Holy grail organic peroxide!

[The_Rsert]

Don't forget to evaporate/destill the remaining unreacted acetone!
But do'nt heat over 65°C, mybe this will let evaporate the phorones also. Acetone boils already at 57°C.

[Mr.ANFO]

ook, you being sarcastic? Sounds like you are making fun of J-scan??? He never got the yeilds I did anyway even though he is a tenant in the same building.. I think he is jelous?
After letting the 2 chems react fully then open the jar up and let it concentrate at room temp.
after several days at room temp put the jar into an ice block and freeze the entire container.

[Rosco Bodine]

Yes that is a good point . At the time when the sealed bottle has developed
that deep red "ruby glass" appearance and the bottle is removed from the bath ,
it would probably do fine to at least uncap the bottle and let the excess acetone
volatilize from the hot liquid . It would probably be better to pour it out in a shallow
layer in a glass tray and just allow it to breathe for awhile perhaps an hour , and then
reurn it to a sealed container and refrigerate it until it is peroxidized . The entire
process should be timed so that the peroxidation can be carried out without delay
once the precursor is ready . From what I have observed , When the precursor has fully
digested , and then likely gone a little past its point where it is optimum , a surface sheen
of an irridescent looking "oily slick" will appear on the surface of the dark red liquid .
If you observe the reflection of a light upon the surface , you can see the effect of "oil on water" with its rainbow colorations , the same effect as when a drop of oil falls onto the surface of still water in the sunshine . At this point the reaction for the precursor is (at least in my estimation) a fully completed reaction , and likely has even proceeded a bit
past the peak concentration for the precursor . Only charting the results of carefully
detailed experiments can tell the story on these visual markers of the reaction progress
and exctly how they translate to differences in yield and purity of product . These refinements will come with further reported experiments . But from my own experiments
so far I believe to a fair certainty it is the "dark red barely clear syrup" stage that is your
purest precursor , and the "black oil" is the staining of the precursor by a resinous impurity
which needs to be filtered before peroxidation , if the mixture was allowed to digest to that point .

[Mr.ANFO]

Yes another point is to look carfully at the black liquid and swirl it in your jar, if the black liquid in the jar stains the sides red then you are ready to peroxidize. The resinous material is that xylitol I was reffering to on Science madness.

[The_Rsert]

I#ve co-precipated DPPP with AP (60:40). The product is completely white. The crystals have no visible differents to pure AP. It smells only completely different to AP and DPPP. It is visible times more powerful than AP. The wonder: It let solid residuums.

[Rosco Bodine]

Has anybody else tried letting the mixture warm on its own exotherm
during the introduction of the first 10-15% of the total peroxide ?

I am not sure that this really accomplishes a damn thing :D ,
it just happens to be the way I chose to do it in order to help
evaporate off any residual acetone from the hot stirred mixture
getting a lot of air circulation across its surface , while nudging the
mixture towards a lower viscosity and getting the chlorination started
while dumping the initial heating to get past that thermal spike , and
into smoother reaction territory . It just seemed a good strategy for
working with the process characteristics , to solve several problems
and have less chance of overheating later , while getting rid of any AP , and
smoothing the heat curve for the remaining reaction . Made sense
at the time to try it that way so that's the way I did it and it seemed to
work fine .

[Mr.ANFO]

Hey R_Sert Have a good look at that coprecipitated AP and you will find yellow crystals! I have copreciped AP AND DPPP and the results are ONLy visible under high magnification ie) microscope. Hopefully when the snow clears tommorow I will got test some devices utilizing DPPP in amounts greater than 80g ... I want some fun :) and take movies and pics!

[Mumble]

I'd like to bring up a point of interest with everybody, and see what they think.

This so called Phorone Dihydrochloride formed by the reaction of acetone and HCl, I believe to be in realitly Mesitylene(sym-methylbenzene). From seeing some of the picture synthesises of this compound, it follows and exact and I do mean EXACT color change as mesitylene. As in if I were to make a picture synthesis of mesitylene, I could take the pictures of the "DPPP" synthesis and use them they are so exact. Mesitylene forms this resinous tarlike material spoken of recently. I have proof of this as my mesitylene preparation has this resinous tarry material right now after sitting out too long.

Mesitylene is commonly prepared by the action of H2SO4 on Acetone. It is referenced as a dehydrating agent, but I wonder if it just need a strong acid to go to mesitylene. If so, this would make the option I propose very plausible.

I tried adding 30% H2O2 to my mesitylene preparation, with mixed success. I got the orange solution previously obtained by others with the DPPP solution. I have yet to be back to check, but it looked as if it had turned a little more yellow and there were possibly some crystals forming. I have heard of a peroxide from mesitylene that is more powerful than AP so this very well could be the recent syntheses instead of DPPP.

I propose two things:
Someone who has made mesitylene/knows it's smell prepare the Acetone/HCl mix. I am out of acetone otherwise I would have done it myself. It takes a bit to get pure acetone around here, expecially with how bad the roads have been.

Someone who has successfully synthesised "DPPP" try the same proceedure, but with H2SO4 instead of HCl. Ideally it would be a third party of sorts as in someone not Mr. ANFO, whom I'm not discriminating against, I just feel he would not take the same care as he wants this to be a new discovery atributed to him. He is welcome to try, but I would still like results from another person.

[Jome skanish]

Wouldn't mesitylene form chloro-mesitylenes in contact with free chlorine?

My knowledge in organic chemistry is not very great but I belive CH3-groups on aromatic molecules is ring activiating, making it easier to add things to the other "aromatic carbons", like in nitrophenol and nitrotoulenes. However the chlorines might be replaced by the peroxi-bonds like in the supposed formation of DPPP from phorone pentachloride.

How would this mesitylene peroxide molecule look like? All I can think up is two mesitylenes on top of each other with three peroxiether bonds between them.

There's got to be a way to distinguish between the two. Anyone with a mass spectrometer or something in that direction?

[Mr.ANFO]

Well ,I you have a good look and organic syntheses web site you will find that Mesitylene doesn't come easily from HCl but is able to be formed by H2SO4 instead.

"Someone who has successfully synthesised "DPPP" try the same proceedure, but with H2SO4 instead of HCl. Ideally it would be a third party of sorts as in someone not Mr. ANFO, whom I'm not discriminating against, I just feel he would not take the same care as he wants this to be a new discovery atributed to him"

excuse me? I have no ego, but maybe you do Mumble. Have you tried making DPPP yet? have you tested it ? Do you DPPP's properties? Cause all of us a science madness have and it works.

[Rosco Bodine]

Not only does it work , but we are very close to having
an optimized synthesis for DPPP . All of the variables
are known and it is just a few details and charting of yields
which remains to be done .

[Mr.ANFO]

I agree. Soo, next question is getting some AP and comparing it under a very high power microscope to "DPPP" and seeing the differences in crystal structure.
next thing the so called gas bubbles that supposidly come from DPPP also come from AP as well. I was just trying the oil submerging test that was done by my roomate. I still don't know why however ammonia/ Ammonium hydroxide attacks it. hmm
Like I said I look up on Mesitylene and came across a reference for HCl reacting with acetone to form Phorone derivatives, were as H2SO4 "dehydrates" Acetone forming pure phorone and Mesitylene. Must be something to do with H2SO4 being a stronger acid?

[Rosco Bodine]

Mesitylene is unlikely to form under mild conditions in an aqueous reaction .

Maybe with concentrated sulfuric and high temperatures you could get that
"cracking" of a long chain acetone polymer precursor , and get ring formation
for mesitylene formation . And maybe some mesityl oxide formation under mild
conditions would be more likely using different acids and conditions . But I just
don't see it as likely for the acetone and HCl mixture that is being used for the
synthesis of DPPP . Those reactions seem to be pretty much consistent with
the reaction diagram in the DPPP patent , with only minor disagreement on a
couple of points which are not significant , where pathway and sequence are
perhaps debatable , but the general reaction is generally correct .

[The_Duke]

Rosco, you said all the variables are known right? So I'm O so curious to know, does it really have a VoD of 9000m/s :) Or is the patent somewhat misleading?

[Rosco Bodine]

The variables I was talking about were with regards to the chemistry .

I haven't fired any of my own sample yet to observe directly and
compare with what I know other high velocity explosives will do ,
but I will get around to such tests later . From what I have seen of
pictures of the tests by others , I'd say that figure is probably high .
But I would doubt that figure because of just looking at the structure
and trying to visualize how such a peroxide would outperform certain
other things like tetrazoles is just a reach on its face so far as I'm concerned .

The way I have looked at it is the figure of "9" is probably a transcription error ,
inverted dyslexia.....typist sees a "6" while typing a "9" you know the story :D
But we can dream can't we . Anyway there are anomalies possible and maybe
this is one of them . So what if it turns out to be only 7600 m/sec ? That will
still make it the baddest peroxide in town .

[Mr.ANFO]

Well I see your point Rosco but, I showed the pictures of AP vs DPPP to a fellow "Doctorate of Physic" at University and his comment was: If Triactone peroxide detonates "3500-4000m/sec" and leaves small indent & smallish metal residue as in this picture we can relate this to the fine metal dust and a gaping dent which is rougly 5.5x the size as TCAP created by this Diphorone Pentaperoxide I would say this patent you talk about is probably dead on "within a few m/sec" if not it may have underestimated the power of this substance as the damage depicted on the picture is astounding for a small shell of that size ".223cal"
Ie) IS it possible we may be looking at a higher velocity than 9Km/sec? maybe? I will go talk with another physicist on Monday, and maybe have more info. The differences in fragment sizes and microshrapnel brass penetrating 2.5mm of hardened steel, all point to an EXTREMLY HIGH velocity.

[The_Rsert]

Yesterday, I made some more pics to my synth.
This time I've got a many times lower yield.
Because I let the HCL/acetone mix since silvester stand on a heatener.
A little ammount of a thicky (like glue) and water insolouble oil was build on the top of the mix. What to hell was that?

[The_Duke]

R_sert
I tried this procedure twice now and more testing is needed but I am convinced that the top layer that forms is waste material and nothing but the desired precursor decomposing into…? Do you notice the oil slick on top of the acetone/HCl solution after excessive heating for an extended period of time? that oil layer upon peroxidation seems to form into the insoluble wax like (glue like) substance in the reaction vessel. I am almost positive that the top layer seems to form from excessive heat, and the decomposition of the desired precursors.


My first attempt I heated the acetone and HCl at 60 C and completely allowed the two to completely react until no more visible changes occurred (About 4 days), both chemical and physical changes were noted (smell, color and viscosity). The yield from this attempt was about 50-60% of what the patent suggested I should have.

I then started another batch and heated at the same temp for a fraction of the time of the first batch until the oily slick started to condensate on top of the mother liqueur, I then removed from heat, cooled and added two parts 30%H2O2 to the second batch. My total yield increased by almost half and there was almost none of the insoluble wax like waste product either, only several small “drop like beads”. I am positive that the top layer that forms is nothing but waste material resulting from the decomposing of the desired precursor resulting in loss of our total yield. Of course as of now this is only theory but it seems very likely to me that this is what is happening and if that is exactly what is happening then we could very easily tell when the solution has reached its end point and is ready for the peroxidation step by the color and evolution of the precursors. Any one else care to back me up? :confused:

[Rosco Bodine]

Phorone Dihydrochloride Precursor :

The sealed bottle reaction has definite advantages . If a bottle or jar
has a metal lid it will not withstand the corrosive effects of direct contact
with vapors of acetone and HCl , and its gasket liner will likely detach
and contaminate the reaction . This can be overcome by laying flat across
the opening of the glass jar , one of the heavier thickness ziplock freezer bags
and then pressing the metal cap downward to engage the threads and tightening
securely . The polyethylene sheets of the bag will act as a gasket and prevent
the inner surface of the metal lid from being attacked by the vapors .
A completely polyethylene or polypropylene cap with compatable liner
or friction seal , or most desirable a teflon seal is actually the best option .
The precursor can be prepared in any shape of bottle , even a wine bottle
and transferred to another vessel of more convenient shape and volume
for performing the peroxidation .

From several slightly different experiments it has been found
the preparation of the acetone and HCl reaction mixture is the
secret for producing good yields of DPPP . The molar ratio of
HCl to acetone must be 2 to 3 , with the HCl limited to only a
very small excess of theory on the order of 2 to 3 % . The volumes
of acetone and HCl must be measured very precisely for the reaction
to produce the precursor in a concentrated and pure form . The
* exact volumes * for HCl 31.45% and acetone to accomplish a
correct mixture are 104 ml of HCl and 112 ml acetone . For convenience
in meaurement using a 100 ml graduated cylinder , for 100 ml acetone ,
use exactly 93 ml HCl 31.45% to accomplish the same ratio .
Small departures from these amounts will produce disproportionately
larger changes in the quality of the precursor produced by the reaction
which appears to be sensitive to pH . If you are using a different
concentration of HCl , then you need to calculate the amount of
your HCl to achieve the same molar ratio as above . The mixture
should be done in a glass jar or bottle and sealed immediately to
prevent the loss of acetone and thereby preserve the reaction mixture
proportions unchanged during the time of reaction , which involves
gentle heating of the mixture . The first heating which occurs is the
exotherm of the self-reaction , immediately upon mixing the acetone
and HCl . This self-reaction is allowed to continue for 1 and 1/2 hours
and then supplemental heating for 2 to 2 and 1/2 additional hours is
performed by placing the still sealed bottle into a 75 C water bath ,
to complete the reaction which forms an intensely red tinted but transparent
solution of phorone dihydrochloride . The beam of a flashlight shined
through the deep red solution gives the appearance of "ruby glass"
and if the solution is swirled so that a thin film of liquid sheets across
the inside walls of the bottle , the thin film appears bright yellow .
This color development is the marker for the endpoint of the reaction
producing the phorone dihydrochloride precursor . The supplemental
heating should be ended at this point and the sealed bottle removed
from the water bath and allowed to cool . A very slight oil slick may be
seen on the surface of the intensely red liquid if light is reflected from its
surface , and it will have the shimmering rainbow irridescent appearance
which is similar to the effect seen when a drop of oil strikes the surface
of still water in sunlight . The trace of oily material is insoluble higher
polymerization and precursor decomposition product which would increase
in amount with continued heating of the acetone HCl mixture , and the
oily surface precipitate therefore represents a loss of the desired precursor .

