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megalomania
October 7th, 2002, 02:54 PM
fatboyvegastj
A new voice
Posts: 8
From:
Registered: DEC 2000
posted December 12, 2000 03:29 AM
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Does Ap really need to be cooled down during the reaction? Thanks
PhatBoy


extreme
Frequent Poster
Posts: 102
From:
Registered: SEP 2000
posted December 12, 2000 04:46 AM
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I think youll cooling it down because you dont want the acetone to boil, but im not sure so please correct me if I'm wrong.


Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted December 12, 2000 08:22 AM
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If it boils you're fucked. You need to cool the solution below 5*C otherwise you'll get the dicyclo version, you want the tricyclo which is more stable and powerful.


CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted December 12, 2000 08:35 AM
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well catually i don't think the DCAP version of AP forms at ANYTHING over 5 celcious. i think at elevated temps it does. (a little higher than 5 degrees C.) but yes keeping the reaction cooled is essential. that is how you produce the tricycloacetone peroxide. this is more stable AND is more poweful. this is what you want, this is what you strive for.
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...Æ


Arthis
Frequent Poster
Posts: 203
From:
Registered: OCT 2000
posted December 12, 2000 12:04 PM
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Logically, the TCAP will be more powerful. Normal as the mol. is bigger.
I didn't know for the 5°C: are you sure, because my AP is not 5°C (maybe 10-15 °C, I never check), and seems to be very stable.

If you don't cool AP you'll have tear gas, and your yield will be VERY VERY low, if you get any cristals, I'm not sure, it depends the quantity of acid you put.


Anthony
Moderator
Posts: 2304
From: England
Registered: SEP 2000
posted December 12, 2000 02:46 PM
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I could be wrong, I was typing from memory, 5*C is about fridge temperature though. 10 -15 degrees C does sound reasonable.


CragHack
Frequent Poster
Posts: 606
From:
Registered: DEC 2000
posted December 12, 2000 04:59 PM
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as a rule of thumb, keep it as cool as you can get it without completely freezing the stuff. thats it. thats all there is to it.
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...Æ


Microtek
Frequent Poster
Posts: 194
From:
Registered: JAN 2001
posted January 06, 2001 09:55 AM
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I usually just cool it with cold tap water
( about 8 degrees ), and I never have any problems. I just pour roughly equal amounts of acetone and 40% H2O2 into a drinking glass add a few ml of 30% HCl stir 10 sec and let it stand overnight. It seems strange to me that you all use so much acid.
I don't think I get DCAP since a Trauzl-block test of my AP gave almost the same result as HMTD (there aren't any inferior HMTD variations right?).

IPN
October 8th, 2002, 09:14 AM
Here is a link where you can find information on the preparation of tetracycloacetoneperoxide which is more powerful and stabil than the dimeric and trimeric forms.
(Ps. sorry for my english.)

The link:
------------------------------------------------
Tried to cut down the length of the link but couldn't - fixed it by adding a www

PDF File ( http://www.rsc.org/CFCart/displayarticlefree.cfm?article=8%2D9%223%24%5D2%5C B%218%27%5D%5CY%28%3E%3C%23S5%3D8%3DP%20P%3D29%23% 3C%0A)

<small>[ October 08, 2002, 12:42 PM: Message edited by: zaibatsu ]</small>

Aaron-V2.0
October 9th, 2002, 01:28 AM
I cant get the link to work, at all! So just take the [PDFFile out of the link above and C&P (Though everyone figured that out quick. :rolleyes: )

I'll just upload the .pdf to Ctrl_C's FTP and for anyone without FTP access who's interested you can file a copy of the .pdf on my very empty <a href="http://aaronewf.tripod.com" target="_blank">site</a>.

<small>[ October 09, 2002, 12:35 AM: Message edited by: Aaron-V2.0 ]</small>

nbk2000
October 9th, 2002, 05:07 AM
In order to get the tetrameric form by using the SnCL<sub>4</sub>*5H<sub>2</sub>O, you need to use something that'll absorb the freed metal ions. That could be EDTA or, more readily available as a photo developing agent, hydroquinone.

