but i thought you were using acetone and not hexamethylenetetramine. acetone wouldnt make HMTD in any way shape or form.

ShockWave
December 3rd, 2002, 12:36 PM
<img border="0" title="" alt="[Eek!]" src="eek.gif" /> <img border="0" title="" alt="[Eek!]" src="eek.gif" />

How stupid of me, I totally forgot, But it looks Like HMTD, and burns like HMTD

THErAPIST
December 3rd, 2002, 01:56 PM
the DPPP stuff burns pretty damn fast with a flash. or at least thats whats stated on madscientists board. ill type the procedure here when i get home from school.

[:edit:]
this is what i got from the other bored. you may want to scale this preperation down a little though since it was said that the final yield was 65 grams

To a 1000 mL erlenmeyer flask add 185 mL of 20% HCL. to a second flask add 100 mL of acetone. to a third flask add 200 mL of 30% H2O2. cool it all to 5ºC. after cooling slowly add the acetone to the HCL and stir the mixture for 5 minutes. (it should turn a slight yellow color over a few minutes). cool the mixture to 5ºC for 2 hours with occasional stirring then let the mixture go to room temp. next stir in the H2O2 over a period of about 10 minutes. the mixture can rise over 40º and the mixture can turn a slight greenish color.
it was said that "second reaction step,formation of pentachlorporon and free Cl with H2O2 as catalyst" dunno what exactly to make of that but it was said.
the DPPP should precipitate on top of the mixture and some fumes bubble off. after all H2O2 has been added, continue to stir for 2 hours or more untill the liquid on the bottom of the flask is clear and no fumes bubble off. then filter out the crystals wash them with 1 L of 10% Sodium bicarb solution and then again with water.
dry the crystals of DPPP at room temp for 48 hours.
the next steps are mportant to remove all traces of acid and AP in the product so that the DPPP can be the safest. dissolve the crystals in a minimal amount of hot ethyl alcohol (60ºC)and then cool it to 5ºC. next add add a large volume of cold water and let it sit for 1-2 hours below 10ºC and filter again. let the DPPP dry and sit at room temp for 1-2 weeks to decompose and evaporate off any AP that may be left.
the final yield was 65 grams. 5 grams of DPPP was slightly pressed into a hard paper blastng cup and ignited with a match. it flashed and only bursted the cup. it will detonate only if heated strongly. a second charge was made which consisted of 50 grams of highly pressed DPPP and was ignited. it detonated and it was felt strongly from a distance of over 50 m away.

i had to kind of translate that since the guy wasnt all that great with his english. i'll havta try this sometime soon. :D

<small>[ December 04, 2002, 08:07 PM: Message edited by: THErAPIST ]</small>

ShockWave
December 5th, 2002, 11:10 AM
I did the same thing, but I never noticed any fumes, and I don't think that I had DPPP, but I kept about 2gram in a small pipe with a fuse, in a safe place and will try to detonated some ANNM in a few months, to see if this stuff is storeable.

static_firefly
December 7th, 2002, 12:37 AM
I just bought some 50% h202 so im going to try thing too at differnt temps and other things. The thing i cant quite understand is how will i know that i have DPPP and not AP.

nbk2000
December 7th, 2002, 04:17 AM
Well, if the DPPP isn't volatile, then a fan blowing WARM (not hot) air over it for an extended period of time (days?) would evaporate off the volatile AP.

Vacuum sublimination would be much faster, but I doubt you have the equipment.

Sure sounds a lot like an AP synth... :rolleyes:

Pu239 Stuchtiger
December 7th, 2002, 01:24 PM
It is definitely not an acetone peroxide synthesis.

I did succeed in getting a very pathetic yield of DPPP once. Maybe 0.5g from around 25mL acetone; I don't remember the exact quantity I used, and I'm too lazy to fetch my lab notebook. It exploded violently with a sharp crack when struck with a hammer - and when sopping wet.

ShockWave
December 7th, 2002, 02:02 PM
what did your DPPP looked like?

Pu239 Stuchtiger
December 7th, 2002, 03:18 PM
Relatively large white crystals; floated in the reaction solution.

knowledgehungry
December 7th, 2002, 04:43 PM
well it would seem that someone finally answered what the floating crystals in my AP where, i always got a small amount of them, i always assumed that they were the dimer form of AP. You learn something new everday.

I have some DPPP going right now but with 3% H2O2 (pool stores are closed for winter :mad: )
I'll let you know results if anyone cares.

kingspaz
December 7th, 2002, 06:11 PM
of course we care! dammit, we need all info. there may be one tiny detail different to your results than somebody elses which allows us to make a better estimate at how to prepare it.

Anthony
December 7th, 2002, 06:48 PM
The crystals which float on the surface of the solution in a typical AP synth are exactly that - AP.

Yak
December 7th, 2002, 06:56 PM
Following on from kingspaz's post:

Its also REALLY great to read what happenes to other peoples experments and makes other people want to try it out for themselfs.

Keep up the good work!!
I think I might try this out, it sounds great

knowledgehungry
December 7th, 2002, 11:28 PM
Ok i'll post what i did, I poured about 5 mls of Acetone into a beaker then poured 5mls of 28% HCl into the solution, i let the mix sit over night in the morning it was nice and yellow. I then poured about 25 mls of 3% H2O2 into the solution. The mixture turned clear in about 2 hours and a few crystals floated to the top i am letting it sit over night to see what i can see. After i get all the supposed DPPP out of it i am just going to let it sit in a petri dish and watch for signs of decomposition if there are none we might be on to something if the stuff disappears though im gonna assume i only created AP and give up on DPPP synthesis for a while.

static_firefly
December 8th, 2002, 03:07 AM
I dont think i the crystals float it is DPPP. The other day i made some AP with 50%h202 and the entire flask was filled up with ap. Cus i had so much i buryed half ( i didnt want it) left a bit out to dry and with the rest i filled the flask back to the top with water. All of the AP floats for me.

vonK
December 8th, 2002, 04:40 AM
You guys say that CTAP sublimes at room temp realatively fast, and I've always believed that. However I must say that I have never noticed any sumblimation happening to my CTAP, ever.
At this very moment I have around twenty grams of CTAP spread on a paper towel, sitting on a shelf in my bedroom. It's been there for around two weeks and I haven't noticed any difference at all in the whole time it's been here.
The temp were I live gets up to 28*C at the moment and I leave my windows open so there's a nice (although hot) breeze blowing through.
I would have thought that if CTAP is as volitial as it is supposed to be then I would have noticed something.
The thing is, the way I see it, you can't rely on the CTAP to be completely removed from your DPPP by sublimation.
I will weigh some CTAP then leave it open to the atmosphere and weigh it again in a week, so that I have some real record, but I'm fairly certain that sublimation is quite insignificant.
I'd love to know if anyone else has ever actually measured losses of CTAP due to sublimation.

Kurt.

spydamonkee
December 8th, 2002, 06:11 AM
i stored 1 gram of AP for nearly two months without a noticable loss, used it for a blasting cap and it worked fine.

was stored on a paper tissue in the cuboard

Pu239 Stuchtiger
December 8th, 2002, 12:24 PM
I think the sublimination is appreciable. I have left containers (margarine tubs) of acetone peroxide uncovered for a week, which caused a noticeable decrease in the quantity of acetone peroxide (I didn't mass it, because it was obvious).

knowledgehungry
December 8th, 2002, 02:23 PM
Ok, I have almost enough DPPP to test it for sublimnination, I dont think that what i have is AP, the crystals are not white as with AP, rather they are clear.They are floating in my beaker right now.

On a totally unrelated but not worth posting by itself note what is the title for someone with over 1000 posts but who is not a mod? Just curious.

Anthony
December 8th, 2002, 03:02 PM
AP sublimination seems to be a fickle thing. Some people, like Pu239 Stuchtiger lose lots, whereas I hardly notice it. The most I've ever lost is about 25% by mass, over six months or so.

knowledgehungry, unless I am mistaken, there isn't a title for 1000+ posts.

kingspaz
December 8th, 2002, 04:38 PM
i think differences in sublimation rate relate to specific batches and the slightly different conditions experienced by each batch during production. as we know these differences account for a varied ratio of dimeric to trimeric AP between different batches. the dimeric form would have a higher tendency to sublimate as it has a much lower molar mass than trimeric (about 2/3 mass of trimeric?).
thus a batch with more dimeric will lose much more mass over 2 weeks than a batch with less dimeric.

nbk2000
December 9th, 2002, 04:18 AM
I was also going to suggest the difference in volatilization was due to varying ratios of the polymeric forms.

If the temps in the mentioned DPPP synth are correct, then if there is any DPPP made (instead of all AP), then the AP impurity would likely be mostly trimeric AP, thus much less volatile than the other forms. So sublimination/volatilization would have to done with the aid of heat or vacuum to drive it all off.

Flake2m
December 11th, 2002, 10:09 AM
I am not sure, but I might have managed to make some DPP. Today just before i filtered out my batch I wrote down some observations:

There appears to be are 3 layers.
The first layer is a white crystaline substance that is less densers than water. The crystals are quite small and are insoluble in water.
A flame test was conducted and and orange flame was seen.

The second layer consist of a transparent dark yellow coloured liquid, possibly a solution.

The third layer is white crystalline compound that appears to be denser than water. It is insoluble in water and the crystals are quite small.

When a sodium bi-carbonate solution was added, the solution effervested and all the crystals rose to the top of the solution and colourless odourless gas was evolved. The transparent yellow colour was diluted out when the crystals where washed & filtered out.

I have yet to test out the crystals as they are still drying.

Anthony
December 11th, 2002, 12:16 PM
*All* characteristics of AP...

megalomania
December 11th, 2002, 01:28 PM
It would seem to me that the possibility of AP formation could be avoided if one isolated and purified the phorone before introducing the hydrogen peroxide. It should not be too difficult to neutralize the excess acid, distill off the remaining acetone, and possibly recrystallize the phorone a few times. I don't know what phorone will dissolve in though, the Merck Index didn't have much data in that regard, but I imagine the usual alcohol culprits or standard lab solvents would work. I would even go so far as to predict the isolation and purification info is in one of the systhesis refs for it, like the Journal of Organic Chemistry 24, 1371 (1959) which I will check this week assuming the library is open during the Xmas break :(

One would then need to modify the DPPP procedure accordingly to reintroduce the necessary acid, rather similar to the AP process but without acetone. Naturally if the reaction proceeds there would be no possibility of any AP forming (assuming no phorone reverts back to acetone, but that is likely to be moot). I know this adds a step of complexity, but in the interests of research where suitable analytical methods are in short supply this method may satisify some curosity. I will do my best to report on the findings of that journal article in short order.

On the subject of AP volitility, the matter is also affected by the purity of the final product. Using lab grade chemicals typicially results in a better product which leads to higher volitility. Furthermore, the volitatlity is not something to be measured against the likes of ether, or other liquid solvent. Think mothballs here, I believe I recently read a reference that said AP volatilizes at a rate of 30% per 1-3 months. That is high for a solid, but by no means noticeable after a mere week. Such volitality is typicially measured against other explosives making AP truly noticeable indeed. The military types wants their bombs to sit around in warm bunkers for years on end, and so in this respect AP is very volitile. For us independant experimenters a few grams sitting for a few weeks will not exactly create a deficit in the quartermasters logs. It's all a matter of perspective I guess.

As to user titles, the list goes like this:
0 newbie
10 A New Voice
25 Bottle Washer
50 Amateur
100 Lab Assistant
250 Researcher
500 Sr. Researcher
1000 Scientist
2000 Scientific Genius
5000 Nobel Laureate

At 1000 posts one is conferred the grand title of "Scientist" glorious in its simplicity, and profound in its import.

It was really starting to irk me figuring out the mechanism for this reaction, then I perused the rest of that German patent and found a proposed reaction scheme and a pic of the target molecule. I drew it out below for all to see. If anyone wants to compare this with AP I have a nice diagram of the reaction on my website <a href="http://roguesci.org/megalomania/explo/acetoneperoxide.html" target="_blank">HERE</a>.
"Our Target Molecule"
<img src="http://www.roguesci.org/images/DPPP.gif" alt=" - " /> <img src="http://www.roguesci.org/images/DPPP_3d.gif" alt=" - " />

<small>[ December 11, 2002, 12:59 PM: Message edited by: megalomania ]</small>

Pu239 Stuchtiger
December 11th, 2002, 08:35 PM
I have never had acetone peroxide float in the reaction solution, not even little specks. Especially all of it.

Megalomania, I recommend reading the thread on this at a different site (link at the beginning of this thread). :)

Anthony
December 11th, 2002, 09:07 PM
I have, HMTD too. It's a rather common and acknowledge phenomenon. Or maybe I've actually been making DPPP all these years?

nbk2000
December 12th, 2002, 12:59 AM
I've had AP floating and sinking, all at the same time. It varies on what you're doing at the time, whether it's offgassing, reacting, crystallizing, whatever.

If it's possible to seperate phorone in a pure state, then obviously one should do that. How complex a task that may be, and whether any acetone is regenerated during the reaction remains to be seen.

Also, is there NO other references to DPPP as an explosive beside the german patent? A single reference is not to be trusted without independant verification.

Well, Anthony, it looks like it's a race between just you and me to see who gets to claim the "Nobel" title. :p

Mega, have you checked your dragon lately? There's an issue I'm curious about knowing.

megalomania
December 12th, 2002, 04:32 PM
I just had a nice reply that got screwed up because of an illegal character :mad: Let’s try this again…
Does anyone happen to have any good results in preparing phorone here? I will try to get that journal from J Org Chem Friday, and while I am there I will do a database search for DPPP. Are there any other names for the stuff out there besides diphoronepentaperoxide? It could help improve my search results.

I noticed in the procedure posted by IPN, and again by THErAPIST, that making phorone at such low temperatures is not likely to work well. It appears that the reaction is an aldol condensation, which requires a high temperature to dehydrate the resulting product and form an a,b-unsaturated ketone. First we get acetone combining to form 4-hydroxy-4-methyl-2-pentanone which is then dehydrated to form its dehydrated product. This chemical either becomes its enol form (good) or acetone does (bad). If we get the good enol we will form phorone, if not we end up with something I think is called 4,6-dimethyl-3,5-heptadien-2-one. That is but one of several mixed aldol condensations that we can end up with, all waste products.

Now then, the product of acetone condensation, 4-hydroxy-4-methyl-2-pentanone, has an equilibrium that forms about 2%. That is quite low, but as we dehydrate that to its unsaturated form we should get more of it. This would seem to imply a series of heating and sitting steps may be the best way to get a better yield.

I would propose refluxing the mix of acetone and HCl. The heat is needed to get the dehydrated product. At the very minimum of the 2% that is converted I would expect the chance of either an acetone enol or 4-hydroxy-4-methyl-2-pentanone enol forming is 50%, so we would expect at least half the total acetone (that reacts) to be our desired product, phorone. Looking at a pic I drew of the dehydrated version of 4-hydroxy-4-methyl-2-pentanone and looking at some data about the equilibrium formation constants of acetone enols, I would expect resonance effects to increase the probability of the good enol forming.

The patent was quite vague about all of this. While I am sure this may be a cheap way, it is probably too time consuming for industrial use. Since we independent experimenters don’t have to worry about a “bottom line” for profit we can wait a bit. A series of refluxing and sitting steps might improve yields over time. Once one was done refluxing they could distill of some of the excess acetone and have only the phorone/crap/acid mix left. This would not require a complete isolation and purification of phorone, and it would limit the amount of acetone to reduce AP formation.

Perhaps nbk had it right when he left his mix set around for weeks, although I highly doubt the formation of phorone would be of much use without any heating. I can’t really say how long one should leave the mix sit around, but I bet it could take awhile. One could judge the rate of reaction by distilling off the acetone and measuring the amount left. It may not even be necessary to reflux and wait, just refluxing for several hours should continually end up with the formation of phorone and waste products.

Hopefully I can find that journal tomorrow and some issues can be explained. The key to this reaction would appear to be phorone production. I have read a little about aldol condensations just now and I have been led to believe only base is used to accomplish such things. It could be that the patent uses acid and acetone in a “one pot” kind of mix so they don’t have to bother purifying anything and can just add in the peroxide. Since they never actually stipulate how much time elapses between the phorone reaction and the addition of peroxide, we must experiment. My vote is the industrial process lets its vats sit around for a week or two, and so must we.

