Sciencemadness Discussion Board - Diphoronepentaperoxide (DPPP)

Diphoronepentaperoxide (DPPP)

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BASF - 28-11-2002 at 03:30

"the determination of blasting power relies on comparative methods. A possibility is the determination of the lead block expansion after trauzl."(roempp)
There is a good picture, but i cannot copy it, i would need a capturing prog.
But i can give you the diameters.
The standard Trauzl block is 20cm in diameter and height and has a vertical hole with 2.5cm diameter 12.5cm deep.
Exactly 10g of the explosive are placed in the hole.

Assuming lead has a density of 11.3g/ccm,
you´ll need at least
11.3*[(10*10*3.14*20)-(2.5*2.5*12.5*3.14)]=68.2kg(!)

You see, it would be quite wise to make a smaller lead block 1-5g.

HLR

BASF - 28-11-2002 at 04:15

I think the sand test would (as vulture proposed) also be a good method to give DPPP some experimental brisance value.
After the detonation, the sand will consist of bigger and smaller particles.

To determine a represantative value i´d propose filling the whole sand into a small bucket and shake it for a defined time, say 15min, so that the bigger sand particles seperate from the smaller ones.
(the bigger ones are on top)

Then determine the big-particles to small particles-weight-ratio by weighing the upper half and the lower half seperately.

HLR

vulture - 28-11-2002 at 09:30

I would think the sand has to be perfectly dry for the sand test, because otherwise water could interfere, not only by absorbing energy, but also by changing the weight. True or not?

BASF - 28-11-2002 at 17:02

For sure, using dry sand would be "a good idea" indeed...

The biggest difficulty in the sand crush test will be the determination of a value that correlates with the size of the particles.
I guess that the shaking of the crushed sand should be done as long as possible, but always for the same time.

And don´t forget: one test is not sufficient.-One test is no test!
At least 3 tests would be necessary to
1)prove the reproducability
2)give a more reliable value

We need reproducable results.
1)the loading density has to be equal
2)the initiation charge has to have a standard size and loading density
3)always use the same sand.
Possibly sand of a particle size of 3-5mm would be best.

BASF - 28-11-2002 at 17:12

Or just juse a sieve to seperate the crushed particles from the rest.....more realistic and better for reproducability.

Crystal Formation

Abramellin - 10-12-2002 at 04:04

Anyone should determine the content of the different AP isomers in the endproduct which formed in the side reactions of the AP synthesis.

tricyclo isomer [ C9H18O6 ] and the
dicyclo isomer [ C6H12O4 ]

How are the size difference between the crystals of the different AP isomers ?

I don`t know it`s possible to make DPPP direclty from pure phorone,
more likely a similar cyclic peroxide from
4-oxoisophorone.

BASF - 10-12-2002 at 06:05

I think the crystal size would be a very unreliable method to determine the content of different isomers...i did not get into thin sheet chromatography, but maybe this would be a thinkable method(has to be UV-assisted as they are colourless).

Further i also believe peroxidation of pure phorone is impossible from my empirical point of view:

Quote:

Peroxidation of commercial phorone

I recently bought 97% phorone at Sigma-Aldrich, which seems to be the only supplier of small quantities.

At first, the phorone was very pure, could easily be melted in a warm water bath and crystallized upon cooling(room temperature) in the form of long yellow needles.

Solubility tests:

-Insoluble in 30% HCl

-soluble in commercial acetone

-exzellent solubility in 98% acetic acid

-Insoluble in commercial ethanol(absolute ethanol needed?)

The phorone does not crystallize at room temperature if surrounded by an aqueous (immiscible) phase.

I tried to peroxidize the phorone(1ml) by first dissolving it in 98% acetic acid (5ml=excess to prevent seperation upon addition of the peroxidation-mix) and then adding a mix of 1ml HCl and 1ml 30%H2O2, but although the batch heated up very strong and this was then later repeated with proper cooling, no precipitate occured.

Maybe the DPPP is very soluble even in aqueous solutions of acetic acid, like phorone.

-Or the reaction just failed.
So i added some ml of water to make it seperate along with the rest of unreacted phorone, but nothing remarkable happened.

The last experiment i did was to dissolve phorone in acetone and then tried to peroxidize both.
I was surprised that the phorone seemed to prevent peroxidation of the acetone(no AP-precipitate).

DeusExMachina - 21-12-2002 at 15:07

I didn't get a chance to read the whole topic because it'sso long and I apologize in advance if someone has alread asked or anwsered this question already but how would you know if you had diphoronepentaperoxide without detonating it when you have it? does it look any different than acetone peroxide or is it just the detonation velocity and a few other stuff that have nothing to do with the appearance of DPPP?

madscientist - 21-12-2002 at 18:30

The answers are in this thread... let's not have discussion going in circles.

ShockWave - 22-12-2002 at 07:45

http://apanshock.tripod.com/phoron_dppp.htm

magnum - 26-12-2002 at 20:20

hi

i did a search on the phonebook and there lives a wolfgang mackowiak in bielefeld (the inventer of the procedure) the phone number is
+49 5 21 33 41 44 . possible he know how it's done. let's call him.

bye

Sublimation and prevention of same

BASF - 7-1-2003 at 12:19

Recently i did a little "study" on the sublimation of "DPPP" and tricyclic AP.
(AP and DPPP were made with great care, using an AN-icebath at below 5°C)

At 21+/-0.5°C samples(filter cakes, thouroughly dried and weighed with 0.01g accuracy) of

1)tricyclo acetone peroxide(TCAP) showed a loss of 26% after 13 1/4 days

2)"DPPP"; 49% loss after 13 1/4 days

To me, this is a strong indication, that the "DPPP"-product is a indeed a different compound, not just another form of acetone peroxide.

I also made two experiments with coating substances to slow down sublimation of TCAP. (Same conditions and time as above)

1)TCAP was impregnated with 16% phorone (from Sigma-Aldrich); the weight loss was now only 15% as opposed to 26% uncoated.

2)TCAP was impregnated with less than 45% of an ethanol-soluble grease(non-volatile) obtained by cooking acetone with concentrated sulfuric acid.

The unexpected result was a weight loss of 38%, even more than of pure TCAP.

lol

Madog - 9-1-2003 at 19:39

thats very tempting, it would be great if someone called him

BASF - 10-1-2003 at 04:57

......and it´s not gonna be me.

It would have to be someone speaking german. I just speak german with a freaky dialect hehe, so i´m not the right one.

But maybe someone could say he examines different peroxides in their capabilities as polymerization starters and spin a story from that....

For sure, if someone could also record the whole thing on tape this would be a cool thing.
Eternal glory to the brave one!

PHILOU Zrealone - 18-3-2003 at 11:43

I have some words to say here!

Tetracene has a density of 1,7 and as a bluk may have a lower density!

I don't have the patent under the eyes but from what I have understood:

(CH3)2C=O + CH3-CO-CH3 -H(+)-> (CH3)2C=CH-CO-CH3 + H2O

Then
(CH3)2C=CH-CO-CH3 + O=C(CH3)2 -H(+)-> (CH3)2C=CH-CO-CH=C(CH3)2 + H2O + (CH3)2C=CH-C(CH3)=CH-CO-CH3 +(-C(CH3)=CH-)3 + ...

