Sciencemadness Discussion Board

Diphoronepentaperoxide (DPPP)

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fatkangaroo - 27-1-2005 at 14:47

Well I have playing with the stuff this morning and I can find no major differences between the 3 substances. I was using medicine capsules for containers each one held less than a gram. I only used fuse for ignition. All I can do different now is try to use a small detonater to see if the DPPP will go to hyper speed. :cool: Anyway I have decided to go back to square one and started a new batch.

DPPP appears intermediate between AP and HMTD

Rosco Bodine - 27-1-2005 at 15:02

That's the way it is looking to me so far at 9.5 mm diameter . The density of the stuff is low and that looks like it could be improved by recrystallization . Or perhaps an ideal condition of acidity , temperature and rate of addition during synthesis would favor a more dense crystal product .
Maybe the addition of a solvent to the reaction mixture , or even a coprecipitated product with AP would have a higher density .

I want to give the film can test a try before you nail the coffin

Matsumoto_Hideki - 27-1-2005 at 16:26

I will try the film can test again, this time with my filtered stuff and see if it doesn't punch a hole in 1/2" steel plate.

Don't give up on it, i might actaully have different stuff than you do?? Like I said I have different results.

PainKilla - 27-1-2005 at 16:37

OK, I hate snow. I am in the process of doing the first part of my experiment. 30% H2SO4 (to equal 30% HCl) was added to acetone, one sample will be held at room temperature, another will be heated exactly the way everyone is doing DPPP. Depeding on the results we can have:

DPPP is made from this method, then the DPPP is really some sort of mesitylene or its derative.

DPPP is not made, no other "special" changes. The product is DPPP or chloroacetone derative.

I will also be attempting to peroxidise chloroacetone sometime. Here is the results of the Room temp h2so4/acetone: *(ill be deleting and updating every few hours)*

+ 0 hours: A clear mixture with reddish haze to it.

+ 6 hours: A slightly yellowed but mostly clear mixture. Still smells LIGHTLY of acetone, but it has some aromatic smell to it, but faint. It is going to be kept stoppered through the experiment.

+24 Hours: Yellowish tint, undescrabable smell.

+48 Hours: I am now REALLy sick, but mixture is yellow like on hideki procedure.... and it has this undescibable smell.... MEANING that no phorone! Too bad.... no Cl garbage either. Bascailly its TeAP or mesitylene or derative peroxide.

Please post any suggestions.

BromicAcid - 27-1-2005 at 17:33

Please, can someone titrate to find the % active oxygen? Find a good density measurement, determine an accurate melting point. These should be easy things that should be known with every compound and are easy to do at home.

More advanced would be for someone to get a solid IR of DPPP and compare it to AP, maybe get a UV spec of the precursor solution. On another site Matsumoto said the key was to distill the solution although he hasn't said so here, if it does have a set boiling point it would greatly limit the amount of compounds form which to select for it's identity. This thread keeps going around in circles, all these witness plates and tests, different procedures and such, everything in the last 15 pages of this thread could probably be condensed into two pages, just fill in the blanks:

Density:
Melting Point:
% Active Oxygen:
Solubility:

IF these were found accurately it would be simple to determine if this is AP or not. Books on organic peroxides give examples on how to titrate and determine the peroxo linkages, they even give AP's values, not that you couldn't just measure them yourself. Someone out there can do this.

Rosco Bodine - 27-1-2005 at 18:15

You betcha I can do density , solubility , and a full and complete melting point analysis , which I shall get around to in due course . It's just that all drudge work and no blowing up shit makes Jack a dull boy ....and Rosco too :D

yellow colour has already been explained

Matsumoto_Hideki - 28-1-2005 at 01:00

Painkilla during all of our synth methods the yellow colour is coming from mesityl oxide which is normally clear but in this case the heat and light cause it to change colour. Mesityl oxide is a byproduct of phorone production from HCl on acetone, as in this case and has a camphor like-odor to it. THIS HAS BEEN EXPLAINED ! WE KNOW THIS FOR A FACT!

Doing some searching on TCAP and HMTD and found that AP (TCAP) is quoted as 5300m/s and HMTD as 4311m/s. So why were some of you telling us that HMTD was more powerful than AP? CLEARLY THIS IS WRONG! DPPP then must be AT LEAST detonating around 6-7Km/s then. AP is reported as stronger than HMTD
by Meglomania, ATF and others.

I quote:"it won't matter though and I will seem very repetitive I assure you. The DPPP may be a little stronger than AP but it is not stronger than HMTD"

[Edited on 28-1-2005 by Matsumoto_Hideki]

WaveFront - 28-1-2005 at 03:28

Matsumoto, VoD and brisance are not the same. Read my post before this. Imagine that you mix a fast thing, like AP, and a energetic thing, like aluminized chlorate powder, and you achieve both the energy and VoD of the pentrite. Well, the brisance of this mix wil not be the one of the pentrite, but much lower, because most of the energy comes from the redox reaction between aluminum and oxigen, wich is slow. Since I understand, the best brisance comes from the energy trapped in stressed molecules.
Just compare AP and HMTD and believe what see your eyes.


It is even possible that certain impurities can act as a binder, improving mechanical transmision of the wave, form denser material , as rosco said, or lead to a more stressed cristaline form?

[Edited on 28-1-2005 by WaveFront]

Rosco Bodine - 28-1-2005 at 06:22

There are several factors which have bearing on the performance of a particular explosive , and the velocity numbers really are only one part of the equation which describes what a particular explosive will actually do under a given set of conditions . Low density is a huge problem to be overcome if any bulk strength and brisance equivalency for "DPPP" is to be demonstrated in comparison with other materials which have double the loose pouring density . Nitrostarch suffers the same problem , and the velocity number for nitrostarch under the best condition is higher than for
other materials which are far more effective at doing actual work upon the target material . The velocity number for a particular material is very much irrelevant when there are more pertinent characteristics to be considered for a particular use , like initiating ability , or cutting ability , or heaving ability , one of which characteristic is particularly good makes that material desirable for a particular use , regardless of what the velocity numbers or other measured values may be . The "work value" of what the material actually does is more significant than what any numbers would suggest it is capable of doing .

As for AP versus HMTD , it doesn't matter what the numbers are for velocity , HMTD is a much more dense material in terms of its pouring density , and its self accelleration across a short distance from point of ignition to reach high order detonation and maximum velocity is certainly greater than AP , which makes HMTD a far better initiating explosive than AP , in a size constrained scenario like a detonator capsule . Regardless of the velocity HMTD is also more brisant , probably because of its density . A more dense explosive is likely to have a higher kinetic energy charcteristic about its expanding plasma upon detonation , and it is that quantity which does the actual energy delivery to the target material , and this is a quite different quantity than the velocity figure for the progression of a detonation wave through the material itself . It's sort of like a drag race between two cars where the car winning the race has little to do with which driver can push the gas pedal to the floor the quickest . It's more a whole lot of other factors which determines what happens in the larger scheme of things .

[Edited on 28-1-2005 by Rosco Bodine]

PainKilla - 28-1-2005 at 09:17

Quote:
Originally posted by Matsumoto_Hideki
Painkilla during all of our synth methods the yellow colour is coming from mesityl oxide which is normally clear but in this case the heat and light cause it to change colour. Mesityl oxide is a byproduct of phorone production from HCl on acetone, as in this case and has a camphor like-odor to it. THIS HAS BEEN EXPLAINED ! WE KNOW THIS FOR A FACT!
[Edited on 28-1-2005 by Matsumoto_Hideki]


Where exactly has this been proven...I would like to see some REAL references and none of YOUR "proven" bullshit observations. As far as I see you claim that you know the by products of a obviosuly very complex process while meanwhile you do not know the difference between the brinsance and VoD. Until I see REAL references I am regarding this as new.

+ 0 hours: A clear mixture with reddish haze to it.

+ 6 hours: A slightly yellowed but mostly clear mixture. Still smells LIGHTLY of acetone, but it has some aromatic smell to it, but faint. It is going to be kept stoppered through the experiment.

+24 Hours: Yellowish tint, undescrabable smell.

+48 Hours: I am now REALLy sick, but mixture is yellow like on hideki procedure.... and it has this undescibable smell.... MEANING that no phorone! Too bad.... no Cl garbage either. Bascailly its TeAP or mesitylene or derative peroxide.

+72 Hours: Mixture has almost no acetone smell, undescribable aromatic. Yellow is darknening very very slightly orange, but still a deep deep yellow. The mixture is also more viscous than it was originally.

chemoleo - 28-1-2005 at 09:52

At what temp is this, Painkilla? If it's room temp, be prepared to wait for anohter couple of weeks.
Add some water, and see if you get someinsoluble oil - which should be mesitylene/mesityl oxide. A yellow precipitate, when neutralised, means phorone.
Did you add h2O2 yet?

Bromic, you are right, the peroxide titration can be done. Will look into the references and post this. This should determine how much peroxide there is per gram of AP, HMTD or 'DPPP'.

IMPORTANT ANNOUNCEMENT

PainKilla - 28-1-2005 at 10:05

This is room temperature, in a sealed flask. I will wait 7 days and see what happens. Depending how fast I fnish this essay for school, I may also heat a sample.

I do believe that Methyl Isobutenyl Ketone PEROXIDE is what we are getting here. I finished one of the essays i needed to do and ehated the mixture same way, everything the same but with sulfuric.... well I got the same results. I have yet to peroxidse the product but I think it is important to realize that it is H+ that affects this not Cl-. This means there is no Cl intermediate and therefore unlikely that any phorone is formed.

Well at least we more or less know what this compound is.... the more important thing to know is whether it is worth making over AP or HMTD. As of now we have no REAL conclusive results besides the makeshifted lead block test. I will try and do some test though, I have no camera and will have to do a more accurate test, which will probably take more time. Still, it is a good finding....

Here is also some important notes:

  1. Almost mineral Acid can be used
  2. The acid must be able to have a good ablilty to add H+ to the acetone
  3. The acid is a catalyst basically, the more you use the faster the reaction will go, you can also use little acid and a lot of acetone
  4. Heating is not neccasary but, 1/2 hour heating at 60-70degreees is equal to 1 day of letting same mixture stand at room temperature


I will do soluibity and stuff of the precursor soon. Then the peroxide.

O yea it tastes like shit, like when I get dust from cleaning my cat's litter box in my mouth... and i cant get rid of it its so fucking gross GAH!


[Edited on 28-1-2005 by PainKilla]

[Edited on 28-1-2005 by PainKilla]

NEw results

Matsumoto_Hideki - 28-1-2005 at 15:49

I don't know what this is but I have made something different that is dark green !