Enough of my ramblings… who would like to correct some of my facts? It could be that a different mechanism is taking place other that aldol condensations and a,b-unsat products (it sure looks like it though).

knowledgehungry
December 12th, 2002, 04:50 PM
Following up on my previous post:
The crystals which i had in my beaker disappeared either back into the solution or into the air. I then heated my mixture until it had boiled down to 1/10 of original volume. No crystals precipitated out of the solution. I let the solution cool. I checked back a day later still nothing so i dumped it. I now have about 10 mls of HCl and acetone sitting in a test tube. It has been sitting for about 2 days, it looks like urine. Should i boil the mixture to try to get out the phorone(it's a solid right)or let it sit?

megalomania
December 12th, 2002, 05:54 PM
I would keep on boiling the mix until you are left with a nice oil. The remaining acetone should come off with little effort leaving the liquid phorone if that's what you have. Let that cool and if you get crystals that may be the stuff. I gather the stuff is soluable in acetone but not in water.

On a related note I have my acetone and acid gently refluxing right now. I noticed in the patent that they use 6 moles of acetone per 1 mole of hydrochloric acid, I decided to go with a 1:1 mole ratio because I think I may lose a little acid along the way. I am not sure (it being in German) but on the page before the formulas it loos like they use 1:1:2 of acetone to hydrochloric acid to hydrogen peroxide. Has anybody calculated any stoichiometry for this reaction?

knowledgehungry
December 12th, 2002, 10:35 PM
stoichiometry, the only thing high school chem is good for.I got roughly 10moles HCl to 6moles Acetone but im quite tired so dont trust me(Casualties show last night)

megalomania
December 12th, 2002, 11:33 PM
Oh no, bad news :( The journal is not at my library, but shipped off to the remote storage place unaccessable to me. I have filed a request to have the article shipped to me, let us hope it arrives in a timely manner. It's a good thing I checked before I went.
Apparently (all of a sudden) just because your not a student, you can't get anything. My remote access to the journal archive was cut (suddenly I may add). The online journal request did accept my submission to have the journal sent to me, so maybe I can slip through the cracks a bit longer. They want a "donation" to remain a patron. Cheap bastards...

One ray of hope, I checked on the other reference in Merck, the one for Zhurnal Obshchei Khimii (Zh. Obshch. Khim.) 22, 632 (1952). I thought I remembered some of those had English translations, well I was right. My library dosen't have back to 1952, but I will try to request it from elsewhere. The problem I have now is whether the English version is called "The Journal of general chemistry of the U.S.S.R. in English translation" or "Russian Journal of General Chemistry (English Translation)." They sound close enough, and how many can their be? :)
I also have a line on the other reference, in Zhurnal Prikladnoi Khimii 34, 1628 (1961) which I think might be "Russian Journal of Applied Chemistry (English Translation)."
Oh, and I almost missed the ref for Zeitschrift fuer Naturforschung 33B, 454 (1978) which sounds like a German one. I gather that is a "B" edition for chemical sciences.

<small>[ December 12, 2002, 11:44 PM: Message edited by: megalomania ]</small>

megalomania
December 13th, 2002, 04:31 PM
Well, my experiment has been refluxing for a total of 6 hours now counting yesterday and today. After only 45 minutes yesterday my solution turned a nice urine yellow. After about 1:30 hours today the solution turned orange, and after 3 hours it became a slight red, now it is a dark wine red. I can see this indicates the progress of some reaction, but I can’t say what chemical is being made. If only I had a HPLC or perhaps a mass spec :)

I believe this is the same color of solution that you referred to nbk, after letting your mix sit around for a few weeks? I did figure out one of the byproducts of this reaction is mesityl oxide, which is what I referred to the first condensation product for lack of a better name. This stuff will boil at 130 <sup>o</sup>C and remains as a liquid under ordinary conditions. This is just something to keep in mind if distilling the reaction mix. It is a colorless honey smelling liquid according to Merck.
Another possible byproduct is mesitylene which boils at 164.7 <sup>o</sup>C. I am quite surprised to find out an aromatic molecule can be made so easily, although I don’t think the conditions of refluxed acetone with HCl are quite right to make too much. A little check of Organic Synthesis shows they have just such a reaction using sulfuric acid and acetone kept cold, rather like the conditions described by IPN earlier in the thread.
I also found it may be a bad idea to neutralize the HCl with a base if trying to isolate it as it can cyclize into a compound called iso-phorone.

I found another reference in Organic Synthesis concerning the preparation of mesityl oxide. There was a footnote about using HCl as one of the condensing; it said it was quite bad as considerable quantities of phorone will result. Looking over the procedure they use gently refluxing diacetone alcohol with a little iodine. By modifying this procedure with acetone and HCl as the footnote suggests, one should get a rather large amount of phorone. It would appear my reflux track is right on the money. The likely byproducts would be diacetone alcohol, mesityl oxide, and unreacted acetone.
Ahh, there it is the bad news… looking up the synthesis of diacetone alcohol I see it required between 96-120 hours to convert 80% of the acetone! Ahh jeez, I can’t afford to waste that much water in my condenser :) A footnote mentions a 70% yield can be obtained at 40-50 hours, that’s a little better. I assume the conversion of diacetone alcohol to phorone proceeds under much the same time frame, with the diacetone being reacted about as fast as it is made. I hypothesized this would take a very long time to react I guess I was right.

FadeToBlackened
December 13th, 2002, 06:11 PM
I've not been following this thread much but I think I've seen "diacetone alcohol" as an ingredient in an aerosol can of antkiller. Raid possibly. I can't remember. It may be worth looking into though (?)

kingspaz
December 13th, 2002, 07:31 PM
hm....that sounds like it may be pentan-3-one but i am guessing :)

Pu239 Stuchtiger
December 13th, 2002, 08:38 PM
Methinks mega has mesitylene.

Syanide
December 13th, 2002, 09:58 PM
I told my friend about this thread and he has decided to synthesize some DPPP today. He will use the Method first proposed by BrAiNFeVeR

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">that's why the most common thought is to first prepare phorone, then dissolve that in HCl solution, and then add the peroxide.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I will post the results and hopefully pictures when the process is completed. :D

nbk2000
December 13th, 2002, 10:05 PM
Yes, Mega, that is the same color progression as I got from letting it sit for weeks (months).

Continuous reflux would do the same thing much quicker but, if you've got the patience, you could always just let a 5 gallon bucket of it sit in a back corner for a few months to let it react on its own time, no reflux hassle needed.

megalomania
December 14th, 2002, 02:06 PM
For those of us who have reflux equipment it works fine, for those of us who do not heating this stuff would be a bit more complicated. I got out some books yesterday and brushed up on aldol condensations and here is what I came up with:

The formation of diacetone alcohol will proceed without heat, achieving an equilibrium mix of between 2% and 5%, meaning that by letting it sit you can end up with that much. Heating will increase the rate of the reaction considerably, but heat is necessary to achieve the dehydration step where the double bond is formed. Once that is done the mesityl oxide that forms (dehydrated diacetone alcohol) is stuck and cannot go back. In essence the equilibrium will shift to product over time. I have read that the conditions required to dehydrate the molecule is only slightly more vigorous than the aldol condensation to begin with. The presence of the carbonyl stabilizes the hydroxyl as it is stripped away, not that this theory is important. Personally, I would not expect any dehydration to happen at room temp, but it is not altogether unreasonable to expect that after many weeks or months that some would form.

From mesityl oxide we are quite likely to get phorone as the principal product. When a molecule of mesityl oxide forms it is more than likely to be surrounded by acetone molecules when it becomes its enol form than an acetone enol is to find a mesityl oxide. The equilibrium (initially anyway) favors the formation of phorone. A second factor is steric crowding. Ketones have a lower formation constant vs. aldehydes of their enols because of the crowded neighbors. An acetone enol going after the very crowded mesityl oxide carbonyl is less likely to happen. A mesityl oxide enol can more easily attack an acetone carbonyl.

In time we would get a very high conversion of acetone to mesityl oxide. It is reasonable to assume that the mesityl oxide forms phorone at about the same rate that mesityl oxide is formed from acetone. These factors serve to limit the amount of mesityl oxide that can react with other things, and thus make the formation of other mixed aldol condensation products, or even mesitylene, a very minor occurrence.

All of this leads to justification of the formation of large amounts of phorone from the reaction conditions I am currently running in my lab. Speaking of which I electrocuted myself an hour ago when beginning today’s refluxing. I didn’t even realize it until a few minutes in. My top condenser hose was not affixed properly and after about 30 minutes in it started to leak. I left the experiment to its own devices for 45 minutes. When I went to check on it there was water all over my electric heating mantle an about 0.5 cm of standing water on my bench. I started to sop it up… and a very strange tingling feeling shot through my fingers every time I pressed down on the sponge. You think I would have stopped… now my fingers feel quite “funny” after being shocked for upwards of 5 minutes as I cleaned the water up. It felt rather like my fingers fell asleep; you know that pins and needles feeling, so that’s what I thought it was. It only happened when I pressed my fingers down, then I did a test press on a dry spot and no pain. I was standing in a puddle of water too. I am alive and well, with a now wire wrapped condenser hose.

ShockWave
December 14th, 2002, 03:09 PM
STRANGE NEWS !! <img border="0" title="" alt="[Eek!]" src="eek.gif" />

A few weeks ago I mixed 1part acetone with 1 part 30%HCL I did the glass in a hot waterbath at about 60C for about 1 hour, it had a urine color but a little darker.

After that hour I let the mixture cool to room temperature and added some Sodium Bi Carbonate straight to the Aceton/HCL, and fillterd out the crystalls, and did this a few times untill no more crystalls were formed, the crystalls should be Phorone but they don't melt at 30C, so I don't what it is.

I disolved a very small amount in 30%H202 and nothing happend, I lay the mixture away for a few weeks and took a look avery week, nothing happend ofcourse.

But, today I looked and their were very big cristals !
The water in the 30%H2O2 evaporated but at this time it is still a bit wet, I also tryed to ignite 2 crystalls but they were not really burning I guess but it did something, more like "SNAP" if they are dry I will test it again !

These crystalls are bigger than sugar <img border="0" title="" alt="[Eek!]" src="eek.gif" /> and have no color !

the pictures of the Phorone and crystalls will be online within a day !!

megalomania
December 14th, 2002, 04:27 PM
I have my pictures ready from my experiment the past few days. Each photo represents the reaction at later stages and clearly shows the color progression.

<a href="http://www.roguesci.org/images/phorone_1hr.jpg" target="_blank">After 1 hour, a light yellow color.</a>
<a href="http://www.roguesci.org/images/phorone_4hr.jpg" target="_blank">After 4 hours, a light red-orange.</a>
<a href="http://www.roguesci.org/images/phorone_12hr.jpg" target="_blank">After 12 hours, a dark blood red.</a>

nbk2000
December 14th, 2002, 09:16 PM
Yep, that's the same exact color progression as my experiment.

Now, if the reaction is self limiting, without heat, to ~2%, what color would that be? Because if 2% is just light yellow, and fully reacted is motor oil, then how did I get to that stage without any reflux?

Bicarb + HCl = Table salt.

Good thing the Forum server info is distributed amongst staff, lest we have lost our illustrious leader in the line of duty and been up shit creek without a password. <img border="0" title="" alt="[Wink]" src="wink.gif" />

<small>[ December 14, 2002, 08:31 PM: Message edited by: nbk2000 ]</small>

megalomania
December 14th, 2002, 11:03 PM
Most likely the presence of HCl has a considerable catalytic effect in the reaction. Since the dehydration requires almost the same conditions as the aldol formation does, having the reaction happen at room temp is not a far stretch. The rate of reaction would be patheticially slow though, evidenced by the fact it takes months to achieve at room temp what I got in 12 hours. Other things like sunlight could play a role as well.

Who wants to be the first to add some of their HCl to their bottle of acetone and sit it out? Report back here on Valentines day maybe? I know this dosn't sound like a fun experiment, most will probably forget. I'll seal up a flask tomorrow and keep it under my pillow...

My fingers still hurt.

nbk2000
December 14th, 2002, 11:32 PM
I figured it was an acid catalyzed reaction. My acetone was saturated with HCl gas, so it would have continued reacting with the absorbed acid as the acetone content was changed to phorone.

The one thing I think simple Mix&Wait would have over heating would be mass quantities. It'd be very simple to mix a 55 gallon drum of acetone with acid and let it sit in the backyard for a few months.

Try doing a reflux on a drums worth. :p

Could have been worse, you could have ended up like some scientists who've fallen on the battlefield of discovery, clutching a test tube in one hand, a retort in the other. <img border="0" title="" alt="[Wink]" src="wink.gif" />

megalomania
December 16th, 2002, 12:17 AM
Actually I could run a reflux on a drum quantity of acetone because I have a pair of gigantic condensers I have never used because they are too damn big. Of course I wasted enough water refluxing 74 mL :p
Not that anyone would want to make such large quantities, that goes beyond personal experimentation.

nbk2000
December 16th, 2002, 12:58 AM
Unless it turns out DPPP actually IS as simple and powerful as claimed

Is so, why fuck around with RDX with all the acids and fumes when you could use cheap solvents and acid, let sit a few months, add gallons of pool peroxide, and get kilos upon kilos of DPPP that has a detonation velocity as high as RDX?

But, life can never be that generous, so there's got to be something wrong with it.

ShockWave
December 16th, 2002, 08:01 AM
Here you can see the weird crystalls that have been formed out of phoron with H2O2

<a href="http://apanshock.tripod.com/Temp.htm" target="_blank">http://apanshock.tripod.com/Temp.htm</a>

nbk2000
December 16th, 2002, 08:16 AM
Have any plans on testing them? Impact, fire, etc?

Those are definately some big crystals. They look rhombic, rather than needle/cubic like AP usually is.

ShockWave
December 16th, 2002, 08:43 AM
I did some tests but it does not really burn, it is hard to test, because they "SNAP" away.

I will wrap them in some aluminiumfoil so that they can not jump away.

nbk2000
December 16th, 2002, 08:50 AM
Are you sure the crystals are totally dry? If not, it may be little steam explosions from trapped water causing the "jumping".

Also, hammer whacks are good to to keep them from jumping. <img border="0" title="" alt="[Wink]" src="wink.gif" />

ShockWave
December 16th, 2002, 08:52 AM
I just did several test but this stuff is worthless !

They only dance when you light them with fire, they don't melt, they don't do anything, they give some smoke and you can smell someting but it is not DPPP :( <img border="0" title="" alt="[Frown]" src="frown.gif" />

Microtek
December 16th, 2002, 10:37 AM
Try these tests:

- Wrap one or two of those large crystals in Al foil and heat in open flame ( protect yourself ).

- Wrap in foil and do a hammer test.

- Grind ( carefully ) and use as base charge in a detonator, place this detonator against a witness plate such as a thick wooden board and mark the length of the detonator on the plate. Initiate the primary explosive ( I suggest HMTD ), recover the plate and see how far down the pipe the detonation propagated.

IPN
December 16th, 2002, 11:10 AM
In the picture the crystals look very wet. Do you have or have you access to a vacuum dessicator. With that it would be easy to drive off the water.

DarkAngel
December 16th, 2002, 12:17 PM
Shockwave those crystals look like Sodium (Bi) Carbonate.
Try to pour some HCl on them to find it out.

ShockWave
December 16th, 2002, 12:47 PM
Crystalls are very dry, the pics were taken about 2 days ago when they were still wet.

My sodium bi carbonate does not look like this, does your sodium bi carbonate looks like sugar?

These crystalls are totally colorless.
The picture shows all of crystalls, as you can see it is not enough to test for a detonation with a primary.

I still have lot's of that some kind of phoron so I can make much more of these crystalls

ShockWave
December 16th, 2002, 04:05 PM
Small update at my site

<a href="http://apanshock.tripod.com/phoron_dppp.htm" target="_blank">http://apanshock.tripod.com/phoron_dppp.htm</a>

Microtek
December 17th, 2002, 04:35 AM
Shockwave: It's easily enough. In fact one tenth of what you have would be enough. I'm not talking about inserting a detonator into a container packed with your crystals. Here is what I suggest:

- First obtain an Al or copper pipe with an internal diameter of 3-4 mm.

- Cut off a length of 3 cm or more and seal one end with epoxy.

- Pack the lower 2 cm of the pipe with ground up 'mystery crystals'.

- Pack the upper cm with HMTD or, if you have it, 0.5 cm rdx and 0.5 cm HMTD.