HQ is also useful as a stabilizer for acrolein.

<small>[ October 09, 2002, 04:12 AM: Message edited by: nbk2000 ]</small>

knowledgehungry
October 13th, 2002, 05:38 PM
In response to the temparature of AP synthesis, I knew someone who knew someone etc. that mixed the acetone, hydrogen peroxide and sulfuric acid together keeping the temp. below 20 C. He ended up with a medium amount of crystals which behaved as AP normally would, i was wondering if using the sulfuric instead of the HCl was what allowed this reaction to occur better than would be predicted? Thanks for any ideas you have to give

Flying Dutchman
October 14th, 2002, 07:15 PM
I use HCl and I only have to cool my solution in the beginning.
It stays under 10.0 C all the time!
but what I do and advice is to first cool your H2O2 and aceton in a salt ice bath. remember it's your safety you probably don't get a second chance.

TheBear
December 23rd, 2002, 04:05 PM
I guess i beat you all (in the temperature point of view that is) 0.5-1 degrees celsius constantly for three days. I add acetone in about 10 portions to the H<sub>2</sub>O<sub>2</sub>and make sure the temp is back at 1C before adding next portion, the temp never goes above 4 degrees celsius during the addition. I use relatively little acid and let it react for three days (I consume huge amounts of ice!). Then I wash it really good and let it dry. Result: fine crytals and not that volatile substanse.

I've also been trying to make an oxygen balanced APAN mixture and I found that the OB balanced mix is 11,7% AP + 88,3%. Is this correct?

Anyway: Does anyone know where to find the density for 19.5% H<sub>2</sub>O<sub>2</sub>?
I would really like to know.

<small>[ December 23, 2002, 03:08 PM: Message edited by: TheBear ]</small>

Arthis
December 25th, 2002, 12:36 PM
I think some have mistaken the need of low temps. :
You don't want to have the coolest reaction ever but you wan't to make a particular form of AP: much more stable powerful etc... If you are at 5°C or at 2°C will not change much.
Particularly when using conc. chemicals, with not much water: remember that 0°C is 273K and 2K (K for kelvin ! you noob ! <img border="0" title="" alt="[Wink]" src="wink.gif" /> ) isn't much.

And cooling too much slows the reaction to a point where resources become too expensive (think about electricity ! and natural resources).

Give us your yield for that we can compare, and eval. the efficiency of such a cooling (i don't think it's useful, but we never know: I never tried personally...)

[EDIT]: I need to learn to speak a better English once for all !

<small>[ December 25, 2002, 11:40 AM: Message edited by: Arthis ]</small>

dave
December 25th, 2002, 02:47 PM
i remember when i started making AP. The first time I made it using no salt and trying to keep the temp below 8*C, I used $2.22 of ice. My last batch I made triple the amount, using already cold water, and tons of salt. I bought a 10lbs rock salt bag for really cheap. I used slightly less then one bag of ice, which is $1.11 dollars each. Ice is the main concern for me when making AP. Ice can really add up to the cost.

Mic
December 25th, 2002, 04:02 PM
why don't you just put some water in a freezer ? water is free ! no ? and I suppose you have a freezer

dave
December 27th, 2002, 05:28 PM
Where I get my ice it depends. If i have it planned out when to make some AP Freeze 1 gallon of water in advance. If i am bored I go buy some ice. It takes 14 pounds of ice sometimes if the wheather is really hot and the chemicals are not precooled. If I leave ice in the freezer too long my mom will throw it out cause she says it is a waste of space.

kingspaz
December 27th, 2002, 07:33 PM
dave, it may be best to plan your synths in advance. that way you are much less likely to forget somthing vital and risk an accident.

Yak
December 27th, 2002, 07:48 PM
Or if you are planning to make it more then once or twice buy more chemicals and store them untill you need them thus more likly to get all the chemicals you need.

dave
December 27th, 2002, 11:02 PM
Sure, I have all my chems stored up in my shed. I got the largest amount I could buy at once without it being too expensive. I am worried about my 27.5% H2O2 decomposing, I have only used 1/3 of the 1 gallon bottle.