150ml of actone were heated with 60ml of HCl @ 31.5%vol

the solution did not change colour until the rest of the 190ml were added, then the solution turned from clear to red then to black-green. any thoughts without flaming. :o

[Edited on 29-1-2005 by Matsumoto_Hideki]

PainKilla - 28-1-2005 at 15:54

I don't think that it matters what color it is. It's just the darkening of the mesityl oxide.

[Edited on 29-1-2005 by PainKilla]

what quote?

Matsumoto_Hideki - 28-1-2005 at 16:07

Mesitylene and Mesityl oxide according that chemsynth site form around phoron, especially during the HCl on acetone reaction.
I beleive this is correct.

Can you prove there is no phorne being produced?


Oh, I think I have a new reaction due to a different colour being produced. It might be signifigant? it might not? don't blow it off.:mad:

[Edited on 29-1-2005 by Matsumoto_Hideki]

PainKilla - 28-1-2005 at 16:11

I am quite puzzled right now, I neutralized one of my mesitylene oxide, and it lost all of its color and turn clear, I got no precipate besides nahso4. How interesting..... nonetheless, because of this i think there is no phorone. I will try freezing this solution.

?What did you use to nutralize it with?

Matsumoto_Hideki - 28-1-2005 at 16:23

What did you nutralize your liquid with?

I am at a loss as to what is happening here.
Some of you are contradicting yourselves with that Dov and overall explosive energy. Why is 9km/sec going to melt through a .75in steel plate, but when AP and HMTD are compaired AP has a higher Dov yet it does less damage, so maybe if this peroxide we are forming is indeed lower energy than HMTD but detonates faster and we have missed this point?

BTW *** How do you explain the micro sized brass dust left from a .233 shell tamped with DPPP vs large twisted metal fragments with TCAP @ 1.6g

PainKilla - 28-1-2005 at 16:31

I used NaHCO3 to neutralize. Regarding your probelm understanding the pwoer....


Brisance is basically how fast an explsoive can gather and realase its under at the max pressure. Or the shattereing effct. It's sort of liek this:

Imagine a propane tank filled with explsoive A and B. Explosive A can build up it pressure really fast and the sudden change in pressure literally shatters apart the metal. This would be like HMTD. Explosive B however, has a low brisance but has a larger VoD. It will basically force the metal to rip apart because of all the pressure thats in there. This is like AP.

Now (dont argue with AP/hmtd just making an example ), while HMTD has a lower VoD, its able to pack more power in its punch I guess. AP final speed is faster, but it releases its enegery slower.

You can almost imagine it as the strong one hit knockout fighter comapred to the weak but really fast fighter.

In other words, it's more dependant on how fast you can release you energy (brisance) than what the maximum speed is.

The thing Im most curios about is its sensitivty.


Quote:

BTW *** How do you explain the micro sized brass dust left from a .233 shell tamped with DPPP vs large twisted metal fragments with TCAP @ 1.6g


AP built up so much pressure it ripped the shell apart like a pressure device. The DPPP relased its enrgy so fast that metal basically shattered itself into little bits of dust, which was helped by the extra output of energy.

[Edited on 29-1-2005 by PainKilla]

Mumbles - 28-1-2005 at 17:41

I get the same result(green-black) when making mesitylene. It is initially the dark red, but on additional standing I get the green. I have a batch that is currently like this. It's easy to see the color when sloshing on the sides of the beaker or pulling the thermometer out. It goes from a dark red layer, to a dark green layer, to a tarish material on top. I don't know what it means either. I assume some polymersation, or something evaporating. Without some very expensive equiptment I don't think we will know for sure.

I am not confirming nor denying the DPPP. I have reason to think it isn't, but I have seen to definate proof in either direction. I think it has been pretty well established that it is acid catalysed, not just HCl. Just making mesitylene will prove this. The colors are exactly the same.

I brought up the topic of a more dilute acid to Pain Killa. That is the only true way to determine if it is acid catalysed or a specific acid is neccesary. 30% Sulfuric acid happens to have the same Normality as HCl. It appears that it is indeed acid catalysed. Since you seem to have the proceedure down very well perhaps you would want to try this and see what results you obtain.

Rosco Bodine - 28-1-2005 at 18:28

Quote:
Originally posted by Matsumoto_Hideki
Some of you are contradicting yourselves with that Dov and overall explosive energy. Why is 9km/sec going to melt through a .75in steel plate, but when AP and HMTD are compaired AP has a higher Dov yet it does less damage, so maybe if this peroxide we are forming is indeed lower energy than HMTD but detonates faster and we have missed this point?
Just for a hypothetical example , suppose we had some ultra high velocity explosive Xenon No-such Pentaperoxide which had a detonation velocity of 30 Km/sec and a density of .01 grams per cubic cm because of the aerogel like crystal lattice structure . How would you suppose the "power" of the hypothetical explosive would compare with PETN ?
Thinking two dimensionally , you would undoubtedly proclaim that the Xenon No-such Pentaperoxide is by far the more powerful explosive since it has more than three times the detonation velocity than PETN ......and you would be absolutely incorrect , because you are not taking into account the other factors besides velocity which apply to determining which material is "more powerful" .
Quote:

BTW *** How do you explain the micro sized brass dust left from a .233 shell tamped with DPPP vs large twisted metal fragments with TCAP @ 1.6g

That is a weight range where the differing plates could be produced by separate firings of the same material , one goes high order and the other doesn't quite get there . Many tests and ignition schemes to rule out this variable would be required for establishing the facts .

I understood this point.

Matsumoto_Hideki - 28-1-2005 at 18:55

Yes but why did you claim that if DPPP detonates at 9km/sec it would drill a hole in .75" steel.? This when you started to confuse me. none the less I still don't undertsand why when I use exactly 1.6g of AP vs DPPP in a .223 rifle shell I get two totally different detonations with totally different energy signatures. the size of the fragmements = power or velocity? Brass penetrating steel pate is idicitive of? as this is what happend in both plate tests.

What about adding Acetone to boiling HCl or the reverse? would this affect the material produced?

[Edited on 29-1-2005 by Matsumoto_Hideki]

Chris The Great - 28-1-2005 at 19:08

Here's what I think about it. Velocity of detonation is not the only thing that effects power, however it is a factor. A high VoD will create a higher brisance, all other factors being equal. However, in the case of AP vs. HMTD, HMTD has a much better OB, hence a higher energy content, as well as a higher density. These allow it to be more brisant than AP.

In this case, although perhaps the DPPP does have a very high VoD, the total energy release would be fairly low as the OB is very poor compared to most other explosives. The low density will also effect the results. Hence something like RDX will be much more powerful due to the higher density as well as the much greater energy content.

Rosco Bodine - 28-1-2005 at 19:12

Matsumoto :

If you understood the point you wouldn't keep saying the same thing and getting the same reply , the legitimacy of which you refuse to accept . You could repeat the test a dozen times , and get one pair of plates showing just the opposite result , or six showing AP and six showing DPPP with better plates . You cannot make accurate conclusions with the variables involved from a single plate test . I don't know what your obsession is about with DPPP , but it definitely impairs your objectivity . This weekend I am going to do the residual peroxide test which will probably show that DPPP is not even actually DPPP , so then what ? Where is the discussion going next if DPPP turns out not to even be DPPP at all ?

[Edited on 29-1-2005 by Rosco Bodine]

Rosco Bodine - 28-1-2005 at 22:52

Okay I never said phorone was a necessary precursor for the formation of a phorone derivative , so what are you going on about ? I have even said flat out several times that I didn't see phorone even being involved in the reactions which may form DPPP , if indeed any DPPP is the actual product . I think we are going to discover that DPPP is not the product , but something else , not necessarily AP , nor DPPP either , but possibly another entirely different organic peroxide , and its detonation rate won't be any 9 Km/sec either , but more like 5.5 to 6 Km/sec .

Phorone made

Matsumoto_Hideki - 29-1-2005 at 00:04

alrighty something strange is going on here, I just did another synth this time Hot 35%HCl to Acetone
550ml HCl to 450ml acetone and an instant reaction took place. Drops of green-yellow phorne started to condense on the upper lid of the pressure canning jar. (all glass) These hardend later into needlike yellow crystals. Phorone if I have ever seen it. Photos will be along shortly.

Chris The Great - 29-1-2005 at 00:21

How hot did you get the HCl? I certainly would hesitate to heat my HCl as it fumes alot already when it's cold....

Can you give more deatils (ie Exactly what you did)?

Even if phorone is formed, keep in mind that it will not form DPPP by being peroxydized.

Atom - 29-1-2005 at 10:43

OMG why do you people keep asking the same question when it's been answered 20 times???? Thats why this thread is so long

YES I KNEW Phorone is a DEAD end

Matsumoto_Hideki - 29-1-2005 at 14:09

HCl was heated to 100c.

Some people are claiming that 1:1 concentrated HCl to acetone does not produce phorone but it is, obviously as there are byproducts being coproduced ie) mesityl oxide.
and mesitylene. I think the problem is that we are not adding enough HCl to get the pentachlorophorone.
Instead we may be geting a trimer or a dimer of Chlorophorone leading to a triperoxide version of the synth? I am very sure that we are not getting a mesityl peroxide..

Mumbles - 29-1-2005 at 14:26

I've said this before over at E&W, and you called me an immoral person, but it is coming true. Evidence is coming out against you, and you refuse to accept it. You keep going on with your stuff and basically ignore the mounting evidence against your compound. I said that you would never want to give it up, because you want this discovery associated with you.

Antisocialite Painkilla

Matsumoto_Hideki - 29-1-2005 at 14:45

Evidence is mounting up against you painfull.

Could you please look at the chemsynth website before posting about the production of mesityl oxide. There is a great BIG synth regarding the action of HCl on acetone. This idicates that mostly phorone and phorone derivatives are in fact the main products instead of mesityl oxide.

DON'T FLAME ME DUDE OR YOU'LL WEAR IT! And don't use the messaging on this page to flame me either!!
]:mad::mad::mad::mad:

[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]

CHEMSYNTH WEBSITE

Matsumoto_Hideki - 29-1-2005 at 15:15

Read what others have posted painfull.
CHEMSYNTH WEBSITE
look up mesityl oxide and you will see the light.
WTF with name calling you immature little shit!