- Add a little silver acetylide, mercury fulminate or lead styphnate to aid DDT, and attach a fuse.

- place the pipe on a plate that is strong enough that it won't be destroyed by the blast but soft enough that it will be dented ( I suggest thick wood ).

- Mark on the board where the beginning and end of the pipe is, and initiate the device.

If the crystals are reasonably sensitive ( more so than TNT ) they will detonate from this treatment as direct contact between initiating and recieving explosives make detonation transfer much more effective ( recall my posts on caseless detonators ). If the crystals detonate, the plate will be dented corresponding to the entire length of the pipe and if they don't, only the section of the plate directly under the initiating explosive will be dented.

As for the amount of crystals needed, let's assume that you can press them to a density of 1.5 g/cc ( as good as industrially pressed RDX ) and you use a pipe 3 cm long with an internal diameter of 3 mm.
You press the crystals into the lower 2 cm which means you need
0.15*0.15*pi*2.0 = 0.141 cc at density 1.5 = 0.212 grams.

knowledgehungry
December 23rd, 2002, 10:56 AM
I would think that maybe we should test the process by using pure Phorone(preferrably bought to make sure of purity) 30%H2O2 and: H2SO4 in one batch, HCl in one batch, Acetic acid in one batch and Acetone + H2O2+HCl as the control batch. anyone have access to phorone???
Ill get around to doin this eventually but not for another month at least.

Donutty
December 26th, 2002, 05:37 PM
Aw.. this poor topic has been abandonned! Ive got a sample vial of a opaque, dark red, oily geranium-smelling liquid waiting to be used, now all I need is the time!

For such a promising development it seems a shame to leave it like this!

frogfot
December 28th, 2002, 09:42 AM
As several people alredy said, first we must develop a way to make phorone. Have anybody actually made it?
Recently i boiled 50 ml acetone + 50 ml 30% HCl in water bath under reflux for 1 hour. Solution got yellow after some minute and then slowly crowled to dark red/brown.
I added 100 ml water and neutralized it with solid sodium carbonate untill it became nearly colourless. Under whole neutralization there formed small ammount of red/brown oil on top, which went over to yellow color when it was neutral.
There were no precepitate.
So, should phorone be that oil? (as i remember it was a solid) Or does it need to be extracted from the oil?

And i just thoat about discussed "patent" on DPPP, if phorone yelds are very small at room temp, then just pouring acid in acetone and then directly mixing with H<sub>2</sub>O<sub>2</sub> would yeld only AP.

<small>[ December 28, 2002, 08:43 AM: Message edited by: frogfot ]</small>

nbk2000
December 28th, 2002, 11:41 AM
Sometimes chemicals form oils, instead of crystals, requiring you to seed it, or freeze it, to get it to crystalize properly.

Indeed, without having KNOWN phorone, you can't be sure that you're not producing AP instead.

frogfot
December 30th, 2002, 09:09 AM
Then its possible that phorone is maby dissolved in acetone to some part.
Collected above named oil, got about 0,6 ml. It got "mixed" smell, so i evaporated it in room temp and funny part was that it started to smell like fir-tree <img border="0" title="" alt="[Eek!]" src="eek.gif" /> If i remember correct, some of self-condensation products of acetone should smell like fir-tree... Does phorone smell like that too?

Will longer reflux time give more oil?

IPN
December 30th, 2002, 10:48 AM
It might give more of that oil, but there is a chance that phorone forms trough the reaction in so small amounts that making decent amounts of it you would need many gallons of acetone and HCl to make noticeable amounts of phorone.

megalomania
December 30th, 2002, 09:23 PM
I am given to understand that phorone is quite soluable in acetone and other common organic solvents. You will have to distill the solvents off to get crystalline phorone.

nbk2000
December 30th, 2002, 11:45 PM
Is phorone heat stable? Or would it decompose, radicalize, polymerize, or some other way get fucked up?

IPN
December 31st, 2002, 04:38 AM
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> The patent don`t say heat at this time and the patent don`t say
some product (phoron) should precipitate from the solution at this time.
If you heat or not, the content of AP are always present at end of the synthesis. On the contrary, if you heat to much or to long, the reaction fails.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I don´t know if this means phorone would decompose on heating but it implies to something like that.

Al Koholic
January 1st, 2003, 05:55 PM
Or since we are just dealing with acetone instead of distilling of the solvent just let it evaporate :-)

Run a current of air over the evaporation dish to speed things up.

knowledgehungry
January 2nd, 2003, 08:22 PM
Yeah but we have the acid too.

IPN
January 9th, 2003, 09:11 AM
If phorone melts at 27C and boils at 198C it should not decompose

(i´m not sure. it´s just a guess)

BASF
January 9th, 2003, 06:01 PM
<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=179&page=5" target="_blank">http://www.sciencemadness.org/talk/viewthread.php?tid=179&page=5</a>

i tried peroxidation of pure phorone(see report on sciencemadness), but it seems to be tricky as phorone can not be dissolved in polar solvents with only one exception: glacial acetic acid.

I still possess several grams of 97% phorone from sigma-aldrich <img border="0" title="" alt="[Wink]" src="wink.gif" /> , i am looking for other ways to peroxidize phorone.

As i see that lots of points already have been discussed in sciencemadness, I would also advocate to interchange more information between the forums, less having the discussion going in circles.

The thread on sciencemadness has grown damn big, but i´ll soon try to pick the most important points out of it for a new thread on the Mackowiak-patent.

Greets to all being curious

ALENGOSVIG1
January 9th, 2003, 08:49 PM
Mabe the reason they're "DDDP" is sublimating fast and burns slower than regular AP is becuase it's the dicycloacetone peroxide isomer.

dicyclo AP burns slow. A 1/2" diameter 1.5" copper tube plugged at one end pressed with dicyclo AP made at 40 celsius just shoots a fireball out the end!

Just a theory though. :)

<small>[ January 09, 2003, 07:53 PM: Message edited by: ALENGOSVIG1 ]</small>

knowledgehungry
January 9th, 2003, 09:29 PM
I agree with alengosvig1. Dppp might have a slower burn rate, (not detonation speed)but it is supposedly non-volatile. If peroxidation of pure phorone has proven so difficult the i doubt that the patent method would have success.

BASF
January 9th, 2003, 11:13 PM
i also made a specific experiment on sublimation, but my "DPPP" was made below 5°C, under these conditions mainly tricyclic acetone peroxide should form.
But it still exhibited a sublimation rate of about 49% per two weeks at 21°C as opposed to TCAP which had a rate of about 26% per two weeks.

<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=397" target="_blank">http://www.sciencemadness.org/talk/viewthread.php?tid=397</a>

Does anyone know what the german patent office exactly examines to grant a patent?
I know at least that european offices want to have evidence on the invention really working, not just evidence wether it is new(like the US patent office also grants patents to inventors of perpetua mobile).
This is what still keeps me being confident about this compound.

Anthony
January 10th, 2003, 06:48 AM
At least in the UK patent offices, all the patent officer has to do is to visualise your idea working with current knowledge and understanding. They certainly don't come to your lab and watch you create and test your invention.

I think we should remind ourselves that an awful lot of shite gets patented and there is a good reason that around 98% of patents never make their owners any money...

It seems that DPPP was originally cited as a high performance, easy to make replacement for AP/HMTD. For that much it has certainly failed due to the difficulty of it's synthesis, assuming that it can be synthesised at all.

Therefore, I think it's being continued as a curiosity only, which would explain why it is getting more attention at ScienceMadness than here. We like our bangs and they like their numbers :)

BASF
January 10th, 2003, 09:13 AM
3D-Structure of the molecule
<a href="http://www.sciencemadness.org/talk/viewthread.php?action=attachment&tid=179&pid=2255" target="_blank">http://www.sciencemadness.org/talk/viewthread.php?action=attachment&tid=179&pid=2255</a>

Chemsketch predicts a density of about 1.3g/ccm.

vulture
January 10th, 2003, 10:34 AM
I recognize that....(I made it duh).
I noticed that Mega posted a structure also, but this was assymetric instead of this symmetric one.
I'm wondering what would be favorable?
If it's assymetric it should polarize light no?
Anyone got a refractometer?

nbk2000
January 10th, 2003, 08:32 PM
The US patent office SPECIFICALLY forbids any kind of "Perpetual Motion" patents. It also requires that the patenter be prepared to defend the validity of their patent application by presenting the device for examination by patent inspectors if there's any issue with the feasibility of the device.

And, I think, the reason 98% of patents don't make money is because:

A) The item is a crappy idea from the start. Though who'd have ever guessed that the talking bass fish plaque would be such a hit. :rolleyes:

B) The patent owner doesn't have the money to market the device sufficiently to make it profitable.

C) They get tied up in court over who owns the idea with someone else who may be suing simply to prevent the device from reaching market. Big corporations do this all the time to suppress any competition.

Anyways, unless someone here has definitively MADE phorone, this topic is closed as it's a dead end without phorone. If anyone HAS made phorone, and has a REPRODUCIBLE synth process to back it up, you can start a new topic to post it.

<small>[ January 10, 2003, 07:32 PM: Message edited by: nbk2000 ]</small>

zeocrash
June 8th, 2003, 05:31 AM
Originally posted by BASF

i tried peroxidation of pure phorone(see report on sciencemadness), but it seems to be tricky as phorone can not be dissolved in polar solvents with only one exception: glacial acetic acid.

I still possess several grams of 97% phorone from sigma-aldrich <img border="0" title="" alt="[Wink]" src="wink.gif" /> , i am looking for other ways to peroxidize phorone.
i heard you can peroxidise things using sodium carbonate peroxide, contained in oxiclean tablets, if anyone has any information on using this, has made AP or HMTD using this method. i'd love to hear it so i dont have to completely wing it.
if otherwise i'm just going to try replacing 30%H2O2 with 30% sodium carbonate peroxide solution, ill tell you how it goes.

vulture
June 8th, 2003, 03:54 PM
IIRC, philou made on post on sciencemadness about the production of phorone which said the condensation reaction should be performed as quickly as possible, because letting it sit would result in higher, useless, condensation products.

yt2095
June 18th, 2003, 01:10 PM
IPN & NBK,

i have tried making phorone with the Acetone and HCL(aq)

both Analytical grade, and have not seen this yellow to red transition? in fact there was no color change at all?

the HCL was 70% and the acetone was 99.98 pure on assay readup
both under 4 months old and had been stored in the correct manour.

i`m intruiged as what causes this coloration. before i was a "newbie" on here i`de done extensive reading throughout this site and should have shares in GOOGLE :)

during this time i set up the acetone and hcl, next day no color change? so i set up 2 more similar.one has heat (when i remember to do it, the other is under constant UV exposer, still no color change?

i realise as a "newbie" it`s probably not best to ASK questions this early on, but i`m left wondering if it`s a flaw in my batch of chems or impurities in yours?

all the above 3 ongoing experiments are at standard RTP.
if there`s any change in state after it`s already 2 weeks, you`ll be the second to know :)

vulture
June 18th, 2003, 01:56 PM
70% HCl? :confused:

zeocrash
June 18th, 2003, 04:02 PM
yeah the highest stable conc of HCl, is about 40%, i have some 36% and that fumes like a motherfucker

yt2095
June 18th, 2003, 04:29 PM
tell me about it!

this stuff is well nasty, that`s why i posted it`s shelf life and wondered wether or not that maybe a factor?
i have no "home lab kit" that`ll give me the conc as it was when 1`st used in my exeriments. but i shouldn`t imagine that it was too far off the 70% mark as labled in 4 months, as for fumes :) :) :)
you`de think the air was composed of pure ammonia gas!
it has an 12 month shelf life, so i would guess that (yes guess and very unscientific of me) that it would change a significant degree after that time (they allow a margin of error).
so i have no real reason to beleive that after 4 month that this should have degraded much below the 70% mark? maybe someone knows more about it p`haps?

but my comment was mainly regarding the production of Phorone and from there the production of "new" type of new compound mentioned in the 1`st post.
all i can say is that i`ve been most unsuccesful in even producing the color change, but i have yet to try the full synth of this compound. i guess i kinda got hung up on this color change.
i constantly remind myself that`s there`s no such thing as a FAILED experiment,,, only more data :)

knowledgehungry
June 18th, 2003, 06:03 PM
you`de think the air was composed of pure ammonia gas! Um HCl is hydrogen chloride ammonia is NH3.

ALENGOSVIG1
June 18th, 2003, 06:08 PM
Im sure he's well aware of that. He was referring to how much fumes are produced when HCl is left around an open container of NH3.

frogfot
June 18th, 2003, 06:10 PM
Is it even possible to have a liquid 70% HCl at room temp.. anyway.. the color change will occur with heat present, but this method suck anyway. Phorone will form as traces and it will condence further to larger products in presence of acid.

Oh, and since this topic came up again.. i have produced mesityl oxide and if you look at it's structure, it's nearly similar to phorone. I used soxhlet extractor and Ba(OH)2 as catalyst. I made an attempt of peroxidation with equal ammount of 30% H2O2 and few drops of HCl (+ MeOH). This reacted about 12h or something.. and after, water was added, a white crystalline product were formed after couple of minutes, which melted in contact with flame. A VERY reliable source said that this is an epoxide of mesityl oxide. The epoxide group is connected instead of double bond in mesityl oxide..
My guess is that phorone will undertake same reaction with H2O2.. so, some other way of peroxidation should be found..

vulture
June 18th, 2003, 06:14 PM
yt2095, your post is very confusing. Could you please clarify.

Are you sure you arent confusing HNO3 with HCl? Because with 70% HCl you should get immediate results and 70% HNO3 is a usual concentration which fumes alot too.

If it's really 70% then it won't be for long, because then the botlle has got to be enourmously pressurized.

yt2095
June 19th, 2003, 08:14 AM
appologies to all, my dummy friend misread the box the ampuoles came in (i got him to photocopy the doc that came with the glass vials and read it my self)

the ampuoles when mixed with distiled water make a 2M solutuion at 72.92g per litre
grams not percent!

ya just can`t get the staff these days!

i`m assuming that these vials are to broken in a suitable vesel and then water added (but that seems rather dangerous as it acid to water and not other way round. so how yer suposed to empty all the contents into 1L of water without personal risk beats me, i just shatered the vial in a beaker and used the stuff neat. still no color change tho?
i didn`t smell like nitric at least not the nitric i make or have used in the past.
i think i`ll start again but make my own HCL and do as NBK sugested and just bubble it through the acetone at least then i know exactly what i`m using and don`t have to rely on anyone else to make mistakes for me (i`m quite capable of doin that on my own, without help) :)

again, accept my appologies and ignore the above few posts i wrote, they were in error

"if you need something doing right, do it yourself!"

vulture
June 19th, 2003, 02:24 PM
2M is already fairly diluted and should pose no problems diluting it further. However, I wouldn't dilute it any further, because 2M is already pretty weak. 2M is the kind of thing you find in school labs, even complete idiots would have to go through considerable effort to hurt themselves with that.

yt2095
June 20th, 2003, 09:06 AM
i probably worded it badly

these Ampoules when added to 1 litre of water make a 2M solution, there are 6 in a box, when all 6 are used it will make the 72.92g per litre

i was given 1 vial, and i used it undiluted to try make 1`stly the phorone then the DDDP.
(not got to the DDDP part yet, i`m still waiting for the color change)

the only noticable effect i have so far is the white frosting effect at the top of 2 of the test tubes, the one i heat (when i remember to) and one i just leave in the room. the other in Cuvvet under UV has no frosting.

appologies if i was a little vague.

vulture
June 20th, 2003, 12:37 PM
What do you mean by frosting exactly?

BTW, UV light is not going to help, as this is not a halogenation with elemental Cl2, merely an acid catalyzed condensation reaction.

yt2095
June 20th, 2003, 01:24 PM
vulture,

the "frosting effect" is like just that.

it will come off with a light touch of fingers, it`s purely a superficial surface effect on the glass.
the tube itself remains unaffected, (i`m using soda glass tubes, tho i think that will have no significance to the reaction)

it`s a white frosting effect at the top of both tubes, i hesitate to use the words "a mist like powder" in case someone decides to jump down my throat and tell me that it`s not a powder at all it`s a "whatever"!

i have only certain frames of reference in which to explain an effect, imagine frosted glass, that goes clear when you run your finger along it.

i`ll PH test it, not now tho, maybe tomorow. the fineness of this surface material, makes me think that it is some sort of condensation forming on exposure to air since it`s not all up the inside of the tube, only about 1cm from the rim, inside and out.

i considered CO2 or tobbaco deposits reacting with HCL vapor, i can`t see how C)2 would cause a reaction as both would be acidic anyway, tobaco maybe???

adjacent chems are all stoppered AND the same effect happens with homemade HCL(aq) if left long enough in a test tube. i know this because i gathered and crushed some iron ore and let is sit in an unstopered test tube for about a week, same effect?

so i`m fairly sure that it is quite strong HCL(aq) that i`m using in this Phorone then ultimately the DDDP trial.

at a loss here as to why i`ts not working re: color change?

vulture
June 20th, 2003, 01:36 PM
Are you sure you are not just simply seeing HCl vapor rising from the testtube.
The only thing I could think of is NH4Cl deposition but that seems odd since there is no ammonia in the air I assume.