Higher acid to acetone ratios and higher reaction temperatures
and longer reaction times increase the amount of the oily precipitate ,
so these factors are to be avoided . The cooled reaction mixture
may be kept in good condition by refrigerating it until the peroxidation step
is performed later . The mixture in the sealed bottle does continue to react
after being removed from the heat , only at a much reduced rate , and the
further reaction nearly ceases under refrigeration . If the reaction has been
allowed to proceed beyond the desired point and becomes very dark from
precipitated material or has a distinct upper layer of oily material forming on
its surface , then it should be filtered through a double thickness of coffee filter
which has been pre-wetted with plain water before filtering . The filter will
trap most of any the oily precipitate and the solution can then be used for the
peroxidation without precipitation of the insoluble impurites which would
otherwise occur if they are not removed by filtration .

Peroxidation of Precursor to DPPP : Generally this has been done by first adding 2 or 3 ml
of fresh HCl to the cold precursor solution before proceeding with the peroxidation .
The greatest exotherm during peroxidation will occur during the addition of
the first 10 to 15% of the total peroxide to be added . The initial exotherm is quite
energetic and must be done dropwise , very slowly with swirling or stirring ,
drop by drop additions are imperative here . This initial peroxidation converts
the phorone dihydrochloride to pentachlorophorone , and the reaction is ten times
as exothermic as is the remainder of the peroxidation . So it cannot be too
much emphasized to go * slowly * with the first additions of peroxide in order to
control the thermal spike which everyone observes to occur at this point in the
reaction . If peroxide is carelessly dumped into the mixture at this point , a
full blown steam explosion has been reported to eject the contents of the mixture
from the reaction vessel . A salted ice bath is a good idea here , and keeping the
reaction below 10 C thoughout the addition of peroxide is good practice . The reaction
mixture is allowed to stand in the cold for at least 30 minutes to complete the precipitation .
One hour would perhaps be better .

I have tried an alternate method which has also worked , using a magnetic stirrer
but I have not compared the yields of the alternate method to the cold method
just described . The alternate method is to perform the initial peroxidation having
the reaction vessel in an unfilled cooling bath containing a shallow layer of plain water ,
and allowing the precursor mixture to warm at a fair rate during dropwise
addition of the first 10 to 15 % of the peroxide , controlling the rate of addition so
that the reaction mixture attains a peak temperature of 65 C at the end of the
addition of the 10 to 15 % of the total peroxide . The addition is stopped and the
bath is filled with ice so that the stirred mixture is cooled below 10 C before the
addition of peroxide is resumed . The rate of peroxide adddition is increased
cautiously so as to maintain the reaction temperature below 15 C to the end of the addition ,
and stirring continued for thirty minutes beyond the last addition .
Stirring is then stopped and the mixture allowed to stand for a few minutes ,
and the mixture is dumped into the now melted cooling bath and neutralized .
Slightly less than the calculated amount of ammonium hydroxide required for neutralizing
is dumped into the well stirred mixture , since it has been observed
that excess alkalinity of free ammonia decomposes the DPPP . Local caustic
concentrations decompose the DPPP , so the neutralization mixtures should be dilute
and mixed quickly , and perhaps it is best to then complete the neutralization using a
small excess of theory of a milder alkali like sodium bicarbonate .

That pretty well summarizes where things are at this point in the experiments
so far regarding the synthesis of DPPP . The material evolves extremely irritating
vapors which should be avoided , as they are quite similar to the irritant effects
of "tear gas" . The effect is noticeable to put it mildly , even at low concentrations
where the smell is not noticeable . There has been consistent observation and agreement
by everyone reporting that good ventilation and / or other protection
is a must . DPPP is one of those materials which will render an area vacant
quicker than a fart filled elevator , you have to experience it to believe it :D

[The_Rsert]

Why are you not writting a exactly senthesis instruction?

[Rosco Bodine]

I haven't yet completed drying and weighing of yields from my last experiment ,
nor have I completed the experiment for the process described above , so
a "Experimental" writeup at this point is premature . I will get around to it
if someone else doesn't do that first . But anyone can take the patent ,
along with the information I provided above , and make DPPP while having
some knowledge of what the reactions are and how the synthesis proceeds .

[Mr.ANFO]

Yes, I will also have to add that the irritating vapours can be dimished by the use of 100% isopropylene alcohol as a solvent to dissolve the irritating byproduct. The end result is DPPP with very little in the way of any smell.
I wonder what this orangy byproduct is?

-- note to all of you skeptics... YOu have got to make a blasting COB out of DPPP just to see how much power this material has !! I am still in a state of shock over it. :)
I would love to see it used in detcord and or in an empty 100g butane can.
BE CAREFUL !

[The_Rsert]

The byproduct is the water insolouble oil (http://www.roguesci.org/theforum/attachment.php?attachmentid=583)
which will form a uppon layer after some days.
But what's the stuff exactly?

[Rosco Bodine]

The oily insoluble substance which gradually forms an upper layer floating on top
of the acetone and HCl mixture , after a long time of reaction is probably a mixture
of phorone and triacetone dialcohol and higher acetone polymer "resinous products" .

Mr. ANFO

The crystals of DPPP which I have been drying for several days are continuing to
gradually lighten in color and lose the irritating vapor which was an unmistakable presence
on the freshly made DPPP . The level of the irritant has steadily decreased around
the crystals exposed to the air , and it is now barely detectable after three days of "airing out" .
When the crystals were freshly made , the irritant vapor was quite overpowering
even several feet away from the crystals resting on the filter and spread out for drying .
And now after several days the vapor has nearly vanished completely , so it is evident
the impurity is volatile , and whatever is the impurity , it is not the DPPP :D ,
but is a nuisance impurity which by some means is accompanying the DPPP crystals
from synthesis , like fleas on a dog . So there is probably some change which can be made
in the way the synthesis is being done , to minimize or exclude the impurity .
Rogue chemist at Science Madness may be correct in that simply letting the mixture stand
will allow the reaction to finish more completely and eliminate the impurity which consists
of unreacted precursor . That looks like a very good theory at this point .

In the early part of the discussion I suggested that reversing the order of addition
may have advantages and this still seems like it may be logical as a possible way
of addressing this specific problem . If the precursor was added very slowly
to the cold peroxide , and the reaction would proceed the same path in spite of this
reversal of the order of addition , then the precursor would be exposed to H2O2
in great excess of its requirement during the early part of the reaction . Normally this
would tend to drive the reaction more assertively in the direction of complete conversion
of the precursor , resulting in a more pure product . And because it appears that the presence
of any unreacted precursor accompanying the end product is an offending impurity
due to its lachrymatory properties , then this provides incentive for formulating a strategy
for reducing or eliminating that unreacted precursor from the end product . I am tempted
to try the reverse order of addition simply to see if this will clean up the reaction .
I know I asked about this earlier and was told that reversing the order of addition produces AP
instead of DPPP , but frankly I doubt the accuracy of that report . What I suppose and hope
could be true is that a white product resulted which was mistakenly identified as AP ,
when it may have actually been pure white DPPP . That would be very nice
if that turned out to be true and clarification on this is no matter of any trivial significance .

[nuclearattack]

I calculated the oxygen balance of DPPP and it is -136 :( , at least is better then AP!
Anyway i wonder how it can reach 9000 m\s or so much power (it is evident from the tests made) with a so poor OB. Well also HMX and RDX have negative OB but generally i know that a good OB is better for performance.
How much the OB is related to vod and power?
However this DPPP seems a very good choice and it should be great if mixed with a positive OB HE.

[Myrol]

I think the Oxygen Balance has no great effect on the VoD.....you say it yourself. AP has a OB of -151,3g O2....It wondered me a long time why such a stuff can be even Explosive under this circumstates....

If DPPP has -136 it should do the Job. HMTD has -92 and has just a better Energydensity as AP.....Someone said AP can reach 6000m/s....I think its a little high but I'm sure 5400m/s are possible...HMTD has his maximum at 5100m/s so th OB might be not that big influence to the VoD.

You see it very good with TNT and NG...TNT has something around -73g O2 per 100g TNT and max 7050m/s, NG +3,5g O2 at around 7600m/s......

I hope to get some very new expieriences with my DPPP. I prepare since Wednesday the Pentachloro Phorone. I used a BIG excess of Hydrochloric Acid 150ml Acetone and 300ml 30% HCl but I want to see the results......The solution must be blood-red until I peroxide it. I also evaporate the remaining Acetone before making the DPPP. Has someone an Idea if its good to neutralize the remaining HCl with Sodium Carbonate? It is perhaps possible to get then pure Pentachlorophorone wich should be result in a very pure product!

About DPPP's irritating odor......I swear it should be Chloracetone wich could form whilst the Chlorination or the Peroxidation to the DPPP....Acetone might be always present, Chloroacetone is a very irritating "Tear Gas" like substance and all symptoms claim that it's really CA. I suffered such a "violation" too. It's very unpleasant (but who cares :D or: screw the innocent)

P.s. If we can separate some pure Pentachlorphorone wouldn't it possible to boil it with some NaOH together to replace all Cl-Atoms with OH-groups?
The finished substance: Pentahydroxyphorone could be Nitrated to a very good Explosive-> Phorone Pentanitrate, who knows?

[VasiaPupkin]

I made some "DPPP" by metod described by The_Rsert. But I have no reflux and I placed acetone/HCl mix in the hermetic bottle on heatener (35-40C). After 20hours I got black non transparent liquid dark red-orange in slim layer. When I prepared DPPP it was yellowish-grey color.
Mixture with crystalls was placed in frige. After 2 day it turns almost white with yellow shade. Then I place DPPP crystalls in open air on few days. DPPP was dissolved in boiling acetone and when half of acetone was evaporated I cool the solution. The precipitated DPPP was an off-white crystalls with weak odor like AP.
I test it on friction. Pure compound was some more sensitive to friction than non puried but less sensitive than AP. Then I place pure DPPP in open glass on heatener (35-40C). And after 3 days its completely turns into very sticky transparent suryp which burns slowly. Damn! :eek: Its looks like decomposition. Or its not DPPP? Other properties is similar as described.

[knowledgehungry]

Well we might have found the reason this explosive isn't used by the military, or anyone really.

[R_Chemist]

I do not think your DPPP is vary pure VasiaPupkin. I have had my DPPP(both the pure white variety and the impure pale yellow variety) sitting at room temperature for over a week now and it has not turned to a liquid. Also Rosco had been doing some sublimation tests of DPPP at around 70C(mentioned on Sciencemadness) which did not yield a syrupy like material. It could be that your DPPP was not very pure and some DPPP sublimated away leaving a residue of unreacted precursor, which would have been trapped within the crystall structure of DPPP, which then dissolved your DPPP leaving the syrupy material.

[Mr.ANFO]

A couple things about DPPP which are recent discoveries and that have been varified by fellow scientists.

1) The smell of untreated DPPP (the yellow colouration) is from mesityl oxide. This chemical has the characteristic camphor-like odor. Mesityl oxide is also photosenstive and thermosensitive and degrades on contact with light and heat to a yellowish colour. (darkens)

2) DPPP has a cubic crystal structure and is very very slightly pale-yellow.

3) Choloroacteone cannot be formed uner the conditions stated by the original patent nor by R_Serts production method. However production of Mesitylene, Mesityl oxide, Phorone HCl, Penta-chlorophorone.... and relatives are and have been detected in the mix I sent to my university.

4) The end peroxide is able to detonate in very small amounts when dry. I seems to act very simular to AP except I am seeing a major energy difference. The peroxide seems to detonating much much faster.

[Rosco Bodine]

There is a patent I posted in the thread about optimizing APAN and it
describes a synthesis of trimeric AP under moderately acidic conditions
which are similar to the conditions of acidity for synthesis of DPPP .

GB620498

Mostly the patent describes the use of sulphuric acid , but does mention
that HCl can also be used in lesser concentrations . On page 3 line 29 of
the patent , it states that too large a proportion of HCl particularly at
elevated temperatures favors the formation of chloroacetone . Of course
there is plenty of free acetone in the reaction mixture of the patent so
it is different in that respect from the reaction mixture for DPPP . Anyway
it would seem possible that any traces of acetone in the DPPP reaction mixture
could also be a source for chloroacetone formation , although the potential
concentration would be lowered . From what I have read about the reaction
of H2O2 and HCl , the reaction takes place only slowly , and produces Cl2 , and
also some HClO by the further reaction of the chlorine with water . I have speculated
that the initial reaction of the DPPP precursor during "peroxidation" which is actually
a chlorination , may be favored by warm temperatures , but at the same time it
is also possible that no advantage may be taken of this if it is true , because of
the undesired simultaneous production of chloroacetone or other undesired byproducts .
This is still an open question not fully resolved for me with regards to the synthesis
of DPPP . If the reaction of the H2O2 and HCl does occur slowly , then the rate of
formation of the pentachlorophorone would be limited by that slow reaction providing
the chlorine . In my estimation the chlorination of the precursor is the least well
understood part of the synthesis of the DPPP .

[Mr.ANFO]

I was not aware that Choloracetone could be formed with HCl and Acetone. Weird.
I was under the impression that Chloroactone could only be formed via free Cl2 and HCl with Acetone. By any chance was this using 37% HCl?

Well as again I will have to say the initial finding of 1:1 Acetone to HCl reaction with 60-65c heat added according to my university favors Mesitylene, Mesityl oxide and Phorone derivatives rather than Chloroacetone. ( this is why the darkening and the camphorish smell led the organic chemists to test for the Mesityl oxide) turns out that in my particular sample gave a signifigant reading.
:confused:

[Rosco Bodine]

Mr. ANFO

Nobody that I know of is talking about the formation of chloroacetone from
reaction between acetone and HCl . What is being described by the GB620498 patent
is that in a reaction system containing acetone along with hydrogen peroxide
and HCl , that increased concentrations of HCl combined with increased temperatures
favors increased chlorination of the acetone to form chloroacetone as an undesired byproduct ,
instead of the intended trimeric acetone peroxide . This is good information
about the reaction condition where hydrogen peroxide reacts with HCl to produce chlorine ,
which is different from the condition where peroxidation would be the desired purpose
for the hydrogen peroxide . The intended reaction for the phorone dihydrochloride is
to be a chlorination reaction resulting in conversion of the phorone dihydrochloride to
pentachlorophorone . The chlorine is being supplied by a side reaction from H2O2 and HCl ,
the HCl being present in some excess in the red phorone dihydrochloride solution , because
more HCl than required by theory was used to form the precursor originally , and/or some
extra HCl was added to the red precursor solution just before the addition to it of the
H2O2 is begun . The production of chlorine is favored by warm temperatures and excess HCl ,
according to the GB620498 patent . And from what I have read elsewhere about the
reaction of H2O2 with HCl , the reaction takes place slowly , therefore it is reasonable that
a very slow addition rate of the H2O2 to the warm and HCl rich reaction mixture would favor
the chlorination reaction preferentially to a peroxidation reaction which would be favored by
opposite conditions , such as cold temperatures and lower concentration of HCl .

