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KABOOOM(pyrojustforfun)
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it formes as an "intermediate" in AP synth. I doubt there's any way to prevent it from further reactions (which form AP) then isolating
it
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Theoretic
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I wonder, is acetone peroxide soluble in anything? 
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Axt
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Conveniently, its fairly soluble in Acetone (I think more-so in DCM), why you ask?
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Rosco Bodine
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AP is fairly soluble in anhydrous isopropanol .
But a more interesting AP solution is coprecipitated AP / MEKP ~ 50/50 , which
separates directly from synthesis as a reasonably pure anhydrous liquid ,
making it easier to isolate than either
AP or MEKP made separately .
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Theoretic
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Just asking, might be useful for storage/separation from the reaction mixture.
[Edited on 20-10-2004 by Theoretic]
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Chris The Great
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| Quote: | Originally posted by sylla
BTW, I've heard that dihydroperoxypropane could be formed using the common acetone/H2O2. I haven't done any search on it (I apologize if it
is the first link on google :p). Have someone tried it ?
It's oxygen balance (-70%) is far better from other peroxides such as the acetone one (di/tri or tetra meric) and DPPP and a bit betterthan HMTD
and TMDD. It's density is around 1.3 (following ACD/ChemSketch software).
But I'm sure with all these properties someone here had already tried it !
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I recently became interested in this peroxide and other non-tradition peroxides. Alot of organic peroxides have not been experimented much with,
mainly HMTD, AP, etc. It forms, as already stated, as an intermediate in AP synthesis. Another peroxide also forms, basically two of these joined
together by a peroxide bond:
HOOC(CH3)2OOC(CH3)2OOH
Both of these are soluble in water, but I think they could easily be extracted using something like methylene chloride or other non-polar
non-water-miscible solvent. I would use methylene chloride because of it's low boiling point.
According to a journal on AP I read, it mentions that the peroxide you mentioned, HOOC(CH3)2OOH was isolated in 12% yield when 50% H2O2 and acetone
where reacted in a 1:1 molar ration in the absence of the hydrogen ion (no acid). Hence, when you mix H2O2 and acetone you get a bunch of non-cyclic
peroxides, the H+ caused them to form cyclic derivatives- the well known acetone peroxide.
When I attempt this procedure, I will mix H2O2 and acetone in a 2:1 molar ratio, with no acid. After several days I will extract with methylene
chloride, and then gently boil if off along with the remaining acetone (the remaining acetone will also be picked up by the methylene chloride) to get
the non-cyclic peroxides.
The Encyclopedia of Explosives gives some information on organic peroxide properties, which is based on structure. It appears that these peroxides
should be quite stable (relative to other organic peroxides that is). For the C(OOH)2 type peroxide, explosive properties are listed as:
Polymeric peroxides formed as a decomposition product are extremely explosive
For HOOCOOCOOH type peroxides, it lists:
Very slight explosive properties
These could obviously be detonated but as organic peroxides go they seem to be quite stable. It will be interesting to attempt to isolate them.
Another interesting thing I noticed in that AP journal was that it mentioned "in the presence of the hydrogen ion, all three abducts have been
isolated with the cyclic trimer being the predominant product in concentrated solutions."
Hence, it would appear that in lower concentrations of H2O2 and acetone, such as with 3% H2O2, the equilibrium shifts over to the non-cyclic
peroxides, and hence a much larger amount of acid is required to push it back towards the cyclic trimer.
I recently picked up a liking for such 'non-traditional' peroxides and hope to prepare a couple of them in the near future. Some other ones
I am interested in are the alkyl hydroperoxides, for example methyl hydroperoxide, CH3OOH. It's a liquid, seems to be sensitive from what
I've read but info is very limited. The Encyclopedia says that it explodes violently (I would think so!) upon jarring or heating.
The explosion should follow:
CH3OOH --> CO + H2O + H2
It is prepared like this:
(CH3)2SO4 + 2H2O2 + 2KOH --> 2CH3OOH + K2SO4 + 2H2O
For the ethyl and isopropyl derivatives it says it is seperated by vacuum distillation but I'm not in a hurry to do that! Doesn't say
anything about isolating the methyl hydroperoxide 
I'm hoping it can be seperated by using methylene chloride as well, as thats simple. Unfortunately, "sensitive to jarring especially at
warm temps" makes me wonder about the wisdom of boiling of a solvent. I think I'll let it sit in a cool dark location to evaporate.
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Axt
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View: http://pulse.webtop100.net/images/methylhydroperoxide.zip 17pg 3.something MB
In German though. I had chemoleo translate some of it quite a while back, guess he wont mind me posting it. This regards the calcium/barium salts of
methylhydroperoxide.
| Quote: | Anyway, it says, 'crystalline barium hydroxide (presumably referring to Ba(OH)2*8H2O), or even calcium hydroxide, is easily dissolved in a
concentrated aqueous solution of methylhydroperoxide.
Salts are formed, which are very soluble in H2O, and which can be isolated by evaporation at as low a temperature as possible (great care to be
taken!)'. |
But in the end, its quite hard to get any decent yield of the alkylhydroperoxides. I think there was a patent related to mixing methanol/H2O2 and
salting out the hydroperoxide followed by distillation, give the patent office a search for methylhydroperoxide etc. but I think it was still <10%
concentration.