[Edited on 29-1-2005 by Matsumoto_Hideki]:mad::mad::mad::mad::mad::mad::mad::mad:

[Edited on 29-1-2005 by Matsumoto_Hideki]

READ THIS PAINFULL

Matsumoto_Hideki - 29-1-2005 at 15:21

There are two general methods for the preparation of mesityl oxide: the action of condensing agents (hydrochloric acid, etc.) on acetone, 1 and the dehydration of diacetone alcohol. 2 The action of acid condensing agents ]is very unsatisfactory; the yields are poor and considerable quantities of phorone and similar substances are invariably produced.

from "Organic Syntheses, Coll. Vol. 1, p.345; Vol. 1, p.53"

other sources
Fitting, Ann. 110, 32 (1859); Heintz, Ann. 178, 343 (1875); Claisen, Ann. 180, 4 (1875); Freer and Lachmann, Am. Chem. J. 19, 887 (1897); Currie, J. Am. Chem. Soc. 35, 1061 (1913); Couturier and Meunier, Compt. rend. 140, 721 (1905); Mannich and Hâncu, Ber. 41, 574 (1908); Bodroux and Taboury, Bull. soc. chim. (4) 3, 829 (1908); Yllner, Svensk. Kem. Tids. 37, 227 (1925) [C. A. 20, 739 (1926)]; Gasopoulos, Ber. 59, 2188 (1926); Brederick, Lehmann, Schönfeld, and Fritsche, Ber. 72, 1417 (1939).


Heintz, Ann. 178, 351 (1875); Kohn, Monatsh. 34, 779 (1913), Ger. pat. 208,635 [Frdl. 9, 62 (1908–10)]; Kyriakides, J. Am. Chem. Soc. 36, 534 (1914); Hibbert, ibid. 37, 1748 (1915); Hoffman, U. S. pat. 1,474,035 [C. A. 18, 401 (1924)]; Locquin, Ann. chim. (9) 19, 32 (1923).
Hoffman, J. Am. Chem. Soc. 31, 722 (1909); Hertkorn, Ger. pat. 258,057 [Frdl. 11, 46 (1912–14)].



[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]

getting back on track to DPPP

Matsumoto_Hideki - 29-1-2005 at 15:40

Lets get back to planet earth shall we. Chemsyth has stated that phorone comes from HCl on acetone along with mesityl oxide as a MINOR co-product. i am sure we have a phorone peroxide but i also beleive that we need to add more HCl to the solution. I think this is going to lead us to our product.
I really pitty those people who can't read a chemsyth report.:P
BTW speaking of spelling, "foick" should be written fuck. hence in the verb "to fuck" or to be "fuck out of luck" example: painkilla was fuck out of luck when it came to reading.


There are two general methods for the preparation of mesityl oxide: the action of condensing agents (hydrochloric acid, etc.) on acetone, 1 and the dehydration of diacetone alcohol. 2 The action of acid condensing agents ]is very unsatisfactory; the yields are poor and considerable quantities of phorone and similar substances are invariably produced.

from "Organic Syntheses, Coll. Vol. 1, p.345; Vol. 1, p.53"

other sources
Fitting, Ann. 110, 32 (1859); Heintz, Ann. 178, 343 (1875); Claisen, Ann. 180, 4 (1875); Freer and Lachmann, Am. Chem. J. 19, 887 (1897); Currie, J. Am. Chem. Soc. 35, 1061 (1913); Couturier and Meunier, Compt. rend. 140, 721 (1905); Mannich and Hâncu, Ber. 41, 574 (1908); Bodroux and Taboury, Bull. soc. chim. (4) 3, 829 (1908); Yllner, Svensk. Kem. Tids. 37, 227 (1925) [C. A. 20, 739 (1926)]; Gasopoulos, Ber. 59, 2188 (1926); Brederick, Lehmann, Schönfeld, and Fritsche, Ber. 72, 1417 (1939).


Heintz, Ann. 178, 351 (1875); Kohn, Monatsh. 34, 779 (1913), Ger. pat. 208,635 [Frdl. 9, 62 (1908–10)]; Kyriakides, J. Am. Chem. Soc. 36, 534 (1914); Hibbert, ibid. 37, 1748 (1915); Hoffman, U. S. pat. 1,474,035 [C. A. 18, 401 (1924)]; Locquin, Ann. chim. (9) 19, 32 (1923).
Hoffman, J. Am. Chem. Soc. 31, 722 (1909); Hertkorn, Ger. pat. 258,057 [Frdl. 11, 46 (1912–14)].





[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]

Can u prove this?

Matsumoto_Hideki - 29-1-2005 at 15:53

Ahh, but you missed one point in that when the H2O2 is added to the PCP we have chlorine being released from the solution. In all my synths this was the case. I think most people have smelled this during their reaction as well.

[Edited on 29-1-2005 by Matsumoto_Hideki]

Chlorine is destinct as a smell

Matsumoto_Hideki - 29-1-2005 at 16:00

well the gas coming from the reaction, besides smelling like chlorine it also acts like chlorine by making white ammonium chloride fumes apon expose to ammonia vapour. well duh it is chlorine. This chlorine is obviouly being used as it is being ejected when the CP is being peroxidized.

BTW spelling helps to. chlroine is Chlorine :P



[Edited on 30-1-2005 by Matsumoto_Hideki]

Stop this now!

Joeychemist - 29-1-2005 at 16:13

I am sick of this flame war. Hideki shut up!

I try to Ignore him, as should everyone else. you are acting like children rather then a matured adult capable of conducting a civilized factual conversation. This thread and the content have deteriorated due to flaming, bullshit and a complete lack of common sense.

What’s next, will you guys be reverting to primates? Will you then throw feces at each other as well?:mad:

Stop it now!:mad::mad:

I would now ask for a moderator to step in, as this has got to stop. Moderators I’m not telling anyone how to do there job, but you do have a job to do, you agreed to keep the forum in order and protect it from disruptions and flame wars. Please, please discipline and order are needed.
:(;)



[Edited on 30-1-2005 by Joeychemist]

vulture - 29-1-2005 at 16:28

I've warned you guys, about 10 pages back I guess, about nutcases like Hideki. But who would listen?

This is what you get for allowing idiots to roam around freely.

This moron is even rude enough to send me reports about other people flaming him, go figure.

I hope you've all learned your lesson.

Hideki has been BANNED.

residual peroxide experiment crystallizing now

Rosco Bodine - 29-1-2005 at 16:34

Earlier today I repeated my synthesis using the method which before produced a nearly quantitative yield of 98 grams of alleged DPPP from a precursor made from 100 ml acetone . And three hours later ,
after the formation of the alleged DPPP , I added 100 ml acetone gradually which caused to temperature to rise again from the - 2 C to 10 C , indication some further reaction is occurring with what is believed to be unreacted peroxide from the DPPP reaction . The ice bath has been refilled and the stirring continued and the batch has been running now for 5 hours since the beginning . The mixture will be allowed to stir at least another 4 hours and then will be left to stand overnight in the melting ice . In a couple of days , perhaps three , I should have a dry weight for the product of this reaction .
The weight of this supposedly "mixed product" derived from a total of 200 ml acetone and 280 ml 27% H2O2 should provide some useful information . Because the peroxide should have been depleted in reaction with the 100 ml of acetone in the precursor if DPPP was produced , and the total theoretical yield possible for that 100 ml acetone converted completely to DPPP would be about 98.5 grams of DPPP . Adding a second 100 ml portion of acetone to the
"spent" DPPP reaction mixture should therefore not result in much of an increase in the weight of any "mixed product" of AP with mostly DPPP already produced , *if* the first product actually was DPPP . If I end up with some much greater amount than 100 grams or so of dried product from the acetone treated "spent DPPP reaction mixture" . then the entire theory for the supposed chlorination route to DPPP is in some serious trouble because of the stoichiometric impossibility presented by
unreacted residual peroxide sufficient for forming an added amount of ordinary AP from the mixture where the peroxide should have been already spent .

PainKilla - 29-1-2005 at 16:44

I thought the theory with chlorination has been disproved already? Will someone neutralize thier mixture because I am getting some interesting results (i mean nuetralize the precursor mxiture the dark red one)

Rosco Bodine - 29-1-2005 at 17:14

Quote:
Originally posted by PainKilla
I thought the theory with chlorination has been disproved already?
Nope the chlorination theory has not been disproven before , but my residual peroxide experiment has the ability to do just that , and more . That is precisely why I am doing the residual peroxide experiment , it is good information provider .
Quote:
Will someone neutralize thier mixture because I am getting some interesting results (i mean nuetralize the precursor mxiture the dark red one)
This was already done in the early part of the thread , and repeated later . I do not see what pertinent information is revealed , or what is the purpose for neutralizing the precursor . I can however see what is the relevance of unreacted peroxide in a "DPPP" spent reaction mixture , when that unreacted peroxide shouldn't be there .

PainKilla - 29-1-2005 at 17:15

If I made something using H2SO4 then no Cl is nessacary, therefore disproven....

[Edited on 30-1-2005 by PainKilla]

Rosco Bodine - 29-1-2005 at 17:29

Quote:
Originally posted by PainKilla
If I made something using H2SO4 then no Cl is nessacary, therefore disproven....
Wouldn't you need to know what the "something" you made actually is , or at least if it is exactly the same product as produced using HCl , having the same consumption of H2O2 involved in the formation of your "something" , in order to conclude that chlorination is disproven ?

PainKilla - 29-1-2005 at 17:37

I did everything the same as the HCl method jsut replaced the acids.... It wil be filtered soon but everything looks *exactly* the same.

Joeychemist - 29-1-2005 at 17:54

Painkilla, as I tried to explain to you over U2U, physical properties are not the same as chemical properties, therefore you can not possibly claim that it is or isn't the same reaction occurring as you have not even collected or tested the precipitate. ;)

Rosco Bodine - 29-1-2005 at 18:04

Interesting , but it really doesn't prove anything so far except that you get a product which looks the same by substituting sulfuric acid for hydrochloric acid . Do you follow what I'm saying ? It is not a useless experiment . However, it doesn't get at the *heart* of the patents described course of reaction for DPPP by way of chlorinated intermediates , the chlorine for which is provided by the consumption of hydrogen peroxide in reaction with HCl . The level of H2O2 in the spent DPPP reaction mixture is therefore a critical evidence for or against the patents claim for the course of formation of the DPPP . If the residual levels of H2O2 in the spent DPPP reaction mixture do not reconcile with the amount of alleged DPPP product obtained , then the course for the reaction is different or the product is not DPPP , because the numbers don't add up . And in chemistry the numbers have to add up .

I Hate you murphy, hate you so much....

Chris The Great - 29-1-2005 at 21:23

Ok, well, I have a few days off school as finals are over for me, but not for others, so no school until next thursday. So, I figured I try to do some experimentation myself.

First, I decided that I will try several routes to the precursor, using different acids; hydrochloric, sulfuric and sodium bisulfate. I would then try to see if the same product was formed by testing each produced peroxide extensivly to either prove or disprove PainKilla's theory.