Early in the discussion of the chemistry of the reactions stated by Mackowiak for the
formation of DPPP , I stated that I had reason to wonder if perhaps the formation of
the pentachlorophorone would be favored by warm temperatures , followed by cooling
of the pentachlorophorone solution for completing its conversion to DPPP . That was
a "guess" about the reaction which is supported by the additional information which
is provided by GB620498 . So it would seem likely that since 6 of 11 of the moles of
H2O2 to be added to the phorone dihydrochloride are consumed in the chlorination
reaction producing pentachlorophorone , that 6/11 of the portion of total peroxide should
be added to the reaction under conditions which favor that intended chlorination reaction .
To reiterate , the conditions favoring chlorination are excess HCl , warm temperatures ,
and slow addition of the H2O2 . Of course it may not be possible to exploit such a strategy
for the chlorination unless the pentachlorophorone is a stable intermediate which may form
in increasing concentration without peroxidative decomposition in advance of the point
where the mixture will be cooled for conditions favoring peroxidation of the pentachlorophorone
to DPPP . Ideally , if the pentachlorophorone is a stable intermediate which cooperates in
accumulating to a high concentration without any further tendency towards decomposition ,
then the formation of the pentachlorophorone intermediate could be accomplished by
performing the reaction *warm* during the time of addition of the first 6/11 of the peroxide
required for the eventual formation of all the DPPP . When all of the pentachlorophorone
intermediate has formed , the mixture would be chilled very cold before the remaining 5/11
of the peroxide is added . So the addition of the peroxide would be done in two stages ,
with the first portion being added to a warm reaction mixture favoring chlorination ,
and then the second portion of peroxide added to a cooled reaction mixture favoring peroxidation
of the chlorinated intermediate having accumulated during the warm first reaction stage .

The volume of H2O2 stated by Mackowiak at 2 volumes of 30% H2O2 for each 1 volume of acetone is deficient the amount of theoretical requirement for the reactions as Mackowiak has the reactions written . A minimum of 2.55 volumes of 30% H2O2 for each 1 volume of acetone would be required for the stoichiometry to be satisfied where 6 moles of acetone are eventually converted to 1 mole of DPPP . Closer to 3 volumes of 27% H2O2 for each 1 volume of acetone would be required by theory . Anyway , I find such an error in stoichiometry found in a patent to not be reassuring since the technical disclosure of chemical reactions is a highly proper place for exactness about such quantities .

[Mr.ANFO]

As most have you have experimented with AP and other HE's, here is a movie of a 80g DPPP shaped punching charge made out of an aluminum butane refill kit cartriage. This was a huge explosion and a 15-20ft visible shockwave!! :)
the blast was strong enough to be felt strongly several 100ft away. There is also a bit of the backstop post shooting away as the can blew threw the 4mm steel pot. Examine this video closely and you will see a bit of post shooting away from the back.
http://www.sciencemadness.org/talk/viewthread.php?action=attachment&tid=179&pid=36242

[nuclearattack]

I'm trying to make DPPP, in this moment 100ml of acetone are reacting with 93ml of 31%HCL on a heater, it is orange but i have to wait some more hours to reach the end of the reaction when the mixture becomes black.
I have some doubts about the amount of H2O2 since i didn't read any precise quantity of the hydrogen peroxide in the precedent posts.
In Rosco last post he writes that 2,5 volumes of H2O2 30% should be added to 1 volume of acetone...this means that i have to add 250 ml of H2O2 since i'm using 100 ml of acetone?

To Mr.Anfo:
there is any video in your link but only a 900kb file with .php extension. :(
Anyway from your description it seems very powerfull for a peroxide, the shaped charge was made with a propane can? Have you got some pictures?

[Dr_Pind]

Well, I was just running through some of the descriptions of the process of making DPPP, and found that one needs 2 moles of HCL for every one mole of phorone to get the Di-hydrochloride-Phorone, right? Now, most of the procedures use around 1oo ml of both HCL and acetone, but only a fraction of HCL (a few ml.) is added to the mixture before the peroxidation. If 100 ml of HCL are needed for making the di-chlorinated phorone, wouldn't one need a lot more HCL in the peroxidation step, to get the penta-chlor-phorone?.. something like 1,5 times the amount of the first amount of HCL?

I mean, if one gets the di-chlorinated product from 100 ml. of HCL, one would need a total of 250 ml of HCL for the production of the PCP.

The math behind my confusion: 100 ml HCL to yield the di-chlorinated product means 50 ml. of HCl for each added Cl right, so if one is to get the Penta-Chlor-Phorone (5 Cl), one would need 5 * 50 ml. of HCL

Can anyone please fill me in on this missing HCL problem? or correct me if I'm wrong about the process... Thanks!

[Rosco Bodine]

In my opinion the pentachlorophorone and the phorone dihydrochloride are not either one distinct intermediates which necessarily must form completely as a distinctly separate step
in the progress of complex reactions believed to occur , if the resulting end product is indeed DPPP . The reactions overlap somewhat especially during the addition of the first half of the peroxide , where the HCl byproduct of chlorination and peroxidation is cycled back into the reaction with the material not yet chlorinated or peroxidized . HCl is involved in the reactions , but is freed again as the reactions proceed , so an amount much less than the total required for the reaction of the entire mass at one time is required . Only sufficient "excess" HCl is needed to be available for the reactions to proceed at a reasonable rate and this has been determined by experiment . For the precursor made from 93 ml HCl 31.45% and 100 ml acetone , self-reacted for a half hour and then heated gently until it becomes orange colored , then allowed to stand for 72 hours at room temperature , and then cooled for the peroxidation , 40 ml of HCl 31.45% added to the cold precursor immediately before the peroxidation has been found to give good results .
This mixture when treated dropwise with 280 ml 27% H2O2 , the beaker cooled in a salted ice bath and rapidly stirred , addition rate limited to control temperature of the mixture in the range of 12-15 C , will produce a good yield . the mixture should be stirred for an hour past the end of the addition and allowed to stand for several hours in the salted ice bath .
The yield of dried crystals is ~ 95 grams by this method . An experiment to follow would be to add gradually another 100 ml acetone to the fully reacted mixture wile it is stirred to a slurry , continue the stirring for another hour and then let the mixture stand in a replenished ice bath for another day , to see what amount of weight increase of AP would be added from any unreacted H2O2 which is evidently present in the "spent" DPPP reaction mixture . A substantially increased weight of yield beyond the theoretical 98.5 grams of DPPP would pretty conclusively *prove* that the first crystalline product is *not* DPPP ,
but some other compound yet to be identified . This weekend I am going to perform this
experiment , because I already know there is unreacted peroxide in the "spent" DPPP reaction mixture which shouldn't be there if the H2O2 had been consumed in the "chlorination" scenarios described by the DPPP patent .

[Dr_Pind]

Thanks Rosco... that really helped my understanding :) Did think about the HCL being recyclet, but thought that the process would need the fully chlorinated product to work... Guess I was wrong :rolleyes: This explosive REALLY sounds promising. A great alternative to AP, powerfull, stable, and made from the exact stuff that AP is made from, and the more complex process really seams to pay off in the end. I will try your procedure in the weekend.

Edit: Isn't one supposed to evaporate off the excess acetone, so that one won't get AP in the finished product?

I read in a post that the amount of DPPP increases if the cold solution is left to stand for some time? Is this true? Is it possible that adding ice cold water to the mixture would increase the yield? It is said that the DPPP is insoluble in H2O, so couldn't one drive it out of solution by adding water?
What about purification? Is the product filtered and washed with cold water while in the filter? And is it necessary to neutralize the trace acid? It has been discussed whether it is necessary to neutralize AP, and some say that the basic environment is worse than a slight acid environment. And isn't the HCL going to evaporate while the product is drying?

How close is this procedure to perfection, conserning the yield. Is it close to the claimed 90% in the patent?..... I know.... It really is a lot of questions in a row, but I would really like to understand the process, and get a good yield. And it wouldn't hurt to hear other peoples oppinions and experience...

Thanks again ;)

[Rosco Bodine]

The best yield which I have gotten is almost quantitative using the conditions
described above . 100 % yield is an improvement over the 90% of the patent .
Of course the patent has a discrepancy regarding the amount of peroxide which
would prevent even 90% yield from being achieved if the patents ratios for the
reactants are followed . There are a lot of unanswered questions about the
proposed DPPP , both questions about the synthesis and the identification
of the DPPP product itself . The study of the process is ongoing . Personally
I tend to seriously doubt the accuracy of the patent , however there may still
be usefulness about the product and the process which may even be improved .
I'm pretty sure there is unreacted peroxide in the reaction mixture which can be
utilized to form a mixed product and I plan to experiment with this idea in the
next couple of days to see what results .

[Mr.ANFO]

1stly about the video. You need the most recent download of quicktime to view the file. Go to mad science and you will find a link to the file on the holy grail organic peroxide thread. I think it is on thread #27?
It is quite the video :) although it proves little. :(

I have been thinking as to why the patent was not clear as to what the substance looked like and other specifics. I really do think this was a deliberate act on the scientists for security measures. If indeed this material has very high brissiliance as is "easy" to manufacture, terrorist groups would love to get their hands on it.

[nuclearattack]

I tried to make the synth of DPPP but...damn! It is very hard to indentify the final product!
I had a very good yeild (i used rosco's ratios) about 90 gr and now the product is drying. Anyway the final product is pure white and it resembles AP, the only difference is the smell...but this is not a good indicator because i usually make AP using H2SO4 and for DPPP i used HCL.
This weekend i'll make a test using two charges on a plate, 1gr of AP vs 1 gr of DPPP, if it is DPPP.
Any suggestion or comment?
Does your DPPP seem like AP?
A note:the final product is pure white even if i didn't wash it, it was white even in the batch.

[Rosco Bodine]

After many experiments it has become evident to me that what everyone has been
calling " DPPP " is actually only trimeric AP , contaminated with a trace amount of
a yellow colored material and containing a lot of entrapped water in a porous crystal
structure , even after the material appears to be a fairly dry powder .

If stoichiometric proportions of reactants are used to account for the formation of DPPP
via the reaction route described by the patent , the "spent" peroxidation mixture will
be found to still contain over half the quantitiy of hydrogen peroxide used , *after* the
supposed "DPPP" has formed . This rules out the patents described "chlorinated" intermediates
which are supposed to be formed from chlorine produced by the consumption
of hydrogen peroxide in reaction with HCl , a reaction which evidently does *not* occur ,
since the unreacted peroxide is still present in the spent DPPP reaction mixture *after*
it should have been consumed in producing the non-existent chlorinated intermediate .
If an additional quantity of plain acetone , equal in amount to that used to originally make
the "DPPP" precursor , is added gradually to the spent DPPP reaction mixture , and allowed
to stand in the cold for an extended time , the weight of "mixed product" obtained is
almost exactly *doubled* , strongly suggesting that *both* products of peroxidation
are trimeric AP . Solubility in toluene , adjusted for water content which separates on solution ,
so that an adjusted solubility figure for the dry crystals is calculated , is found
to be about 35 grams per 100 ml toluene for the DPPP produced by a non-mixed product
reaction where no plain acetone was added for reaction with residual peroxide .
Comparable solubility of a control sample of bona fide trimeric AP made by the usual method
is also found to be 35 grams per 100 ml toluene . The presence of the unreacted
peroxide in the spent " DPPP " reaction mixture , and the comparable solubility of the
alleged " DPPP " product with the solubility of trimeric AP , are compelling evidence that
the Mackowiak patent is without validity .

[nuclearattack]

Do you think that DPPP is only a fake?
How do you explain the greater power that some tests have demonstrated?
Expecially the test of the metal plate?

[Rosco Bodine]

Do you think that DPPP is only a fake?
Yes the patent is *bogus* . It does not withstand scrutiny . Even the
proportion of hydrogen peroxide to acetone specified in the patent does not
square with the amount which stoichiometry would require for producing the
compound claimed to be produced in 90% yield . From a standpoint of
mathematical analysis , the patent does not withstand scrutiny from the start
and the discrepancies and contradictions get worse from there as the results from
experimental evidence is added .


How do you explain the greater power that some tests have demonstrated?
Expecially the test of the metal plate?
The results of a few tests or a single test do not provide an accurate picture .
You can do numerous tests of the exact same material under conditions where
certain variables apply , and have test results which are misleading . There are certain
conditions where it is a coin toss whether the detonation will be low order or high order ,
and a dozen tests of the same sample material could produce good plates or poor plates
as a result of unidentified variables peculiar to that one loading , or to a range of loadings
where the same anomalies occur .

I am certain that anyone who carefully and honestly examines the Mackowiak
patent , to a level of thoroughness required for arrival at scientifically valid conclusions ,
will also dispute the validity of the Mackowiak patent for the same reasons . I am sure
that my science will be at odds with the opinions of some others who would choose
to disregard the science and go with their opinions . When they get deeper into the
scientific aspects of the experiments and the tests there will be reached a point where
the things I have said are confirmed by their own data .

[knowledgehungry]

I have long doubted the validity of this patent, however might not a different product be formed rather than AP or DPPP. There is no doubt that many different products are formed by the reaction of HCl and Acetone. It is likely that these products may react with H2O2. I personally have not succeeded in creating DPPP. Most of my failed reactions result in no precipitate I'm going to research what products are formed by HCL and Acetone and then take a look at how those products would likely react with H2O2.

[knowledgehungry]

I just stumbled across this at sciforums.com

DPPP mystery is cracked !! THE KEY FOR MAKING DPPP IS THE DISTILLING OF THE BLACK_RED LIQUID INTO THE MOST CONCENTRATED YOU AN MAKE IT.. Should have a concistancy of lite motor oil.
DPPP has a plate like pentagramlike crystal structure and is (dark yellow orange) almost umber coloured. kinda reminds me a bit of (wulfenite)
My synthesis was correct and WOW I even have pics and video of a micro amount deflagrating and one of a melting- to semidetonation. It deflagrates at an amazing speed as well. at least 3x faster than TCAP does in a small amount. DPPP also is totally smelless when it detonates and has a tiny amount amount of soot was seen in the deflagration.. however when it actually detonates no soot is formed... interesting. As the patent says it also detonates when contaminated ... I mix 50% with very fine saw dust an it detonated like AP... but with the smell of hot wood...