Might be worth trying to extract dimethylolperoxide (formaldehyde/H2O2) with a more volatile solvent, as it wants to detonate if evaporated from water
.. know that first hand. I think theres a Pb salt of this in PATR2700. Theres a soluble hydroperoxide of hexamine as well, also an insoluble one by
using HNO3 check vol.8, H82.
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Chris The Great
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| Quote: | | But in the end, its quite hard to get any decent yield of the alkylhydroperoxides. I think there was a patent related to mixing methanol/H2O2 and
salting out the hydroperoxide followed by distillation, give the patent office a search for methylhydroperoxide etc. but I think it was still <10%
concentration. |
I can't read German but at least that gave me a good idea of the synthesis as well as the yields. I guess 100g dimethylsulfate --> 7g methyl
hydroperoxide is pretty poor. Couldn't find the patent but I would prefer to prepare it in the pure form, to make other interesting compounds
and also for a small explosion test. I certainly don't want to make these to make big booms, I just wanna make them because they are interesting
and unusual.
Thanks for the info! Can someone kindly translate the synthesis, which starts on page 12? It's fairly short. I can get the general idea but it
would be nice to know exactly what they did, and not just generally what they did. Doesn't look that hard but it would be problematic if a
sentence that I thought meant stir vigoursly actually means stirring causes detonation, etc.
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((Blasta))
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organic peroxides
Chris, sounds like you have some great ideas. Have you tried producing Methyl Ethyl Ketone Peroxide yet? I think you'll find that the VoD of this
stuff is pretty good...and when mixed with Ammonium Nitrate can be quite powerful. Never mind TCAP...
use caution---explosives in transport
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Chris The Great
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No, unfortunately I have not....
I haven't found MEK here (at least not in a product that it could be easily extracted from), but I haven't actually looked that hard.
If I see some I will definately pick some up though.
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((Blasta))
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| Quote: | Originally posted by Chris The Great
No, unfortunately I have not....
I haven't found MEK here (at least not in a product that it could be easily extracted from), but I haven't actually looked that hard.
If I see some I will definately pick some up though. |
It is avaliable, but getting scarcer due to its effects on health. Try Industrial Plastics and Paint, Cloverdale Paints, ICI paints, General Paints**
I know they have a tonne of the stuff at dirt cheap prices. MEKP with an addition of a NITRATE is very fun to detonate. Its quite powerful oh, mixed with finely powdered Ammonium Nitrate 9:1 ratio proves to be awesome. No
idea on the VoD...can't help you on that one. I bet it is more powerful than commercial PowerGel for rippin' a part rocks.
[Edited on 17-8-2005 by ((Blasta))]
use caution---explosives in transport
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C6(NO2)5CH2CH(CH3)N(NO2)2
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acetone peroxide/AP/triacetone triperoxide/TATP/TCAP/peroxyacetone from 3% H2O2!
So, the day before yesterday, I tried to make AP with 3% hydrogen peroxide disinfectant. I've heard of other people doing it before, they never gave
their specific reaction conditions, and others saying it failed, and I wanted to know if it was possible. My first attempt failed, but the second I
put about 70ml of disinfectant in a bottle, and left it in the freezer an hour until a bit of ice formed. Then I took it out, put 4ml acetone, and 7ml
10% hydrochloric acid and put it back in the freezer. My hope was that the low temperature (~-20C) would freeze some of the water out of solution, and
make concentrated H2O2 in situ.
After 20Hrs, the mixture looked like a solid block of ice with a couple drops of free liquid. In reality, the block of ice was likely porous, with
concentrated AP reaction mixture between the crystals. taking the bottle out of the freezer for an hour caused some of the ice to melt, although there
was still frost forming on the outside of the bottle. The remaining ice rose to the top, while white particles settled to the bottom of the container.
Then, before all the ice had melted, I added sodium bicarbonate until it stopped fizzing. Today, I filtered part of the mixture, and flame-tested the
white sediment. Even when damp, it burned in a series of "puffs" of flame. After drying a piece slightly smaller than a rice grain, I put it on a
piece of newspaper and touched it with a hot steel wire. It decomposed in a fraction of a second without burning the paper.
The yield from this procedure wasn't great, a gram or two I think compared to the theoretical 5+, but the material is definitely energetic. Just
thought I'd share this method of using low concentration Hydrogen Peroxide.
Put that in your pipe and smoke it!
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MineMan
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Interesting!
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caterpillar
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In our shops "hydroperite" is sold. It is the complex of hydrogen peroxide and urea. Add some acetone and a few drops of HCl. wait, wash and dry.
Women are more perilous sometimes, than any hi explosive.
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Rocinante
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Interesting. More details like ratio, yield and procedure would be welcome.
TATP can be formed via air/light oxidation of diisopropyl ether, too.
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caterpillar
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Quote: Originally posted by Rocinante  | Interesting. More details like ratio, yield and procedure would be welcome.