It seems very advisable to isolate the phorone!
The more you wait, the more crotonisation will occure!
If you let aceton and concentrate NH4OH stand for monthes it will make yellow, then orange, then brown then a black solid precipitate...thus a high polymer of the kind
(-C(-R)=CH-)x.

Thus phorone is made aside with other trimers condensate and the more you wait; the more you go to higher polymers!

Phorone is submitted to addition of 2 molecules of HCl and follows markovnikov's rule!The phorone resonates and display CH3 inductive giver effect and enol-cetone shift-both effects goes in the same way!
(CH3)2C=CH-CO-CH=C(CH3)2 + 2HCl -->
(CH3)2CCl-CH2-CO-CH2-CCl(CH3)2
Then HCl oxydises with H2O2 and heat to generate Cl2!
2HCl + H2O2 --> Cl2 + 2H2O
Cl2 may react directly with phorone to add 2 moles of Cl2!
(CH3)2C=CH-CO-CH=C(CH3)2 + 2Cl2 --> (CH3)2CCl-CHCl-CO-CHCl-CCl(CH3)2
Anyway assuming the way they propose is right:
Cl2 and HCl will yield monohalogenation of hydrogens alfa oriented vs the ceto carbon!
Looking at ((CH3)2CCl-CH2-)2C=O the more favourable sites of halogenation is thus the inner methylene and not the external CH3 that are far from the C=O!
And this said it bring to the same as Cl2 addition on phoron!
((CH3)2CCl-CH2-)2C=O + 2Cl2 --> ((CH3)2CCl-CHCl-)2C=O + 2HCl
This is a good assumption since the phoron is symetrical molecule why would it give an unsymetrical product now?
I don't see a reason why if they have terminal halogenation on one side why not on 2,3 or 4 terminal CH3?
Anyway:
((CH3)2CCl-CHCl-)2C=O + 4H2O2 --> ((CH3)2C(OOH)-CH(OOH)-)2C=O + 4HCl

As a conclusion, you see that ALL HCl involved is recovered and it serves as a catalyst!
Thus there is no significant increase of acidity; also in 33% HCl pH = -1, no pHmeter can work well in such concentration; since it is in excess, you will not notice any change!

Finally if this works for phorone it should work aswel with Cl-CH2-CO-CH2-Cl to replace the Cl by peroxydes to get 3,4dioxacyclopentanone (DACP) then peroxidise it to cyclotri(DACP).
With Cl-CH2-CH=O

It should also work with the intermediary
mesityl oxyde (CH3)2C=CH-CO-CH3 via the chlorinated (CH3)2CCl-CHCl-CO-CH2Cl

So in this patent basic organic rules seems to be broken!
The best way to make the stuff is to isolate intermediaries!
Mesityl oxyde, phorone (via distillation) then add HCl on both; then isolate the chlorocetons; then chlorinate with Cl2 bubbled in H2O2 solution of the chlorocetons!

The trauzl test is a bit tricky because it deals with 10g of explosive!So if you have an explosive that is 10 times denser than another one you will compare let say 10 ccm of a HE of density 1 and 1ccm of a HE of density 10!
Of course this explains why high density lead primaries display so bad in Lead Block test vs pure HE of much lower density!
A good alternative would be to make both LBT with same weight and with same volume of HE and with molar weight multiple!

Same problem with brisance it is based on a given sample of known weight!

IgnorantlyIntelligent - 23-3-2004 at 18:01

Damn where was I while this thread was so hot and in testing??? Damnit! Well this compound interests me even though I seriously doubt DPPP is a possibility. 9000m/s? Come on now, if the germans really invented a compound THIS easy to make and this powerful they'd either tell no one or it would become their new main HE for blasting and such. If it truly has th properaties described earlier than it would not be hard to make it fairly insensitive by the addition of NC paste or something. 9,000m/s is..to say the least, aww inspiring.. I will begin tests tomarow. I read somewhere that the HCL/acetone mix must sit in a warm place for about 72 hours atleast for the phorone to form. You all talked about just letting it sit for 10 min or so...I doubt that would work.

[Edited on 24-3-2004 by IgnorantlyIntelligent]

Blind Angel - 23-3-2004 at 19:31

Not registred, this thread is over 1year old and has procreated to create some offsprings

IgnorantlyIntelligent - 23-3-2004 at 20:51

A year old..... smeone must have a conclusion. IS or IS IT NOT possible?

Polverone - 23-3-2004 at 21:51

I don't think the compound, as described, exists. But of course this is just my opinion. It's been a year, and many people have tried this one way or another and failed. But if the challenge were "perform a total synthesis of quinine," everyone here would fail too. That is no proof that it is impossible that a substance having the claimed properties of quinine exists. Still, I think DPPP is a chimera, since it has unusually good claimed properties and a given synthesis that either does not work at all or that works only by some tricky modification not mentioned in the patent.

Phoronsynth. Still works:-)

braegler - 26-4-2004 at 02:19

Hallo,
mix 100ml Aceton and 100 mlHCl konz (37%).
Boil under reflux for 2 Hours (70°C schould be best).
Cool down to 5°C an slowly add
48 g powdered Sodiumhydroxyd until the liquid becomes yellow and the pH is >7.
Cool meanwhile, so the Temp cannot rise above 10°C (realy good cooled and slowly added).

Cool down in a Ice/Salt-Bath to appr. 0°C and filter.

To wash the residue, rinse with Icewater at 0°C.

The yield of Phorone is not bad in this way.

BASF - 26-4-2004 at 10:28

? is this from a book or what ? ... its not quite scientific to write sth without naming any source or at least saying "this is just an idea of mine or this from the Organikum or book xy"...
however, it seems to be a detailed procedure to me.
I have once bought some phorone; if someone wants to make a DC-comparison and lives in Germany or Austria, i could eventually send him some mg in a letter or something...

shadeT - 23-5-2004 at 05:10

BLAST_X wrote --------------------

I've tested preparation of DPPP and i can say it`s a very interesting and varied explosive.
You can use it as a primary explosive and as a high energetic secondary explosive.
You can never classify DPPP in the same category as AP or HMTD.
The question is, at which density you use DPPP and at which method you use to ignite DPPP.

preparation:
To a 1000 ml erlenmeyer flask add 185 ml of 20% HCl (i don`t
have 35% HCl at this time). To a second flask add 100 ml of aceton.
To an third flask add 200 ml of 30% H2O2. Cool all to 5 C.
After cooling, slowly add the aceton to the HCl and stir the mixture
for 5 minutes.(very slight yellow colouring over a few minutes)
The patent don`t say heat at this time and the patent don`t say
some product (poron) should precipitate from the solution at this time.
If you heat or not, the content of AP are always present at end of the synthesis. On the contrary, if you heat to much or to long, the reaction fails.
Cool the mixture to 5 C for 2 hours and stir occasionally.
After standing, set the mixture to magnetic stirring at room
temperature and slowly (over 10 minutes) add the H2O2 to the
aceton/HCl mixture. The temperature can rise over 40 C and
the mixture become a sligth green colouring.
(second reaction-step, formation of pentachlorporon and free
Cl with H2O2 as catalyst)
The DPPP should precipitate on top of the mixture and some fumes bubble of.
You can distinguish this of AP crystalls, which formes in the reaction-mixture and which are a bit larger than crystals of DPPP.
I`ve look at the crystals exactly through a microscope.
(look at attachment DPPP.jpg)