The author was Hideki Matsumoto. If what he says is true then this can not be AP. Acetone would most certainly be boiled off first.

[Chris The Great]

Well, it certainly isn't DPPP though I think that name is stuck to it :P

I have alot of precipitate, I'll filter it out later tonight as I didn't have time on the weekend. I'll then try peroxydizing my thick, motor oil like stuff made with 97% H2SO4 instead of HCl (reaction happens very fast, it's done in maybe 10 minutes without heating, it drives itself).

Anyway, copied my post from sciencemadness on my results and conditions etc.


Yes, that may convince me, although I will want to confirm it myself, after all I have a small batch of 'DPPP' in the works, and wow, this stuff sure gets full of crystals! One of my mixes is nearly solid! Details below, as details are good.

My HCl and acetone mixture, which had been sitting for approximatly 3 days, and was a light red orange colour, was put into a hot water bath for about 1 hour, with about 10 minutes out of the bath because it started boiling without enough room to condense. Half was poured out and the jar was resealed with a plastic baggy (polyethylene). Heating continued until the mixture was a black colour, although exposure to very strong light showed it was a red colour. A small amount of oil was seen floating on the surface.
http://img41.exs.cx/my.php?loc=img41&image=heating2nl.jpg
This was put into the freezer along with my H2SO4 mixture and the ruby red HCl mixture I poured out 20 minutes in, as well as my H2O2 to get it nice and cold.

12mL of the red stuff was put into a 125mL jar in a saltwater bath (-10 degrees).
http://img41.exs.cx/my.php?loc=img41&image=step19tf.jpg
Picture mainly to show contrast to later images.
10mL of H2O2 (35%) was added over a peroid of about half a minute with another syringe, with swirling. The temperature rose to 10 degrees. The jar was capped and labelled A.
A second 125mL jar was put into the salt water bath, and 12mL of the red stuff was added, followed by 1 mL muriatic acid. 10mL of H2O2 (35%) was added over a peroid of half a minute with swirling. Temperature was about 12 degrees afterwards, however the precursors had warmed up somewhat before hand.
30 seconds later:
http://img41.exs.cx/my.php?loc=img41&image=30sec3aa.jpg
Maybe 2 minutes later:
http://img41.exs.cx/my.php?loc=img41&image=mins8ds.jpg
A fair amount of crystals had already formed at this point.

About 2 hours after this, the mixtures are both white. A is a near solid mass of crystals, while B is much more runny. Both smell nothing like AP, and have a strong smell that burns my nose if I inhale right over the jar. I'm going to leave it for at least 12 hours before filtering and washing, rinsing with alcohol and drying.



It seems to me at least that adding HCl before H2O2 reduces the yield, though I can't confirm it at this point due to not having enough H2O2.

[megalomania]

Allow me to interject some reason here if I may. I have not been following this thread since I made my original posts a few years ago, and back then I was only concerned with phorone. I have since re-read this entire thread and I would like to point out a few things.

First of all it is quite apparent to me that any reaction done in the presence of any quantity, other than trace amounts, of acetone is invalid. The formation of TATP is something that cannot be ignored and will always affect your results. It is only yesterday that knowledgehungry finally brings up the point of purifying the phorone. Actually The_Rsert first mentioned it somewhere around page six, but none of his experiments ever utilized the tactic. I am not saying have super pure phorone, all I am saying is have it be substantially free of acetone. A fractional distillation will take care of that. If there is no acetone there can be no TATP. Early on there was mention of pure phorone not working in this reaction. Some other inert diluent can be used like methylene chloride, chloroform, carbon tet, perhaps even methyl, ethyl, or isopropyl alcohol. Even toluene or xylene would likely work.

My second point is that many of you have been using anecdotal observations and wishful thinking to gauge the VOD of this explosive. One guy did a plate test, fine, but one test is hardly definitive proof of a VOD at 9000 m/s as Rosco has pointed out several times. For his test to be even remotely trustworthy there should have been several trials to gauge repeatability and eliminate sources of error. Also, a plate test is not a good way to establish a true VOD, it only gets you in the ball park. Anecdotal guesstimates of VOD certainly do not count, even though you might convince yourself that an explosion looks more powerful. Psychologically we want DPPP to be more powerful, and we can convince ourselves of this fact.

I am rather doubtful as to the mechanism of this reaction published in the patent. Phorone is a symmetrical molecule, so why does it form a pentachloride instead of a hexachloride? I can see why it forms 5 and 6 membered rings because ring strain is lessened. If hexachlorophorone is formed this would make a third 5 membered peroxide ring giving us phoronetriperoxide.

I am afraid that a bit more modern scientific proof is required to sway me as to the existence of DPPP. By that I mean mechanistic characterization and spectroscopy reports. I will be doing an analysis of phorone formation by gauging the progress and extent of the reaction via 1H and 13C NMR, FTIR, and GC/mass spec. I am surprised no one has tried to run a TLC on the phorone.

I have requested as much literature as I can get on the synthesis of phorone. I have one journal article right in front of me that uses zirconium chloride to form phorone (among other things) from acetone. The included IR results show what I would expect: phorone, mesitylene, diacetone alcohol, triacetone alcohol, mesityl oxide, and 2,2,6,6-tetramethyltetrahydro-1,4-pyrone (the authors mention this as the source of camphorlike odor).

I also did a Chemical Abstracts search for DPPP. I did manage to find it this time. There is only one reference to it in the past 100 years, and that is the German patent we base all this on. Not one scientist since 1969 has published so much as a mention of DPPP. I find that curious. I don’t even think the Encyclopedia of Explosives and Related Items bothered to mention this stuff, although I am not done searching for different combinations of its name. I apologize because I do not know where I put the information I acquired from CAS. I could not save the files to my keychain drive, so I wrote it down, but the paper is awol. I will get the info in a few days, which is the CAS number, the proper IUPAC name, and the molecular structure.

EDIT: Having just read The_Rsert's procedure I am reminded of an error that both he, and some time back that Rosco, have made. Dichlorophorone does not form except in the presence of free chlorine. The free chlorine is enabled by hydrogen peroxide. How can dichlorophorone be formed merly by refluxing HCl and acetone (except maybe in trace amounts)? And I quote The_Rsert:

Two hundred ml of fuming HCl (hydrochlroc acid, 37%) are mixed with 200 ml acetone and heatened with hot water under reflux. The flask and the attached reflux-condenser are stored on a heatener for 15 h, whereby the temperature in the flask is about 30°C. The fluid dichlorhydrogen phorone is formed. The acetone must be evaporated at 60°C. The remaining dark (like oil) fluid is stored for the next 12 h at 20° to 30° or more without reflux or a stopper. If possible, add some more fuming HCL. This converts the dichlorhydrogenphoron to pentachlor phorone; furthermore, the remaining acetone is converted. The oily fluid is cooled down to -10°C, 50 ml hydrogen peroxide (30%) is added slowly. The temperature should be slightly below 0°C. When the temperature decreases to about -10°C, black crystals precipitate, which are heavier than the solution. If no crystals precipitate, then ice-snow must be added cautiously until crystals begin to precipitate.

Surly the formation of dichloro and pentachlorophorone happens only AFTER you add hydrogen peroxide. At least this is what the patent leads me to believe.

[knowledgehungry]

Personally I highly doubt that this patent is valid, currently I trust members experience more than the patent.

To anyone out there who has access to IR, NMR, or Mass Spec please run a test on the final product and send the results to me, I am rather good at interpretating them, my teacher was amazed at how quick I picked it up.

Mega could you either post the results of your mechanistic analysis or send them to me? I would greatly appreciate it.

[The_Rsert]

Do you think that DPPP is only a fake?
How do you explain the greater power that some tests have demonstrated?
Expecially the test of the metal plate?

I prepared a stuff ("DPPP") which does not smell like AP, which does deflagrades on air times faster and which has another crytalls structure. I tested also the explosion power of it on air against the double amount of AP. "DPPP" is stronger. You can see a little video as evidence here (http://members.fortunecity.de/potatoguns/versusDPPP.html) if you don't believe me.

The metal plate tests may show you also that that the "DPPP" has a greater power even when it's pressed in a cap and I heard that some (Russian) people has tried it's sensitive to friction with the result that the "DPPP" is less sensitive than normal AP.

DPPP does definitly exist, but the in the patent described procedure will never form pure DPPP so the patent is more or less bullshit.

To get pure DPPP we have to purify the needet products(dichlorhydrogen phorone) of the HCL/acetone mix.
Has anyone the time and the glasware to destill it fractional?

So we can say that the stuff which we (I) made may be not pure DPPP but a co-cristallized mix of some different organic peroxides which is stronger than normal AP.



One note/question:
If you cool you acetone free acetone/HCL-mix-product, after standing for some days, to less than -10°C you will get much of a black crystalline precipate after adding some drops of H2O2.
(look at the attached pics). Which stuff is it? :confused:
Is it pure pentachlor phorone? :D
THX!

[nuclearattack]

My acetone/HCL mix wasn't so black, maybe that i have to wait more next time before use it.
Next time i'll let the remaining acetone to evaporate after the black compound is formed.
Should i add fresh HCL before starting the peroxidation or i should add H2O2 to the pure black substance?
Anyway if the final product is not DPPP but it is more powerfull then AP it is good for me! :D

[megalomania]

Maybe you guys could try TLC with a sample of the suspected DPPP and a sample of TATP prepared the usual way. This should at least tell us if we are dealing with a mixture of TATP and something else, just TATP, or something else entirely.

Ward’s sells TLC plates individually for $2. Check them out at http://wardsci.com/category.asp?c=1451&sid=GOOGLE&eid=GL327 There is also currently an Ebay auction for a pack of 25. The bold might be able to make their own. A slurry of silica gel will stick to glass plates coated with plaster of paris. Aluminum oxide is the other plate coating of choice.

[Chris The Great]

I also think the patent is crap, I made some 'DPPP', with 12mL of my HCl and acetone mix, and 10mL 35% H2O2, and there was no acid present during washing. According to the patent, there should be alot of acid. I also tried adding 1mL of HCl to it before the H2O2, got a smaller yeild and it was very acidic afterwards. However, both resulted in the same substance, as far as I can tell.

But the stuff is pretty interesting, I have done no real tests other than deflagrating some, which releases alot of black smoke and seems to burn with more violence than AP, and a small 1 gram piece underwent DTT and detonated with a large amount of noise and blast, though little brisance as it was a small piece in the open, and no distinctive AP smell was noted. I'll post some details later, as it's late, they're upstairs, and I want to go to bed :P

But, it is certainly not AP. I also highly doubt it is DPPP, as sulfuric acid and even NaOH work to make the precursor, although I have not reacted my H2SO4 mixture with H2O2 yet, and have not tried the NaOH method. Peroxidizing the H2SO4 mix is for tommorrow.

[The_Rsert]

The "DPPP" has a great "initiative" power! I blasted a mix of about 100g AN, 30g NM, 5ml PGDN and 5g Al without a problem with a really little blasting cap with less than 0,2g "DPPP" in a little drinking straw with a 2mm ID.
I got a really, really big crater!

[megalomania]

As promised, here are the details of diphorone pentaperoxide from CAS.

CAS #: 32619-19-5
common name: diphorone pentaperoxide
acronym: DPPP
CAS name: 1,2-dioxolo[4,3-c][1,2]dioxepin-8(3H)-one

[Rosco Bodine]

The "DPPP" has a great "initiative" power! I blasted a mix of about 100g AN, 30g NM, 5ml PGDN and 5g Al without a problem with a really little blasting cap with less than 0,2g "DPPP" in a little drinking straw with a 2mm ID.
I got a really, really big crater!

What you got is a talent for storytelling :p :eek: :(

And about the CAS registry , maybe somebody should ask
how many other compounds they have listed which don't even exist :D

[hereno]

Me think so too...

One of them 2mm ID drinking straws :rolleyes: Reading here and on sciencemadness it seems the only ones reporting the greatness of this "DPPP" are the ones that are greatly and blatantly inflating claims.

[megalomania]

It has just occured to me that one not need go to all the trouble of running a HPLC or GC/MS to insure a proper seperation of DPPP from AP when a simple FTIR or NMR will be able to identify the presence of a carbonyl. If no carbonyl peak is indicated, then there is no DPPP. I would run a sample up to the lab tomorrow, but I have no H2O2 :( Since we are in the off season for pools I'll have to pay through the nose for a chem supplier to send some.

[Chris The Great]

So, I filtered out my "DPPP" last week, and it was dry enough to do some tests on this weekend.

Filtering was somewhat problematic for me, I lost alot of the product from the A batch.
The A mixture was poured into the filter, and distilled water was used to get the rest of the crystals out of the jar. A small amount of sodium bicarbonate solution was poured onto it, however there was no acidity, so I stopped pouring it and rinsed it again with distilled water. Then, it was rinsed with methanol, which caused about a third of the product to go through the filter! I was somewhat upset, so rinsed again with distilled water and then with isopropyl alcohol (99%). The isopropyl went through the filter very slowly however it did not take a bunch of crystals with it as the methanol did. I squeezed the rest of the isopropyl alcohol out of the filter by hand and put it in a small dessicator.
The B mix was dumped into the filter and distilled water was used to get the rest of the crystals out of the jar. A large amount of sodium bicarbonate solution was required to nuetralize, and it foamed a large amount during nuetralization. After the product stopped foaming when sodium bicarbonate solution was added, I rinsed it with distilled water and then 99% isopropyl alcohol. After most of the alcohol had gone through the filter I squeezed out the rest by hand and put it into another dessicator.

This weekend I had time again, so I went out to check on the "DPPP". It has dried completely in the dessicator, and both the A and B mix seemed to be exactly the same thing. A few deflagration tests also gave that impression.

About 1 gram of "DPPP" in the form of many small chunks was ignited on a spoon, with a very nice think black smoke ring being formed. I then deflagrated ~1 gram of each the A and B mixtures on a piece of wood. Both burned very quickly, seemingly more quickly then AP, with think black smoke being formed each time.
A then took a pill sized piece, also approximatly 1 gram, perhaps a very small amount more, and had it DDT with a very large amount of force. I had put in hearing protection for these tests, as I didn't know exactly how easily it was to detonate, so my ears only had a very slight ringing that quickly faded away. Although it was very loud, and I felt a substantial shockwave hit my hand which was in a leather glove about 4 inches away, there was only a small 1cm dent on the soft particle board. No smoke was produced, and the distinctive smell of detonating AP was not smelt.
I detonated a small <0.5 gram AP initiator I made to test, and the smell was very strong, indicating that what I have was definatly not AP.