Glass is normally not attacked by HCl.

I sincerely hope you didn't mistake HF for HCl! But that seems rather impossible, as I don't think you would still be here typing replies then...:eek:

The color change is easily noticeable after an hour at 40C using 37% HCl.

yt2095
June 21st, 2003, 06:37 AM
Vulture, your an absolute genius!

Ammonium chloride... you got me thinking along those lines of possible air contaminants.
Ammonia, but i have no Ammonia???

But i DO have 3 cats! and the litter tray does need changing more often than it gets changed, and the weather here of late has been less than comfortable because of the heat.

the "frosting" is Chloride of cat piss! :)

who`de have thought it eh :)

nice work.

rooster
June 21st, 2003, 08:32 AM
Humans, and probably cats also, do not produce NH3 directly, as it is poisonous to them. Instead they convert it to urea. The only solution i can see is that some decomposition product of the cat piss is ammonia. Maybe urea is converted to ammonia?

yt2095
June 21st, 2003, 09:17 AM
Rooster,
your 1`st assertion is quite correct.

Urea does indeed breakdown to NH3 then almost imidieatly to NH4(aq).
but you know as well as i that even the (aq) version sticks like hell! :(
and so does this room when the litter tray gets overlooked and the weathers hot.
common toilet bleach in a watch glass or my chlorate manufacturing usualy counters this, the price you pay for for having a wife that will only enter the Lab, with writen permission or to bring me another beer :) (just kidding)

but Vulture was quite right, i never even considered the ambient ammonia untill he suggested it.
Hmmm... a thought just occured to me, perhaps if i poured dilute niric acid in the litter tray and let it dry with some fuel oil... :)

fayll
July 22nd, 2003, 03:59 PM
This is the original German patent for DPPP in german language :


DPPP01 (http://vanphai.free.fr/DPPP/DPPP01.pdf)
DPPP02 (http://vanphai.free.fr/DPPP/DPPP02.pdf)
DPPP03 (http://vanphai.free.fr/DPPP/DPPP03.pdf)
DPPP04 (http://vanphai.free.fr/DPPP/DPPP04.pdf)


--------------------

bloodbob
October 18th, 2003, 05:33 AM
Assuming the phoron density is less then water then the best way to make the phoron is with dean-stark condensor ( I'm assuming we are doing condensation reactions ) .

nitric63
October 19th, 2003, 12:52 AM
Originally posted by THErAPIST
oh... an update since i had the idea. i put 90 mL of 6% peroxide into a mason jar and then i added the 5 heaping teaspoons of hex along with 2 heaping teaspoons of NH4NO3 and another 45 mL of 30% H2SO4. when i added the sulfuric the whole thing turned yellow like orange juice and then got really really cloudy, so i let it set there for a few minutes. within about 10 minutes i had some yellow fluffy precipitate on the bottom and top of the liquid, so i let it sit there another 3 hours. then I went and filtered and washed the stuff. the stuff was yellow to start with but the more i ran water thrue it the more white it got. then when i added the 10% sodium bicarb it got pretty much pure white. so i dried it and all and then went and pressed 2 grams (i made 2 batches) into a plastic drinking straw. I fused it and then took it and an acorn squash out into the woods. i stabbed a hole in the squash with a pencil when i was on the way there. when i got there i put the extremely large blasting cap inside the hole, lit the fuse and trotted off about 100 feet. when it went off it didnt make much noise at all but ill be damned if the squash didnt get obliterated. the biggest piece i found was about as big as a marble, and not ona those big marbles either. not to mention the piece was some 70 feet away. the dirt where it had been sitting was pretty messed up too. in my opinion it was more powerful than HMTD but i dont know how to conduct many tests to prove this. im gonna make a gram charge of both and set them on the same thing to test bristance and such sometime soon though. the crystals seem to be slightly smaller than those of HMTD also. anyone care to give me some ideas on how to test the stuff? or maybe make a batch yourself and test it? whatever. just makin an update. ill get the pics up when i can. cant find my fire wire <img border="0" title="" alt="[Frown]" src="frown.gif" />


<small>[ December 02, 2002, 12:07 PM: Message edited by: THErAPIST ]</small>

Perhaps along with some HMTD there was hexamine dinitrate formed. Perhaps you should try this again but leave out the xNO3 and see what happens.

The point of posting this was my small response about the hexamine dinitrate which I had accidentally put inside the quotes.

blindreeper
October 19th, 2003, 01:36 AM
nitric63, may I ask what was the point of posting that?

me234
October 20th, 2003, 10:54 AM
I have just read through all 3 pages of this thread and noticed that so far no-one has mentioned trying the DPPP with H2SO4. Many moons ago I was making a small batch of AP, approx. 5ml's worth, and for a change I added the acid to the acetone first, I think I might have read somewhere that this was a better method for making AP (Sadly, I suspect a kewl site at play here). The acid I used however was concentrated H2SO4, and after a few seconds I had an ever darking solution the same colour as mega's was after an hour, I was just wondering why not try refluxing using sulphuric acid, it does have the added effect of dehydration, I just thought this might be nice as mega's synth of phorone stated that a dehydrated product was neccesary. However I am a newbie and I may be well off the mark, so I hope the idea was useful.

My apologies, Boob Raider also mentions having used H2SO4 as his acid. Boob Raider, what strength sulphuric did you use?

McGyver
October 20th, 2003, 08:23 PM
Just an idea, how about contacting the guys behind the patent "I was woundering..." :D

T_Pyro
November 1st, 2003, 01:20 AM
On a number of occasions while making some AP, I had noticed that the acetone started turning yellow when it came into contact with conc. H2SO4. I was clueless as to what the compound was, until I came across this thread.

Well, I took about 20 ml of acetone and 20ml of 98% H2SO4. In about 1hr 30 mins, a dark reddish brown viscous, oily liquid had formed, which was lighter than water. Also, this compound had a very strong sweet kind of smell of acetone, but far stronger than acetone itself. This substance (phorone?) was cooled to 0*C, and 200ml H2O2 (at ~4*C) was added slowly, while stirring continuously. The mixture was left aside for 96 hours at room temperature, at the end of which I noticed yellow fluffy crystals on the sides of the beaker, and floating on top of the liquid. These crystals deflagrated when lit, giving out flame "tongues" about 3cm long. The fierce "whump!" that accompanies the deflagration of unconfined AP was missing. I haven't tested the compound under confinement yet.

For the conversion of acetone to phorone, does the Cl- ion of HCl play a part too, or is it just the H+ ion which brings about the polymeristaion? I've read through the previous posts on this forum, as well as the "other" forum, but I was unable to come to an unambiguous answer. None of my organic chem books deal with phorone or the polymerisation of ketones, either!

me234
November 27th, 2003, 12:58 AM
Has no-one here been able to buy phorone? a place near me sells iso-phorone (their name) for a few dollars a kilo, you guys think this might work ok for the synth? is there anything wildly different about the iso- form that might screw things up majorly if I try this?

PyroNitrate
November 27th, 2003, 08:45 PM
Depends on purity.... There could be other ingredients inside it which could totally mess up the experiment, or even harm you.

Sorry didnt see your end statment, Check the percentage, if it has other ingredients, you should probley extract the phor from the other ingredients.

knowledgehungry
November 28th, 2003, 06:54 PM
Umm, isophorone would be a different isomer of phorone, not a mixture of different chemicals.

T_Pyro
November 29th, 2003, 08:00 PM
Usually, the prefix "iso-" means the presence of a (CH3)2 group, or 1,1-dimethyl group. But how this figures in the structure of phorone, I have no clue whatsoever!

me234
December 3rd, 2003, 01:28 AM
the place I'm going to get it from generally has pretty good stuff, if it's not 100% or there abouts they'll tell me, I'll post % if I try it any time soon, nobody have more info?, I know it'll be a different stucture, I'm just wondering if it might not still work somehow. Anyway

Desmikes
December 4th, 2003, 01:57 AM
Earlier in the thread it was mentioned that someone did purchase PURE phorone but still wasn't able to make DDDP.
Now that I started posting, I'll tell about my experience with synth. All three chems that I used were very pure lab reagents all of which were spec (or whatever) tested. My HCL was 37.5% and 35%H2O2. After weeks or may be even months I added H2O2 and here's what I got: for uncontroled tempr reaction (which heated up a lot and was even spitting for a little while) I got brown oil that was not at all soluble (5% of total volume). For a narrow (2 cm) and long tube that was fully submerged in crushed ice + H2O, I got some yellow precipitate, which soon filled up almost the entire volume of chems but apparently dissolved or shrunk to about a half the V by next day. That's after sitting for roughly 24 hrs at room temp.
after drying that orange-yellow crap for DAYS, it still acted like putty. It didn't make AP whoosh when set on fire and produced some black smoke.
I think that it wouldn't dry very well and produced black smoke b/c of that oil. Does anyone know what that oil is?

The_Rsert
November 14th, 2004, 04:28 PM
Well, I took about 20 ml of acetone and 20ml of 98% H2SO4. In about 1hr 30 mins, a dark reddish brown viscous, oily liquid had formed, which was lighter than water. Also, this compound had a very strong sweet kind of smell of acetone, but far stronger than acetone itself. This substance (phorone?) was cooled to 0*C, and 200ml H2O2 (at ~4*C) was added slowly, while stirring continuously. The mixture was left aside for 96 hours at room temperature, at the end of which I noticed yellow fluffy crystals on the sides of the beaker, and floating on top of the liquid. These crystals deflagrated when lit, giving out flame "tongues" about 3cm long. The fierce "whump!" that accompanies the deflagration of unconfined AP was missing. I haven't tested the compound under confinement yet.

You had'nt made DPPP!
H2SO4 and aceton will from some propyl ethers which will form peroxides like AP in contact with air or H2O2.
I have heard that pure diisopropyl ether will form pure (maybe mono-) AP in contact with air under reflux.


Maybe another way:
A few weeks ago I have heard that 2l 10% pure percarbonate solotion, 300ml 20% HCL and 300ml or less Aceton will form after 4 days about 70g pure DPPP (after recrystallising).

Then I have mixed 1l bleach ("Ace - Milde Bleiche", contains 5-15% oxygen based bleach) with 200ml Aceton and 250ml 24%HCL in a 5l canister.
After 3-4 Days i had 36.8g (after recrystallising) of a white explosive powder with a very low density. Maybe it's pure DPPP!

Another idea to separate AP from DPPP:
Make an emulsion of your stuff in water and cook it for a few minutes, AP does decompose in water a 90°C, but DPPP will decompose over 180°C.

FUTI
November 15th, 2004, 04:07 PM
I do not agree about propyl ether formation from acetone and sulphuric acid. Also ethers make their own kind of peroxides on standing on air and light exposed through radical mechanism without hydrogen-peroxide added at all. I saw once the result of mixing sulphuric acid and ketone similar to one described so I do not doubt the report made here. What is the structure of product is diferent issue. I would bet on condensation if I have to...but I wouldn't like to test my fortune with explosives soo...

I liked the percarbonate idea although the numbers are little confusing for me. It looks like it is very low percent peroxide solution during reaction after all. If you say it is so, I will trust you, but it seems then that somehow salt made during reaction forces reaction to making large organic molecule that are salted-out of solution to form precipitate. Enthropy is miraculous sometimes isn't it?

EDIT: Mumble said it true you can obtain mesitilen from acetone but I thought it needs high temperature. Was that acetone dried?

Mumble
November 16th, 2004, 01:09 AM
Well, I took about 20 ml of acetone and 20ml of 98% H2SO4. In about 1hr 30 mins, a dark reddish brown viscous, oily liquid had formed, which was lighter than water. Also, this compound had a very strong sweet kind of smell of acetone, but far stronger than acetone itself. This substance (phorone?) was cooled to 0*C, ....


I can solve this mystery. Your mystery substance is none other than mesitylene(1,3,5-trimethylbenzene). It's an aldol condensation of acetone catalyzed by acidic or basic conditions. Mesitylene is a redish liquid with a density around .88 with a strong sweet smell. I'm thinking we have a ringer here.

If you don't believe me have a look for yourself. http://www.worldwideschool.org/library/books/sci/chemistry/OrganicSynthesis/chap11.html
Your ratio is almost the same, and you allowed adequate time to react and adequate heat. I'm assuming from your post that you didn't cool this part of the reaction at all. To form this compound some heat is required.

Myrol
November 16th, 2004, 12:14 PM
A Month or so ago, I have made DPPP. The high VoD and being a easy Peroxide.......I tried it once. I didn't remember the amounts of Acetone, 30% HCl and Hydrogen Peroxide but I have done it this way:

The Acetone and the Hydrochloric Acid was mixed 1:1,5 by Vol. and tempered to 60°C for over four hours. I got an deep red solution wich smelled ABSOLUTELY different as Acetone. I prepared the mix for the peroxidation and added under very strong chilling (5kilos of Ice-Salt!! :eek: ) small amounts of H2O2. I never had seen this before but even with this huge Icebath the temperature rose a little after I added 10ml H2O2 to the mix!!!!! White crystals appeared, the mix lost his red colour. After being ready, I bumped the mix on a big Filter and washed him with lots of Carbonate sol. and cold Water.

The Yield was unsatisfying, a blame for this effort. Something around 60g but Im sure my Batch contained over 600ml liquids. And the next thing why I hate DPPP-> it stinks terrible, burns and irritates almost everything, the eyes, throat, nose, skin and your lungs. Im sure it was freed from Acid but DPPP is extremly volatile so thats why I think it irritates so strong!

knowledgehungry
November 16th, 2004, 12:58 PM
If DPPP really is as volatile as some people claim that would explain why such a seemingly great explosive is very uninteresting to explosive experts in general.

The_Rsert
November 20th, 2004, 09:07 PM
My explosive powder (made of sodium percarbonate solution) don't stinks.
But it's lighter than normal AP and the dust of it burns in my nose.
The normal AP dust don't burn in my nose.
:confused:

Now, who has made really pure DPPP ??? :confused:
:confused: :confused: :confused:

Another Idea :cool:
When DPPP is acescent, maybe it will form explosive salts.
If anyone have time, please test it salts for properties, and features for example of the DPPP sodium salt.
(mabe it can be prepared by mixing of anhydrous NaOH(39.9971 g/mol) and DPPP(2838.8579 g/mol) in much anhydrous ethanol. Then recrytallize the the salt if it's possible.
:rolleyes:

Mumble
November 20th, 2004, 10:29 PM
EDIT: Mumble said it true you can obtain mesitilen from acetone but I thought it needs high temperature. Was that acetone dried?

Just the heat of the sulfuric and acetone mixing is heat enough. If you pour the acid in the acetone, you will notice it becomes very hot, and may even spot boil. Within probably 30 seconds it turns an orange shade and has a familiar aromatic odor being emited. If you let it cool back to room temp, and dilute with an equal volume of water you will see the redish-orange layer on top. Trust me, I tried this just last night, I need mesitylene for another project of mine. I think any water in the acetone sort of catalyses the reaction by providing heat from dehydration with sulfuric acid, and then the conversion to mesitylene produces even more water so it just continues on.

The method used, just mixing the two, isn't the best method for the preparation of mesitylene, but it does in fact work. If you actually want to produce the compound, I suggest following the proceedure from the link I provided.

FUTI
November 24th, 2004, 05:50 AM
to Mumble: Thanks. I figured this out myself. After all how much you can heat the mixture containing acetone to acetone boiling point at best. I agree with all said on that issue.