After all H2O2 is adding, continue stirring for 2 hours an more till the liquid on the bottom of the flask are clear and no fumes bubble of.
Filter out the crystals, wash them with 1 L of 10 % sodium bicarbonate solution, and again with water.
Dry crystals of DPPP at room temperature for 48 hours.
The next step are very important to remove all traces of acid and AP in the product, that you can handle safe with DPPP.
Dissolving the crystals in minimum amount of hot ethyl alcohol (60 C),
let cool to 5 C, filter, add a large volume of cold distilled water, let sit for 1-2 hours below 10 C and filter again.
Let dry DPPP at room temperature for 1-2 weeks to decompose and evaporate the rest of AP on the air.
final yield: 65 g
(at this reaction temperature and with delute 20% HCl, i think you can get much more yield with reaction temperatures below 10 C and a longer reaction time, the patent say around 90%)

Be careful with large quantities because DPPP is somewhat sensitive
to friction, shock and heat.

I`ve tested the DPPP in 3 different charges.

1. I`ve made a blasting-cup (hard-paper) with 5 g charge low pressed
DPPP and ignite with a match.
No detonation, only flash, the blasting-cup bursts only.
Consequently, if you ignite DPPP at powdered density or with flame,
it`s flashes only, you can use it as a primary explosive similar
to AP and HMTD, it detonates only at this density when strongly heated.
(very storage stable and lower sensitive to friction and shock)
2. I`ve made a stable blasting cup (hard-paper) with 50 g charge high
pressed DPPP and ignite with a match.
It datonates hazardous and i`d feel strong the detonation pressure
still the distance of over 50 m between the blasting-cup and me.
3. I`ve made a stable blasting cup (hard-paper) with 10 g charge high
pressed DPPP and ignite with a match.
It datonates correctly as well.
Consequently, in high pressed density or under pressure in a
stable blasting-cub - DPPP is a high qualtity and high energetic
explosive, it detonates without a primary igniter.

Disadvantage:
- somewhat sensitive to friction and shock
- low detonation temperature, ~ 200 C
- density of DPPP are not very high

Advantage:
- required chemicals for synthesis are cheap
- it`s easy to produce (no expensive lab-equipment required)
- large volume of gas and high explosive velocity, ~ 9000 m/s
(conditioned military usage, cut of steel ...)
- storage stable and great chemical stability

DPPP is my new favourite peroxide. It`s safer to handle as AP or HMTD and more powerful and brisant.
It`s a very good primary explosive to ignite very insensitive explosives (hexogen,octogen,TNT,HNIW) or a energetic single explosive.

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

Does this procedure actually work and did anyone try to make DPPP by this method ?

KABOOOM(pyrojustforfun) - 24-5-2004 at 02:59

<blockquote>quote:<hr>After cooling, slowly add the aceton to the HCl and stir the mixture
for 5 minutes.(very slight yellow colouring over a few minutes)
The patent don`t say heat at this time and the patent don`t say
some product (poron) should precipitate from the solution at this time.<hr></blockquote>the mixture needs to stay for days to obtain a considerable amount of phoron. plus phoron is just slightly soluble in water so if he had no precipitate it simply means he hadn't much phoron in his solution (just enough to give it a very slight yellow colouring

.
heating the aceton/HCl mix has the advantages of accelerating the reaction and removing the unreacted aceton (tho I'm not sure about the former)

<blockquote>quote:<hr>Disadvantage: .... - low detonation temperature, ~ 200 C ....<hr></blockquote>as mentioned by others already it's the temperature at which it explodes when it is heated slowly (with a particular rate).
<blockquote>quote:<hr>Advantage:
.... - large volume of gas and high explosive velocity, ~ 9000 m/s (conditioned military usage, cut of steel ...)
- storage stable and great chemical stability<hr></blockquote> almost everyone agreed that 9000 m/s is too much for such explosive.... I bet 9000 f/s is closer to its real VOD

(not meaning it had been a misprint or such).... BASF's experiments proved DPPP to be even less storage stable than AP!

shadeT - 24-5-2004 at 08:47

Can you explain a bit more storage sensitivity ?

is there maybe a site somewhere where i can find more info about this explosive ?

Do you have experiences with DPPP ?

KABOOOM(pyrojustforfun) - 24-5-2004 at 19:37

see <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=397" target="_blank">DPPP-the legendary Mackowiak patent </a> and <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=1506" target="_blank">Diphoronpentaperoxyd & Chloroacetone</a> .

no for some strange reason I can't experiment much

shadeT - 27-7-2004 at 07:56

I tried a method that shockWAVE described in this thread before .

10 ml pure acetone was added to 15 ml 19% HCl , that was left to stay an hour ( no color change ) and then later i added in 20 ml 30% H2O2 . After about 20 minutes i come back to see whats happening and i see incredible yield of powder formed on the top of the solution ...

I was very suprised, i left it so 40 more minutes, but not much was formed later ... The smell reminded me a bit on MEKP, and i noticed some bad fumes there and it affected my eyes that started to realy hurt during neutralization.

After it was properly neutralized, i filtered the christals and let them to dry.

Details about the powder - Bad smelling, a little bit diferent than AP. It looks more like a powder than chrystals, as shockWAVE said no sparkling on light ... Tried to ignite some of it when still wet, when i put it on flame it WHOOMP a few times then the rest melts and doesnt to anything ( but thats maybe becose it was still wet ... )

[Edited on 14-6-2011 by quicksilver]

Isophorone?

J_O_H_N_Q - 4-8-2004 at 21:22

Isophorone is the stuff right?
Because I can get it for about $3 (US) a kilo.
Does this sound good to you guys? I think I'll dream a DPPP synth using isophorone sometime, might be fun.

The_Davster - 4-8-2004 at 21:39

Isophorone has a different structure than regular phorone so it cannot be used.

successful synthasis of DPPP explosive

Dr. BOOM - 15-12-2004 at 19:55

I went home to my lab yesterday and began working on several ways to make DPPP from Acetone/HCL/H202:

Be very careful! The reaction tends to run-away very quickly so always mind the temperature. DPPP forms just before the reaction runs away so you will have to act quickly and neutralize the acid. This is a bizzare chemical reaction which could REALLY hurt you!! be safe!

Procedure:
Take 250mL of acetone and add to 250mL HCL (muratic acid)
----add 110 C heat until liquid color change to dark reddish-orange color~almost black (process should take 20minutes or less)
next cool the Chloro-phorone to -1C for 30 minutes.

get ready 500mL of chilled H202 (+2C) and very slowly add liquid to dark Chlor-Phorone. Be EXTREMELY careful to monitor the temperature---if you add too much the reaction will run away violently!
Color change will be evident and a mass of solid cystals will form at the bottom...continue adding in the H202 until the flask is filled with yellowish-white precipitate ...this is cystalline DPPP. Dump the solution into another flask via a filter. The filter will be used to trap all the crystals. Wash these crystals in a solution of bicarbonate/water to neutralise any left over acid.