Al Nobel
December 28th, 2002, 11:39 AM
I like winter, no cooling problems for three months.I produced my last batch of AP a week ago on my balcony and it worked great.

TheBear
December 30th, 2002, 03:44 PM
Arthis: I know all that (and please don't try to make jokes like those K stands for kelvin 'noob', they can so easily be misread).
I just want to minimize the precense of the dimer form of AP by being so close to the freezing point as I can. And as for now I don't need to freeze the water in the freezer (as I'm writing it's -19C outside). When it comes to yields here's some facts from last batch:

107 ml acetone (84,7g)
200 ml H2O2 (19,5%)
20ml HCl (30%)

Yield: 73.8g AP

I'm pretty pleased with the yield. I might be imagining all this but the shock sensitivty seems to be lower (due to smaller chrystalls?) than for high temperature manufactured AP, BUT I've only tested it with the classical hammerblow test.

The AP were not dryed in one huge pile but i spread it out over 6 filterpapers.

Oh I forgot to mention, that about a less volatile product were probably not true in my last post (it's pretty cold now and I compared with the volatility of my AP last summer when it was +30*C in the shade) so I can't make a statement regaring it's volatility.

Helos
December 30th, 2002, 06:57 PM
According to pyro 2000 (swedish text by swedish infomania)
using HCL as a catalyst means that both the dimer and trimer form is created, this is not the case with H2SO4 for example.

Anthony
December 31st, 2002, 05:31 AM
It's been long established that dimmer/trimmer formation is governed by temperature, not catalyst type.

TheBear
January 1st, 2003, 03:15 PM
Although hundereds (slight exaggeration) of threads have covered this:

Using H2SO4 might result in formation of H2SO5 (H2O2 + H2SO4 ---> H2O + H2SO5). H2SO5 + actone gives the dimer version _only_

Pyro2000 is an excellent collection, but the organic peroxides file (written by thallion) contains several false claims (HCl not working to catalyse production of HTMD for example).

Off topic: Helos could you please mail me (the mails I send you was automaticcly replied saying your email doesn't exist)

EP
January 28th, 2003, 10:42 PM
Everyone (well hopefully everyone) knows about rinsing in bicarb solution to neutralize any remaining acid in the finished AP, but I've heard from some people that the basic conditions created by bicarb aren't much better than the acidic conditions of unwashed AP. Is there any truth in this? If so, it a final good rinse with plain water sufficient to remove NaHCO3 traces?

metafractal
January 29th, 2003, 01:05 AM
While I always neutralize my AP with a weak alkali solution, from personal experience I have noticed little difference in the sensitivity when such procedures are taken. You can read about my experience when my unneutralized AP seemed unbelievably insensitive to shock in <a href="http://d106112.u27.qwknetllc.com/cgi-bin/ewforum/ultimatebb.cgi?ubb=get_topic;f=2;t=000447#000000" target="_blank">this</a> thread, towards the bottom.

Notice to the future: This link was supplied while roguesci was on a temporary address, so if this link fails, simply replace the d106112.u27.qwknetllc.com with <a href="http://www.roguesci.org." target="_blank">www.roguesci.org.</a>

xyz
January 29th, 2003, 03:02 AM
I wash my AP with Bicarb, then wash it several times with water so that if there is any acid left, or if the AP is now basic, then it gets as close to Ph.7 as possible.

frogfot
January 29th, 2003, 06:41 AM
I have a standard procidure when washing peroxides lesser than 10g AP or HMTD. 200ml water, 100ml 5% bicarb solution and finally 200ml water. Cold tap water is used.

It would be great to have a scientific paper on di/tri AP yields depending on temperature. Something like the pdf on tetra AP above. But everytime i search google it finds kewl sites instead of something useful..

<small>[ January 29, 2003, 05:43 AM: Message edited by: frogfot ]</small>

X-Wulf
January 29th, 2003, 04:48 PM
I wonder if any papers have been published on the subject of yields w.r.t. reaction temperature? Even the one on tetra-cyclo in this topic is related to the catalyst and not so much the temp.