But I have another question...can mesitylene form peroxide?...explosive one?...I know cumene can form hydroperoxide so there is a slight chance that mesitylene can to...but does anyone know for sure how this work with mesitylene?

knowledgehungry
November 24th, 2004, 08:34 AM
When DPPP is acescent, maybe it will form explosive salts.
If anyone have time, please test it salts for properties, and features for example of the DPPP sodium salt.
(mabe it can be prepared by mixing of anhydrous NaOH(39.9971 g/mol) and DPPP(2838.8579 g/mol) in much anhydrous ethanol. Then recrytallize the the salt if it's possible.


If you look at the structure of DPPP I doubt you will find a way for it to form a salt very easily. For a compound to form a salt it needs to be able to pick up either a negative or positive charge, neither of which are very likely in this compound.

The_Rsert
November 24th, 2004, 11:45 AM
OK, "knowledgehungry", Now I see, too! :eek:
But how does it look with HMTD, I have heard that it will form very unstbale salts in contact with metals...maybe it exsists a stable salt of it. But that fits not to this thread... :)

To the way with the sodium percarbonate :cool: :
A lab lab assistent, I asked meant, that the bleach "Ace - Milde Bleiche" will form the peroxid very slowly, in cause of the precipating NaCL and the low H2O2 concentration. So that the acetone go to phoron first. Thats all.
You will never get really pure DPPP by this way I think. :(
But its an good compromise, because(pressed) its better than normal AP.

I have just made it again, with the same bleach but with less HCL so that the phoron will not formed so fast. The product was much more like the typical AP than/as before.
This supports the theory of the lab assistent.
:( :( :(

And now again, who has made really pure DPPP?


I'm sorry about my bad english.

knowledgehungry
November 25th, 2004, 08:44 AM
HMTD has NH2 groups on it which are much easier to form a salt with. Salts in general are less stable than their organic counterparts.

The_Rsert
November 25th, 2004, 09:44 AM
The Yield was unsatisfying, a blame for this effort. Something around 60g but Im sure my Batch contained over 600ml liquids. And the next thing why I hate DPPP-> it stinks terrible, burns and irritates almost everything, the eyes, throat, nose, skin and your lungs. Im sure it was freed from Acid but DPPP is extremly volatile so thats why I think it irritates so strong!

Maybe, you have destroyed your phorone in the solution incause of the long heating period.
Was it under reflux? Because acetone does boil at about 57°C.
In the original German patent it says, that the yield should be over 90%.
Has somebody fuming HCL?
Because in the original patent it says, that you will need high concentrated HCL and not 25% or 30%. And there it says nothing with boiling or heating. :)

Here is my link to the original patent:
http://members.fortunecity.de/potatoguns/



To "knowledgehungry":
OK, maybe I will test carefully to make some HMTD salts by myself in the next weeks, bacause the stbale salts will not form other more unstable salts so fast as normal HMTD. :p

Joeychemist
November 28th, 2004, 01:39 AM
Has somebody fuming HCL?
Because in the original patent it says, that you will need high concentrated HCL and not 25% or 30%. And there it says nothing with boiling or heating.

Rsert

I had a problem once with fuming acid while attempting DPPP, I ran out of lab grade 35% HCL acid so I went out and bought muriatic acid containing 31% HCL acid and added it to my acetone, The mix began to fume off what I’m pretty sure was all of the chlorine and hydrogen gas that was in the acid, It did not change to phorone, it did not even slightly turn yellow, I let the first mix fume for awhile, then heated until the acetone was just starting to bubble then I tried a mix in the freezer. No phoron was formed.

After I added the 6% peroxide and it did not even form a small amount of AP. This is how I know that all of the chlorine and hydrogen separated from the acid into gas insted of polymerizing the acetone to phorone. If the chlorine and hydrogen would not have separated from the acid, it would have still acted as a catalyst to form the AP. I have not had this problem before until I used the muriatic acid. Either the 31% HCL acid in the muriatic acid is not concentrated enough or contains an impurity other than water.

Dose anyone have an explanation as to why the chlorine and hydrogen was separating from the acid into gas form? I must say, I was gasping for air after I got a nice whiff of the chlorine. :eek:

nbk2000
November 28th, 2004, 10:01 PM
The peroxide oxidizes and the chlorine is released.

Joeychemist
November 28th, 2004, 10:23 PM
The peroxide oxidizes and the chlorine is released.

Mr. NBK

I did not add peroxide to the mix for it to start releasing all of the gas, I just added the 31% HCL muriatic acid to the acetone and it started releasing all of the gas. 31% HCL acid should be enough to polymerize the acetone to phorone. Like I said I’ve never had this problem with my lab grade 35% HCL while making DPPP and I never have had the problem since. It was only the muriatic acid Maybe it was just a nasty side reaction caused but the contaminants in the muriactic acid. I will try a different brand of muriatic acid to see if the same reaction occurs.

FUTI
November 29th, 2004, 03:06 PM
Just a thought but since HCl is already leaving solution at any concentration higher than about 20%, maybe it was just HCl that make you caugh. When you mix two different solvent, certain amount of energy is released and that would lower solubility of gas in water. You can try mixing alcohol and destilled water...you will notice bubles leaving solution on their mixing. Maybe this is what "burn" you during that attempt, if it is as you said happend before you added H2O2. Percent of acid get to low in solution due to "evaporation" and reaction was slow and you couldn't "salt-out" the product. Just a thought...

Joeychemist
November 30th, 2004, 12:25 AM
if it is as you said happend before you added H2O2. Percent of acid get to low in solution due to "evaporation" and reaction was slow and you couldn't "salt-out" the product. Just a thought...

Futi

The acetone did not polymerize to phoron so I didn’t even have a chance in hell of “salting out” DPPP, AP was not even formed. That is what has me so damb convinced that all the HCL turned to gas. (I should have measured the amount of liquid left in the bowl).

I wish it was just a small amount of gas released but I’m sure all the chlorine separated and turned to gas. There was only 300 ml in the bowl and my garage was filled for fifteen minuets with very thick white gas that floated close to the ground. The reaction was very violent and produced much more gas then a regular reaction dose.

I understand fully that during the reaction chlorine is freed which bonds with three hydrogen atoms of the phoron to give 3 HCL and then bonds with the phoron. I also understand that adding the peroxide forces the chlorine off and bonds itself to the phoron, thus creating more free chlorine.

I was just wondering if anyone else has had this problem with muriatic acid while attempting DPPP. It was two failed attempts and since then I make a note of it not to run out of the 35% HCL. 31% should have worked but didn’t, instead it (for some strange reason or another) reacted violently. :confused:

FUTI
December 5th, 2004, 04:09 PM
Now I'm lost. Did you or didn't you added peroxide to solution...NBK2000 already asked this and you said no, now you answer me something different that AP wasn't formed. If there was no peroxide how it could form in the first place? Sorry if I miss something in your post but it didn't match the way I see it. Rest of the story is OK. Gas produced heavier than air could be both Cl2 or HCl.
Does anyone know can CaCl2 added to that solution with slow adding of sulfuric acid generate good mixture of HCl that will compensate the troubles. You will have to remove CaSO4 and purify the product but if it works better...

edit: NBK2000 proposed chloride being oxidised by peroxide (this is real reaction). You also wrote at first about hydrogen and chlorine evolution (highly unlikely to occure here), posibly as your first conclusion; but then later reported that gas evolution starts even without peroxide. And that caused the problem with my understanding of what you posted (like there was not enough of it already in that reaction).:(

If you gona use ZnCl2 use it in conc. HCl like Lucas reagent. :D

You are right about CaSO4 being hygroscopic, but as you gona use it in water solution it will form dihydrate, this could reduce the chemical absorption problem but could make the nasty slurry and trap your reactants in physical way. Mix it all well and filtrate the mixture trough a flutted filter paper, wash the precipitate with small portion of water or acetone, and leave it until product start crystalize out of solution. I had the impresion that product do not separate during initial mixing, but on prolonged standing so this procedure could work in that case. I just hope that solid formed do not somehow catalyticaly promotes product formation (but I doubt it) and entrap it in CaSO4 precipitate, but even in that case you can obtain product by precrystalisation. Happy hunting! :)

Joeychemist
December 5th, 2004, 07:02 PM
I did not add peroxide to the mix for it to start releasing all of the gas, I just added the 31% HCL muriatic acid to the acetone and it started releasing all of the gas.

FUTI

I think I might have messed you up. If you read word for word I added the peroxide after the gas was formed and dissipated, and that’s how I came to the conclusion that my HCL turned into gas. That’s why not even AP was formed. Because the there was no catalyst left in the solution when I finally added the peroxide to the solution. I knew that DPPP would not be formed because phorone was not formed. I simply used AP as a reference to the HCL separating from the solution.

About what you said though FUTI, I was thinking maybe ZnCl2 or CaCl2 could be used along with the slow addition of dilute sulfuric acid too!

But I think because concentrated H2SO4 would be too strong it would lead to carbon and the H2SO4 itself would react with acetone to form mesitylene.

Also would the CaSO4 not absorb some of the phorone due to the fact the CaSO4 is a bit hygroscopic?

The only way to know for sure is to test the theory, because after all it’s only theory until it’s proven a fact!

Joeychemist
December 7th, 2004, 08:40 AM
You are right about CaSO4 being hygroscopic, but as you gona use it in water solution it will form dihydrate, this could reduce the chemical absorption problem but could make the nasty slurry and trap your reactants in physical way. Mix it all well and filtrate the mixture trough a flutted filter paper, wash the precipitate with small portion of water or acetone, and leave it until product start crystalize out of solution. I had the impresion that product do not separate during initial mixing, but on prolonged standing so this procedure could work in that case. I just hope that solid formed do not somehow catalyticaly promotes product formation (but I doubt it) and entrap it in CaSO4 precipitate, but even in that case you can obtain product by precrystalisation. Happy hunting! :)

FUTI

I almost didn’t see you’re edit. I’m glad you and I are on the same page now. :cool:

I also think that SnCl4 (Stannic chloride) should work, I don’t have any ZnCl2 or CaCl2, so I will buy some Stannic chloride and try using that. Which should actually be more eficient than CaCl2. Which if the CaSO4 dose turn into a nasty slurry it would be a lot of work compared to other methods.

I will try using SnCl4 this week and post my results. Next week I will try some others methods, just for the hell of it. :D

FUTI
December 8th, 2004, 02:45 PM
Thanks for mentioning SnCl4 Joeychemist...I was thinking what is neat way to produce good amout of SnCl4. And I found answer where I weren't expect. School lab drills;)
If you mix SnCl2 with methyl-orange and expose it to sunlight you get Sn4+. I just hope to find the way to get rid of the balast compunds. I do know that there are beter ways, but SnCl2 is easy to make from solders, and methyl-orange is IIRC sold at stores as indicator for water pools.

megalomania
December 8th, 2004, 06:01 PM
How do you make SnCl2 from solders, and what exactly is a solder anyway?

K9
December 8th, 2004, 06:52 PM
I would assume he means reacting a tin based solder (for welding) with HCl.

Joeychemist
December 8th, 2004, 08:48 PM
SnCl2 is easy to make from solders

FUTI

I hope you know that solder is an alloy, right, Most solder is a mix of 60% Sn 40% Pb, silver can also be used along with other metals. So FUTI I suggest finding a more pure form of tin to make your SnCl2 with. Have you thought about using tin cans maybe.

FUTI
December 9th, 2004, 06:28 AM
I thought that tin cans contain only thin layer of tin accros other metal made through electroplating. And yes I though about alloy of tin...I need to find a silver based one since it will give near pure SnCl2 made through dissolving in hydrochloric acid. PbCl2 isn't much soluble in water and AgCl even less. HCl further reduce solubilty of those and can enhance solubility of SnCl2 through complex formation. PbCl2 can also became more soluble in warm acetic acid solution, so I guess it also can be mede more soluble through complexation. I read somewhere on this forum that there are Cu based solders? Any hint for me where to look for specific solder type, I guess some of you guys more experienced in electronics and welding can help me. I didn't say I made SnCl2 from solders, I'm sorry if it sounded that way...but I certainly will try to do it.

BTW I forgot to say earlier if anyone will try anhydrous ZnCl2 and try making Lucas reagent as I proposed with concentrated hydrocloric acid...I forgot to say it makes a lot of heat and HCl fumes on mixing. Precool that acid before making reagens...and if posible it is good idea to melt ZnCl2 in flask under vacuum and cool it down without exposure to water.

nbk2000
December 10th, 2004, 07:36 PM
McMaster-Carr sells elemental tin in various forms for about $10/pound, last I saw.

kingspaz
December 10th, 2004, 10:03 PM
Solder is normally an alloy of tin and lead, or tin and silver. Lead free solder is however 99% tin. The only problem with using solder is the removal of the flux. I'd imagine this could be done relatively easily by simply melting the solder and allowing the flux to boil off.

Mr.ANFO
December 24th, 2004, 01:14 AM
alrighty, I think I have made DPPP in relatively pure form see this http://community.webshots.com/user/matsumoto_hideki
... what % I am not sure but it looks a hell of a lot like Ap with the exception that it has a distictive yellow colouration to it.
My method was via the 1:1 2:1 H2O2 method HCl@35% to Acetone then adding heat taking this liquid down that black-red colour (VERY DARK) and then letting this liquid sit for a few days to a week in the open to cool and let some of the unreacted acetone to vapour off. I then took this liquid and chilled it for several hours in a freezer at -25c ie) below -5c is good enough!
The Peroxidation is the hard part since the moment the peroxidation occurs the heat really being to climb rapidly, I find you have only a few secs between the formation of YELLOW precip and the secondary reaction which intitiates a complete boil over...
So as soon as you see the precip form wait 3-5 secs then nutralize the reaction with Ammonium Hydroxide.
Precip is yellow to yellow white and has way more power than AP! I have a few movies of AP and DPPP going off in the same amounts and the results are clearly visible. DPPP also seems to detonate in much smaller quantities than AP does and doesn't seem to sublime at all at room temp ( It does have a sharp odor simular to AP but more fruity). weird stuff. Please tell me what you think :)

The_Rsert
December 24th, 2004, 06:26 PM
I have just found this:
http://www.sciencemadness.org/talk/viewthread.php?tid=1031&page=2

"...Another high order explosive that I have tried with sucess is D.P.P.P.D or D.P.P.P.
It is called chemically Dipherone Pentaperoxide (Diamine) and has the highest detonating velocity of all Organic peroxides at 9.8Km sec.
This is made my adding Acetone to HCL and heating it to around 40-50c the mixture turns green/yellow and smells pungent. leave this to sit/evapourate and collect the yellowish crystals from the residue after the precip has formed. This process is long 12-48hrs and needs careful inspection!!!
Add Hydrogen peroxide to the crstalline mass and chill immediatly in a freezer.
the end result is a greenish soild crystalline mass. Dry this out and it becomes an extreamly powerful heat sensitive explosive with a det velo of nearly that of PETN! BE CAREFUL WITH THIS STUFF AS IT IS ALSO HIGHLY TOXIC AND FRICTION SENSITIVE// DONT PUT IT IN A SCEW CAP CONTAINER OR IT WILL DETONATE!!..."

This way of synthesis seems to work fine.
No I have 38% fuming HCL. I will test it tommorow.
:)

Joeychemist
December 24th, 2004, 07:10 PM
Mr. ANFO, (AKA;J-scan, hidiki matsumoto, cato-exp,and Dr.Boom) was recently banned from Sciencemadness discussion board for being a liar and a k3wl, He is not a credible person, and I strongly suggest you question everything he says. You will find this forum much stricter than the other forums you have k3wled up with you’re bullshit. Hideki Mr. ANFO whatever you call yourself I don’t like liars and I don’t like you :mad:


R Sert

What the hell are you smoking??? Read that thread very carfully. The person that posted that was banned for being a liar and for flat out being a stupid tard. Actually it was Mr. ANFO (the idiot above your post).

After 48hrs of heat phorone crystals will form. That’s all. The moron who posted this was just trying to act k3wl at another forum (where that quote was taken from).

That is just another DPPP synth, only instead of acid/acetone/phorone you use pure phorone crystals. It should work still just the same. You might even get a better yield.

Barnacles
December 24th, 2004, 07:39 PM
Hey joey if you dont like liars don't lie yourself I found you on someones page claiming to be admin here and threatening to ban him. I thought I'd post this because I cannot mail any mods http://community.webshots.com/scripts/guestbook.fcgi?albumID=232298508
If hes a filthy liar the people here would find out after very few posts. So don't ruin it for him here quite yet.