I tested a 5 gram brass AP charge beside my newly found DPPP, and the two substances are totally different in terms of power. I blew a dime size hole in some mid grade sheet steel whereas AP couldn't scratch the surface.

Too much heat

Joeychemist - 15-12-2004 at 20:35

Dr Boom

First; you never pour chemicals into acid (unless it’s unavoidable) because you risk splashing acid all over, instead add acid to the acetone. (Just trying to help).

Second; you’re giving the mix to much heat, Acetone boils at somewhere around 56.5°C.When you use to much heat some of the phorone will decompose altering you’re product yield.

Third; unless you purify the phorone you’re end product will still contain small amounts of AP. How much DPPP did you use to blow a hole into the steel and how thick was the steel?

O and DR.boom,I'm sure that there are other threads about DPPP you could have posted this in.

Rosco Bodine - 15-12-2004 at 22:03

Hmmmm , hold on there mini-moderator if you please . If Dr Boom has cracked the mystery of the holy grail peroxide , who are you to interfere or criticize ? If the reported experiment is reproducible and the fellow has succeeded , then he has done more than many others who have tried and failed , including those of us who have dared to add things directly to concentrated acids and lived to explain why that may in some cases be exactly what you do want to do , even though it may not be generally a good safety practice to do it recklessly or without reason . So let's see where this thread may go , and if it is a classic or detritus can be left to the real moderators .

Please stay out off this,unless you wish to help

Joeychemist - 15-12-2004 at 22:38

Rosco
I didn’t know that the DPPP code had not been broken yet.

I was simply trying to help Dr. Boom and help this thread progress. You should try that instead of criticizing me for trying to help this man increase his over-all yield. I'm not trying to play "mini-mod" I was simply telling Dr. Boom my advice. So unless you have something to add to the thread or you can disprove me or my advice, please stay out of it.

Rosco Bodine - 15-12-2004 at 23:17

Quote:

Originally posted by Joeychemist
Rosco
I didn’t know that the DPPP code had not been broken yet.

Now you know more than you did before , because the matter has certainly not been solved . Unless someone has contacted the inventor personally for the details and clarification of the process described only in general terms in the patent , so far there has been little in the way of answers and no one has confirmed the process described by the patent , by any reported experimental results . ( until now with Dr Boom )

Quote:

I was simply trying to help Dr. Boom and help this thread progress.

No , you were tutoring Dr Boom in matters you do not understand , unless of course you have succeded yourself in the quest for the holy grail peroxide and have therefore perfected the process to a level where you can tutor Dr Boom in how to improve his results to match your own . My take on things is that you never made the compound in discussion , yet you propose to instruct someone else on the finer points of doing something you haven't done yourself.

Quote:

You should try that instead of criticizing me for trying to help this man increase his over-all yield.

I wouldn't presume to speak to the heart of matters I do not understand as if having expertise I did not possess . But you would do that in a half second which is exactly what you have done here .

Quote:

I'm not trying to play "mini-mod" I was simply telling Dr. Boom my advice. So unless you have something to add to the thread or you can disprove me or my advice, please stay out of it.

I did add something , but the point was lost on you . More interesting contributions to this thread would be to ask about the heating of the acetone hydrochloric acid mixture , and when the temperature was measured , was the temperature ramped to that peak , or held there for a time , or is that the bath temperature . What concentrations for the reactants , and what was the weight of the charge and the target specifications and in what manner was the charge initiated ?

Those would be more pertinent interests , before giving advice about what you have not accomplished and already yourself resolved .

just made DPPP... quite a bit different than AP

Dr. BOOM - 15-12-2004 at 23:54

This DPPP stuff is quite fascinating. I started with equal
parts 1:1 Acetone to HCL and heated it until the reacted product turned dark red. I then transfered this product to a freezer where I took the temp down to around -30c
The Dichlorophone turned almost black/very dark red-brown when it was fully cooled.

I was running into problems with the peroxidation process and kept getting the DCP reverting back into acetone, HCl with a massive releasal of heat. Anyone know why this is?

I however found a way of quickly filtering the crystals and the results were very satisfying

Alright, I got a better yeild with lower heat!

Dr. BOOM - 16-12-2004 at 00:20

Ok, I heeded the advice of a lower temp for the production of Dichlorophorone ( or Chloroacetone?)

Once Crystalized (this takes 3-4 secs) the substance must be immediatly filtered and nutralized in Ammonium Hydroxide and then transferred into a bath of ice cold water. The crystals I see are light lemon yellow and are incredibly fine, about the size of cerium oxide polish.

Sorry

Joeychemist - 16-12-2004 at 00:30

Rosco
You’re right about me not asking if the temperature of the solution was set at a steady temperature of 110°C or any other crucial details that would have helped me further understand his procedure or the methods of which he used. You’re point was not lost on me Rosco and I apologize for not being more thorough in my post. It is however very wrong of you to assume that I have no experience or have never performed this procedure or several others in the past in the quest to understand this explosive. Though I have had many troubles, I have overcome most.

I would like to get back on track here Rosco, if you wouldn’t mind I would like to drop this now and just continue on.

I strongly recommend the slower approach to heating this solution, I usually heat mine in a water bath, I heat until the water is almost boiling, (about 98c) then keep at a steady temperature. I never let the solution itself boil. Then I heat for about two hours until the solution is very dark in color, and there are very little crystals floating on the top. (You can’t heat the solution too long or at to high of a temperature or some of the phorone will decompose). To make the DPPP collected free of any (most) TCAP, I Make an emulsion of the collected crystals in hot water and cook it for a few minutes, AP decompose in water at 90°C, but DPPP will not decompose in water until about 180°C. I really hope that this helps.

Rosco Bodine - 16-12-2004 at 06:33

Joeychemist , Sorry for my tone earlier . I was at the end of a rough day and running out of my usual surplus of patience and good humor . I saw you were on your second post here and that Dr Boom was on his first post , and that didn't help either . Agreed to get back on topic , and for certain the details are important . Hydrochloric acid is not a dehydrating acid and will not pose the same order of addition hazard as for sulfuric acid and water , but even that can be managed with good stirring and special technique . The hazard encountered there is basically something overstated for the protection of chemistry novices or the careless who will soon find trouble there in mishandling a delicate procedure whose thermodynamics appear more quickly than their skill or understanding at managing such manipulations involving strong acids . However , in the area of chemistry involving nitrations of energetic materials for example , there are times when it may be risky but necessary to add other substances to strong acids , or to gradually and cautiously dilute such mixtures , for reasons that may be valid , even though contradicting the usual safety protocol . So it is a rule to be broken in special circumstances where the order of addition may have bearing on the product , or the order of dilution may have bearing on product isolation .
Seeing this may be one of those "special cases" I supposed that it may be Dr Boom's departure from convention which had bearing in his reported success , and wished that we look more closely at that possibility , and other details which could go to reproducing his reported success.

The temperature during or following the peroxidation could indeed be critical for producing and isolating the product free of impurity with AP , and the pH , or avoiding the precipitation of any insoluble intermediate may also be critical . One of the things which may have been a wrong assumption in other threads is the idea that somehow obtaining pure phorone as an intermediate was necessary , when in fact many compounds named as derivatives of some parent compound cannot be made by any means from that parent compound which is not a valid precursor , but a "parent" compound in name only and referenced only as an example of structure related to its "derivative" . Thus it may be possible to make the peroxide "derivative" of phorone from acetone , while it may be completely *impossible* to make it from phorone itself .

sylla - 16-12-2004 at 07:03

I've done some DPPP, actually I'm not sure it is really DPPP but I can tell you it is NOT AP.