I then tried dissolving it in toluene to check the moisture content, as Rosco had found his full of water. About 3 grams where dissolved in 25mL toluene, and absolutly no water was seen. So, whatever it is, it's pretty pure.

I am hopefully going to try peroxidizing my precursor prepared with sulfuric acid instead of hydrochloric acid tommorrow.

[Mr.ANFO]

:)
Well I think I have finally figured out somthing about DPPP and it's synthesis. 1:1 ratio HCl 37%vol to acetone is in fact correct however we get the yellow-redding effect of byproduced mesitylene as the main reaction starts to take place. You will notice that after the entire reaction has ceased there is a precip that refuses to let any light through. This is indeed in fact the target Chlorophorone as a sample was taken to my university and tested. When this suspended material has hydrogen peroxide 35% added to it there is a releasal of Cl from the chlorophorone and depending on the temperature of the liquid you can get a wide range of phorone peroxides forming in the end product along with mesityl oxide.
Now I have done two different sytheses one at a warmer temperature -5c and one at -30c.

Alright so now about the velocity, I have had an ex-forensics officer test fire a brass shell loaded with 1.23g AP and got 5180.34m/s by using an infrared VOD "Usec chronometer". My "DPPP" hit 8460.90m/sec at 1.23g. clearly we now have numbers to play with. This was done at a secure location at a test range as a university project of mine. I do not have pictures that I can post on this forum. sorry, you can tell i am full of shit but I don't care at this point. The other thing that gave the VOD away is the metal casing shrapnel from the two explosions. look at the test.pdf on this forum and you will see what I mean. Clearly the difference in size indicates a faster explosion

[The_Rsert]

What you got is a talent for storytelling :p :eek: :(


Hey, that's no only a story! :mad:

The PGDN and the Al makes the composition more sensitive than normal ANNM! 0,4g HMTD is strong enough to initate 25% ANNM.

So, why can't a very little drinking straw, filled with a little amount of "DPPP" initiate a near fuse sensitive composition.
It does work great! Try it by yourself!

Don't forget, the mix does contain PGDN and Al which makes it some times more sensitive than usual ANNM.

[Rosco Bodine]

you can tell i am full of shit but I don't care at this point.

Now there is one * conclusive finding * which has already been reached
some time ago , and for many good reasons , that indeed YOU ARE FULL OF SHIT !
You are absolutely correct you are full of shit , and it's really pretty sad that
anyone would be so obsessed with a science experiment that it has
become a kind of mindless calling for them to convince others a lie is true .
You can't tell enough lies that are variations on a theme to get past
some fundamental facts which dispute the formation chemistry for the
theoretical and speculative compound DPPP . You can't pretend that
working with your mason jar and estimated quantities that somehow you
have found the "secret" conditions which result in the successful synthesis
of a compound which by all indications from experiments , and by chemical
and physical tests has been shown * DOES NOT EXIST * except in wrong
theory , backed up by wrong math , and of course accompanied by chlorine
evolution which never occurs either .


So, why can't a very little drinking straw, filled with a little amount of "DPPP" initiate a near fuse sensitive composition.
Because 2 mm is smaller than the critical diameter required for self detonation
of the " DPPP " and also for most other explosives , to reach high order detonation
in any reasonable distance . There are only a very few explosives which would have
2 mm capability and the " DPPP " isn't one of them . Critical diamneter is
one of the things I tested , and it was found to be 5.5 mm . So convince somebody else
with your story , somebody who doesn't know any better than to eat up all the shit you are shovelling .

[The_Rsert]

Grrrr!
A detonation is not required to initate PGDN/AN/NM/Al mix! A stronger blasting will be (off course) better, but it does work!

I used some times drinking straws as blasting caps! 1time for pure NG, 2times for a fine ANNM compositions (I used a 5mm ID drinking straw for the forst one of them) and one time for pure PGDN! It does work fine!
I'm also using metal detonators with a 9mm ID but it does'nt make a big difference for this explosives. I had only one two misfires with prilled ANNM and drinking straw blasting caps.

Make PGDN, put a little blasting cap made of a little drinking staw and AP or DPPP in it and light it! It does work!

A blasting cap made of a drinking straw filled with pressed AP will be even good enough to initate APAN!
My blasting cap looks very smilar to the one in this PDF: http://members.home.nl/icexool/Shaped%20Charges.pdf

It does work fine! Believe me! Try it by yourself! I'm not stupid as Mr.Anfo!

[Mr.ANFO]

Rosco you are the type of person to NOT beleive anything as your world is completely false, what would it matter if I was telling the truth anyway? You would still say that anything except your calculations or observations are correct! My test was done in precision manner and too fucking bad rosco as you hadicapped your own research by switching the topic at science madess to making isopropyl peroxide instead of DPPP! THAT WAS STUPID! as clearly DPPP and phorone peroxides exist. SO CALL ME A LIAR, I DON'T CARE !

PURE AND SIMPLE THE VOD IS VERY HIGH FOR DPPP and is close to what was reported in the patent. It just does not seems to have the high heat that HMX or PETN has.
Those are my finding weather you like it or not.

You can dabble in theory any day Rosco. I don't, I do TESTS.

BTW I agree with the R_SERT as PGDN/AN/NM/Al DOES NOT require a detonation to go off.
have you tried this Rosco or was that pure theory again?

What the hell is this 2mm bullcrap for DPPP? that is just shit.. All you need is enough compressed DPPP to form a ciritical mass in mgs. DPPP detonates in very small amounts around 15-20mg.

[The_Rsert]

Mr.ANFO, the VOD has nothing to do with the power of the explosives! RDX has a lower VOD as HMX, but they have a very smilar lead block expansion.
Pressed AP has VOD up to 5400m/s, HMTD "only" 4511m/s but AP has a lead block expansion of 260ml and HMTD a 340ml leadblock expansion.
One of the most powerful explosives (Si and liquide Oxygen) has only a VOD of about 4000m/s but is 7times stronger than TNT. Also most other mixes of liquide oxygen have a low VOD but a high power. Many liquide explsosives has a low VOD but a very high power (for example EGDN, ethyl nitrate,...) And so on...

I think that "DPPP" can never reach the power of PETN or RDX, even if the VOD is very smilar.

Don't lie like a idiot. You're storys are many times to corious.

[festergrump]

Anfo,

Get a clue that nobody is buying your claims as they are not proven but merely insisted on. If you have proof of your claims, please present them to us, but don't conspire different ways to make us believe that you have achieved what has not been proven. We are beyond taking your word that your teacher said it was as you believe, you had an ex-forensic scientist use a chronograph on it, your "roomie" J-scan saw it, ect... Picture proof is required of you to be listened to with any more than serious doubt.

From my short time here I have witnessed the fact that this Forum will not tolerate multiple personas or the wrecking of threads with blatant unproven claims and intent of leading other members astray.

Please don't wreck this thread for the rest of us interested in learning from people willing to go the mile and prove their findings. If you want to self destruct and end your learning expirience here thats your own business, but do it quickly so the rest of us may get back to topic and members can actually benefit from having read this thread.

[Rosco Bodine]

Mr. ANFO :

The " type " of person I am has no particular bias about any particular
chemical compound used for any purpose or made in any particular way , any more
than a mechanic would favor any particular size or type of threaded fastener for
some particular assembly , beyond what is needed for the job .......it is all just
" nuts and bolts " engineering to me . I couldn't give a shit less what is the
critical diameter for a particular material , until I am assembling some device in which
I want to know that value so I will know the device will work , or has a chance of
functioning as intended . If I want to shatter metal with a device or cut metal , then
I don't give a rats hairy ass what the velocity number is , but what I care about is whether
the metal intended to be shattered or cut is acted upon by the particular charge
to accomplish the task desired .

If someone proposes a synthesis for a composition of matter and they want what they
communicate to be taken seriously , then do a serious description of the synthesis details
so that anyone can reproduce your results , or otherwise don't post your fairy tales on
the web and not expect to be ridiculed .

BTW , I do not believe I ever posted anything online anywhere about " isopropyl peroxide "
Maybe you know as much about what you are talking there , as anywhere else .



The_Rsert :

Are we up to 5 mm now from the earlier 2 mm ?

Add another .5 mm and then you will be closer to reality .

( closer , but still a long way from being there )


This thread has descended into the same kind of classic nonsensical AP thread
of arguing stupidos that has graced every online forum where kids can wrap their
minds around mixing peroxide , acetone , and HCl to get something that makes a bang .

Really I have better things to do with my time for experiments with other materials
where the power and the level of discussion is simply in another orbit of technology .

So with that , I'll say farewell , and leave others to ponder the great mysteries of AP ,
and complex ways of making it which convince everyone through months of experiments
with " colored " AP reactions mixtures , that anything else other than contaminated and
crystal modified AP is the product .

[knowledgehungry]

Rosco I think that the critical diameter for explosives is pertaining to secondaries, I might be wrong but you can get a 1mm by 1mm amount of AP to detonate by hitting it with a hammer.

[SweNMFan]

IF DPPP was the ultimate explosive I would think that someone would use it as it is dirt cheap to make. There must be something wrong with it, since its still NG, PETN, RDX,HMX and TNT that rules.

Oh and a MacDonald drinking straw(8mmID) with 1g HMTD have never failed me.. And I never dared to pack it more that 0.8-0.9 g cm3...

[megalomania]

Progress in science is not dictated by the lone experiment of a single scientist. Your results may indeed be correct, Mr. Anfo, but the results will still require independent verification. The same goes for Rosco, his results may be off.

However, there is the issue of credibility to deal with. I trust the scientific veracity of Rosco Bodine, but I have doubts about Mr. Anfo. Perhaps my doubts are unwarranted, but they are there all the same.

In this situation I will not be satisfied until I have done my own tests in the lab. I consulted a chemist today and he suggested an IR study would be the best bet to identifying a carbonyl group. I may also run a liquid/gas phase chromatograph in about 2 months. I am going to speak to another scientist about reserving a block of time with some real analytical equipment soon. If my qualitative spectroscopy results seem to show the presence of DPPP, or something besides AP, then I’ll run it through the chromatograph, which has a mass detector that can identify quantitatively what we have.

I will sum up with one of my favorite quotes:
“An infinite number of experiments can prove your theory true, but it only takes one experiment to disprove everything.”

[Guerilla]

I think that the critical diameter for explosives is pertaining to secondaries, I might be wrong but you can get a 1mm by 1mm amount of AP to detonate by hitting it with a hammer. Every explosive has a critical diameter, at a certain density. It is the diameter at which the detonation front is strong enough to sustain a continuous detonation. The strenght of initiation affects the time needed for the explosive to achieve its maximum VoD at given density but other than that its of little importance; you certainly can detonate the other end of a long 1mm ID tube of ap but the detonation velocity will quickly drop down aborting the detonation. Officially the CD of an explosive is determined through numerous trials and errors till the diameter at which, on average, 50% of the cords detonate completely, is found. Hope I wasnt stating the obvious here..

[knowledgehungry]

Thanks for clearing that up for me guerrila. If DPPP is what it is claimed to be my guess is that it is not used because it is an organic peroxide. Organic peroxides are not used often for obvious reasons. Even if DPPP had a VOD of 9000 m/s I still wouldn't use it for a main charge, and neither would any military or commercial business. You don't want a large amount of a powerful explosive that will go off if you look at it wrong.

[The_Rsert]

Rosco, here's the demonstration that it does work.
First I measured the ID of the drinkng straw exactly: 2,5mm :rolleyes: :p :D

I put some of my "DPPP" in the drinking straw (I stoppered one side first) and pressed it a little bit with a little wooden rod. I placed the blasting cap on a metal sheet and lighted it (by a fuse).
It cracked loud and now theres a little hole in the sheet.
It's definitly strong enough to initiate PGDN layered ANNMAl!

See the pics of the archive I've just made and attached if you don't believe me.
http://www.roguesci.org/theforum/attachment.php?attachmentid=633

Please, don't call me a liar anymore!

[Rosco Bodine]

Hot Toluene is a good recrystallization solvent - density improver for the AP / " DPPP "

When toluene is * heated * in a sealed jar and then the crude AP / DPPP is is added ,
it literally will form a syrup which is two thirds or more by weight the dissolved
organic peroxide . Any water trapped in the fluffy crude crystals separates and rises
to the top of the hot solution where it can be decanted or ladled off . If the hot saturated
toluene solution is allowed to cool slowly while being stirred slowly on a magnetic stirrer ,
gritty anhydrous crystals of much improved density gradually precipitate . I tried adding
denatured alcohol to the toluene solution hoping that this would speed the precipitation ,
but this was unsuccessful because the alcohol / toluene mixture exhibited a cosolvent effect
and no organic peroxide precipitated . The alcohol did form an upper layer containing the
water in solution , along with a fair amount of the organic peroxide also in solution .
Upon evaporation , this separated moist alcoholic solution also deposited gritty crystals
of much improved density .

The crystals obtained upon cooling of the hot saturated toluene solution are coarse enough
to drain easily and most of the supernatant toluene can be decanted from the slug of crystals
and the AP loaded toluene tailing can be saved for the next recrystallization batch . The
filtered and blottered crystals still damp with toluene dry much more quickly than the
crystals ordinarily obtained from an aqueous mixture , and the loose material has a higher
density and larger size granulation . The anhydrous crystals from toluene are a
" gritty crystalline form " as opposed to the much less dense " fluffy powder " sort of product
obtained from aqueous systems . Even with this density improvement for the crystals
obtained from the cooling of a hot saturated toluene solution , the bulk density of the
uncompressed loose crystals is only 0.6 .

A mixture of AP and " DPPP " crystals dissolved in hot toluene to the point of saturation
and then cooled slowly while stirring resulted in a mass of crystals uniform in size and
physical appearance .

From 100 ml of heated toluene which was then saturated with the organic peroxide in solution ,
75 grams of the dried anhydrous crystals were obtained after decanting
the cooled toluene residual solution and filtering and drying the product .

[Child-of-Bodom]

Megalomania, I can do LC-MS on the phorone right now, and I am willing to do some beginning small tests.
LC-MS is very good in getting single masses, which gives absolute info on the molecular formula of the molecule.
I doubt wheter GC-MS is usefull, as you need temperature stable compounds up to 250°C. (injection temp.)

If you think this is usefull, please post/email a procedure you were to follow for the NMR, then we do at least the same thing, there are already enough misunderstandings...