So, I got out some jars, cleared my very messy lab, and starting working. First, I measured out ~115mL acetone into each jar.
Then, 105mL 32% HCl was added to the jar with the plastic lid (plastic won't be attacked by the HCl fumes). It heated up and maintained a nice warm temp. I set it aside and measure out some 97% sulfuric acid (60mL) and 300 grams of solid toilet bowl cleaner (40% sodium bisulfate....work with what you have :P ).

http://img199.exs.cx/my.php?loc=img199&image=0016sk.jpg

I figure I can afford to lose some of my hard to get sulfuric as it's going to help us understand this mystery....so I thought :mad:

Well, this is about where things got really really bad and murphies law basically....pissed me off.

I slowly poured the sulfuric acid into the acetone to be greeted by the acetone exploding out of the jar in a blast of acetone vapour, somewhat like pouring hot acid onto a carbonate. I rushed to clean the acid/acetone of my hand and digital camera, and succeeded somewhat, although I had to pour water all over my hand as it had started to burn.

The mix, after reacting for 20 seconds had turned a nice, deep ruby red and was boiling quite nicely.

http://img199.exs.cx/my.php?loc=img199&image=0026sx.jpg

Well, that was nice, except another 20 seconds later it was deep black and still boiling.

http://img199.exs.cx/my.php?loc=img199&image=0036kv.jpg

Time to clean this up and cap this. So, I put on my rubber gloves and.....spilled the shit all over my bench! The jar was slippery as hell because of all the acetone!

http://img199.exs.cx/my.php?loc=img199&image=0046mo.jpg

This is where my messyness worked against me. Usually I will clean my bench up very good if I'm going to do somethign dangerous, but this was supposed to be a slow reaction that requires hours to complete with heating!
The stuff was horrible to clean up, it got everywhere. I stuffed paper towels underneath the crack between the thick boards that made my table, to keep it from puddling on my microwave, and spent 15 minutes cleaning this stuff up. About this time the reaction had finished, and it smelt AWEFUL. Bad enough I felt sick. But I had to keep cleaning.

I then decided to put the jar outside since it was really smelling bad and white fumes where coming off it. I spilled it again, this time it was really thick and foamy. AAUUGGHH. This spill was smaller though, since it was thicker. But it smelt HORRIBLE.

The next 20 minutes involved me taking all the stuff out from under my bench, wiping tons of this stuff off it, feeling sick to the stomach and getting really mad as the experiment was ruined.

In the end, I got a nicely stained workbench. Someday this thing is just going to explode from all the built up chemicals in it.

http://img199.exs.cx/my.php?loc=img199&image=0058yr.jpg

I left the pile of toilet cleaner next to it to help counter the horrible smell.

I'll try the stuff again tommorrow, and maybe do the sulfuric acid reaction again in a big jar so it doesn't boil over and make a video of it....it WAS pretty cool except for it getting everywhere and making me feel sick....

Sorry for ranting here, but hopefully someone can learn from my really bad luck.

EDIT: Heh, I just noticed that the 4th picture kinda looks like blood sprayed out of my face all over my experiment :P

[Edited on 30-1-2005 by Chris The Great]

Del Rocco - 29-1-2005 at 23:46

Please pardon me, guys. I have been reading through this thread for some time trying to make heads or tails of it, but I must thank the person who made it now able to be read from Matsumoto's last post on out. Though I offer no valuable contribution to this thread, I must say this:

Thank you, Vulture, for putting a stop to Matsumoto/Mr. Anfo/whatever he will be next week. I mostly frequent the E+W Forum due to their compatablity with weapons (which I am more prolific with), but I do many times enjoy your forum here, though, and am glad to see "Mr. Asian Polymorph" go bye bye. He has insistantly spewed his falsities at E+W with posts about how HIS DPPP detonates at 9000 mps (regardless of actual proof) in more than one thread. I'd be willing to bet he's not roomies with J-Scan other than in his head (or pants, your guess).

Mumbles was right. But now that Matsumoto is banned here we have to hear his insistance moreso over there, I speculate.

If I might be so bold as to offer a bit of advice: If it's possible to do an IP ban on Mr. Matsumoto, do it now, and be done with the whole bunch of personas in his head. Rogue Science will sick of him soon and do the same.

There is no LAN. They are all one and the same.

I'll retire to my place in the shadows to learn, now. (AHEM, who do I return the soapbox to?).

Obersturmführer - 30-1-2005 at 07:48

I have read this entire topic, over and over. I have also talked to people here in sweden, I have read other pages too. DPPP is almost sulphur coloured fine powder. I have tried to make it. First time i got white powder, 2nd time grey, and the final time skin coloured. What am I doing wrong? My powder is finer than AP and has another colour, but it smells like AP and has the wrong colour. Has anyone here made it and succead? And if, could he/she pleas explain exactly how?

P.S. Excuse my bad english, hope you at least understand what I mean .

[Edited on 30-1-2005 by Obersturmführer]

"mixed" product from residual peroxide experiment

Rosco Bodine - 30-1-2005 at 09:24

The product obtained from my experiment has been filtered and is drying . Of course I will have no actual weight until the product has finished drying , but from the volume of the crystals it is plainly evident there is a massive increase in the "mixed product" obtained by adding a second portion of acetone to the supposedly "spent" DPPP reaction mixture . As a strictly visual estimate there appears to be at least a 50% increase in the product and perhaps a 75% increase or even more . I can't tell for sure how much until the productt is dried . But just from what I am seeing as a result from this experiment , the entire matter of the DPPP as a composition of matter obtained by the route specified by the Mackowiak patent is in serious doubt because of the evidence of unreacted peroxide in the DPPP reaction mixture , in
an amount that makes the reaction scheme specified by Mackowiak *impossible* . The dry weight of the "mixed product" will likely shed some further light upon what is the probable material which we have alleged is DPPP .
At this point it would surprise me none at all if the supposed "DPPP" turns out to be nothing more complicated than a variant of AP , or something very close to AP , if not indeed simply AP which has been "tinted" slightly by some polymerized acetone impurity . Can everyone almost hear Axt chuckling at this point , saying uh huh I told you so ?

PainKilla - 30-1-2005 at 09:50

Lol, that is what I said too, but nooone lsitens. I am going to filter out my stuff later today hopefully. Also of interest is this:

Acetone with NaOH, makes the same yellow color!

Puzzling eh?

Look on the bright side , good information obtained

Rosco Bodine - 30-1-2005 at 10:06

Serendipity has its worth in experimentation . One thing I did learn from my experiments is how to get AP to initiate picric acid in an unreenforced detonator , use a generous amount in a larger diameter than usual , and kick it good at the start with a ball of AP putty .
That's a piece of information worth knowing that I didn't know before , and haven't seen it mentioned anywhere else either . There's so much bullshit been published both in print and on the web ,
about all sorts of energetic materials . I love it when an experiment develops a piece of *good information* tried and true , which can be added to my own *no bullshit* files regarding such things as have been confirmed by my own experiments and then known for damn sure from direct observation and direct personal experience . Nothing quite like a good eyewitness report for your own convincing , when the eyewitness is yourself :D

Volunteers wanted

vulture - 30-1-2005 at 12:28

Painkilla made a good suggestion of summarizing this topic to get rid of all bloated speculation, but unfortunately I don't have much time on my hands right now, so therefore I'm asking if there are a few members who'd like to condense this into a new thread.

Sounds like a job for 9 KM/sec No-such Pentaperoxide Man , no , ....wait a minute ... he got banned .

Rosco Bodine - 30-1-2005 at 13:06

The printable text only word file for this thread is 256 pages long and is 1.4 MB ,
converted to pdf is not much smaller .
Please give everybody a chance to archive the complete thread before it gets edited or locked or whatever else fate is contemplated for it . There are still a few test results like density and melting point to do , but that could be added later .

chemoleo - 30-1-2005 at 13:13

I was thinking of removing needless unrelated/flaming/arguing posts to reduce the amount of gibberish in this thread.
But a good summary, with the experiments attempted, and the respective results, might be a wise idea. For instance, right in the beginning of this thread, Brainfever tried this very method of heating acetone/HCl, and claimed that the product seemed like AP. There is a lot of redundancy here.

But please no random speculations such as 'THIS IS mesityl oxide', 'this is mesitylene' if the only evidence is its aromatic smell or whatever.
There are way too many chemistry -related claims in here, with little experimental confirmation other than theories...

Rosco don't worry, the essence of this thread won't be changed. That wouldn't be in anyone's interest.

[Edited on 30-1-2005 by chemoleo]

PainKilla - 30-1-2005 at 13:33

I am gonna filter out my "DPPP" soon. I think giving it a new name would be approtiate also. I am positive no phorone is involved. The reacion procedes seemingly with NaOH and any strong acid. I will test crystals and if this is true, then no phorone is used. Therefore, IMKP I think it sould be called (isobutenyl methyl ketone peroxide, to alliveiate peopel thinking its methyll iso butyl ketone) While I have no direct evidence that it is this, its obviosuly not phorone nor is there proof anywhere that phorone is ever made....


Or it can simply be TeAP, sicne it could be this too.

In a very real sense this thread is a " Classic "

Rosco Bodine - 30-1-2005 at 13:39

It may serve a useful purpose to just leave the thread as it is , because it shows the contrast between scientific method and tests designed to develop pertinent data versus intuition and anecdotal but non-conclusive approaches ,
applied to the task of learning an unknown by experiments intended to reveal what is secret . Reading through the thread , there are portraits of various persons struggle with methods and tools for investigation , verification or dismissal of a set of reactions descrbed by an obscure patent . The result is an "epic" work , which is sort of
the "War and Peace" of organic peroxide threads :D

PainKilla - 30-1-2005 at 13:42

Yes, I agree, but I do think we should at least make some sort of new thread or maybe a document with the info. I can happily do this. Just let me finish my experiments with H2SO4. I have a strong feeling this is TeAP or IMKP. IDK, I think we should see what all my acetone condesntation experiments work out to be. So far we have these agents that do something:

H2SO4
HCl
NaOH (presumably KOH, BaOH etc if its not too strong)
any other acid

I think we should try using salts and see what happens.

Rosco Bodine - 30-1-2005 at 13:52

I keep reading your posts but you aren't making it clear what is the purpose of your experiments , or how the results of your experiments tend to support or otherwise have bearing on what you are trying to prove or discover . There are "shoot in the dark" sorts of experiments , and then there are very focused sorts of experiments which serve to reveal one very specific piece of information . It is difficult to know where you are going with your experiments unless you are very specific what is your purpose and how the particular experiment is relevant .