I've mixed 1vol HCl 30% with 1vol Acetone, mixed them well and cooled it. Then I added 2vol H2O2 slowly keeping the temp low.

You can notice several things between this chemical and AP, first it does not sink into the solution like AP does. I have been able to separate AP from "DPPP" using a mix of both, acetone and water. Using specific amount of water and actone you can have three layer : on the bottom AP, on the middle the solution and on the top the unknown chemical.

Note that when this compound explodes there is not the caracteristic smell of AP and it is way harder to blow it up with a hammer !

I finaly noticed that this compound was twice more soluble than AP (tested in methanol, acetone and ether).

Of course I cannot prove it's DPPP and I have no idea of the structure of the mol but I'm pretty sure it is not AP...

Btw, I don't believe DPPP to have such an amazing power. When I do theoretical expectations from enthalpy and density (both approximated using other theoretical expectations rules) I find that DPPP would be a little bit less powerfull than AP (these approximations give me the same power for all AP's but I know TeCAP is more powerfull and "safe" to handle than DCAP).

Why did the author say it is soooo powerful ?

So, considerating all these things I do believe in DPPP but I see it more like a problem rather than a holy grail peroxide.

Rosco Bodine - 16-12-2004 at 07:48

Maybe "inventor's euphoria" caused inflated claims . I don't know what the story is about the material . I haven't attempted the synthesis for reason I found something I considered better and easier in a liquid mixed peroxides which is coprecipitated AP/MEKP . The DPPP could possibly be wetted with or form a eutectic with the mixed peroxide , to form an interesting composition . Or , because of its lowered volatility DPPP may have usefulness where AP does not . Tetrameric AP is a distinct improvement over AP in regards to volatility . I have made the tetrameric AP so I can report that much is true . It is slightly more powerful than the trimer . The melting point would be a definitive property for
DPPP as compared to AP . Solubility and
crystal examination by microscope should be revealing also . Solubility in isopropanol is one thing I would check . Impact sensitivity is another identifier . Response to ignition ,
critical mass for unconfined DDT , could be useful distinctions . And a final point of interest for me is related to the possibility of coprecipitation of a mixed peroxides containing DPPP , possibly by sequencing the peroxidation to produce a mixed product deliberately , wherein the presence of AP would be an expected result as a component in the product , rather than an impurity needing to be removed . Different proportions of a mixed product could result in a solid or plastic or liquid composition .

[Edited on 16-12-2004 by Rosco Bodine]

Well, look at the link below!

Hideki Matsumoto - 16-12-2004 at 10:02

http://community.webshots.com/user/matsumoto_hideki

read the captions, Dr.boom is right this stuff looks nothing like AP or TAP. It is way way more energetic.
if not DPPP what the hell is it?

Very interesting!

chemoleo - 16-12-2004 at 12:32

I think at last we are on to something here, good work!

A couple of questions/points:

What was the yield? You use a rather large amount. Also you don't specify how much H2O2 you added to your 500 ml of reaction mix.

Secondly, regarding the crystallisation: You mention that it crystallises out immediately, yet you seem to add the H2O2 very slowly to avoid a massive temperature increase. If you add it slowly, how then can you finish the whole addition of such a large volume in less than four minutes (as you advise on the web page)? In other words, could you please describe what exactly you did? How much H2O2 did you add, how did you achieve such rapid cooling, and under what conditions do you get this secondary decomposition reaction that redissolves the crystals to produce something lachrymatory?
Please describe it as good as you can, as the step of H2O2 addition in terms of amounts, temp, and time seems quite crucial.

In terms of evidence we seem to have the following:

- smells different (which I find very convincing - seriously)
- Crystals form RAPIDLY, unlike AP/tAP, where you leave the batch for hours in the cold (or are there some methods where this is not the case?)
- Crystals redissolve in the reaction mix if left unchecked, unlike AP once again.
- Solubilities - could someone please point out exactly what AP is soluble in or not, versus DPPP?
- Volatility - AP was reported to lose 0.9% of its mass per hour at room temperature at air (from a paper in Propellants, Pyrotechnics and Explosives) - DPPP presumably isn't volatile?
- Power - yet needs to be confirmed.
- Impact sensitivity - seemingly lower for DPPP?

Oh, and I don't see as much a problem of pouring acetone into HCl, after all, what causes the heat and acid spitting is the heat caused by hydration of the acid. Not so much the case with acetone, being water free. Of course, one never knows had one never tried this before, so I guess that it's advisable to add the acid to the acetone rather than vice versa.
Anyway, this is an oldschool chemistry advice, and I myself have done it a few times the other way round, but never had a problem. Probably one of those things where a few people got hurt who did it uncarefully, and this then made it into every chem book.

At last... tsts DrBoom/Hideki, noone is doubting the validity of your claims at this point, so no need for an extra alias to add extra substance to your work!

[Edited on 17-12-2004 by chemoleo]

sylla - 16-12-2004 at 14:47

I've checked my notes and I tested AP to be 200g/l in acetone while DPPP was only 100g/l. I only tested it in a few ml because of the hazardous chemicals.

With methanol is was about 50g/l for both.

With ethyl ether it was 100g/l for DPPP and I lost the result for AP (didn't write it :/)

So it seems solubility in acetone is the good test ! If someone have "DPPP" and AP it would be fun to have a better value.

Btw, can these compound peroxidize the ether into the dangerous ether peroxide ?

These results are poor but seems to show they have different sollubilities in acetone which is a very good thing in favor of DPPP

if you have a sample of both, mix them, dissolve it in acetone and add water, they really do separate

[Edited on 16-12-2004 by sylla]

What i used to make this stuff with.

Hideki Matsumoto - 16-12-2004 at 16:14

alrighty then.

Acetone to HCL 1:1
heat until the liquid changes to a dark red,brown, then
cool off down to as cold as possible..
H2O2 is 2:1 250+250=500 (Pentachlorophorone) + 500ml H2O2 = DPPP

example I have 500ml of Chlorophorone (dark liquid)
I add 490-500ml of 35% H2O2

You will instantly get a yellow- white precip let the reaction continue for ~3 sec and then immediatly filter the crystals out and dispose of the filtered liquid.
YOU MUST USE ammonium hydroxide bath to nutralize the HCL in the DPPP or you'll have a runaway reaction. This whole process must be done in seconds.
Yeild is defently 80-90% or thereabouts. high effecientcy.

You can either slowly add the peroxide or fudge it.