[K9]

I think I'd like to try this out to see for myself (as I finally have some time) to see what the deal is all about. What I'd like to know though is, what it actually is if it's not DPPP and it actually is more powerful than regular AP at least.

[Myrol]

Wouldn't it be clever to manage some tests between AP and DPPP?

I mean, there are some nice posibillities to compare AP's and DPPP's performance.

I have now a four week old Acetone-Hydrochloric Acid mix (large excess HCl used 150ml Acetone and 300ml 30% HCl) wich is nearly as red as a dark Cherry. But hey....there are no different layers in this mix...its entirely one sirupy fluid. So I think I will Peroxide that as soon as I have time.....300ml 35% H2O2....is that to much?

With this "DPPP" I can then make some tests wich doen't cause to much effort to me. The plate dent test should be ok, or the brisancy against concrete and metal. But theres a thing wich would be great to see, but I have not the necessary space to do that. A big block of "porous concrete" with a drilled hole in the center and a defined amount of AP and DPPP. The explosion should rip something like a small crater out of the concrete, because porous concrete isn't so prone to cracks as ordinary concrete.

Ahh yes....and an Aquarium test should also be very useful! 2g of DPPP or AP fired under water beside a copperplate. The plate must be around 3cm away to create a useful dent, direct contact would rip the metal into pieces!

And last but not least...a test with bigger amounts: "Membrane blow-out". A sample of your Explosive placed into a big room. Around the Explosive are lots of small Al-Foil or plastic membranes placed hemispherically around the Explosive. Thin squares of glass would be even better. To target of this test is to compare the pressure created by the Explosion wich ruptures a unknown amount of membranes or windows. The farer away membranes rupture, the higher the Pcj and VoD because the Density of DPPP is relatively well known (or could be measured with a Pycnometer).

An Example: 50g of DPPP broke 20 1square-inch wide and 0,3mm thick windows and the farest was 90cm away. AP just managed 12 Windows with maximum 65cm. Both Explosives have relatively similiar densites so the VoD and the "Blast" must be in case higher from the DPPP if the easy formula Pcj=0,25xDensity ExplosivexVoD² is right. I know this test cause a lot of effort......I had this Idea after seeing it how precisely Explosion blow out Windows compared to the distance. :o

[megalomania]

I scanned the book "Test Methods for Explosives" which explains the various ways to charachterize such things as VOD, sensitivity, etc. I have not edited the scanned images yet, but I will make it my next book. I am sure the information will help those willing to test AP vs. DPPP.

[Child-of-Bodom]

I would like to do some tests on AP/'DPPP' with LC-MS, but I've ran into a small problem. For this technique, I need to dissolve the compound in a polar solvent... is AP/'DPPP' soluble in acetonitrile or something like methanol? This is needed for the so-called electrospray principle.
Even if it dissolves in only very, very little bits it is no problemo, concentrations of 1mM are the max. for this thing.

If this is not possible, I'll might give it a try at the GC-MS, but is their any spectrum known of AP? I can run a standart of course, but a prove with a nice library hit would be much nicer. The only tricky about this is the injection temperature, it needs to be over 150°C (IMHO), is AP so stable? If it alsready decomposes in the injection port is doesn't have too much use...
I don't have time or possibility's to do much testing, so I want it good in once.
I think this is a better approach then testing the compounds over and over... and to finally prove there's DPPP yes or no.

[Rosco Bodine]

A melting point test of the product from the " DPPP " recrystallized from
a toluene solution saturated at 85 C and allowed to cool , compared
with a melting point for a sample of authentic AP also recrystallized in
the same manner from a hot saturated toluene solution will likely give
an identical melting point .

TLC is likely to confirm the implication .

Temperature instability for the sample is going to complicate getting
meaningful test results where decomposition may skew the results .

[Detonate]

So wats up? Does DPPP exist or not? In my oppinion it does. The material I made is different to AP in many factors. Its density is lower than that of AP, its not as senstitve to flame as AP, the smell ist completely different (but this could be because the presence of any byproducts such as mesthylene oxide). The crystals I got are also a good piece smaller than the AP crystals. I havent made any tests on power because my DPPP (or what ever) is still damp. And to anyone who knows: Is the reaction wich is showed in the patent possible or not? :confused:

[Detonate]

So wats up? Does DPPP exist or not? In my oppinion it does. The material I made is different to AP in many factors. Its density is lower than that of AP, its not as senstitve to flame as AP, the smell ist completely different (but this could be because the presence of any byproducts such as mesthylene oxide). The crystals I got are also a good piece smaller than the AP crystals. I havent made any tests on power because my DPPP (or what ever) is still damp. And to anyone who knows: Is the reaction wich is showed in the patent possible or not? :confused:

[Detonate]

So wats up? Does DPPP exist or not? In my oppinion it does. The material I made is different to AP in many factors. Its density is lower than that of AP, its not as senstitve to flame as AP, the smell ist completely different (but this could be because the presence of any byproducts such as mesthylene oxide). The crystals I got are also a good piece smaller than the AP crystals. I havent made any tests on power because my DPPP (or what ever) is still damp. And to anyone who knows: Is the reaction wich is showed in the patent possible or not? :confused:

[megalomania]

Unscientific qualtative tests are doomed to innaccuracy. There is a chance this process leads to a different crystal form of AP. There are many explosives that have a wide varity of crystal forms that affect their density depending on how it is allowed to crystallize and what with. Certainly having solvents or byproducts trapped in the crystal during crystallization would lead to differing densities, color, smell, detonation velocity, etc. Something as simple as a different rate of stirring, or mixing the chemicals too rapidly could lead to different crystals forms.

Since there is no consensus as to what procedure to use (like there would be in a journal) none of us have an established procedure we can use to attempt to reproduce EXACTLY the same conditions. Twenty different people doing the same reaction in twenty different ways is bound to produce seemingly 20 different substances. Make AP twenty different ways and I bet many of you would have conflicting reports about odor, color, density, and detonation velicity.

These compounds, AP and DPPP if indeed there is actually any DPPP, are too close in physical properties to differentiate from one another without using some more precise scientific tools and methods of analysis. Unfortunatly most of us can only use 18th century means of analysis.

[megalomania]

Unscientific qualtative tests are doomed to innaccuracy. There is a chance this process leads to a different crystal form of AP. There are many explosives that have a wide varity of crystal forms that affect their density depending on how it is allowed to crystallize and what with. Certainly having solvents or byproducts trapped in the crystal during crystallization would lead to differing densities, color, smell, detonation velocity, etc. Something as simple as a different rate of stirring, or mixing the chemicals too rapidly could lead to different crystals forms.

Since there is no consensus as to what procedure to use (like there would be in a journal) none of us have an established procedure we can use to attempt to reproduce EXACTLY the same conditions. Twenty different people doing the same reaction in twenty different ways is bound to produce seemingly 20 different substances. Make AP twenty different ways and I bet many of you would have conflicting reports about odor, color, density, and detonation velicity.

These compounds, AP and DPPP if indeed there is actually any DPPP, are too close in physical properties to differentiate from one another without using some more precise scientific tools and methods of analysis. Unfortunatly most of us can only use 18th century means of analysis.

[megalomania]

Unscientific qualtative tests are doomed to innaccuracy. There is a chance this process leads to a different crystal form of AP. There are many explosives that have a wide varity of crystal forms that affect their density depending on how it is allowed to crystallize and what with. Certainly having solvents or byproducts trapped in the crystal during crystallization would lead to differing densities, color, smell, detonation velocity, etc. Something as simple as a different rate of stirring, or mixing the chemicals too rapidly could lead to different crystals forms.

Since there is no consensus as to what procedure to use (like there would be in a journal) none of us have an established procedure we can use to attempt to reproduce EXACTLY the same conditions. Twenty different people doing the same reaction in twenty different ways is bound to produce seemingly 20 different substances. Make AP twenty different ways and I bet many of you would have conflicting reports about odor, color, density, and detonation velicity.

These compounds, AP and DPPP if indeed there is actually any DPPP, are too close in physical properties to differentiate from one another without using some more precise scientific tools and methods of analysis. Unfortunatly most of us can only use 18th century means of analysis.

[Silentnite]

Ah, I am rather confused. Hopefully someone may help.

I had some spare time, and some spare chemicals. So I proceeded to try making DPPP, or failing that, tried and true TCAP.

I added 1:1 ratio of Acetone to 37%HCl . I then put this over a bunsen burner. During which time it turned yellow and had little bubbles rising like in champagne. Smaller then that of course but close enough. It slowly faded to orange. Then to Red. And finally a deep reddish color.

I then poured some off and capped the rest to play with later. The minute amount I poured off was then a darkish orange and lighter then the original quantity was. To this I added an equal(maybe 1 1/2) amount of 3% H2O2. The solution quickly turned Yellow. No heat from that process though. It is now looking like lemonade, or concentrated lemon juice. No precipitate, nor anything else for that matter. At some point should this form crystals or did I do something wrong.

I personally believe(after reading all 7 pages) that DPPP doesnt exist as said. Maybe an alternate form of TCAP such as the Dimer version suggested earlier. But I should have some precipitate in a few days at least to find out and compare.

BTW, during the entire process it smelled slightly of acetone, and had the burning associated with HCl. Although after I pulled it off the flame, I accidently spilled some of the liquid and it had an aroma I would compare to a weak chloroform.

[Silentnite]

Ah, I am rather confused. Hopefully someone may help.

I had some spare time, and some spare chemicals. So I proceeded to try making DPPP, or failing that, tried and true TCAP.

I added 1:1 ratio of Acetone to 37%HCl . I then put this over a bunsen burner. During which time it turned yellow and had little bubbles rising like in champagne. Smaller then that of course but close enough. It slowly faded to orange. Then to Red. And finally a deep reddish color.

I then poured some off and capped the rest to play with later. The minute amount I poured off was then a darkish orange and lighter then the original quantity was. To this I added an equal(maybe 1 1/2) amount of 3% H2O2. The solution quickly turned Yellow. No heat from that process though. It is now looking like lemonade, or concentrated lemon juice. No precipitate, nor anything else for that matter. At some point should this form crystals or did I do something wrong.

I personally believe(after reading all 7 pages) that DPPP doesnt exist as said. Maybe an alternate form of TCAP such as the Dimer version suggested earlier. But I should have some precipitate in a few days at least to find out and compare.

BTW, during the entire process it smelled slightly of acetone, and had the burning associated with HCl. Although after I pulled it off the flame, I accidently spilled some of the liquid and it had an aroma I would compare to a weak chloroform.

[Silentnite]

Ah, I am rather confused. Hopefully someone may help.

I had some spare time, and some spare chemicals. So I proceeded to try making DPPP, or failing that, tried and true TCAP.

I added 1:1 ratio of Acetone to 37%HCl . I then put this over a bunsen burner. During which time it turned yellow and had little bubbles rising like in champagne. Smaller then that of course but close enough. It slowly faded to orange. Then to Red. And finally a deep reddish color.

I then poured some off and capped the rest to play with later. The minute amount I poured off was then a darkish orange and lighter then the original quantity was. To this I added an equal(maybe 1 1/2) amount of 3% H2O2. The solution quickly turned Yellow. No heat from that process though. It is now looking like lemonade, or concentrated lemon juice. No precipitate, nor anything else for that matter. At some point should this form crystals or did I do something wrong.

I personally believe(after reading all 7 pages) that DPPP doesnt exist as said. Maybe an alternate form of TCAP such as the Dimer version suggested earlier. But I should have some precipitate in a few days at least to find out and compare.

BTW, during the entire process it smelled slightly of acetone, and had the burning associated with HCl. Although after I pulled it off the flame, I accidently spilled some of the liquid and it had an aroma I would compare to a weak chloroform.

[cyclonite4]

This DPPP thing seems to have gained alot of interest (especially at SM, the topic is 23 pages long). Generally I have no idea whether DPPP exists or not, but I have this wierd feeling it may all be a hoax, although I am hopeful it isn't.

I tried a few months ago. After leaving the HCl in the acetone for a day or two, smelling it would burn the nasal passage (apparently it is a good chance that chloroacetone formed instead). I poured excess 6% H2O2, and got a temperature rise of 6-7C, a few hours later, a precipitate was noticed to form, which stopped precipitating at the end of the day. Due to the similarity to AP, I was under the impression I had formed dimeric AP, thus chucked the product away in fear of it's infamous instability.

[cyclonite4]

This DPPP thing seems to have gained alot of interest (especially at SM, the topic is 23 pages long). Generally I have no idea whether DPPP exists or not, but I have this wierd feeling it may all be a hoax, although I am hopeful it isn't.

I tried a few months ago. After leaving the HCl in the acetone for a day or two, smelling it would burn the nasal passage (apparently it is a good chance that chloroacetone formed instead). I poured excess 6% H2O2, and got a temperature rise of 6-7C, a few hours later, a precipitate was noticed to form, which stopped precipitating at the end of the day. Due to the similarity to AP, I was under the impression I had formed dimeric AP, thus chucked the product away in fear of it's infamous instability.

[cyclonite4]

This DPPP thing seems to have gained alot of interest (especially at SM, the topic is 23 pages long). Generally I have no idea whether DPPP exists or not, but I have this wierd feeling it may all be a hoax, although I am hopeful it isn't.

I tried a few months ago. After leaving the HCl in the acetone for a day or two, smelling it would burn the nasal passage (apparently it is a good chance that chloroacetone formed instead). I poured excess 6% H2O2, and got a temperature rise of 6-7C, a few hours later, a precipitate was noticed to form, which stopped precipitating at the end of the day. Due to the similarity to AP, I was under the impression I had formed dimeric AP, thus chucked the product away in fear of it's infamous instability.

[Silentnite]

The liquid now looks like Squirt or some other such Citrus-y beverage. No precipitate. I think I shall add some acid and maybe some more H2O2. More H2O2 as I am using only 3% and maybe it needs a little more. And more acid due to the fact that it has been sitting quietly in my fridge for a day now, and maybe needs a kick in the ass.

On the other hand, my batch of AP is coming along nicely. So I say Screw DPPP, and I shall stay with TCAP, howerver *great* DPPP is.

TCAP is my friend. Reliable, and easy to make. Next foray will be HMTD:D

[Silentnite]

The liquid now looks like Squirt or some other such Citrus-y beverage. No precipitate. I think I shall add some acid and maybe some more H2O2. More H2O2 as I am using only 3% and maybe it needs a little more. And more acid due to the fact that it has been sitting quietly in my fridge for a day now, and maybe needs a kick in the ass.

On the other hand, my batch of AP is coming along nicely. So I say Screw DPPP, and I shall stay with TCAP, howerver *great* DPPP is.