[Edited on 30-1-2005 by Rosco Bodine]

PainKilla - 30-1-2005 at 13:59

I am trying to see what effect other chemicals ahve on acetone, like H2SO4 vs HCl. I am trying to see whether it is HCl that causes that peroxidisation or no. Obviosuly, this is not the case. Now that I know no phorone is made (sicne Cl is not used, and also no solid precipate etc) I am trying to see what will turn acetone into this yellow stuff. Obviously, H2SO4 has been used to make mesitylene/oxide so I think it could be a derative of it. If NaOH, works then I shall try and find literate on what NaOH condesnes acetone to. This will give us insight on what to call this.

I care more about what this is than how powerful it is. Properties of the prodcut don't interest me unless its a lot less senstive than AP, which will most likely remain my choice primary since it's so easy.

If we can figure out the precursor, then we can figure out the name molecule, OB etc. it will make much more useful things. Since any mineral acid works seemignly, then I think I shall try bases too, just for the hell of it. Obviosuly, this has similair results too. If I can peroxidise the NaOH'd acetone then almsot defiently no phorone is made.

Rosco Bodine - 30-1-2005 at 14:12

It is already known that acetone reacts with NaOH to produce triacetone dialcohol , particularly at cold temperatures . A patent was posted describing this many pages back in this thread . As for the mesityl peroxide angle , why do all those speculative experiments when a good yield of whatever is the "unknown product" has been obtained by an HCl process whose quantities have already been carefully worked out ? The present yield of whatever unknown energetic material we have is a mixture so filled with crystals as to be impossible to stir . The reaction mixture sets up like ice cream , a semisolid sludge of crystals . Are you investigating a new compound or simply looking at alternative methods for what is probably the same compound , and very likely is trimeric acetone peroxide ?

PainKilla - 30-1-2005 at 14:15

Well, I got no small amount of crystals etiehr, I have maybe 2mm of liquid and the rest is a slur of crystals that IS hard to stir actually. The yeilds with H2SO4 are jsut as good. I am just trying to see what precursor forms peroxides. The more choices we have common with many chemicals the more liekly it will be that. If the NaOH stuff can be peroxidsed and we have soemthign in common with all of them then it will be that. I think this is jsut TeAP, not trimeric. Or IMKP.



[Edited on 30-1-2005 by PainKilla]

Just another shot in the dark...but

Mickhael - 30-1-2005 at 14:40

Just to make mention of it, I took the several week old mixture of black fluid (supposedly phorone but now who knows what...)

100ml of that ^
100ml MEK 99%
50ml HCl 31.5%
350ml H2O2 35%

Drip added the H2O2 and have now left it stirring in a -15c freezer for getting close to 24 hours now. The results will be posted below...I hope this isn't too useless to tell, I'm hoping to see whether it ends up as all liquid peroxide possibly = MEKPAP

PainKilla - 30-1-2005 at 14:55

Actuallly that is intersting, I would like to see what happens with ketones in general because perhaps in the end most simple ketones form this same black goop that cna be peroxidised.




[Edited on 31-1-2005 by PainKilla]

Chris The Great - 30-1-2005 at 15:55

Hmmm, since I have a big stack of the thread in paper form sitting on my desk that I am reading through, I'll also help sum up the thread.

I think a summary thread, seperate from this one could be made, where the results and findings of everyone can be summed up, ignoring all anectodal evidence (well, not ignoring but presenting it as "so and so found that DPPP did such under such non-controlled situations";). It probably wouldn't be too hard to reduce the entire thread to two pages (although Rosco insists on having such big, long descriptive scientific posts! Why must he make things hard! )

Painkilla, I'll contact you over AIM, since we are kinda doing to same type of experiments with acetone + acid (though you don't seem to have you'r boil over and spill all over), and make sure we don't both sum up the same parts of the thread.

Now, some thoughts on me accident with sulfuric acid. I hypothesize (I do not conclude, I'm making educated guesses) that it reacted too quickly because I had as many moles H2SO4 as there should normally be HCl, thus twice as many H+ ions. I may go slower (realative to that) with maybe a quarter the amount, and end where it should (nice red colour). I say a quarter as HCl can keep reacting to far as well, so perhaps less could be used with sulfuric acid, the much faster reaction time being able to make up for the less acid used. More tests, of course.
The reaction occured in anhydrous conditions, and reacted extremely fast, so perhaps the water slows down the reaction rate. Perhaps another test can be conducted using a drying agent to pull water out of the reaction. I'll try to test this later today.

I think that regardless if this produces can explosive, it is still useful knowledge. We can learn what to be avoided in making DPPP, try to figure out exactly WHAT is going on in the reaction, since we really don;t know for sure, and we might even stumble completely accidently onto a better way (unlikely however).

Also, just thought I'd point out that methyl nitrate has a very low density (1.2) but still detonates over 8000m/s. I mean, it's highly unlikely DPPP does this, but density doesn't always determine VoD. I mean, I don't think DPPP is anywhere near what it's claimed to be, but I thought I'd mention this.

Rosco Bodine - 30-1-2005 at 16:41

Quote:
Originally posted by Chris The Great
Hmmm, since I have a big stack of the thread in paper form sitting on my desk that I am reading through, I'll also help sum up the thread.
The whole thread converted to pdf is a whole lot easier to navigate . I could upload the
pdf version of the thread if anybody wants it .
Quote:

I think a summary thread, seperate from this one could be made, where the results and findings of everyone can be summed up, ignoring all anectodal evidence (well, not ignoring but presenting it as "so and so found that DPPP did such under such non-controlled situations";). It probably wouldn't be too hard to reduce the entire thread to two pages
*TWO PAGES* ??? You gotta be kidding .
Quote:
(although Rosco insists on having such big, long descriptive scientific posts! Why must he make things hard! )
Hard ? How about thorough , attentive to detail in a realm of things where details are important . There has to be a certain formality about the descriptions of experiments for clarity , and I plead guilty to being long on details so if it takes a page to describe a process , then there aren't needed ten more pages of questions from other people about precisely what I did and why .
Quote:

Now, some thoughts on me accident with sulfuric acid. I hypothesize (I do not conclude, I'm making educated guesses) that it reacted too quickly because I had as many moles H2SO4 as there should normally be HCl, thus twice as many H+ ions. I may go slower (realative to that) with maybe a quarter the amount, and end where it should (nice red colour). I say a quarter as HCl can keep reacting to far as well, so perhaps less could be used with sulfuric acid, the much faster reaction time being able to make up for the less acid used. More tests, of course.
The reaction occured in anhydrous conditions, and reacted extremely fast, so perhaps the water slows down the reaction rate. Perhaps another test can be conducted using a drying agent to pull water out of the reaction. I'll try to test this later today.
Never just dump together reactants for experiments where you are unprepared for boilovers or explosions from a reaction which is unfamiliar . It is good practice to go little by little with additions and have a thermometer or otherwise watch for unexpected exotherms , evolution of gases , or explosion hazard . Small quantity test reactions on a small scale are a good precaution since the magnitude of any surprise is also on a reduced scale .
Quote:

I think that regardless if this produces can explosive, it is still useful knowledge. We can learn what to be avoided in making DPPP, try to figure out exactly WHAT is going on in the reaction, since we really don;t know for sure, and we might even stumble completely accidently onto a better way (unlikely however).
This is still an interesting thread , and an organic peroxide energetic material is produced in good yield , whatever it may turn out to be . Acetone is converted entirely to acetone dialcohol by refluxing through a Soxhlet apparatus whose thimble is filled with barium hydroxide . It would be an interesting experiment to see what product may result from peroxidation of acetone dialcohol , and if that product might be trimeric acetone peroxide , obtained by rearrangement during peroxidation of the acetone dimer . Something similar may be occuring from the precursor made from acetone and HCl , which simply acts in peroxidation as an acetone contributor , substituted for ordinary acetone and reacting the same as if it were ordinary acetone to form the same end product .

PainKilla - 30-1-2005 at 17:14

I filtered my H2So4 stuff, It looks exactly the same as every describes. I got a good 30-40g estmating, dry. It smells like AP, but not as pleasent. I will weigh it out ocne it dries and test it out.

Which book has the procedure for TeAP. I think it's urbanski, but I am not sure. I know it uses H2SO4. I can't recall the procedure though.

I started off using 70ml of the dark red mixture. I added 100ml of H2O2 30%. I am also peroxidsing the left overs, just in case.

More interesting results, the mixture left over from the IMKP or AP, was the light color mixture that didn't peroxidise! I think then that it is that final thing that NaOH seems to make also, that is the thing being peroxidised. This Polymer? probably breaks up with the addition of H2O2, and forms peroxide bonds. This is MOST likely TeAP! In fact, now that I think about it this IS TeAP. Urbanski had some properties of it and it would be wise to compare them.

EDIT: Ah damn it wasn't tetrameric it was tri, and it was in Koehller. I do think it is some sort of polymeric peroxide. (like teap or pentaAP or something who knows)

[Edited on 31-1-2005 by PainKilla]



GOOD GOD, I HAVE SEEN THAT PAPER. I KNOW. STOP saying like I dont know what TeAP is. I am still saying it is possible. Not as much anymore. I think its probably a ketone polymerization peroxide.

I don't know why it cant be and why everyone is so stubborn to suggestions.

[Edited on 31-1-2005 by PainKilla]

Rosco Bodine - 30-1-2005 at 18:26

Quote:
Originally posted by PainKilla
Which book has the procedure for TeAP. I think it's urbanski, but I am not sure. I know it uses H2SO4. I can't recall the procedure though.
It's a journal article . Japanese IIRC . The catalyst is tin chloride , not sulfuric aicd . In fact the presence of mineral acid prevents the formation of tetrameric AP and results only in trimeric AP being formed as the product .
Quote:

More interesting results, the mixture left over from the IMKP or AP, was the light color mixture that didn't peroxidise! I think then that it is that final thing that NaOH seems to make also, that is the thing being peroxidised. This Polymer? probably breaks up with the addition of H2O2, and forms peroxide bonds. This is MOST likely TeAP! In fact, now that I think about it this IS TeAP. Urbanski had some properties of it and it would be wise to compare them.

No , sorry the product is not tetrameric AP , no way , no how , not even maybe . If tetrameric AP was even discovered at the time of the last Urbanski publication , it would be news to me .

Chris The Great - 30-1-2005 at 18:34

Quote:
*TWO PAGES* ??? You gotta be kidding .

Well, as a thread, not as actual paper! By comparison this thread is on it's 31st page, so 2 is a substantial improvement. Of course, the total length will still be long but at least it will be nice and easy to navigate.
Quote:
Hard ? How about thorough , attentive to detail in a realm of things where details are important . There has to be a certain formality about the descriptions of experiments for clarity , and I plead guilty to being long on details so if it takes a page to describe a process , then there aren't needed ten more pages of questions from other people about precisely what I did and why .