Hideki Matsumoto - 16-12-2004 at 16:28

Sure slowly adding the peroxide will only delay the onset of the final decomposition. Either way you will have a decomposition reaction if you leave the reaction too long. i find by chilling both chems down to as cold as possible say realistically -2c , the reaction chugs along but the crystalization is very slow. as soon as the crystals appear the heating beings. the temperature shoots way up and after 4 secs the liquid turns clear and the secondary reaction occurs, reverting the DPPP into acetone, Phorone, HCL, Cl2 and water vapour into an irratating acid cloud which will burn your face shut. You have to filter out the crystals before the liquid turns piss yellow and nutralize the HCL using Ammonium Hydoxide. As I said again all this must be done in a matter of seconds. YEILD IS EXTREAMLY GOOD!! up to 90%

Rosco Bodine - 16-12-2004 at 16:55

If you are experiencing that sort of thermal effect , it may be useful to perform the peroxidation step in a shallow
layer , something like a Fernbach culture flask or even a glass baking tray , either
of which would be prechilled to a freezing
cold temperature and set upon a salted layer of ice or in a salted ice bath . Then
the reaction mixture could be quenched by
dumping it into a large amount of cold water or onto crushed ice , perhaps even dumping the mixture directly into the same cooling bath . 3 or 4 seconds is not much time and perhaps using a shallow layer with greater heat exchange area would provide a longer time window , and lessen the chance of a sudden decomposition from overheating . A teflon coated aluminum pan would give better heat transfer , but of course it would not be transparent , so a white teflon washer
or rod , perhaps the stirring rod , would need to be placed in the solution to see the color change to clear . I wonder if you have tried anticipating the endpoint by simply dumping the mixture when it clarifies , knowing that in a few seconds the reaction will go to decomposition , or do you wait for the yellow color to begin to reappear and then dump the reaction ?

[Edited on 17-12-2004 by Rosco Bodine]

chemoleo - 16-12-2004 at 17:03

Can I just ask, are you therefore getting about 200 grams of this substance??? That would very roughly equate to 90% yield. This would be an incredible yield by the way... and sounds rather optimistic to me.

And let me get this straight: After four seconds, you filter. Filtering takes several minutes. While it's filtering, you are adding the ammonia, to neutralise it? When do you do your neutralisation step?
Or are you neutralising after 4 seconds, and then filtering?

Rosco Bodine - 16-12-2004 at 17:14

I just thought of a good idea for a neutralizing salt bath . If you make
a solution of ammonium nitrate and
mix in some hydrated lime with it ,
you get a mixed solution of calcium nitrate
and ammonium hydroxide . Dump this over crushed ice and you have a salted
ice bath reeking of ammonia , and the
byproducts of neutralization would be
highly soluble and not interfere with the
filtration of the DPPP .

DDDP reaction

Dr. BOOM - 16-12-2004 at 17:23

the production of the crystalline mass = 70% of the liquid solution...some chlorine was liberated, but not much---

I did another detonation test and have concluded that the substance created is not AP. It doesn't have the smell nor the unstable properties of AP...crystals are different too. It is a sharper explosive.

yup 90% yeild ... not 70%

Hideki Matsumoto - 16-12-2004 at 18:47

You can pour the ammonia over the crystals.... yes this method also works. I willl take all your pieces of advice. The shallow pan method sound interesting, though it will have to me made of pyrex. I expect the same results.
I got about 454.7ml = maybe 80-100g due to the density being very very low.

PainKilla - 16-12-2004 at 19:08

I am going to try this tommorow and post comprehensive results with VoD testings etc, I doubt pictures but if my freind can grab his camera, hopefully I can get that too. Hideki, I have a couple of questions....

How Senstive to AP is this?
Is it volatile, flammablity the same, more friction/schock sensitive?
The ratio of acetone/hcl is 1:1 and h2o2 is 2:1.... do you mean 2:1 when they are combined or seperate...

IE

50ml acetone+50ml HCl + 100ml h2o2, or
50ml acetone+50ml HCl + 200ml h2o2...

Also, does the NH4OH have to be a particular concentration or does regular supermarket 3% work?

Thanks!

Rosco Bodine - 16-12-2004 at 19:14

The sudden heat you describe as occurring simultaneous with crystallization could actually be heat of crystallization ,
and it may be possible to moderate the effect by seeding the reaction with a few crystals from an earlier batch , early in the addition of the peroxide . This could possibly also have undesirable effects or no effect at all .

Distill the solution first.

Joeychemist - 16-12-2004 at 19:26

Dr Boom.

There is no way you can have 90% DPPP yield, when you did not purify the phorone. The key to this explosive is the production of the phorone first. :cool:

. Almost all of the AP formation can be avoided if one isolates and purifies the phorone before introducing the hydrogen peroxide.

This could be done by distillation. One would then need to modify the DPPP procedure accordingly to reintroduce the necessary acid, rather similar to the AP process but without the acetone. In theory if the reaction proceeds there would be no possibility of any AP forming (assuming no phorone reverts back to acetone) thus creating pure DPPP.( you can then remove any AP that did form by decomposing it in hot water,(because DPPP dose not decompose in water until about 185c, as I said above.) Have you tried to purify you end product yet.

70-90% of the volume becomes DPPP,yes

Hideki Matsumoto - 17-12-2004 at 01:39

sorry no, the volume of PCP ( pentachlorophorone) becomes the DPPP. Usually in my yeild this is about 90% of the liquid volume. HCL acts as a catalyst only. i yeild 100-300g per batch.

Tried a DPPP charge today against an AP charge

Hideki Matsumoto - 18-12-2004 at 00:40

Yes, now that I have some results!!
I tried an AP 50g charge of equal weight and size against a 50g DPPP charge and I have to say the results were awe striking!! The AP detonated with a bright orange flash and loud sharp crack that we all know and love.
The charge was placed on a piece of 1" thick metal sheet and the blast from the AP charge was strong enough to put a dinger in the sheeting. However the DPPP charge cut right through the sheeting as though it was butter. there was also very little flash during detonation. weird stuff....

Higher Vod

Joeychemist - 18-12-2004 at 01:19

Quote:

Originally posted by Hideki Matsumotothere was also very little flash during detonation. weird stuff....

There was no flash or noticeable fireball because the DPPP has a higher VoD than AP dose at around 5000 m/s. I'm not sure how high, (as no one actually knows). but I think that the very small crystal size plays a large part in this explosives high VoD because it's not the density that gives it such high a VoD as DPPP crystals have around the same density as AP dose (It’s to hard to tell with my crappy scale though).

crystal size influencing devol?

Hideki Matsumoto - 18-12-2004 at 09:08

Well I would expect that the DPPP detonates at roughly the same speed a PETN, this due to the fact that I have seen PETN go off before, and know its characteristic cutting power. DPPP acts in much the same way and will cut as well. It also detonates at much faster velocity than MEKPAN and other organic peroxides. This DPPP detonates so fast it looks like a light blur, and has an extreramly sharp crack when it goes off. Again I am just eyeing it to make a rough estimate here. Blast fragments are WAY smaller (dust sized) than MEKPAN or other peroxides. So I do beleive the patent was right about 9Km/sec.

Rosco Bodine - 18-12-2004 at 11:51

Now I really have my curiosity peaked , wondering if the DPPP would be stable when wetted with the syrupy liquid mixed
peroxide AP / MEKP . If it is chemically compatable , as it well might be , then there is potential for a much greater density composition of wetted DPPP having no dead airspace between the particles , or there is even possibility of a tertiary eutectic high density solid or plastic or liquid . Such a composition could be a relatively stable organic peroxide "super explosive" , never before described .

yup , de dip , dipdip

It could even be a "superduper explosive"

H2O2 concentration

Smoer - 18-12-2004 at 13:48

I saw there was used 35% H2O2,But I have only30%.So,will this work too?and do I have to ad more then or will the same amount as with 35% be ok?

cheerz
Smoer

The_Davster - 18-12-2004 at 14:17

It should work just add more. Calculate to get the volume of 30% you would need.

superduper explosive

Joeychemist - 18-12-2004 at 14:18

Rosco

Ok, let’s just say that this primary has a VoD of 9000 m/s and is by far more stable then AP. What explosives would be the best choices to use to try to create are "superduper explosive"????