TCAP is my friend. Reliable, and easy to make. Next foray will be HMTD:D

[Silentnite]

The liquid now looks like Squirt or some other such Citrus-y beverage. No precipitate. I think I shall add some acid and maybe some more H2O2. More H2O2 as I am using only 3% and maybe it needs a little more. And more acid due to the fact that it has been sitting quietly in my fridge for a day now, and maybe needs a kick in the ass.

On the other hand, my batch of AP is coming along nicely. So I say Screw DPPP, and I shall stay with TCAP, howerver *great* DPPP is.

TCAP is my friend. Reliable, and easy to make. Next foray will be HMTD:D

[cyclonite4]

I like HMTD myself (having a large supply of hexamine :D ), but to get any decent yeilds, you need to use 30%+ H2O2, and I've yet to find a place that sells it both locally, and at a reasonable price ($40 is sky-fucking-high price for a litre :O ).

Don't forget to call TCAP by its structural formula ;) : 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexoxonane (according to ChemSketch)

[cyclonite4]

I like HMTD myself (having a large supply of hexamine :D ), but to get any decent yeilds, you need to use 30%+ H2O2, and I've yet to find a place that sells it both locally, and at a reasonable price ($40 is sky-fucking-high price for a litre :O ).

Don't forget to call TCAP by its structural formula ;) : 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexoxonane (according to ChemSketch)

[cyclonite4]

I like HMTD myself (having a large supply of hexamine :D ), but to get any decent yeilds, you need to use 30%+ H2O2, and I've yet to find a place that sells it both locally, and at a reasonable price ($40 is sky-fucking-high price for a litre :O ).

Don't forget to call TCAP by its structural formula ;) : 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexoxonane (according to ChemSketch)

[Silentnite]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

[Silentnite]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

[Silentnite]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

[K9]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

Every 10 volumes is about 3%, makine 50 volumes 15%.

[K9]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

Every 10 volumes is about 3%, makine 50 volumes 15%.

[K9]

When you are talking about H2O2 and the bottle says 50 volume is that the same as 50%? I cant seem to find a reference anywhere. If it is, then I can get it relatively easily. But it would usually be 40 volume.

Every 10 volumes is about 3%, makine 50 volumes 15%.

[me234]

Oh well, I guess it's time I share my stuff with the rest of the world before someone else does something similar:
Can anyone here help me with converting some pictures (scanned) from paint/word format to something a little more compact: as at present the word format has one pic at ~9mb and the other at something similar.
The reason why I post this here, is that, drum role please: The first picture is a scanned copy of an FTIR spectrum run of trimeric acetone peroxide; and the second is an FTIR on (very) badly made DPPP (which I will be attempting again later as I do not trust this to be the right stuff now).
Now I expect a certain amount of scepticsm to greet my claim, but I shit you not. If you guys want I'll even post the instrmentation details.
So, can anyone help me, or should I just post some huge fucking pictures on the thread? If you can PM me and I'll e-mail you the spectra.
Thanks for any help guys.

P.S. Coming to a thread near you this summer: NMR on Trimeric AP an alleged DPPP!!!

P.P.S. I PM'ed Mega and NBK about this, but neither have replied so far. And holding onto something this exciting for a few weeks is damned hard!

[me234]

Oh well, I guess it's time I share my stuff with the rest of the world before someone else does something similar:
Can anyone here help me with converting some pictures (scanned) from paint/word format to something a little more compact: as at present the word format has one pic at ~9mb and the other at something similar.
The reason why I post this here, is that, drum role please: The first picture is a scanned copy of an FTIR spectrum run of trimeric acetone peroxide; and the second is an FTIR on (very) badly made DPPP (which I will be attempting again later as I do not trust this to be the right stuff now).
Now I expect a certain amount of scepticsm to greet my claim, but I shit you not. If you guys want I'll even post the instrmentation details.
So, can anyone help me, or should I just post some huge fucking pictures on the thread? If you can PM me and I'll e-mail you the spectra.
Thanks for any help guys.

P.S. Coming to a thread near you this summer: NMR on Trimeric AP an alleged DPPP!!!

P.P.S. I PM'ed Mega and NBK about this, but neither have replied so far. And holding onto something this exciting for a few weeks is damned hard!

[me234]

Oh well, I guess it's time I share my stuff with the rest of the world before someone else does something similar:
Can anyone here help me with converting some pictures (scanned) from paint/word format to something a little more compact: as at present the word format has one pic at ~9mb and the other at something similar.
The reason why I post this here, is that, drum role please: The first picture is a scanned copy of an FTIR spectrum run of trimeric acetone peroxide; and the second is an FTIR on (very) badly made DPPP (which I will be attempting again later as I do not trust this to be the right stuff now).
Now I expect a certain amount of scepticsm to greet my claim, but I shit you not. If you guys want I'll even post the instrmentation details.
So, can anyone help me, or should I just post some huge fucking pictures on the thread? If you can PM me and I'll e-mail you the spectra.
Thanks for any help guys.

P.S. Coming to a thread near you this summer: NMR on Trimeric AP an alleged DPPP!!!

P.P.S. I PM'ed Mega and NBK about this, but neither have replied so far. And holding onto something this exciting for a few weeks is damned hard!

[grendel23]

Obtain a copy of Paint Shop Pro, readily available on P2P networks with crack. Use the "resize" function to scale it down. I would also experiment saving in both jpeg and gif formats to see which looks better at a smaller size with your images.
I am sure most other image manipulation software will work as well, PSP just seems a bit nicer than most to me.

[grendel23]

Obtain a copy of Paint Shop Pro, readily available on P2P networks with crack. Use the "resize" function to scale it down. I would also experiment saving in both jpeg and gif formats to see which looks better at a smaller size with your images.
I am sure most other image manipulation software will work as well, PSP just seems a bit nicer than most to me.

[grendel23]

Obtain a copy of Paint Shop Pro, readily available on P2P networks with crack. Use the "resize" function to scale it down. I would also experiment saving in both jpeg and gif formats to see which looks better at a smaller size with your images.
I am sure most other image manipulation software will work as well, PSP just seems a bit nicer than most to me.

[metafractal]

No need to use Paint Shop Pro - just use the "paint" program supplied by windows.
Open paint, then
1. File->Open->Select image file
Then, resize your image to a reasonable size by going
2. Image->Stretch/Skew
And type in an appropriate number for vertical and horizontal (same number)
eg Horizontal: 15%
Vertical: 15%
3. Then go File->Save As
Select JPG format and type in a name.
The image should now be much smaller.

[metafractal]

No need to use Paint Shop Pro - just use the "paint" program supplied by windows.
Open paint, then
1. File->Open->Select image file
Then, resize your image to a reasonable size by going
2. Image->Stretch/Skew
And type in an appropriate number for vertical and horizontal (same number)
eg Horizontal: 15%
Vertical: 15%
3. Then go File->Save As
Select JPG format and type in a name.
The image should now be much smaller.

[metafractal]

No need to use Paint Shop Pro - just use the "paint" program supplied by windows.
Open paint, then
1. File->Open->Select image file
Then, resize your image to a reasonable size by going
2. Image->Stretch/Skew
And type in an appropriate number for vertical and horizontal (same number)
eg Horizontal: 15%
Vertical: 15%
3. Then go File->Save As
Select JPG format and type in a name.
The image should now be much smaller.

[me234]

Sweetness, thanks metafractal, I can seem to save as jpeg, but I used 50% by 50%, and the file is now damn near a tenth the size.
Shit, I can't save as jpeg or anything else the forum will accept.
OK I'm gonna have to work on this one.
Give me time, and a really long lever.

[me234]

Sweetness, thanks metafractal, I can seem to save as jpeg, but I used 50% by 50%, and the file is now damn near a tenth the size.
Shit, I can't save as jpeg or anything else the forum will accept.
OK I'm gonna have to work on this one.
Give me time, and a really long lever.

[me234]

Sweetness, thanks metafractal, I can seem to save as jpeg, but I used 50% by 50%, and the file is now damn near a tenth the size.
Shit, I can't save as jpeg or anything else the forum will accept.
OK I'm gonna have to work on this one.
Give me time, and a really long lever.

[Silentnite]

I don't know what format you started with, but Paint should be able to save it in an alternate format, just use the drop down box right under where you type the name in.

However, if that doesn't work(and for some formats it won't) then do a quick search on google for a picture converter. If I recall NBK's choice of picture attachment is a .gif, but provided it's small enough it ought to be ok.

[Silentnite]

I don't know what format you started with, but Paint should be able to save it in an alternate format, just use the drop down box right under where you type the name in.

However, if that doesn't work(and for some formats it won't) then do a quick search on google for a picture converter. If I recall NBK's choice of picture attachment is a .gif, but provided it's small enough it ought to be ok.

[Silentnite]

I don't know what format you started with, but Paint should be able to save it in an alternate format, just use the drop down box right under where you type the name in.

However, if that doesn't work(and for some formats it won't) then do a quick search on google for a picture converter. If I recall NBK's choice of picture attachment is a .gif, but provided it's small enough it ought to be ok.

[me234]

Ladies and gentlemen, I have finally converted it to some useful size.

FTIR analysis of trimeric acetone peroxide:
2 parts 50% H2O2
5 parts acetone
0.5 parts HCl ~30%

Acetone and peroxide mixed, cooled to ~5 Celcius, maybe lower.
HCl added over a 15 minute period, left 1 night.
Very little AP floating, indicating (hopefully) >90% trimeric isomer

FTIR run as thin film technique on a KBr disc, chloroform solvent.







Peaks identified:
Group expected range actual position present
-CH3 1355 --> 1395 1362.71 Yes
-CH2 1430 --> 1470 1471.19 No
-C=O ~1750 N/A peaks NO
-C-O 1080 --> 1300 1186.44 1200.00 doublet Yes


Numerical values given in wavenumbers


Maybe not too conclusive, but if anyone has a sheet with a large no. of functional group peaks ranges and wouldn't mind sharing...
The most important part of this I think is the definite lack of carbonyl groups and
-CH2 groups, both of which DPPP should have.
Up next should hopefully be a DPPP IR, as soon as I have 'made' (?) some.
Opinions please, waddaya thunk?

[me234]

Ladies and gentlemen, I have finally converted it to some useful size.

FTIR analysis of trimeric acetone peroxide:
2 parts 50% H2O2
5 parts acetone
0.5 parts HCl ~30%

Acetone and peroxide mixed, cooled to ~5 Celcius, maybe lower.
HCl added over a 15 minute period, left 1 night.
Very little AP floating, indicating (hopefully) >90% trimeric isomer

FTIR run as thin film technique on a KBr disc, chloroform solvent.







Peaks identified:
Group expected range actual position present
-CH3 1355 --> 1395 1362.71 Yes
-CH2 1430 --> 1470 1471.19 No
-C=O ~1750 N/A peaks NO
-C-O 1080 --> 1300 1186.44 1200.00 doublet Yes


Numerical values given in wavenumbers


Maybe not too conclusive, but if anyone has a sheet with a large no. of functional group peaks ranges and wouldn't mind sharing...
The most important part of this I think is the definite lack of carbonyl groups and
-CH2 groups, both of which DPPP should have.
Up next should hopefully be a DPPP IR, as soon as I have 'made' (?) some.
Opinions please, waddaya thunk?

[me234]

Ladies and gentlemen, I have finally converted it to some useful size.

FTIR analysis of trimeric acetone peroxide:
2 parts 50% H2O2
5 parts acetone
0.5 parts HCl ~30%

Acetone and peroxide mixed, cooled to ~5 Celcius, maybe lower.
HCl added over a 15 minute period, left 1 night.
Very little AP floating, indicating (hopefully) >90% trimeric isomer

FTIR run as thin film technique on a KBr disc, chloroform solvent.







Peaks identified:
Group expected range actual position present
-CH3 1355 --> 1395 1362.71 Yes
-CH2 1430 --> 1470 1471.19 No
-C=O ~1750 N/A peaks NO
-C-O 1080 --> 1300 1186.44 1200.00 doublet Yes


Numerical values given in wavenumbers


Maybe not too conclusive, but if anyone has a sheet with a large no. of functional group peaks ranges and wouldn't mind sharing...
The most important part of this I think is the definite lack of carbonyl groups and
-CH2 groups, both of which DPPP should have.
Up next should hopefully be a DPPP IR, as soon as I have 'made' (?) some.
Opinions please, waddaya thunk?

[frogfot]

me234, nice that you have some analysis data, but IR is not that representative.. Since you've got access to a lab do H1 NMR experiments instead. I think it will resolve different CH3 groups much better than IR.. this is valuable if you wanna see the ratios between dimer/trimer/tetramer. This would also be the "ultimate" way to assign the DPPP.

[frogfot]

me234, nice that you have some analysis data, but IR is not that representative.. Since you've got access to a lab do H1 NMR experiments instead. I think it will resolve different CH3 groups much better than IR.. this is valuable if you wanna see the ratios between dimer/trimer/tetramer. This would also be the "ultimate" way to assign the DPPP.

[frogfot]

me234, nice that you have some analysis data, but IR is not that representative.. Since you've got access to a lab do H1 NMR experiments instead. I think it will resolve different CH3 groups much better than IR.. this is valuable if you wanna see the ratios between dimer/trimer/tetramer. This would also be the "ultimate" way to assign the DPPP.

[me234]

Bastards! Unfortunately, the prof that let me use the FTIR said he'd rather not let me run personal NMRs. Can't really say I blame him all that much though, considering what I'd be running it on!
Before you UTFSE me, I've looked though pretty much every spectroscopic data book I could lay my hands on, and unless I missed something and should feel stupid about it, I cannot find any reference to an IR peak for organic peroxides. Not a damned one.
However, I am sitting here staring at a doublet in the ether region on the IR I got for AP.
So anyway, IR absorptions occur due to changes in dipole moments. But in AP the O-O bond is perfectly symmetrical, no permanent dipole moment. Now, please forgive my stupidity/forgetfulness/laziness, but for Ir absorption, must there be a permanent dipole moment to absorb, or can no dipole moment absorb to give a DM?

OK, so back on topic. Several people have described their acetone/HCl mixes forming this, for lack of a better term, black shit, either when heated for long enough, or on addition of H2O2.
What I was wondering was, what was the longest your, um, black shit, has ever taken to develop.
The reason I ask is that I've had this world's-simplest-ketone/HCl mix sitting on a shelf for several months now, and only a small amount of that black material has formed. For the most part it's a liquid mass that's the traditional red/orange/dark colour, but with a small amount of a black solid just floating around.
Basically this rant was just to ask if someone could maybe help me attribute various colours to the various compounds, mesitylene etc.
Thanks for any help.
P.s. Sorry if the post sounds confused an unordered, just a reflection of my state of mind.