I meant that as a joke, it's great to have such detail that you provide. The more detail that is provided the happier I am. I love reading about an experiment that has very detailed observations compared to more general ones.
Quote:
Never just dump together reactants for experiments where you are unprepared for boilovers or explosions from a reaction which is unfamiliar . It is good practice to go little by little with additions and have a thermometer or otherwise watch for unexpected exotherms , evolution of gases , or explosion hazard . Small quantity test reactions on a small scale are a good precaution since the magnitude of any surprise is also on a reduced scale .


Yes, that is much better laboratory practice. I'm kinda lucky that I learn all these things that hard way with fairly benign reactions.

The_Davster - 30-1-2005 at 20:41

For PainKilla's sake, I have attached the TeCAP file. There is no way "DPPP" and TeCAP are the same.

I also find Rosco's in depth write ups very beneficial. They are also better than such "writeups" by Hideki that are a few sentences, but prompt dozens more posts acking for clarification.

[Edited on 31-1-2005 by rogue chemist]

Attachment: TetramericAcetonePeroxide.pdf (95kB)
This file has been downloaded 1503 times

Here's another file of interest

Rosco Bodine - 30-1-2005 at 21:17

There are some interesting pieces of information regarding solublility in various
solvents , ect. in the attached file .

Attachment: TATP.pdf (139kB)
This file has been downloaded 4771 times

Chris The Great - 30-1-2005 at 23:05

Well, more experimentation, this time without catastrophic failure :)

Earlier today I added the 300g toilet bowl cleaner (40% NaHSO4) to 115mL Acetone, which is kinda like slush now. The colour changed in about 6 hours to a very light yellow, signifying it is reacting slowly. The NaHSO4 picked up a lot of water however, and was very moist, so this may be slowing down the reaction.

My mixture of 105mL 32% HCl and 115mL acetone had turned yellow in the 24 hours it had been sitting, at a temperature of approximatly 10 degrees.

My remaining sulfuric acid/acetone (115mL acetone, 55mL H2SO4) had turned a black colour with a very think black oil floating on the top after sitting outside in occasional light rain for 24 hours. I added water to the mix and it formed a orange, opaque colour, the oil floating to the surface. The stuff is very thick and sticks to glass very well, it took some time to clean out the jar it had been sitting in (it has a lid that fits, and so I needed it for the next experiment). The oil formed a grey colour when being rinsed out with water, similar to the opaque orange formed from the liquid and water. It seemed to have solid gunk in it too, this was removed with methanol and acetone.

Next, I measured out 55mL of acetone and put that into the jar, then added 14.5mL of 97% H2SO4 over a peroid of about 30 seconds using a syringe. The acetone did not boil at all this time. I rapidly screwed on a metal cap to prevent the acetone from evaporating away from the reaction. The liquid had turned the colour of my HCl mix at this point. The mixture heated up very rapidly, but did not boil. The colour deepened to a deep red after a minute, and acetone was condensing and running down back into the mix very rapidly. After two minutes the colour was deep enough that it could not be seen to be red without a strong light source.
The mixture kept 'refluxing' for about ten minutes before acetone stopped noticably condensing. The jar felt very hot to the touch. The colour at this point was even darker than before.
After 15 minutes the mix was hot, but not hot enough to be uncomfortable, perhaps about 40 degrees on the outside. I think this is where the reaction was done, as the temperature had fallen very rapidly in the last 5 minutes. After 30 minutes the temperature was about room temperature on the outside. It was very dark at this point, it needed to be swirled so the mixture would run down the sides in order to see the red colour with a bright light. No seperate layer was formed, it seems to be a single liquid, though this may change. When only traces of the liquid remains on the side after swirling it seems to be more of an orange colour although this may be because there is just a trace of it left when it looks orange.
The smell is very strong and unpleasant, although not irritating to me. I opened the jar and smelt the vapour, there was no trace of acetone at all, so the reaction is complete. Because the smell was very strong it was seeping out from the metal seal (it's not perfectly airtight it seems) and it needed to be sealed with electricians tape as it is now in my room.

Holy shit!

Joeychemist - 31-1-2005 at 00:41

I got exactly the same results as you Chris when the H2SO4 was added to the acetone, a very thick viscous solution results, (thick like cold glycerin). The temperature difference is also definitely greater than that of the HCl/acetone.When I added water to clean out the beaker received two layers.

I added 5 drops of 35% H2O2 the H2SO4/acetone precursor while stirring and received instant boiling and ebullition which consequently produced a lot grey and white smoke and it splashed the precursor all over the place. I then allowed the precursor to cool down while I cleaned up. I the began to introduce the H2O2 drop wise very slowly while stirring vigorously, the temperature continued to rise at an astonishing rate even after adding only a few drops. I was going to water the precursor down and continue but I decided to forget about it, and dumped it out.:mad:

I don’t recommend adding high% H2O2 to this solution, whatever it is as it seems kind of dangerous. Any way others are welcome to try but be warned and take cautions.

Chris The Great - 31-1-2005 at 01:03

Hmm, perhaps the solution can be diluted by adding it to a small amount of water before adding the H2O2. According to Painkilla, he still had a large amount of acid present after the polmerization (using 25% H2SO4) and so a large amount of the heat could be from H2SO4 sucking up water.

latest results....

Mickhael - 31-1-2005 at 02:22

20 hours of being stirred in the -15c freezer, has left a slightly milky looking yellowish liquid, with several large globes of dark red liquid sitting on the bottom of the container. And there seems to be a very thin layer of another clearer liquid on the surface. No crystals of any kind to be seen, unless they are extremely fine suspended within the liquid, there are also various small globes of clearish liquid hanging in the main mass of milky yellowish liquid.

32 hours after synth (left at 18c for 12 hours) Dark red globes on the bottom of the container have now risen to the surface and for a very pale red upper layer, seemingly mixed with a yellow clearish layer just above it, yellow milky liquid still remains as 90% of the total liquid, small bubbles noted to be rising from the bottom, no other layers noted besides the 3: Estimated %

| |
| Pale, clearish layer ^ 4% |
| |
| Light red layer ^ 6% |
| |
| |
| |
| |
| |
| |
| |
| Yellow milky layer 90% ^ |



Small plastic dipstick was inserted into the top layer and the 2 drops roughly, that cling to it where lit with a lighter…it instantly deflagrated in a 5 inch fireball…absorbed and contained firing tests to come soon.

Any thoughts on what I’ve made, and how I should try to separate it? I have no plans on neutralizing the batch until I know more, for fear of destroying needed research liquid.

Quince - 31-1-2005 at 02:42

Greetings everyone, new guy here. I've been lurking around this thread for a while, and finally decided to register.

I became interested in acetone peroxide because I can't find any OTC nitric acid, which seems to be necessary for most explosives, and I'm only interested in small amounts anyway.

It's not clear from this thread (which I did read in full) whether the faux-DPPP really has any more power than AP.

I also want to ask about peroxide strength. The only thing I've found here (Vancouver, Canada) is 3% peroxide. Is it at all possible to use this in the procedures that Rosco made, just increasing the volume? Or does the concentration maybe dilute the acid too much or something?

I tried making regular AP by chilling all chemicals in the freezer then mixing them in the usual AP order, and letting it sit in the fridge. Out of 40 mL total liquid (using this weak peroxide) I got 1/8 tsp translucent crystals floating at the liquid surface, and it took two days in the fridge. I pressed that in a bit of aluminum foil, hit it with a hammer and -- nothing. Putting it over a gas flame, however, did the trick -- large flash and the aluminum foil was in pieces.

As I was reading this thread, I got excited at the prospect of something I could also make with things easy to obtain, but more powerful. You can imagine the disappointment. But I may still try, even if there's only a small increase in power. So, can I use the weak peroxide, or if not, I hope someone from BC can suggest a source of a stronger one.

Thanks.

PS Does anyone know if it is possible to have the email notification be on for all my replies by default? I've seen such an option in most other forums, but I can't seem to find it in the Control Panel here.

[EDIT] Has anyone tried reversing the order of mixing for other peroxides, such as MEKP (i.e. ketone and acid first)?

[Edited on 31-1-2005 by Quince]

PainKilla - 31-1-2005 at 05:17

Joeychemist: You need to dilute the acid before starting anything unless you want an accident like Chris. I am sure you can add the acid but it would need to be done very slowly, and you WILL experiance the heat of it sucking the water when you add H2O2. This may not be a bad thing though.

Mikael, so let me get this stright did you or did you not get a product from what you were making?

I think it was Rosco who mentioned that this was an intermidiate between HMTD and AP. I agree with this, but I am not sure yet what it is. I have a feeling we shall know soon... :D

----------How very interesting. I am came up with this during my bio midterm. It seems right, and even more right since it is known that acetone can turn into isopropanol. Please don't flame me I am still learning organic chemistry and this is an educated guess. it could still be just AP. But I am doubtful.

The acetone first polymerizaes, forming an alcohol, then continues to do so, until the H2O2 is introduced. The OH then forms a peroxide bond. I will try doing the same procedure, substituing the acetone for isopropanol. Hmm.... Even more interestingly is that isopropanol is now used to make acetone, so it is possible that we are getting a mix of this alcohol polymer, various oxides and mesitylene. It also seems much more liekly. Bromic says he had a paper on ketone polymerization, Ill see how well it corresponds to this.

Also, I am not sure why isopropanol does not do this on its own, probably due to more reactivity from the acetone. Also, the presence of the all strong acid/base seems to do something. Isopropanol boils at 85C, and that is about where I started to get some serious boiling. I really think this should be investigated.


la]

[Edited on 31-1-2005 by PainKilla]

Yes I made a peroxide...

Mickhael - 31-1-2005 at 11:00

Yes I do appear to have made some type of liquid peroxide, whether it is the tiny clearish layer, or the larger pale red layer, OR that it is mixed into the remaining yellow milky fluid is something I have yet to determine, I have a pretty tight work schedule so I will get to more tests as soon as I can.

Hello guys, another new person interested in your project.

responsible blaster - 31-1-2005 at 11:55

I have been in contact with a fellow by the name of The R_Sert on Rogue science and he gave me a link to this sites DPPP synth page.
I have produced some of the material in question, and the yeild is very good. It is also far more powerful than AP or APAN or MEKP. I think this materials full power can be realized when it is highly compressed and blasting cap placed at dead center of the device.

dry weight of "mixed product" from residual peroxide doubled

Rosco Bodine - 31-1-2005 at 12:07

The weight of the dried "mixed product" obtained from subsequent reaction of an additional quantity of acetone after the "DPPP" reaction was complete , is double what the yield is obtained by only the reaction of the acetone contained in the "precursor" .