A few come to mind, like DPPP putty, Dissolve DPPP and Nitro cellulose in acetone. Then let the excesses acetones evaporate. Or I have a friend who re-crystallizes his AP with MHN that should work with DPPP. These are definatly not our superduper explosive but they should work fine.

I have also thought about dissolving DPPP and RDX in a solvent like acetone and allowing the mix to recrystalize to create a high explosive putty that can be detonated by fuse but is also stable, safe and easy to make.

Smoer, 30% H2O2 will work just fine. :cool:

Smoer - 18-12-2004 at 14:29

OK thanks.

So,
For the phoron I used 10ml HCl(29%) and 10ml aceton.
I should use 23,33=23.5ml H2O2 30%.

This is just a test so I use small quantities.

Rosco Bodine - 18-12-2004 at 15:41

Quote:

Originally posted by Joeychemist
Rosco
Ok, let’s just say that this primary has a VoD of 9000 m/s and is by far more stable then AP. What explosives would be the best choices to use to try to create are "superduper explosive"????

Already said it twice before in this thread that what I have in mind is a tertiary composition with coprecipitated MEKP / AP . As for stability , AP is actually quite stable within it's known limitations . So is MEKP .

Quote:

A few come to mind, like DPPP putty, Dissolve DPPP and Nitro cellulose in acetone. Then let the excesses acetones evaporate. Or I have a friend who re-crystallizes his AP with MHN that should work with DPPP. These are definatly not our superduper explosive but they should work fine.

Yeah all the other ways in which AP is used , the DPPP may possibly substitute for AP .

Quote:

I have also thought about dissolving DPPP and RDX in a solvent like acetone and allowing the mix to recrystalize to create a high explosive putty that can be detonated by fuse but is also stable, safe and easy to make.

Maybe , but there you may have compatability problems . What makes you think a plastic composition would result ?

Quote:

Smoer, 30% H2O2 will work just fine. :cool:

Axt - 18-12-2004 at 17:07

Quote:

Originally posted by Joeychemist
Ok, let’s just say that this primary has a VoD of 9000 m/s and is by far more stable then AP. What explosives would be the best choices to use to try to create are "superduper explosive"????

It's possible that peroxidation of acetylacetone would result in a polymeric energetic plasiticiser, viscosity could be varied by addition of MEKP. The product should be more powerful then AP being a larger molecule with better oxygen balance. Thats purely theoretical, i've no idea on the actual consistancy of acetylacetone diperoxide, and I have no desire to go kneading a polymeric peroxide.

As to the issues with your credibility Hideki, since you have pictures of its synthesis, I suppose you have no problems providing pictures of a 1" plate cut "as though it was butter", lest your experiances will be left with the fantacious ring of felled trees around the bonfire you have <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=1031">spoken of</a>. I've never seen the orange flash from AP that "we all know and love" you speak of either, many inconsistancies here Hideki, I hope you can set these issues straight.

oh the picture I have !!!

Hideki Matsumoto - 18-12-2004 at 17:49

Ok you don't beleive me... oh don't worry when I get some time to upload my photos you'll see....
i have already provided some pics about the production of DPPP now I will have to give you an AP vs DPPP shot.
no problem/

As for that orange flash when AP detonates... it aways happens although it is not very bright....

[Edited on 19-12-2004 by Hideki Matsumoto]

Joeychemist - 18-12-2004 at 18:19

Quote:

Originally posted by Rosco Bodine but there you may have compatability problems . What makes you think a plastic composition would result ?

Rosco

I’m not completely sure that DPPP and RDX would re-crystallize to form putty or a plastic, it might even form a liquid or a solid crusty cake. But if incompatibility is not a problem then the mixture should have a very high density and would be able to be detonated by fuse. If the mix were to form into a solid crusty cake after the solvent evaporates, it could still be poured into molds to fit the purpose of its use.

Hideki, did you press the DPPP charge that cut through the 1” piece of steel. If so, did you calculate the density of the DPPP after it had been pressed? How much did the charge weight? What was the charge in total made of??

Axt - 18-12-2004 at 18:55

Quote:

Originally posted by Hideki Matsumoto
Ok you don't beleive me...

I dont believe, nor disbelieve you. Since you are inflating claims, why would I have blind faith in your credibility.

Quote:

Originally posted by Hideki Matsumoto
...with a bright orange flash

Quote:

Originally posted by Hideki Matsumoto
...it is not very bright

See my point.

Checking PATR for acetylacetone diperoxide (AADP), properties are: very explosive, not volatile, glassy syrup. OB is nearly the same as DPPP. Seems that it would form a plastic mass, though safety is still a concern. Its syth is the same as AP.

If DPPP were to have the properties as claimed in the patent, in combination with AADP a "superduper explosive" should result :cool:

The_Davster - 18-12-2004 at 21:07

Well I tried DPPP a try....Mixed sucess.

25mL of acetone was mixed with 25mL of HCl. It was heated on a salt/water bath for 45 min with the temp between 50-70 degrees the entire time. I recieved a light orange colored solution. This was then heated for 15 min at a higher temp than befor eto drive out excess acetone. This was then cooled via freezer till it was at -20, the solution was a medium orange color, not light, not dark, just orange. It was much lighter than the pic on that site. When it had reached -20 it was transfered to a 1.5L beaker( Using Roscoe's surface area idea) in a salt ice bath. 50mL of -20 35% H2O2 was very quickely all poured in in a circular motion. Strange....10s has passed by and there has still be no ppt and the solution is still the same color. At this time I am terrified that it is going to suddenly runaway on me. After 20s has passed by the solution is still the same as at 10s...I am full of adrenaline...For reasons I can no longer remember I dump in my neutralizing solution( 400mL commercial ammonia +7g NaOH). There was no ppt

.

I go to satrt the washing of the glassware and in my haste i put the last drop of H2O2 in the beaker in which the DCP was cooled in (150mL), there was still a single drop of DCP solution in there. So I get back to the lab bench after washing the graduated cylinders and the 1.5L beaker, I grab the 150mL beaker to go wash it and in that small drops of reactants in the bottom, crystals have appeared

. I have filtered this and am drying it as I type.

In hindsight I should have let the DCP and H2O2 react a bit longer... My cooling must have been too effecient

for such a small volume. Oh well, I wil try again in a few days.

Maybe heat longer

Joeychemist - 18-12-2004 at 21:21

Rogue chemist

I would suggest heating the acetone and HCl longer, I would go so far as to say twice as long at the same temperature will do you good. every time I make phorone it is not orange but a very dark red color.

PainKilla - 18-12-2004 at 21:42

I am curious.... while the original procedure may be easy, I think that this could be easier and less dangerous in terms of filtering, with the chlorination of the dichlorophorone.