[me234]

Bastards! Unfortunately, the prof that let me use the FTIR said he'd rather not let me run personal NMRs. Can't really say I blame him all that much though, considering what I'd be running it on!
Before you UTFSE me, I've looked though pretty much every spectroscopic data book I could lay my hands on, and unless I missed something and should feel stupid about it, I cannot find any reference to an IR peak for organic peroxides. Not a damned one.
However, I am sitting here staring at a doublet in the ether region on the IR I got for AP.
So anyway, IR absorptions occur due to changes in dipole moments. But in AP the O-O bond is perfectly symmetrical, no permanent dipole moment. Now, please forgive my stupidity/forgetfulness/laziness, but for Ir absorption, must there be a permanent dipole moment to absorb, or can no dipole moment absorb to give a DM?

OK, so back on topic. Several people have described their acetone/HCl mixes forming this, for lack of a better term, black shit, either when heated for long enough, or on addition of H2O2.
What I was wondering was, what was the longest your, um, black shit, has ever taken to develop.
The reason I ask is that I've had this world's-simplest-ketone/HCl mix sitting on a shelf for several months now, and only a small amount of that black material has formed. For the most part it's a liquid mass that's the traditional red/orange/dark colour, but with a small amount of a black solid just floating around.
Basically this rant was just to ask if someone could maybe help me attribute various colours to the various compounds, mesitylene etc.
Thanks for any help.
P.s. Sorry if the post sounds confused an unordered, just a reflection of my state of mind.

[mediumcaliber]

I had a major fuckup with this today. I have a roommate who's hard of hearing and otherwise should just not know about all this fun; he has his own room so I have a reasonable amount of privacy. Yesterday I mixed about 3/4 L of the dark red liquor with an equivalent amount of 27.5% peroxide over the course of the day in a 3L screw-top glass jug. Mixing was accomplished by swirling at every addition, and the jug was kept on ice. Everything went well, but before I got around to filtering out the product, I tested a small portion from an earlier batch by placing it on foil and heating from below with a match. Direct ignition of this earlier batch got exactly the same reaction seen by others and the product had the characteristic "bug spray" smell. When heated on the foil, the product melted and detonated, which is exactly what I didn't want, since my roommate was right in the other room. He sounded startled, said something to himself, and left the apartment.
So everything was put away in short order, and since reaction was finished, the jug of acid and DP (I'm calling it "Different Peroxide" at this point) was placed in the back of the top shelf of my closet. About 7 hours later, the cap blew off the bottle. I left the room and waited for the HCl fumes to air out, which should not have taken long since both windows were open. The air in the room was clear, but strongly smelled of HCl and burned eyes within a few seconds. I quickly got goggles and gloves out, however goggles still allowed enough air in that my eyes burned within 30 s of entering the room. My roommate was still asleep. I wrapped a wet towel around my head to breathe through and cover the vents and gaps of the goggles, and found the bottle. It had two liquid layers, no solids, and was hot to the touch. The lower one was bubbling a small amount of gas up through the upper layer in one place, or so it appeared -I couldn't look at it long. I dumped it in the shower and turned on the water, but the bathroom still burned my eyes more then 10 minutes after rinsing the liquids down the drain, and this was solved by washing the bottle. My closet was splattered, and I took out some stuff with the most splatter and bagged it, and then began washing the closet walls, but gave up because the air near the closet overpowered my wet towel and goggles. It took three hours from the burst to get that far. Having poured the HCl without breathing protection, I don't think the <400 ml of HCl present in the bottle could have been responsible for this; I'm betting that it somehow reacted further to produce chloroacetone.
So the moral of this story is, one of the more hilariously bad things that can happen to an amateur chemist is to accidentally produce tear gas.
Also, do not leave your DP in acid.

One completely different note from a few months ago when I produced gram quantities of DP with 3% peroxide, I found that recrystallizing from acetone with some mixed gunpowder produced a greenish powder that qualitatively appeared softer -kind of squishy, not like the more powdery straight product that forms a stiff paste when wet. It appears to be less crystalline. I don't know what I could do with it since I'm looking to use DP with AN and I don't need something to make it any less sensitive, but I thought it was interesting.

[mediumcaliber]

I don't know if anyone's particularly interested, but I continued with some success and have a few other things to add. The remainder of my H2O2 (27.5% peroxide pool treatment, $17/gal) was used up in three reactions conducted in parallel. The red liquor was prepared in ~1L quantities in three 40oz "malt liquor" bottles. These were glass with lined metal caps, and despite the mixture coming in repeated contact with the caps, no corrosion was observed. Malt liquor bottles in the four brands I've tried are all the same shape but have very slight differences that indicate they are not made by the same company; as this must apply to the cap seals, YMMV. Two of the reactions were carried out in 2L plastic soda bottles in an ice-water bath, and the third in a 5qt ice cream tub. The peroxide was placed in the tubs and chilled red liquor was added. Since I am almost totally without instrumentation, I metered the addition by color, adding enough red liquor to the reaction mixture when it was light yellow to turn it dark orange. Using a candy thermometer I estimated the temperature rise in the tub was 4-6 centigrade, and it approached the bath temperature and the appropriate color within 10 minutes. No signs of degradation of the plastic vessels were seen.
I filtered the precipitate out by pouring the mixture through two paper towels in a strainer until the filter capacity was approached, then pressed out the last of the liquid and washed the cake. The liquid was kept in case more precipitate might form, and a small amount did. The washed precipitate was transferred to a bucket and washed further with sodium bicarbonate, which seems not to have been a very good idea at this point, as the CO2 turned the whole thing foamy. The pool peroxide had surfactants in it.
A much better way of filtering was to place a pillow case over the strainer and dump the mixture over it; this eliminated the need to replace torn filters, increased filter capacity, and allowed the product to be wrung out much more thoroughly than the paper towels did. This method was used to recover the neutralized product.
The damp DP is very firm, but probably contains 20-50% water. When it's mixed with AN, a thin paste is formed. This paste produced a deflagration flash when flame was applied, but only the area near the flame reacted. When damp DP was ignited, it deflagrated and left a few water droplets behind.

I have a few tests set up to test mostly dried DP vs DP-detonated DPAN, and the DPAN slurry, so more results may be forthcoming.
Sorry if I'm rambling a bit much. My sore throat and nose from Wednesday's events have turned into a nasty case of bronchitis, and I may still have a fever.

[Pb1]

It appears that all of this controversy has finally been laid to rest. In this thread (https://www.sciencemadness.org/talk/viewthread.php?tid=179&page=36) over at SM, ordenblitz conclusively compares the product of DPPP synthesis with TATP via FTIR. Not suprisingly, the two are the same. To summarize,

DPPP is a Crock

I guess that this wild goose chase is finally over.

[FUTI]

As much as I would like that final word has being said on this subject I have to ask some questions. FTIR is good method for confirming that one compound is identical to other only if you have FTIR spectrum of pure compounds. So the question is: Has anyone confirmed the chromatographic purity of those products, melting points etc.? Fingerprinting IR domain should be conclusive evidence if they proved that they have pure compound (which is as you know very hard to do with AP making mostly mixtures of dimeric and trimeric product). If it is truth then apparent difference in VoD is maybe caused by different crystal lattice of chemically identical product so it does open a new subject - how to make AP of certain crystal packing/density?:) Work never ends.

[me234]

If DPPP is a crock, then why did someone (can't remember who) post the CAS no., IUPAC structure and name for a compound refered to as "Diphorone pentaperoxide"?

Could someone please instruct me as to why the attachment isn't working, Jpeg gives the size of the file as under the specified maxima...

[FUTI]

I just stumpted on interesting info on one of the sites that speaks on rocket technology etc. I won't post the link since I did that already. Anyway info from that site says that Russians had a major rocket failure (on one of its reliable rockets in 20 years use) and found that the culprit was the replacement of tin based solder seal with the lead based one that cause disaster in H2O2 lines /oxydant/. Now I'm much less prone to experiment with obtaining tin from solders for making any kind of peroxyde based explosives.

[HoS]

I tried this yesterday. I mixed 80 ml HCl and 80 ml Acetone and let it start to react.

I then heated the Acetone/HCl mix till it was a deep yellow color (took it down from 160 ml to 50 ml) let it cool and finished heating my peroxide (this maybe where I went wrong).

I mesured out 100 ml of the still hot peroxide and added it. I then added a splash of HCl and let it react overnight. Come morning I look in to the reaction container to see no solid formations.

So the ever loved 0% yield for me.

+++++

Work on your Grammar. NBK

[c.Tech]

HoS, use common sense.

Why would acetone react with HCl?

Acetone boils at a very low temp - 56.3 °C, if you heated it you would cause it all to evaporate, your HCl probably did too. Ultimately you were just adding water to your peroxide.

Why heat anything if nobody else does it? Most people cool an acetone/H2O2 mix before adding the acid because it forms the more stable and stronger isomer of acetone peroxide.

If your not smart enough to make the explosive I would hate to see what happens when you try to use it.

If your lucky you wont make huge bombs and get yourself killed like an ex-user (phone) on this forum. Do a search for him.

EDIT: apologies I didn’t read the previous posts on the 1st page.

[Chris The Great]

This isn't about making AP the normal way though. This is about making the most likely AP peroxide the interesting way.

You need to keep the liquid from evaporating, most of the acetone evaporated and didn't react. When I did this, I did not have a reduction in volume of any significance.

However, you are not supposed to heat the peroxide, so I would agree that that is where you went wrong.

[sprocket]

Why would acetone react with HCl?

Acetone boils at a very low temp - 56.3 °C, if you heated it you would cause it all to evaporate, your HCl probably did too. Ultimately you were just adding water to your peroxide.
Acetone reacts with HCl to form, among other substances, mesityl oxide and phorone via aldol condensation. You will notice this if you add hydrochloric acid to acetone and let the mix sit for a couple days (less if heated) as the liquid turns from clear to yellow to dark red.

Acetone does indeed boil at a low temperature, phorone and mesityl oxide don't. Their boiling points are 199°C and 127°C respectively. Though, the acetone/HCl mix should still be refluxed.

[Zajcek]

I always see people trying to make phorone from acetone and HCl. Why don't someone buy pure phorone and try to make it's peroxide? My chem supplier sells it, but I don't have any money to buy it. It is about 5 euros per gram ( to expensive for me )

Someone with higher budget could try to buy it. And then simply add some HCl as catalyst and then slowly add H2O2. I have read that photon is not soluble in water, but if you add some HCl, it is. :eek:

If I didn't crash my car, I could buy some phorone and try it myself, but I have so save every penny to buy a new one.

[Chris The Great]

Because it's been tried and it does not make a peroxide when reacted with H2O2 and HCl.

[A.Scriabin]

I've tried to make dppp last night,but happens a very strange thing:first I added the same amount of HCl(30%) to Acetone,and nothing happens,still clear.After I put H2O2 30% and the liquid started to heat and became white,so I cooled it and 2 minutes later,it formed white ad relatively big cristals(I think TATP,not DPPP) with an enourmus yield,at least 80%.The strange thing is that required ONLY 2-3 minutes to precipitate!could it be the dimer?

[Zajcek]

You have made AP, the most possibly dimer.

It precipitated so quickly because of big amount of catalyst used ( HCl )
and because of higher temperature of the reaction.

[Chris The Great]

Yes, that's how I always make mine. Usually it takes a few hours for the crystal mass to turn solid. It doesn't matter which order you add the ingredients if you want it to react hot and fast.

Surprised most of the acetone didn't evaporate first. I might have to try it with some more acid and see if I can get the same kind of results...

[DONMAN]

Ok, I mixed equal parts 27%~HCl and Acetone a year ago. Totally for got about it, then I read this and I remembered it. Found it.

This is probably the most complete and total reaction noted so far between the HCl and acetone. It is so oily and dark! Currently I am doing a test with about 5mL of the Phorone and excess 24~%H2O2 in a salt-ice bath. I am letting that sit over night. In the morning I will wash it and compare it to some Ap that I have crystalizing right now.

When I added the H2O2 I noticed within minutes I had some white precipitate forming.

[camelslaper13]

I recently mixed cooled 25 ml chilled acetone to 20 ml chilled HCL 30% in an icewater/ammonium nitrate bath. I stirred it but never heated it up, it stayed under 30 C. the entire time.

About a half an hour later it had turned yellow, so I slowly poured 25 ml H2O2 30% in and it instanly turned white, and after a minute of stirring it was a thick paste. I left it for 2 hours and then filtered the crystals out with a paint strainer.

The crystals are all white. I have no idea if they are DDDP crystals or just all AP (if so its probably mostly trimers since it formed at such a low temp with such strong acid).

Something I noticed when I packed it into a .17 shell was that it turned green when it touched the brass. Another thing, when I stuck a fuse in I heard fizzling which might have been residual HCl reacting with something in the fuse... but I'm not sure, any ideas as to if that was dangerous and what it was?

All I know is it freaked me out...

[Alexires]

Camelslaper - *sigh*. When doing AP, I keep the temperature under 0ºC.

30ºC is unacceptable really, if it is anything like AP.

Do some thinking. You have just added something with an acid and an oxidiser to a metal (brass). I'm willing to bet my left nut that you didn't wash your product, or if you did, you didn't do it properly.

What is brass made of? What colour are the oxides of the constituents of brass? Does this explain the green colour?

And fuck that. If you push ANYTHING into an energetic material and it FIZZES, I sure as hell would want to be doing it behind a big, thick piece of plexi-glass.

Go read up on explosives safety and go search for pictures of people who made mistakes and paid for it in our hobby.



It's nice that you are interested, willing to do some experimenting and not just shooting your mouth off, but this isn't like school.

If you fail here, you might not get another chance. If you are lucky, you will have a near miss and think to yourself; "Fuck me, I need to be more careful. I could have died".

Please be careful Camelslaper. We don't want you to become another statistic.

[megalomania]

If you get the jist of this thread then you will notice the proper identity of DPPP will require some serious analytical hardware such as IR, NMR, and X-ray characterization. The original DPPP patent is the only reference in the entire Chemical Abstracts database. There are very few of us who have access to such equipment, fewer still who would be able/willing to do the characterization. Maybe some kind soul at Los Alamos will hear our plea, but most likely only (predominately) suicide bombers would ever use this explosive. The military does not use unstable and volatile primary explosives.