In a previous experiment a precursor made from 95 ml HCl and 100 ml acetone was treated with 40 ml additional HCl and then peroxidized with 280 ml 27% H2O2 .
The yield was 98 grams .

The experiment was repeated with the same quantities and conditions , with a subsequent addition of an "extra" 100 ml portion of plain acetone , 3 hours into the supposed reaction for DPPP . There was a massive increase for the yield of "mixed"
product produced by the reaction of the added 100 ml acetone with residual unreacted peroxide contained in the original mixture . The weight of the thoroughly dried " mixed product " is 198 grams . A 100 % yield of ordinary trimeric acetone peroxide from 200 ml acetone would be 201.5 grams . There are different ways of interpreting the result depending upon what the product is believed to be , * If * the product is trimeric acetone peroxide , then the yield represented by the 198 grams of product is 98.25% of the theoretical 201.5 grams .
So at the very least an extremely high yield process method has been devised for trimeric acetone peroxide . The product may be a mixture of trimeric acetone peroxide with some other unidentified organic peroxide formed in the first three hours of the reaction .

But in either case , the weight of mixed product absolutely disproves the Mackowiak specified reaction route involving chlorination , where any chlorine produced would consume the same hydrogen peroxide , as was found instead to be unreacted in the "DPPP" reaction mixture , and utilized in subsequent reaction with additional acetone , to double the weight of "mixed product" .

The result of this carefully done experiment disputes the validity of the Mackowiak patent for the claimed compound " DPPP " .

[Edited on 31-1-2005 by Rosco Bodine]

chemoleo - 31-1-2005 at 13:28

Interesting.
A couple of questions: You added the acetone straight to the putatiive DPPP crystals, right? YOu didn't first remove the crystals, then use this supernatant to add another 100 ml of acetone into? Because as such it may well be possible that the 'DPPP' is 'over-peroxidised', meaning the DPPP could well react with the acetone to form a lesser peroxidised species. To find this out, you'd have to try addition of acetone to the filtered CLEAR solution of supernatant, which is the leftover after the 'DPPP' reaction.
Another thing - having done plenty of experimental chemistry and such, it seems extremely unlikely that anyone would achieve such high yields, simply because even IF a conversion is 99%, one'd lose at least a couple of percent during the purification, if not more (it sublimes, you have to filter, dry it etc). If you claim that you miraculously have a purification loss of 1% I simply won't believe you :P:P
Therefore I should think that the 'theoretical yield' does not apply here with respect to AP, simply because the molecular masses etc are not correct to start off with. In other words, the final mixed product cannot be AP because yields such as this are impossible to achieve, and thus it has to be a species that is DISTINCT from AP.

Anyway, let me know whether the supernatant can be peroxidised. That'd truly indicate that there is leftover H2O2 (even though that could be easily determined anyway by adding MnO2 or something, after neutralisation).

[Edited on 31-1-2005 by chemoleo]

FrankRizzo - 31-1-2005 at 14:22

Be extremely careful when mixing concentrated sulfuric acid with hydrogen peroxide in the presence of an organic material like acetone. Mixtures of sulfuric acid and high-test peroxide (piranha bath) are used to clean things like chromatography columns, and MANY accidents have resulted because of residual acetone catching fire/exploding.

Rosco Bodine - 31-1-2005 at 15:02

Quote:
Originally posted by chemoleo
Interesting.
A couple of questions: You added the acetone straight to the putatiive DPPP crystals, right?
correct
Quote:
YOu didn't first remove the crystals, then use this supernatant to add another 100 ml of acetone into?
No, because of the thixotropic nature of the slurry , separation would have involved manipulation losses , so the residual peroxide from the DPPP synthesis was reacted in situ with the added portion of acetone .
Quote:
Because as such it may well be possible that the 'DPPP' is 'over-peroxidised', meaning the DPPP could well react with the acetone to form a lesser peroxidised species.
Unlikely for any such amount of excess H2O2 to be somehow "adsorbed" on the DPPP product , especially since if the DPPP product was DPPP formed by the chlorination route , there wouldn't be any residual peroxide there to be "adsorbed" or to participate in some sort of "transperoxidation" scenario .
Quote:
To find this out, you'd have to try addition of acetone to the filtered CLEAR solution of supernatant, which is the leftover after the 'DPPP' reaction.
You can believe that if you want to , I don't . Testing for the presence and activity of reactants contained in mixtures without separation is a common practice and only rarely produces skewed results from unlikely side reaction scenarios as you suppose occurs .
Quote:

Another thing - having done plenty of experimental chemistry and such, it seems extremely unlikely that anyone would achieve such high yields, simply because even IF a conversion is 99%, one'd lose at least a couple of percent during the purification, if not more (it sublimes, you have to filter, dry it etc). If you claim that you miraculously have a purification loss of 1% I simply won't believe you :P:P
So I can't slip that one past you , okay . You are correct about the drying losses and when I said well dried , I did not say anhydrous and recrystallized from toluene . Both samples were dried the same way to an apparent level of dryness based upon the elimination of lumps and the material becoming a free flowing powder . Also there was a weight loss on drying "curve" observed where there is a sudden decrease in the weight lost from water evaporation and the weight loss enters a low loss per hour where sublimation is predominating . Technically , because of the concurrent sublimation and evaporation of the last few percent of water , there is no way to *completely* dry the material without substantial sublimation losses . So for consistency , the drying and the yield calculations were performed the same way , so that the amount of error for occluded moisture is about the same for each sample , and a fair comparison is achieved . If you wanted the absolute figure for sublimed samples or recrystallized material rendered *absolutely* anhydrous , the aliquots which I have tested would put the actual yields for the anydrous organic peroxide at closer to 85% for the isolated pure product . But then it is also true that
manipulation losses occur there also . So
to be precisely accurate is impossible without resorting to an actual chemical determination . Split the difference , the actual yield on a molar basis for the anhydrous product is ~ 90 % . Anyway ,
the range of error will never reach an amount for any measuring adjustment sufficient to explain the "doubling" of the mixed product comparison .
Quote:

Therefore I should think that the 'theoretical yield' does not apply here with respect to AP, simply because the molecular masses etc are not correct to start off with.
My stoichiometry is valid and double checked . If it is wrong then you tell me where and where exactly , in more words than just saying "the molecular masses are wrong" , because I use good numbers and I know what I'm doing .
Quote:
In other words, the final mixed product cannot be AP because yields such as this are impossible to achieve, and thus it has to be a species that is DISTINCT from AP.
I get yields in organic peroxide reactions always in the 80-90% range , sometimes a bit higher , with the exception of course for tetrameric AP which runs about half that percentage .
Quote:

Anyway, let me know whether the supernatant can be peroxidised. That'd truly indicate that there is leftover H2O2 (even though that could be easily determined anyway by adding MnO2 or something, after neutralisation).
Certainly it is the supernatant which is the unreacted peroxide . And the first clue that made me aware of the unreacted peroxide was when I brushed a thermometer against my skin and was actually given the "white burn" which skin receives from any substantial concentration of peroxide . The thermometer had been removed from a supposed "spent" DPPP reaction mixture which should contain very little residual peroxide , and yet it was evident it was still loaded with unreacted peroxide which should have been consumed in the chlorination reaction and subsequent peroxidation of the chlorinated precursor to DPPP . Because there was still a lot of unreacted peroxide in the "clear liquid" of the spent mixture , this was when I first began to doubt the entire matter of DPPP , and devised the "residual peroxide" experiment to confirm those well founded doubts . Anyone is welcome to repeat the experiment and adjust the drying and yield calculations to suit their own satisfaction . The final conclusions will not be affected , only the figures supporting the same conclusions will vary slightly from my own . But since the figures are comparative from one reaction with the next , the errors introduced by method will cancel , so long as the same method is followed for each reaction being compared . I am perfectly satisfied
with the accuracy of my conclusion regarding the lack of validity of the Mackowiak patent . The process does not follow the reaction course Mackowiak describes , and the first clue you will observe for this resides in simply watching the thermometer and seeing that the thermal curve for the reaction is not where it should be in relation to the quantities of peroxide having been introduced . The exotherm diminishes well before it should and the temperature begins falling rapidly , when it should still be rising during the peroxidation . I have a lot of experience with syntheses and with observing such clues , and honestly the thermal curve raised an eyebrow for me the first time I did this synthesis and every time thereafter . The thermal curve simply never reconciled with the reactions described by the patent , not at any range of temperature where the reaction was run , and I covered my bases there too , trying many different combinations to give the reaction every chance to work as advertised , if it was going to work , but it simply does not proceed in the way Mackowiak has declared .

Can u guys boil down what you are finding as it takes too long

responsible blaster - 31-1-2005 at 15:48

I am finding that I am loosing my train of thought reading all the academic jargon. Please tell me weather or not anyone of you have actually tested this material in an electronic velocity testing rig? Also to add you your academic material I beleive that it is the addtion of 1.5x more HCl during the 1:1 synthesis and addition of heat to what we are currently doing that causes addition oxygen to bond with the phorone HCl from the 35% H2O2. My opinion on the DPPP done so far is infact we have a low grade Phorone peroxide derivative and is not infact DPPP or DPHP.


I filter my so called "DPPP" out and the crystalline material is yellowish, I then run isopropylene alcohol through the crystals and let them dry out completely, crystals are white-greenish tinted. I am find something interesting here, the more additional HCl added to the percusor "phorone HCl" beyond the 1:1 ration outlined by the patent the more brisilliant the ending peroxide becomes. AM I ON TO SOMETHING HERE? or shall I call it a fluke? :o

Rosco Bodine - 31-1-2005 at 16:00

Sublime any of the colored material and you will get white crystals and a colored residue which does not sublime . It may only be a trace , but it will be left there , the impurity responsible for the color .

And Hideki , the only thing you are "on to" is playing with mommy's computer or maybe a friends , or the one at the library or cafe .

There's no magic to making DPPP since it isn't DPPP that you get anyway . How about some solubility and melting point data to tie things up nice and tidy , or would that be overkill at this point ?

PainKilla - 31-1-2005 at 16:03

No I think it would be a satifactory conclusion to this thread. Unless of course you get MP's that are really wierd.

Quince - 31-1-2005 at 16:30

Sorry, but as no one answered my questions, I ask again: can I use 3% peroxide, and do I adjust the amount of HCL besides putting in more peroxide? And, is there any conclusion as to whether there is ANY difference in explosive power between this and AP?

Thanks.

Rosco Bodine - 31-1-2005 at 16:42

I just happen to have on hand 4 liters of spectrophotometric grade toluene . That should give some good solubility data . I'll try to do the solubility test tommorrow , unless the cold I am fighting has other plans for me .