Joeychemist
December 24th, 2004, 07:47 PM
The nerve of you shawdow, I did not claim to be an admin or a moderator for this forum. I said this was my forum and I would kick him out if he continued to lie. And by that I meant let the proper people know what’s up. I was angry and wrote that post off rather quickly. Don’t you dare put words into my mouth shawdow :mad:

The_Rsert
December 24th, 2004, 07:58 PM
Of course I know, that the bad boy who wrote that AP has 200% of the power of TNT has smoked to much musket.
I meant the way, to use the solid phorone.
Maybe the, in the orignial patent described, DPPP yield of 90% is based on the solid phorone?

nbk2000
December 24th, 2004, 09:23 PM
On December 23, 2004 at 8:00 am, joeychemist wrote:
Hidiki,DR boom whatever, I noticed you joined the explosives and weapons forum under the name j-scan today.well i just want to tell you that I love the E&W's froum and I will not have you lying or blowbaging or triple posting in my forum. I noticed you were reading the FAQ's today, I suggest you read the rules. I am willing to let this go. I will not tell my forum members that you were caught lying at MSDB. bUT IF i (WTF? :rolleyes: NBK) catch you lying or talking out of turn or if I'm even having a shitty day, belive me,I will kick you out of my forum! I hope you read this and really do become a part of the family.I do belive you made DPPP and I am glad you show a willingness to learn.I also notice you're from canada,please contact me at nbk-1killer@lycos.com Joeychemist


He used way too many possessive articles in his sentences, implying that he had the power to make such a decision. That, and the e-mail addy he used belonged to a member that was previously banned for stupidity. :rolleyes:

Too bad he didn't have the good sense to know better than to even come close to implying he was staff, let alone ME. :p

Though how anyone able to read above the elementry level would confuse me with him, considering his abysmal grammer and spelling skills...;)

Oh well. He'll no longer be a shadowing our doorsteps here. :)

j-scan
December 24th, 2004, 11:11 PM
I believe their is some confusion here. First of all, I am the host for a network of computers. I run a single IP addressed LAN with multiple users off a HUB. The administrator over at Science Madness went and and banned the entire IP address without looking at the individual user accounts. 1 user was at fault for blacklisting my entire IP..now nobody can join. not good! I explained my situation and was called a lier. This really bothered me! I was met with pure hostility...I couldn't even explain myself first. No...you will not see me "j-scan" double posting at all in this room.

Hopefully, I can somehow speek to the admin of "science madness"and explain the situation again.
------------------
DPPP synth: for which I was called a lier for---->

I was very critical of my roommate for posting material that had not been fully examined. I to tried to prove him wrong by creating a batch of supposed "D.P.P.P". The crystalline mass at the end of the reaction was light yellow and formed instantly when the Hydrogen Peroxide came into contact with the Chloro-Phorone. Chlorine gas was expelled from the reaction. I was able to test 2grams of supposed D.P.P.P product against 2 grams of cold formed AP (dicyclo acetone peroxide I believe--could be wrong) and the results indicated that supposed D.P.P.P. had a significantly higher detonation velocity through examining blast fragments from a soup can detonation. Sure the method is crude, but I have a ball park figure and i know this material is more powerful that standard AP.

megalomania
December 25th, 2004, 09:10 PM
All right, the show is over, nothing to see here. Lets keep this thread ON TOPIC from here on in. If anyone feels the need to discuss this little soap opera make a post in the water cooler. Unless its about explosive peroxides, it does not belong in this thread.

Mr.ANFO
December 26th, 2004, 01:20 AM
alright all those who think I lie all the time... explain this ... Why doesn't Phorone directly peroxidize in an HCl soultion? *****YOU CANNOT PEROXIDIZE PURE PHORONE IT DOES NOT WORK******.. Others have tried and failed miserably. The method as I stated using 30-40% HCL seems to work just fine, because the phorone is bonded to 5(Cl2)'s = AS THIS IS ALSO EXACTLY WHAT THE GERMAN PATENT USES
thanx... And yes the crystals are yellow when you are finished.
AND As I said again, it is better to overestimate (as I have done on some occasions, I admit) an explosive than to underestimate it. Underestimating an explosive usually leads to DEATH or severe injury! Joey and R_sert. NO HARM DONE IN OVERESTIMATION, HOWERVER THE REVERSE IS ALWAYS TRUE>

Rosco Bodine
December 26th, 2004, 11:17 AM
Mr.ANFO ,

Please give a very precisely accurate and thorough step by step description of your method for DPPP ,
so that others may easily reproduce and confirm your results . If you keep things matter of fact and
tell it like it is , then people will respect you , and a flamewar will not waste the bandwidth we are allowed
to use for sharing good information .

j-scan ,

If you have confirmed the method for DPPP , please share your own description
of the method giving all the details as accurately as possible .
It is understandable to become excited when succeeding at an experiment
which has failed for others because of simple details that have not been
fully identified as being important to the outcome of the experiment .

The quantities and order and rates of addition and temperature of reaction
and the times for reactions may be very critical to reproducing good results .
And what may seem simple to someone having succeeded , may include a detail
which confounds a dozen others who cannot duplicate the result because of
a single critical factor which they did not know was essential . Please be precise
in describing times for example , " a few days to a week " is *not* a good indicator
of a reaction time for a mixture where a polymerization is occuring . It would
be better to say some number of hours at a certain temperature . You should
understand the conventional way of describing how a synthesis is performed ,
in the usual style of technical writing which is attentive to the essential details .
Perhaps you could assist Mr.ANFO in doing a proper writeup so that anyone else
can reproduce his reported results .

nuclearattack
December 26th, 2004, 02:23 PM
I'm with Rosco, please Mr.ANFO and j-scan give to us a good description of the procedure! I want to replicate the synth and make some tests with this DPPP, if you are right someone (perhaps me if i'll be able to do DPPP) will confirm your claims and your reputation will rise a lot. :) Personally i don't believe to people that make bad claims on other persons so i want to follow your procedure and see once for all if you are right.
Science is not only theory but experiments and incontrovertible results!

SweNMFan
December 26th, 2004, 02:37 PM
Did try it today. Mixed 50ml acetone with 60ml 30% HCl and heated it in a salted water bath for maybe 30min, the solution turned yellow and did fume and smelled not very nice.. anyhow the solution finally stopped producing the white vapour so I placed the flask in my freezer. It still had dark orange colouring when I took it out. not as red as in the pictures. But it was -8 C and still a solution. It now had a volume of 74ml. So I slowly started to add 32ml 30% H2O2. After the first drop the solution started to get milky as crystals formed. The temp rose from -8 to 9° C after first 3ml of H2O2 (And I did have a salt, ice bath) So I dumped in the rest of the H2O2 and then dumped it in the filter, which was a bad thing to do as the H2O2 bleached thru my coffee filter in 2 sec and the whole batch went down the toilet..

So

The crystals that formed looked more like HMTD than AP and they were slightly yellow.

Don't use synthetic coffee filters when doing this experiment.

The_Rsert
December 26th, 2004, 04:20 PM
Just a little tip:
When you are thinning the milky solution with water before filtering, you can use a normal coffee filter. That's easy and it does work very fine.
This is sometimes also very good for the yield, because sometimes there is some DPPP/AP dissloved in the acetone which will be precipated, if you will add some water.

j-scan
December 26th, 2004, 06:09 PM
Here is my write up...

I started with a 1:1 ratio of HCL and Acetone and added heat until the color changed to a dark orange. I continued the boil on a low setting and got the color down to a dark red -black) and then cooled it down over a period of days "freezer would have sufficed just fine".. The solution changed color again and the viscosity also changed to a motor oil consitency(very thick). This oily liquid is relitivly pure Pentacholorphorone (dark yellow orange.. looks black in standard light) say 90-95% and about 10-5% H20.. Ok I am guessing here... It has not much acidity to it anymore. You then have to add a few mls of HCL to get the peroxidation happening. After adding the HCl you then add H2O2 and give the solution a stir.
Cl2 is immediatly ejected from the solution (you can smell this)which turns bright yellow ( heat climbs up rapidly) and a yellowish orange precip is immediatly formed at the bottom of the flask... this then eventually migrates to the top of the flask where you can scoop it out with a plastic spoon. The more pure the liquid the better the yeild.. a small flask say 100ml SHOULD optimally yeild you around 80ml of crystals.
---problem occured the first time I tried this: because the solution was not completely reacted , TC AP formed with the DPPP... ALL of the left over acetone must be evaporated in open air for their to be pure DPPP.

-------------------------------------
more info and improved method as of 11pm Dec 25th:
--------------------------------------
Please follow carefully:

For the best results--->

200mL Acetone
300mL Muriatic Acid (30% HCL)

Mix together into a glass container and place into a hot water bath to 100C
Boil for 45 minutes until solution changes to a dark orange-red. Remove heat.
Allow the solution to cool off to 2 C or so for at least 10 hours without a lid. I left my solution for 24hours at room temperature. The solution should at this time be almost black as the HCL will have converted the majority of the acetone onto thick viscous Chloro-Phorone. Left over HCL content should be minimal.

The next step is to reintroduce 30ml of HCL catalyst into the Chloro-Phorone solution and add 500mL of chilled 35% H202. Chlorine gas will be expelled. A mass of yellowish -orange crystals should appear almost instantously, The temperature should increase slightly but should not boil over.
Dry the crystals using distilled water and ammonia/ or bicarbonate solution. rinse and dry.
-----the end product is quite stable when dry---not as shock sensitive as AP but highly explosive in the presence open flame or any surface temperature above 190C.

j-scan
December 26th, 2004, 07:14 PM
?In terms of filters I use good old fashioned paper towl .. it works well. just don't let the filter paper dry pit or you'll have C4 paper when you go and burn it in the incinerator.

Rosco Bodine
December 26th, 2004, 09:21 PM
j-scan

Your description is making sense to me .
The dark red-orange oily product you obtain as a * residue*
from the heated digestion , followed by evaporation of the
acetone / HCl mixture , according to the patent's reaction equations ,
is phorone dihydrochloride . If the patent is correct , this is next
converted to the pentachlorophorone by free chlorine , provided
from the separate side reaction between added HCl and H2O2 .
Evidently the pentachlorophorone formation then releases half
the same amount of HCl as was required in the earlier side reaction
between HCl and H2O2 which provided its 3 added chlorines .
The pentachlorophorone then reacts further with H2O2 to precipitate
DPPP , and also releases its chlorine in the form of HCl , in an amount
which corresponds to the other half of the HCl required for the
earlier production of free chlorine from HCl / H2O2 , along with the
HCl which was first bound with the phorone to form the "red oil"
phorone dihydrochloride precursor . Therefore the combined HCl contained
in the phorone dihydrochloride formed in the first part of the reaction
is released again as HCl upon the formation of the DPPP as a preciptitate .
It is this "extra HCl" being released which is causing the reaction rate to
"ramp" upward and the heating acelleration to be observed . The other
HCl present in the reaction system would be purely catalytic , but since
the concentration of the "catalyst" is always increasing as the reaction proceeds ,
then the reaction becomes "autocatalytic" , and inclined by nature towards
runaway . This sort of reaction has a high potential for disaster unless the
quantity of the reaction mass is limited to what cooling capacity can keep
within safe limits , and the shape of the reaction vessel and cooling surface area must
regard the thermodynamics of a particular "reaction mass" . These sorts of
reactions do not "scale up" directly so great caution should be observed .
For example a 250ml reaction mixture may be perfectly safe to manage ,
but there may be no power on earth which could keep a 25 liter reaction mixture
under control . This is the sort of reaction which must be adapted to continuous
flow and small reacting quantity "reaction zones" instead of any "vat process" for
a single large batch .

Have you tried the reverse order of addition to see if the exotherm is more manageable ?
For example , have you tried adding a catalytic amount of HCl , a few ml perhaps , to
the prechilled H2O2 , and then add the "red oil" to the cold , slightly acidified H2O2 ?
This would allow for the larger volume of the H2O2 to function as a "heat sink" by
virtue of its thermal mass , and serve to more greatly dilute the added HCl being released
as an aggravating autocatalytic presence . A simultaneous drip of a separate stream of
some HCl neutralizer might be started to help control the reaction mixture acidity ,
or perhaps alternately a buffer in the H2O2 could be useful in this reaction .

j-scan
December 26th, 2004, 09:43 PM
Have you tried the reverse order of addition to see if the exotherm is more manageable ?
For example , have you tried adding a catalytic amount of HCl , a few ml perhaps , to
the prechilled H2O2 , and then add the "red oil" to the cold , slightly acidified H2O2 ?
This would allow for the larger volume of the H2O2 to function as a "heat sink" by
virtue of its thermal mass , and serve to more greatly dilute the added HCl being released
as an aggravating autocatalytic presence . A simultaneous drip of a separate stream of
some HCl neutralizer might be started to help control the reaction mixture acidity ,
or perhaps alternately a buffer in the H2O2 could be useful in this reaction .
Reply With Quote
.

No, I haven't tryed this way yet. I have some Chloro-Phoron brewing and I will try your alternative method and see if the temperture remains more stable. :)

---go to upload those photos :)

Mr.ANFO
December 27th, 2004, 12:57 AM
Yes, my roomate and I.. jscan tried this and the results were not as good. Looks like Pentachlorophorone must have HCl added to catalyze it, then H202 added to PCP+HCL to peroxidize. Not the other way around or too much heat will be produced and it reverts back to acetone and a lower phorone %ile is observed. For some reason I keep getting TCAP in the method you suggest.. I am wondering why this is?
As you suggest keep the reaction small and better yeilds will be produced. OK .. good idea...

Rosco Bodine
December 27th, 2004, 01:50 PM
About the scaleup , not necesaarily keep the reaction small ,
as there could be a problem introduced by going either microscale
or macroscale . Until more is understood about precisely what
is occurring in the various reactions , keep the scale moderate
for safety and don't attempt a gallon jar sized batch .

Hydrolysis of the phorone dihydrochloride in preference to its
further chlorination to the pentachlorophorone could make the
reverse order of addition problematic . This process is evidently
affected by small changes , and precisely why so many people
have had problems with experiments to produce DPPP . The
frustration of many failed experiments not properly post mortemed
is likely responsible for many short tempers related to DPPP .
It has been something of a Rubick's Cube for organic peroxide experimenters :eek:

Another thought which occurred to me is that it may be useful to
dilute the "red oil" with cold methanol before adding to it the
H2O2 . And perhaps to divide the amount of HCl added for the
peroxidation catalyst , adding some to the "red oil" and some to
the H2O2 . By such manipulations of the conditions , and by varying
the rates of addition , the reaction can probably be made predictable
so that scaleup can be managed safely . The crystal form of the product
would also likely be improved if the precipitation could be slowed by
such methods .

j-scan
December 27th, 2004, 02:31 PM
this is an interesting idea with Methyl Alcohol....and I should try it.

Last night I created several new batches of phorone diHydrogen Chloride...and today I will peroxidize it all and take some pictures of the process. Hopefully no problems will arise.

stay tuned...

The_Rsert
December 28th, 2004, 09:32 AM
I made last evening some chlorphorone.
I heated 200ml fuming HCL with 200ml acetone to 30 min. 50°C and let it sit for 15h at 30°C. The solution turned very dark.
I heated the solution to 60-70°C to evaporate the remaining acetone.
I've just put 3ml of the chlorphorone solution in a test tube and them I've added 5ml 35% H2O2. Some "fluffy" cristalls precipated.
I put in the column and I let it stand for 5min.
When I've turned back, the solution boils, and in the same second, I've heard a loud pop (detonation). The test tube chrushed.
My ears are ringing now ;).

j-scan
December 28th, 2004, 02:47 PM
From your description you forgot to add HCl to get the reaction going again. Then you add your H202 at 30-35% concentration. Do not add too much H202 or you will not get the DPPP forming. You'll get fluffy TCAP as the heat increases rapidly to near boil over. Try and add a little H202 at a time---- you'll see what I mean. The solution will go bright orange and this is the DPPP precipiate forming. You should get a fairly decent yield*

DPPP is bright yellow-orange and smells nothing like AP when burned-It has a very weak smell--- I guess the closest think to it would be nitrocellulose. It will detonate with shear power if the material warms up past 200C.

nuclearattack
December 29th, 2004, 11:07 AM
To Rsert:
so the reaction works, the only thing to take in big consideration is to cool down the phorone and H2O2 or it will ignite.
I bought the chemicals next week i'll try with the synth. :)

The_Rsert
December 29th, 2004, 11:59 AM
I've made a batch DPPP.
I mixed 150-200ml acetone with 200ml 37% hydrochloric acid in a round 500ml flask and attach a condenser (Liebig cooler).
I put the flask in 90°C hot water and put everything on a radiator. After 20min the solution becomes yellow. I hold temperature between 25°C and 40°C for 15 hours. I removed the condenser. Evaporate the remaining acetone bring the solution to boil at 60°C for a few minutes). I let everything sood for 12 hours again at room temperature. The solution was near black coloured. I cooled the solution to -10°C in a ice bath and added 50ml 30% hydrogen peroxide. I waited 10min. The solution turned into two layers. One was (not completely) clear, the other (lower) layer was near black an contains black cristalls (a phorone). I poured off the clear solution into another container. I added slowly 250ml 30% hydrogen peroxide to the lower layer. I don't let the temperature rise over 5°C. When the addition was finished, I thinned it with the clear solution.
After a few hours (I was on edge, so I left it only for one hour) I filtered it. Then I washed the DPPP with sodium carbonate solution.