TATP can be formed via air/light oxidation of diisopropyl ether, too. |
I used 30% H2O2. I'm talking about the experience of my friend. But the procedure is very simple. I think you should have an excess of H2O2. Make
simple calculations. The aforementioned compound is sold as a big round tablet. You even do not need to smash it to pieces- only make it wet with
acetone and drop HCl. Wait for one day, wash and dry.
Women are more perilous sometimes, than any hi explosive.
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C6(NO2)5CH2CH(CH3)N(NO2)2
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acetone peroxide, AP, triacetone triperoxide, TATP, ,APEX, TCAP, peroxyacetone from 3% H2O2, more data.
On November 23, 2019 I tried a somewhat more "systematic" test of the effect of freezing during an AP synthesis with diluted precursors. I Chilled
containers of acetone, hydrogen peroxide (3% disinfectant) and muriatic acid (hardware store/technical grade, 31.45% HCl labled concentration) to
under 5C. Then, I poured an identical mixture of the ingredients into three different 1 liter pete plastic bottles. I used 50gm (give or take 100mg)
of peroxide solution, 2.56 gm (30mg tolerance) of acetone (assumed to be almost 100% concentration), and 1.73gm (30mg tolerance) of hydrochloric acid
in each bottle. The amount of hydrogen peroxide was chosen arbitrarily, the amount of acetone was supposed to give a 1:1 molar ratio with the 1.5 gm
of hydrogen peroxide already in solution, and the weight of hydrochloric acid was selected to give starting concentration of about 1% by weight HCl.
One bottle was left in a heated building, where the temperature was between 18 and 13C.
Another was left in a refrigerator where the temperature was about 3C.
The third was left in a freezer with an estimated temperature of -15 to -20 C.
Only I had access to the refrigerator/freezer, and I closed the bottles tightly and put them inside socks and then plastic bags to contain any
leaks. I had previously tested one of the bottles and found that the cap began to leak profusely at a pressure of about 3 atmospheres. Fortunately no
noticeable pressure formed in any of the bottles, and they stayed sealed.
On November 30th, 157 hours later, I checked the containers again. The "refrigerator" and "room temperature" specimens had no sign of precipitation,
while the "freezer" one had just one big piece of ice and very little liquid. Almost all of the liquid was either frozen or absorbed into the ice
block. I neutralized the clear liquids with baking soda and poured them down the sink. I left the "freezer" sample in the room to thaw.
After it thawed, but before it rose to room temperature, I checked it and found a lot of white precipitate at the bottom of the liquid. I added baking
soda until it stopped releasing carbon dioxide. All of the fizzing caused gas bubbles to stick to the precipitate, bringing it to the surface. I
diluted the mixture with water, filtered it, and washed the inside of the bottle with water to get the last bit of precipitate out.
The wet paste was scraped off the filter, and weighed at 2.7gm. After standing in open air for 12 hours, it weighed roughly .95 gm. after 11 more
hours of drying, it still weighed .9gm, suggesting that drying was largely complete. The paste had still kept its shape from when it was wet, but I
didn't try to break it up or check its consistency, for safety reasons.
a small (less than 20mg) piece of the product responded to flame with a very rapid deflagration, and no visible residue.
I may try to det. a few hundred mg. of my product, but that property is already well known and I'm fairly confident that it could work. The mechanism
and optimisation of the reaction needs more attention.
The next test will be to re-wet the product, and take a ~100mg piece and test it with an acid, to confirm that it had little to no baking soda in it.
assuming that it is almost entirely AP, the yield was about .9gm out of a theoretical 3.25, or only about 28%. This is much better than with the
shorter duration experiment, but is still fairly low.
When I filtered the mixture, the liquid that came through still had a lot of hydrogen peroxide in it, and bubbled as it went down the drain. This
would explain the low yield. I suppose that a longer reaction period would help change this. Assuming I am right about freezing changing the
concentration, It also might help to use less hydrochloric acid, since this lowers the freezing point and leads to a bigger more dilute volume that
remains liquid. Acetone and hydrogen peroxide might do the same thing, but they get... precipitated as the reaction proceeds.
I am coming up with ideas of how to test my hypothesis about why freezing starts the reaction. I am thinking of trying a reaction at 3C with 10 or 20%
hydrogen peroxide, and if that is successful we know the barrier at 3C is just low concentration. Then, assuming it is successful I could try the same
at -20C but with a freezing point depressing salt. If it is still successful I would no that the salt had no effect on the reaction. Then I would try
3% at -20C, while using salt or some other inert freezing depressing agent to keep the whole solution liquid. If that reaction failed after the others
were successful I would know that the main reason that freezing helps is that it "removes" water from the reaction and forms higher H2O2
concentrations in situ. If the reaction was successful with a completely liquid, salt protected 3% solution at -20C, that would mean some other factor
was at play, perhaps there is a competing or AP-destroying reaction that happens at warmer temperatures.
[Edited on 6-12-2019 by C6(NO2)5CH2CH(CH3)N(NO2)2]
[Edited on 6-12-2019 by C6(NO2)5CH2CH(CH3)N(NO2)2]
Put that in your pipe and smoke it!
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