Quince :

3% peroxide is insufficient concentration for getting any decent yields from peroxidation reactions . 40 volume hair bleaching peroxide , "clear developer" sold at beauty supply shops is about 12% and is still not going to produce any good yields , but way better than the 3% . You are much better off using 27% or 30% for
peroxidations .

As for the power , that remains an open question . The results of those tests done so far are promising but not conclusive , as there are variables other than the chemical identity of the test material which could account for the few positive test results . It may be slightly more powerful than AP made by usual methods , but not as powerful as HMTD in small diameters and quantities .

[Edited on 1-2-2005 by Rosco Bodine]

Quince - 31-1-2005 at 19:11

Mickhael, I noticed you are also in BC. Where did you get your peroxide?

Chris The Great - 31-1-2005 at 19:29

Rona sells 35% in 1L bottles, that's where I get mine (I'm in BC too....we should have a blast off or something :P ).

18 hours after the 14.5mL H2SO4 was added to the 55mL acetone, the mixture has thickened and become even darker. I took up 2.5mL of it with a synringe and squirted it into my sink which was filled with water. The water turned black with stirring, and a slight amount of oil floated to the top, though very little. However, some greenish gunk that is very sticky got stuck to the sink and the tip of my syringe which I used to stir it. This stuff is sticky like glue, and sticks to everything. It is obviously a contaiminant, but by my estimate it maybe makes up only 5% by volume of the mixture at most. I will atempt peroxidation tonight.

The HCl and acetone mixture is now a nice orange, which a redder layer near the top.
The NaHSO4 mixture has turned yellow, it appears to be going at the rate as the HCl, perhaps because the NaHSO4 had gotten wet before being added.

Now, I just had an idea. Some people bought phorone and tried to make DPPP from that, with no success. It MAY just work.
http://www.sciencemadness.org/talk/viewthread.php?tid=80
No more needs to be said. This could be a method to produce 'true' DPPP.
This process may also work starting with acetone and HCl, although I have no electrodes that would be able to do this, so I can't test it.

Rosco Bodine - 31-1-2005 at 19:48

Evidently the myth of DPPP is going to die hard .

Never the less , I am inclined to kill it dead .


Have test tube , Will Travel :D

Wire Rosco , Science Madness ;)

"Hello guys, another new person interested in your project."

Del Rocco - 31-1-2005 at 20:06

Translation: "Hello guys, please don't notice that I'm back."

Responsible Blaster,

Has J-Scan's LAN extended a bit or are you simply the next incarnation of Matsumoto Hideki/Mr. Anfo/J-Scan? Sure, your tune has changed minutely but I cannot help but notice the obvious (one might say I have a rather keen eye for it):

1. Your first post you overcompensate your guilty feelings for coming back yet again where you are obviously not welcome by immediately offering explanation of how you supposedly got here.

"I have been in contact with a fellow by the name of The R_Sert on Rogue science and he gave me a link to this sites DPPP synth page." (RS has been inaccessable for at least the past 24 hours.)

2. "It is also far more powerful than AP or APAN or MEKP." AND "I am find something interesting here, the more additional HCl added to the percusor "phorone HCl" beyond the 1:1 ration outlined by the patent the more brisilliant the ending peroxide becomes."

Still defending it to the bitter end are you, Hideki? Why does this patent require our attentions so badly? Did your daddy write it? (BTW, the word is "brisant" not "brisilliant". I know this because I know an expert in-- "Word-iology". ;)

3. "Please tell me whether or not anyone of you have actually tested this material in an electronic velocity testing rig?" (Does anyone really need to GUESS where he's going with this one next? It HAS to be at the very least 9000 MPS!)

I'll shut up, now, and take my lashings like a man if I am wrong, but there is only one way to tell... A mod needs to check his IP against that of his other incarnates, that's all.




[Edited on 1/2/2005 by Del Rocco]

Toluene solubility comparison test results

Rosco Bodine - 1-2-2005 at 15:24

In two 100 ml volumetric flasks was placed carefully weighed 50 ml of toluene
and a micro stirbar was placed into each .

The solubility of trimeric AP was found to be 18 grams in the 50 ml toluene . A small
amount of water separated and appeared
as tiny scattered droplets adhering to the walls of the flask . The amount of water was very small , insufficient to actually coalesce into a single drop or settle to the bottom of the flask , just a few barely visible specks of free water , indicating the sample of AP was very dry .

The solubility of the " DPPP " was also 18 grams in the 50 ml of toluene . However ,
there was a huge amount of trapped water , slightly more than one third the weight of the apparently "dry" crystals of DPPP was entrapped water , which separated when the DPPP crystals were dissolved in toluene , and formed a distinct lower layer of separated water .
The separated water was measured and subtracted from the weight of
" DPPP "which had been dissolved in the toluene to determine the non-water portion of the "DPPP" sample which dissolved as 18 grams .

These 18 gram per 50 ml solubilities are actually slightly into the cloudy range , a bit oversaturated and showing a tiny amount of undissolved "grit" of crystals , so the "formal solubility" may be a fraction of a gram under 18 grams per 50 ml , or based upon the more usual 100 ml of solvent , a bit less than 36 grams per 100 ml toluene . That's as close as I am going to get it . Anybody wants a more precise figure can do the test themselves using recrystallized anhydrous samples .

Seeing how much occluded moisture persists in the " DPPP " has pretty well shitcanned any further interest for me in this material because there's too damn much water trapped in the stuff . This makes for tedious work recrystallizing to get rid of the water . And the solubility
being identical to trimeric AP pretty well
says that "DPPP" *is* trimeric AP any damn way , which can be easily made in a much more pure and *dry* form without any elaborate purification required .

I think any further interest for me with experiments concerning " DPPP " is finished after this toluene solubility test .
For me " DPPP " is going into the file
entitled " No-such Pentaperoxide " along with a few other other lame patents .

PainKilla - 1-2-2005 at 15:36

Well then, thats that :). I guess everyone should thank each other (and especailly rosco) for spending thier time and hard work in pursuit of this topic. 3 Years now is it? And the validity of DPPP is disproved! I guess I will use this method since I can store the red/yellow much for a long time and make the peroxide whenever. I guess we can conlude its AP, but a "better" form of it, which is not a bad thing.


I thank everyone for spending their time on making this! I guess now we can disprove IPA Peroxide now :). I bet you it COULD work via that reaction mechanism I posted.

O yea, I think using the H2SO4 helps prove that this is indeed AP since we know AP is also made via H2SO4 and that no chlorination is indeed involved.



O yea, BYE HIDEKI!!!!



[Edited on 1-2-2005 by PainKilla]

Serendipity one more time

Rosco Bodine - 1-2-2005 at 17:08

The good solubility of AP in toluene at room temperature is likely even better when the solvent is warm . And the solubility of AP in alcohol is about one tenth the solubility in toluene . So this provides a possibility for securing the AP in anhydrous form pretty easily .
If the AP still damp from neutralization and filtering was dissolved in warm toluene , then any water present would simply separate from the toluene solution of AP . If alcohol was slowly added to the separated toluene solution of AP , the AP should crystallize out in anhydrous form , and being wetted only with anhydrous solvent which should evaporate quickly from the filtered crystals , which would be obtained water free . This could certainly expedite the process of obtaining AP in pure and dry form . The AP contaminated
filtered solution of toluene alcohol need not go to waste , as it would make a very good solvent-fuel / detonation catalyst for wetting AN , especially if any nitro compounds
such as picric acid , or dinitrotoluene , or nitronaphthalene were added to the AP/toluene/alcohol , and then the AN dampened with such a mixture . The anhydrous AP crystals could be used for the detonator / booster and any leftover AP simply blended into the sensitized AN mixture . Waste not want not , and no leftover material to cause any unsightly clutter in storage areas :D

[Edited on 2-2-2005 by Rosco Bodine]

Chris The Great - 1-2-2005 at 21:26

So, we're going to ignore the different crystal shapes, the fact that it doesn't small like AP, and the fact that it, at least according to those who have made it, that it is more powerful?

I mean, the stuff sure doesn't seem to be AP to me. I mean, sure the patent is crap, but this definatly isn't AP. Sure, it might not be superpowerful ultimate explosive, but it seems to be something new.

There are simply to many open ended questions just to say it's AP.

Now, if someone does and NMR or mass analysis on this stuff, and it turns out that yes it IS AP, then ok, I'll believe it. No such test has been done and it seems to have so many differences to be AP. If the crystals where the same, then I'd believe them. But the crystals are different! I've done alot of close looking at my AP, and ever description of 'DPPP' I've read says, in big bold letters "NOT AP."

Since I mixed up some of my own, I'll test it myself, scent wise, crystal shapes and explosive power, and tell you. The method of formation looks different, the smell is different, etc.

Not to seem like I am thinking like Hideki, but this stuff really seems to be a new peroxide, definatly not 9km/s or even close, but more brisant than AP. And with rosco finding it so full of water, it might be more powerful if the time is taken to recrystalize and dry the stuff.

I am certainly not going to give up this stuff. I want to know what it is! And even if it isn't DPPP, I think we should at least preserve the name as this whole thing really is an epic project.

How about a mixed product recrystallization from toluene

Rosco Bodine - 1-2-2005 at 23:03

Well that's next on my agenda . I have 18 grams of AP dissolved in 50 ml of toluene and I have 18 grams of " DPPP " dissolved in another 50 ml of toluene .

If I mix the two toluene solutions , and start adding alcohol , or just dump the solutions out in a glass tray and let the toluene evaporate , either way I'll bet anything only one variety of crystals is obtained , lovely snow white crystals of AP , and no crystals of anything else .

Chris The Great - 2-2-2005 at 00:37

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.jp...
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.

Quince - 2-2-2005 at 19:58

Can standard AP and the new version be used to detonate nitroglycerin/nitrocellulose gel? Should it be loose crystals or compressed?

Also, will it still detonate if I mix in a bit of polystyrene dissolved in acetone to bind it together?

[Edited on 3-2-2005 by Quince]

Joeychemist - 6-2-2005 at 13:19

Look what Mega has found, it is not that important but it still merrits a post;)

dppp.jpg - 32kB

The_Davster - 6-2-2005 at 13:38

Now that does definatly merit a post. :o

However, the properties of the "DPPP" that has been prepared in this thread tend towards it being standard CTAP. Looks like we are in for another 30+ pages added on to this thread in the quest for the actual DPPP.:D Unless what we have really is DPPP which seems quite doubtfull at the present time. I really would like to see NMR or mass spec done on "DPPP" and CTAP.

[Edited on 6-2-2005 by rogue chemist]
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