The yield looks promising. :) But it's not dry now. It's also not weighted yet.
And I think that it's possible to improve the yield. :)

You can see some pics here: http://members.fortunecity.de/potatoguns/DPPPSyn.html

j-scan
December 29th, 2004, 08:05 PM
YEEEHAWW!
This is what I got when I made my first successful batch of DPPP. Same colour.

The_Rsert
December 29th, 2004, 09:29 PM
I don't no why exactly but the "Edit" function does not work.
So I have to post here my news:

In the filtrate of the DPPP (was clear after filtering), which I've left for 9 hours, much more DPPP is precipated now. :)
So the yield grows up and up and up! :)

And I've just uploaded also the German synthesis instructions: http://members.fortunecity.de/potatoguns/DPPPSyn.html

Next day, I will write a working English synthesis Instruction.
:) !

kingspaz
December 29th, 2004, 09:35 PM
Well done :)

It would be useful once the DPPP has dried if you could give some explosive properties data. Possibly a comparison with AP? This is more good news.

The_Rsert
December 30th, 2004, 09:52 AM
I'm just uploading a video which schows you the different bettween DPPP and the double amount AP.
DPPP is many times better than AP!
You can download the video here when the upload it finished (I have only a old 33kb modem) there:
http://members.fortunecity.de/potatoguns/DPPPSyn.html

knowledgehungry
December 30th, 2004, 11:21 AM
Is the AP double by volume or weight?

The_Rsert
December 30th, 2004, 11:49 AM
By Volume. But AP has a smilar dumping volume to DPPP.
PS: DPPP will make cracks in nearly every ammount.

I've just co-recristallized/co-precipated some AP with some DPPP. The prdoduct is white.

knowledgehungry
December 30th, 2004, 11:59 AM
Next time you do tests could you do it by weight please? This is more accurate than volume for determining relative power of an explosive. Your doing great though, don't take that as criticism, so far you've done some real good and useful work.

The_Rsert
December 30th, 2004, 12:27 PM
No, my weighing machine can't weigh so little ammounts.
The weighing machine needs a minimum of 0.5g and has a annulment of 0.1g.

Mr.ANFO
December 31st, 2004, 02:59 AM
I just tried The_Rsert's DPPP production method and I have to say I have never yeilded as much DPPP in one sitting. From a 250ml container I got about 110-100g of DPPP. I hink once it drys though It may be only 70-80g ? Of course then I have to purify this further.
My dry DPPP is brilliant sulphur yellow-green how about yours R_sert? Can you please tell me your material looks like?

The_Rsert
December 31st, 2004, 10:08 AM
I've made converted the synthesis instructions to the PDF formate.

The_Rsert
December 31st, 2004, 08:23 PM
Mr.ANFO
Yes, my looks sulfur-like-green, too.

I've just made a test with less than 30g DPPP charge (in a paper beaker). The target was a butane tank (exactly 15cm away).
See the picture! I've also made a video, which I have to upload next day. Or I will upload only the sound...(size... :( )
And I've also filled a rocket (reaches a high of 100m) with exactly 2.5g DPPP. This was one of the loudest rockets, I've ever heard! (I will also upload a video or the sound!)

And I've made also a 1.5kg ANNM detonation. (no sound, no video, just a crater :) ) and some FAE tests (This videos I#ve uploaded already to http://www.roguesci.org/theforum/showthread.php?p=68572#post68572)

Tommrow I will make some more DPPP.


Ohh! I love silvester! :D

Mr.ANFO
December 31st, 2004, 08:46 PM
aha! DPPP is indeed yellow-green. (Sulphur yellow) Ok.
For an experiment I have uploaded on scimadness.org videos compairing small amounts of DPPP vs TCAP.. Also please go see my webshots account as I have new pics there http://community.webshots.com/user/matsumoto_hideki

Notice the yellow crystals in the jar in the last photo? almost the entire glass was full of them 250ml of liquid and 180-190ml of DPPP. Ouch. Just weighed the DPPP, still has not fully dried yet but it looks like a good 110-125g yeild... WOW
NEXt project for me will be making DPPP detchord ... .. next thing .. could you please give me access to your videos and pics of your DPPP crystals. thanx.

The_Rsert
January 1st, 2005, 06:55 PM
My DPPP looks very smilar to your's!

I've co-precipated DPPP with AP (1:2). The product is completely white, and it has no good visible differents to normal AP. So the colour is not a great indicator!

With the videos..., I've still some problems! My encoding program (Dr.DivX) is on strike with my normal video-camera (can't make pictures). The aground of the problem is my MP3-codec, I think.
I can only make videos without sound or sound without videos :(

The videos and pictures, I've uploaded before are from another (borrowed) camera (can make pictures). :(

Mr.ANFO
January 2nd, 2005, 03:51 AM
Here are pictures of a .223 remington mag cartrige test against steel car sheeting 2.5mm thick.
Holy shit... I just did a velocity test and look at this pic

Everyone ... drop your shit and look at this picture of my .223 shell velocity test against thick steel.

Both mini shaped charges were full of AP and or DPPP..
You can clearly see which subtance has more power.

1# AP charge with exactly the same # of grains as DPPP
detonation was strong enough only to nipple the primer and propell it and the base of the shell into the metal. primer was still in the bottom on the caseing which was retrieved later.


2# DPPP charge was strong enough to punch a BIG crater in the steel and propell the primer almost completely through the target. BIG blast marks are visible in the target surface indicating a MUCH higher velocity and energy signiture. I have pictures of the recovered metal fragments from the AP, whereas there was nothing left of the DPPP casing. The primer in the DPPP charge was atomized as well, but only the very bottom case rim although mageled was left! YES !!! THIS PROVES THE PATENT'S CLAIM!!!

Child-of-Bodom
January 2nd, 2005, 10:36 AM
The R_sert, for how long did you reflux the acetone and HCL?

The_Rsert
January 2nd, 2005, 11:02 AM
To Child-of-Bodom:
First for 15min at about 70°C (to start the reaktion) and than for about 15 hours at about 30°C.

I've just made a new DPPP detonation. The destruction of 10g DPPP looks like the destruction of 50g APAN! This suff is defenitly times more powerful than normal AP. The synthesis is very remunerative (I hope, this is the right word ;) ).

And it's less sensitiv piezo-sparks than AP. (pure DPPP does not iginite when it's hit by a electric-piezo-spark). This schould be a better indicator for the purity as the colour.

Mr.ANFO
January 2nd, 2005, 12:10 PM
Gee, good news R_Sert I couldn't beleive it myself about just how much power this stuff has, I as I was told by some people on Science madness I was full of shit and that I was using picric acid or something like RDX/PETN to do the damage I showed. I was nearly able to punch a hole in thick steel flooring (2.5mm) (I thought it was 4mm) thick with just about 1g of compressed DPPP wereas the compressed AP just barely scratched the surface. Another thing to note was that the brass casing bits actually punctured the steel in the DPPP test. This stuff has got to be detonating well beyond 6000m/s per gram (at least 9km/sec in my estimate) WOW looks like the patent was OTL after all.

Rosco Bodine
January 2nd, 2005, 04:36 PM
Gee, good news R_Sert I couldn't beleive it myself about just how much power this stuff has, I as I was told by some people on Science madness I was full of shit and that I was using picric acid or something like RDX/PETN to do the damage I showed. You misunderstood what was said there , because I agreed the DPPP witness plate starburst evidenced higher brisance than AP , because the impact welding of brass fragments into steel is typical of brisant explosives like picric acid or better , and not typical for AP . I was nearly able to punch a hole in thick steel flooring (2.5mm) (I thought it was 4mm) thick with just about 1g of compressed DPPP wereas the compressed AP just barely scratched the surface. Another thing to note was that the brass casing bits actually punctured the steel in the DPPP test. This stuff has got to be detonating well beyond 6000m/s per gram (at least 9km/sec in my estimate) WOW looks like the patent was OTL after all.The actual velocity is going to depend upon the column diameter and length , strength and rigidity of the confinement , and the manner of initiation . Very likely the peak velocity cannot be reached with a 1 gram charge , and also very likely there is a minimum critical mass where brisance
sufficient for use as an initiator is efficiently achieved . If a half gram is below that threshold , then a 2 gram charge could do three or four times the damage of a 1 gram charge ...if that makes sense . But that sort of math does not follow for much larger charges only for detonator sized amounts in the case of a material such as DPPP . The effect of increased charge weights is disproportionately increased after a certain transition point , which is a sort of "critical mass" for making the leap to high order detonation . Below and in the near vicinity of that
quantity , the stuff is "just playing around" in terms of what double that amount will do under the same conditions .

Mr.ANFO
January 3rd, 2005, 01:13 AM
Agreed, Rosco and by now you must have heard about today's test involving approx 30grains ~1.93g of DPPP & TCAP under ~2kg compression in a .223 shell? Were you able to download Pyroz's .pdf file? My ears are still ringing after that test...
I am going to give Science madness a rest for a while as I get too excited/ passionate and makes me go crazy. crazy + explosives = danger :)
This will be my domain and Pyroz my host will have his own space on Science madness from now on for a bit.

mr.pyro
January 3rd, 2005, 03:21 AM
I just tried the written synthesis by Rsert. The oily substace appeared after heating for 2 hours at 50 C and then heating for 15 h at 30 C. I cooled it to -10 C and Added 50Ml H2O2. IT was cooled back down to -10 C but no black crystals came out, because there was already a heavy yellow precipate. I waited for about 1/2 hr to see if any balck crystals would precipitate out, none did, so I added 200 ml more H2O2 and the precipitate was similar looking to Rserts pictures.

Edit

I just filtered what ever precipitated out and after neutralization, can not be more then 10g of DPPP. This seems like a shitty yeild from more then 400 Ml of Reagents. I think that the initial adding of 50 mL H2O2 might have been to much to fast, and instead of causing the seperation of layers, caused the DPPP to precipitate.

Mr.ANFO
January 3rd, 2005, 05:12 AM
really. If the solution is fairly pure and uniformily heated you will not be able to get any "black crystals" as these "crystals" are polymerized Phorone and Phorone HCl and are relativly inert. If you get these it usually means you have overheated the acetone and HCl mix.
Hold your black liquid to the light, if no light passes through it you are ok, if you see a red colouration at the bottom you have either leftover unreacted acetone or HCl and need to add more acetone or HCl accordingly.
----TIP****It may be nessesary to add an additional 5ml of HCl if the pH is too low inorder to get the DPPP to form properly.
If you had left your DPPP to form in a freezer and VERY slowly added you H2O2 over the course of several hrs say 4-6hrs between the first peroxide addition and the remainer peroxide you would have had a MASSIVE yeild! I had 250ml of Phorone HCl and yeilded just shy of 100g.
I am just warning you that DPPP is incredibly powerful so 2g is roughly equivalent to the same amount of PETN. Check out Science madness forums and download the test.pdf on DPPP as it will show you just what kind of power this stuff has.

My synth: I added 5ml HCl chilled the entire mix to about -25 to -30c then added 38ml H2O2 and gave it a good stir. I then left it to sit for 5hrs to form the seed crystals. 5hrs later the Solution was HOT orange colour, I then added all my remiander H2O2 slowly taking 5-10mins and stiring while I was doing this to observe any heating between applications, I then left the entire solution to settle for another few hrs. By this time the solution was neon yellow, "this is pure DPPP colouration" and then filter and let it warm up and nutralize all the acid.

nuclearattack
January 3rd, 2005, 05:36 AM
Wow! The plate test is amazing! :eek: :eek:
This stuff is incredible not only for detonators but also for APAN (DPPPAN) or DPPP putty. ;) :D
It should be interesting making a power comparison test beetween Tetrameric AP and DPPP.

To Mr.ANFO:
why don't you attach the test.pdf file on your post? ;)

The_Rsert
January 3rd, 2005, 02:12 PM
I just tried the written synthesis by Rsert. The oily substace appeared after heating for 2 hours at 50 C and then heating for 15 h at 30 C. I cooled it to -10 C and Added 50Ml H2O2. IT was cooled back down to -10 C but no black crystals came out, because there was already a heavy yellow precipate. I waited for about 1/2 hr to see if any balck crystals would precipitate out, none did, so I added 200 ml more H2O2 and the precipitate was similar looking to Rserts pictures.

Edit

I just filtered what ever precipitated out and after neutralization, can not be more then 10g of DPPP. This seems like a shitty yeild from more then 400 Ml of Reagents. I think that the initial adding of 50 mL H2O2 might have been to much to fast, and instead of causing the seperation of layers, caused the DPPP to precipitate.

Yes, maybe. But I'm not sure about this :confused: . Add the H2O2 more slowly and stop when the phoron will begin to precipate.
Another reason is that maybe the phorone is semi-solouble in acetone/water, so evaporate the acetone better and maybe and add some ice.
Was your reaction between HCL and acetone under correct reflux?

Mr.ANFO
January 3rd, 2005, 02:42 PM
Ok here is the .pdf file. I was just reviewing all the properties listed on the patent
Properties: I have commented beside them..

a) insoluble in water (yes)
b) still explosive when heavily contaminated (yes)
c) detonation velocity approx. 9000m/s (indeed it has got to be)
d) low detonation temperature approx. 200°C (yup)
e) does not develop smoke upon detonation, does not smell, no solid residues. (YES)
f) ignition by fire, blasting cap or electric (yup)
g) does not decompose at long storage (we will see)
h) yield of manufacturing process approx. 90% (yes 70-80% is typical, but 90% is realistic as well)

My DPPP observed properties

g) Colour is BRIGHT yellow and looks white-yellow when moist/wet.
h) Needs a good jolt ( a hard strike) to set it off unlike most other proxides
i) Has a rather irritating camphor-like odor
j) Does not seem to react with metals to create metal peroxide salts.
k) Black soot and some brown residue apon deflagration as well as an odor.

Rosco Bodine
January 3rd, 2005, 03:18 PM
Agreed, Rosco and by now you must have heard about today's test involving approx 30grains ~1.93g of DPPP & TCAP under ~2kg compression in a .223 shell? Were you able to download Pyroz's .pdf file? My ears are still ringing after that test...Yes these tests seem pretty conclusive that DPPP is a more brisant explosive than AP . All of these experiments are interesting , as we gain some little perhaps useful detail towards a good understanding about DPPP and discover its secrets .
I am going to give Science madness a rest for a while as I get too excited/ passionate and makes me go crazy. crazy + explosives = danger :)
This will be my domain and Pyroz my host will have his own space on Science madness from now on for a bit.It is always a bit of a thrill when a plan comes together , just try to keep objective so that the subtleties of observation are not made complicated by any inaccuracies which cause a description of the
facts you "catch" from your experiments to become like the dockside telling of a "fish story" that is the temptation for every successful fisherman . That is expected as a tradition among fisherman , to see how big the lies can get in good humor so eveyone may laugh at the absurdity . All my fish stories are true of course , especially about the even bigger one that always got away ;) But science is by nature a sort of "dry" and trudging , meticulously accurate sort of endeavor . Be dull and objective until all the good data is proved and analyzed , then later be as excited as you like . We all get excited too when an experiment goes well , but have to keep a certain reserve to do good science and get all the details down straight , so we can "certify" the method and guarantee the "repeatability" of the results , even if just for ourselves to benefit the next time we do the same experiment .

Baquacil is a very storage stable product indeed . I just did an accurate density
measurement to determine the actual H2O2 content on a half full jug of Baquacil thathas been sitting at room temperature for 3 years . The fresh material was 27.5 % H2O2 by density measurement , and after 3 years storage the strength is 26.6% which is a reduction of just under 1% . That is excellent stability indeed for peroxide after 3 years at room temperature .

The_Rsert
January 3rd, 2005, 05:17 PM
I've just bought some .223 remington mag cartriges. I will make some tests with DPPP against AP, HMTD (yes, I know what I will do), tetrammincopper(II)-persulphate, lead styphnate, some co-precipated products (http://www.roguesci.org/theforum/showthread.php?t=4463), maybe RDX, maybe MHN, maybe CTMTNA and maybe PETN if possible.

mr.pyro
January 3rd, 2005, 09:37 PM
Was your reaction between HCL and acetone under correct reflux?

No, I left it uncovered. It vapored off probably about 1/4 of the total Acetone/HCL mix. It did form a thick oily substance that was described though.

I am retrying it, because I tested .1g of my total 5g precipate from the first batch, and confined with only Al foil made quite a bang, about the same as 1g of Flash in a tube. I have started the reaction, heating the Acetone/HCl at 50 C for 2 hours covered by Saran wrap, but with ice on top to condese the vapor. Little % of the solution was lost. It is now still on heat at 50C approaching the 2.5 hr mark, but is an opaque black but with a red tinge when viewed from the bottom. I will let it heat under these conditions until 3 hrs is reached. Then take it off heat, boil as 60C for a few minutes, per Rsert's sythesis, and then continue to heat uncoved at 20-30C overnight.

Mr.ANFO
January 4th, 2005, 03:58 AM
If one is making detcord, for the binder what would one need in theory? Or is DPPP fine enough to be used all on its own compressed in a clear 1cm dia vinyl tube?

The_Rsert
January 4th, 2005, 01:50 PM
You can powderise DPPP very easy very fine. Just put it in into a zip-plastic bag and kneat it with your fingers. You will get a very fine powder. Wear industrial gloves!

Edit: The DPPP must be 10000000% dry!

SweNMFan
January 4th, 2005, 02:41 PM
If one is making detcord, for the binder what would one need in theory? Or is DPPP fine enough to be used all on its own compressed in a clear 1cm dia vinyl tube?

PETN detcord doesn't have a binder, just loose PETN in the middle and my nations armys detcord have 10g/m..

If DPPP is as powerfull as reported you will not make a detcord with a 1cm tube, you will end up with something else, like something to cut holes in doors, small safes or the side of a armoured money transport..

Mr.ANFO
January 4th, 2005, 07:26 PM
Yes, indeed DPPP is as powerful as reported..
9000m/sec = ~31,000ft/sec 9Km/sec isn't fast enough for detcord??
you are shitting me about only 10g/m since that is too a weak a detcord & it wont do a dam thing. 110g/m detcord is used all the time for taking down trees and such. I think that is what you mean?

knowledgehungry
January 4th, 2005, 09:56 PM
What he is saying is that a 1 cm diameter detcord of an explosive as powerful as this is assumed to be would be overkill. He is saying that it is too thick for a detcord.

Mr.ANFO
January 5th, 2005, 01:04 AM
oohk... Sorry I ment .5cm dia 1cm cic tubing for wine making. That is more realistic?

SweNMFan
January 5th, 2005, 03:34 AM
you are shitting me about only 10g/m since that is too a weak a detcord & it wont do a dam thing. 110g/m detcord is used all the time for taking down trees and such. I think that is what you mean?

No standard issue swedish army detcord only have 10g/m . Why waste explosives on trees when we had 2 chainsaws issued..

As PETN have a VOD of ~8500m/s DPPP will probobly work too..

xyz
January 5th, 2005, 04:47 AM
Mr. ANFO, cutting down trees is more of a novelty use for detcord...

It's main use is to connect a series of seperate charges together, so that they can all be detonated simultaneously (give or take a few fractions of a second) from a single detonator.

Basically, it allows you to detonate multiple charges with a single detonator and fuse, something that would usually require multiple detonators and an electrical ignition system.

Of course, there are also heavier grades of detcord for demolition and "forestry work" :D

Mr.ANFO
January 5th, 2005, 01:06 PM
I do know about the main uses for detcord thanx, but I was looking at the BIG detcord that was used in the high explosives/cutting trees with detcord thread on this forum.
I thought primacord was what was used for connecting charges together?
I though PETN had a detvol of 9.3Km - 10.4Km/sec?

SweNMFan
January 5th, 2005, 01:26 PM
Primacord is a trademark , just a brand name for one company’s detcord

a single pure PETN crystal with the density of 1,77g/cm2 have a vod at 8500m/s .. PETN detcord usually lay around 7000m/s as there is air between the crystals.

Oh and I seen some DPPP references saying that the VOD is around 6600-6800m/s but I can't find it again now..

The_Rsert
January 5th, 2005, 04:01 PM
I thought, that (pressed) PETN has a maximum VOD of 8700m/s.
Detcords a better for make round holes in doors as for cutting trees.
:).
Maybe I will make some MEKP to mix it with DPPP. This schould give a very powerful explosive!

Mr.ANFO
January 5th, 2005, 10:04 PM
oh, now I am confused Detcord and Primacord are the same thing? then what's the stuff called that is used for taking down 20inch dia trees that is 1cm dia? detcord?
Well as far as DPPP's detvol the original german patent states 9km/sec clearly. As far as PETN I was almost certain that detonated above 9Km/sec.

BTW MEKP isn't something I want to make as it is soo incredibly mutagenic/immediatly toxic absorbing through the skin.

Microtek
January 6th, 2005, 05:56 AM
"Detcord" may once have been a trademark for a specific product, but these days it is usually simply referring to a length of hose filled with explosive. It comes in various sizes for different purposes but is usually used for detonating blasting charges simultaneously, such as in charges employing colliding shock waves.
Detcord is also sometimes called "detonating fuse" and a version known as mild detonating fuse exists which contains less than 0.1 g/m of PETN in a metal hose. This is usually used as a delay in warheads when very precisely timed detonations are required.

As for the detonation velocity of PETN and DPPP, well, DPPP is not known with any degree of certainty but PETN lies in the 8300-8500 range depending on confinement and charge dimensions ( although PETN isn't nearly as dependent on these factors as is RDX ).
As detonation velocity is so very dependent on density, I find it extremely unlikely that any explosive with a density of around 1.1 could possibly reach a VOD of 9000 m/s. There is only a handful of explosives that cross this line in the first place and they ALL have densities from 1.8 to 2.x.
I know that the patent claims VOD = 9000 m/s but many patents contain exaggerated claims, so I am not convinced of this VOD until someone actually measures it.

Please understand that explosives don't need an extremely high VOD to be very powerful; so claims like " A small amount of this explosive made a large hole in this target, so VOD must be at least 9000 m/s" are completely misleading ( regardless of whether the VOD actually IS at least 9000 m/s; its the logic that is flawed ), and tend to make knowledgeable members very sceptical of your other statements.

Rosco Bodine
January 6th, 2005, 05:03 PM
What is still needed is a detailed technical writeup for the synthesis of DPPP ,
having no ambiguities about measured amounts of materials , their purity and concentration , the conditions for their admixture including temps and order of addition ,
reaction times and method of stirring , heating , cooling , neutralizing , filtering , drying ,
and the weight and percentage yield based upon what precursor , as is the information
supplied by a usual description of an experimental synthesis . That is the sort of definitive information which allows for others to duplicate reported results , instead of having a
hundred questions about the details . So perhaps these people who report having made hundreds of grams of DPPP could make notes carefully as they perform the synthesis
and then share the detailed information . I have done some preliminary experiments and
the results from those experiments are indicating that the details are important for achieving any good yields of DPPP . I do not believe that the synthesis of DPPP has yet been adequately described so anyone who is having good success please share any of the
more detailed information you may offer , along with any refinements to the process which
you may have devised .

The_Rsert
January 6th, 2005, 06:26 PM
I remember, that one member of the Sciendemadness Forum evaporated the acetone to hot from the solution. The solution turned clear.

Now, my questions: Is it possible, that the oily liquid is only chloracetone (in my chemistry bokk it says that it has a low boling point and is near black and oily) and not dihydrogen chlorphorone is?

Is is it possible that the stuff we have made maybe chloracetone peroxide is and not DPPP?

Mr.ANFO
January 6th, 2005, 09:37 PM
If indeed we have made chloroactone peroxide then why is chlorine given off when H2O2 is added?
As far as I know Chloroactone has a boiling point around room temp and if you had made it, you woulden't be around to post here on the form as it is a blister agent and very deadly!
Chloroacetone is also a translucent deep yellow, not thick and black red.

Rosco Bodine
January 7th, 2005, 01:50 AM
The DPPP which I just successfully made has a pale yellow tan color ,
and a fine crystalline texture almost like pumice but a bit more coarse .
The freshly precipitated material is fine enough that it cakes when wet
but coarse enough that it filters easily and rinses well . It gradually floats
to the top of the peroxidation mixture , from trapped small bubbles of oxygen
from the hydrogen peroxide , forming a floating raft of crystals which can be skimmed
from the surface using a spoon and transferred to a filter for rinsing .
In its physical texture it resembles fine crystalline HMTD more than the
coarser crystals of AP . It is sensitive to alkaline pH , decomposed by
ammonium hydroxide so it is preferable to skim it from the acidified peroxidation
mixture and rinse it with plain water , then neutralize any residual acidity under
only mildly alkaline conditions , perhaps using 2% baking soda , I'm not sure for
not having tried that yet . The odor is very aromatic , something similar but
different from eucalytpus oil , or sassafras , spicier than menthol or wintergreen ,
a "caphorous aromatic essence" a very distinctive aromatic odor , difficult to characterize because it is a distinctive fragrance of its own , like trying to say what turpentine smells "like" ? ( well it smells "like turpentine" :D ) and the same for DPPP , it smells like DPPP , a very distinctive odor . I believe it is physiologically active . Good ventilation
would be wise precaution , and I wouldn't recommend getting a deep whiff of the stuff
to confirm what it smells like . Perhaps the feshly made material is perfumed by traces of
byproducts and the scent will diminish upon drying , but I'm telling you to my nose the stuff
absolutely reeks . A dog could smell a teaspoon of DPPP a mile away . So this could be
the deficiency that would make this material undesirable , the odor and probable toxicity
are not things which commend DPPP . The properties of DPPP otherwise are worth investigating , and bindered compositions , or mixtures might remedy those deficiencies .

Mr.ANFO
January 7th, 2005, 03:16 AM
YEs Rosco then you have exactly what I have, as Mine has a sort of a camphorish odor to it... sort of Pineish sort of eucalyptusy......? can't describe it really. It is also highly irritating to the eyes and nose.. careful. I really do not think it is toxic however as most phorone relatives are quite safe. Phorone is listed only as an irritant. However don't go by that.. It does burn the skin like most organic peroxides. My fingers go burn after touching it (typical peroxide burn), i know not really that safe.. however I am reffered to as the human ginea pig.

I really think that the camphor odor is in fact the actual DPPP.. the stuff we wanted to synthesize. I will take a small sample next week to university.

knowledgehungry
January 7th, 2005, 08:39 AM
Rosco, you ask for a detailed write up of the synth but you have succesfully made it yourself? Maybe you would like to do the write up? I'm sure we would all appreciate that very much, considering your experience. I am going to work with DPPP as soon as I get some time, but for me that may mean a month from now.

Rosco Bodine
January 7th, 2005, 09:39 AM
Okay , here's what I know or believe is likely true at this point about DPPP .

Many more experiments will be required before some ideas can be regarded
as conclusive findings about the synthesis of DPPP , however I am willing to
go out on a limb early with a few ideas so that others may do their own tests
to see if these ideas square with their own results .

First of all the molar ratio of HCl to acetone is important , as is the time and
temperature they are reacted before the peroxidation . Maintaining the proportion
of acetone and HCl requires a sealed bottle for the digestion of the mixture .
Otherwise the acetone evaporates and results in a variable mixture . Not
much pressure is developed and the reaction sufficiently rapid having a bath
temperature of about 75 C. If a metal threaded lid is used , then a heavy
ziplock "freezer baggie" placed flat over the container under the metal cap
before it is secured will prevent the cap liner from being destroyed by the
fumes and contaminating the reaction mixture when it detaches . A bottle
having a plastic and polyseal cap is best for the sealed bottle digestion .
It is the soluble or finely dispersed portion of that digested acetone HCl mixture
which will be reactive with the peroxide . The resins or oils which may precipitate
represent a loss of precursor and should be filtered before peroxidation using a double
thicknes of coffee filter wetted with water before filtration . There isn't much
of anything to be gained by excessive temperatures or extended hours of heating
the acetone and HCl to the point it becomes so dark as to contain suspended
or separated resinous precipitate . Such "black oily" material will not be converted
to DPPP , but will only precipitate as clumps of sticky insoluble goo contaminating
the more and more aqueous peroxidation mixture . This is why filtering before
peroxidation is a good strategy for removing the bulk of such suspended material.
Molar ratio of HCl to acetone should be 2 to 3 , with only very slight excess of theory
for the HCl on the order of 3 % seems in the ballpark . Using more HCl or heating
the mix too high or too long causes resinous insoluble products to precipitate and this
should be avoided to the extent possible . Exact optimums for ratio and times have not been yet determined so this can be an area for close measurement and comparison of
results .

The greatest exotherm during the peroxidation occurs during the addition of the first
10 to 15% of the total peroxide to be added . This initial peroxidation should be done
with efficient stirring and slow , even dropwise addition of the peroxide . I have used no
cooling during this initial addition , or only a shallow plain water bath , and allow the
stirred mixture to heat up from the exotherm to about 65 C . The addition of peroxide
is stopped and then ice is added to the bath to cool down the mixture to 10 C , the stirring
being continued the entire time , and then addition of the peroxide resumed more rapidly
at such a rate as to maintain about 15 C to the end of the addition . The stirring is continued for thirty minutes after the end of the addition and stopped . The crystals
will form a floating raft , from adherent bubbles of oxygen which make them buoyant and
may be skimmed from the surface using a plastic spoon and transferred to the filter .
The crystals should be rinsed on the filter , and neutralized with only dilute alkali . Strong
ammonia will decompose the DPPP . The material is very aromatic and the vapor is irritating
and perhaps intoxicating , and should not be considered harmless until more is known .

An experiment is in progress , and this was posted earlier over at Mad Science .
Honestly , to my old eyes , this forum is damn near unreadable in the new
BombShock color scheme . I get a headache trying to read this reverse contrast
tiny text , and can't understand why anyone in their right mind would prefer this
illegible nonsense or pretend they do to please the management here . Sorry
but I call it like I see it and take my knocks if I must . Anyway , the information
here is pasted from my post at the other forum where the topic really started .

I have a new batch of acetone and HCl reacting , in which I made a far less excess acidity than the earlier batch that I think I scorched with too much acid .
I remembered when I was observing the first sealed bottle experiment that I had the idea that this reaction is pH sensitive , so I tried to measure very carefully the acetone and HCl to achieve
just a 3% excess of theory of HCl to acetone . The results are distinctly superior in terms of color development and the purity of the color is striking at
3 1/2 hours . The color is that of "ruby glass" pure red , brilliant red , not any "tea color" to this batch . I have a good feeling about this ratio just based on
the clarity and depth of color . If nothing else it is pretty . What I used was exactly
112 ml acetone and exactly 105 ml HCl 31.45% , mixed and allowed to stand in a sealed bottle for 1 1/2 hours without supplemental heating , and then heated for 2 hours still in the sealed bottle , in a 75 C water bath . I have removed it from the bath , and am allowing it to cool and stand overnight .

I must say that quite different reaction rates and color developments are being observed with small changes in the acetone to HCl proportions , so obviously
some exactness is needed about these
measurements and reaction times and temperatures . And then when to proceed with the peroxidation and at what rate and temperature and other conditions are important also . This synthesis is not one which is likely to work across a wide range of conditions ,
as is the synthesis of regular AP . So please , those of you who are having success make careful and detailed notes of what you are doing and what you are getting out the other end as yields .

Mr.ANFO
January 7th, 2005, 11:24 AM
I reveresed your amounts Rosco leaving a slight excess acid to actone made my yeilds jump up like crazy! My last batch was 249ml HCl 35% to 246ml Acetone. A little bit of excess acid seems to make the reaction run a little quicker, as well no extra acid is needed during peroxidation had the amounts been reversed.
Keep on producing there Rosco and save all your DPPP, nutralize it, dry it out and stick it into a double plastic bag and store it in a cool dry place.