Would it be possible to follow Hideki's method to dichlorophorone and then bubble chlorine into the mixture, to form pentachlorophorone? It seems that will all the multiple reactions occuring, much heat is produced.

Dichlorophorone--->DPPP step obviously produces a lot of heat, and probably adds to the decomposition rate of the whole mixture... Especially the HCl+H2O2-->Cl reaction, though I am not sure.

I propose a direct chlorination of the dichlorophorone followed by a peroxidation. This adds an extra step, but allows easier management of calculations/cooling etc....

Basically---->
The original reaction:

Acetone+HCl--->DCP

Catalyst HCl
DCP+ H2O2 ---> lots of side reactions-->DPPP

We can change this too-->

Acetone+HCl--->DCP
DCP+Cl -->PCP (pentachlorophorone)
PCP+H2O2 -->DPPP

This is simplified for viewing obviously, but with the chlorination, we can control the temperature much much easier, as instead of going from DCP-->DPPP, we add the extra steps in and PCP-->DPPP instead.... This would also possibly remove the whole possibilty of all the stuff decomposing, and any other hazards....

Of course, working with chlorine isn't the safest of things either, and it must be important to see whether chlorine will affect the end products as Cl+DPPP-->boom, will not be good, or extra chlorine possibly destroying the entire structure of DCP (unlikely)....

Input please?

I agree about adding steps !!

Hideki Matsumoto - 18-12-2004 at 21:51

Actually that is probably what is happening to me. The rapid relasal of Cl is probably causing the majority heating. hmmm well I will give it a shot. I still have to get those detonation pictures of the AP vs the DPPP on the webshots.com account. Somepoeple think I am exaggerating... well once those pics are posted, well see... Anyway ... by adding steps to the production of DPPP we may actually get little heating, I will have to try this! This would be a +!!

Yes My PentaChlorophorone is almost black-red color, never orange. I tried while it was cooling to add 2-3 drops of H2O2 and the color changed to a lighter shade. I came back 3hrs later and the stuff was back to dark-red but had a punjent smell of Cl2. when I used my peroxydation method I got my best yeild, to date..

[Edited on 19-12-2004 by Hideki Matsumoto]

PainKilla - 18-12-2004 at 23:40

Ah, good to see I'm not totally stupid lol. I have bought a hotplate and ammonia to try this out monday, hopefully with the Cl method, but I will try the other one if I can't do the Cl way.

I defeintly think its the H2O2+HCl-->Cl2 side reaction that makes the temperatue extremely high and all that fun stuff. It would be preferable I think to do as both methods involve Cl gas and better to get a more controlled reacton by using Cl than not using it and getting a possible cloud of war gas :x....

How much ammonia does this need to be dumped in BTW?

right on Painkilla!

Hideki Matsumoto - 19-12-2004 at 00:05

Yup, i just tried a micro small batch of DPPP and got same reation as what painkilla is describing... I compaired this to HCL and h2O2 reaction and they are with out a doubt identicle. So Now i have to find away of making this reaction either occur slower or stop it all together..
hmmm.

just a though, use chilled ammonia to cease reation?

$0meb0dy - 19-12-2004 at 09:00

I just tried it.
It's drying know, but when burning a bit while it's wet is doens't even look like AP.
There wasn't even a flame.
I'll do some more test when it's dry.

But my yield was crap and they aren't super fine cristals.
But still it could be normal AP maiby, we'll see...
[Edited on 19-12-2004 by $0meb0dy]

[Edited on 19-12-2004 by $0meb0dy]

PainKilla - 19-12-2004 at 09:23

I will be trying this today, probably using the Cl method, but if someone could review this quickly because I have to use a makeshift Cl generator....

Will Cl eat through or cause adverse reactions to plastics (soda bottle plastics and the fish tank tubing)?

I will try the other way if this way becomes unavaible.... Unfortently I have only 22.4% colored HCl, but it seems pretty pure aside from the surfactant and coloring, I hope it works :/.

The_Davster - 19-12-2004 at 10:31

Fish tank tubing works fine, although it will become coloured white on the inside. I use it for bubbling chlorine all the time.

Low temperature chlorophorone production!

Hideki Matsumoto - 20-12-2004 at 17:58

Wow!! Just decided to take heat out of the equation for Chlorophorone production... results are looking good.
this must be the cold forming method in the other patent they were talking about.

[Edited on 21-12-2004 by Hideki Matsumoto]

DPPP breakthrough!! Video proof!!

Hideki Matsumoto - 21-12-2004 at 12:16

Hello, I have just made a video compairing the power of AP vs DPPP and the results are truly amazing!!

I will be finding a host for these videos shortly.

------1 post needed NOT THREE!

Dr. BOOM - 21-12-2004 at 15:11

grrr...stop triple posting, man...it gets rater annoying!

( :mad:

Edit by Chemoleo: AND YOU STOP POSTING FROM TWO USERNAMES! GROW UP!)
-------------------
righty then, Hideki can't control his excitement and its understandable because heres why:

I think hes onto something:

I did a test with AP & DPPP yesterday and the energy level is considerbly higher with the supposed DPPP product. The color is noticeably different too. My DPPP is creamy yellow---in comparison to DiCyclo Acetone Peroxide which is bone white crystalline mass. When placed in an oven with an air temperature of 195-200 C the DPPP product explodes spontaously. In comparion DiCyclo acetone peroxide which just sits their and melts--then vapours off without igniting. Weird stuff. When confined DPPP acts like Dicyclo Acetone peroxide and detonates...

Clearly their was a difference in energy released.

I tried 2.5 grams of high density DPPP vs 2.5 grams of high density Acetone Peroxide packed into a .458 winchester mag shell case with flexon plasticized ignition cord and crimped. Each device was placed into a metal soup can to contain high speed particles--- the results were remarkable.

DPPP device tore the soup can into extremely small-sharp pieces while the Acetone Peroxide device had a harder time tearing through the metal container---soup can looked like it was peeled apart but it was still in one piece, more or less.

[Edited on 21-12-2004 by chemoleo]

90% DPPP yeild

Hideki Matsumoto - 21-12-2004 at 19:49

Condensing the Pentachlorophorone at 60c turns out the best results!

This picture is of the yeild with that method.. look at the soild mass of yellow crystals!

90% DPPP.jpg - 138kB

Video

Hideki Matsumoto - 21-12-2004 at 19:57

look at this !
fist movie is of .01g (pea sized) lump of DPPP going off unconfined!
the explosion was strong enough to blow a hole in the metal foil and created a small shock wave

Something else to metion was the disappearaing metal foil plate... this explains the bright white flash as most of it was blown into small dust particles which added to the explosion. This also indicates the high velocities metioned in the german pattent.

[Edited on 22-12-2004 by Hideki Matsumoto]

Attachment: 100_2453.MOV (940kB)
This file has been downloaded 1864 times

video DPPP production in a container

Hideki Matsumoto - 21-12-2004 at 20:12

Here is video of DPPP being made in a container. I have just added the H202 and then 2sec later this happend. a second after this shot was taken 400ml of Concentrated Ammonium Hydroxide (aq) was added to the solution to nul the reaction.

The result was about 250-300g of DPPP crystals.
More than enough to make a powerful cutting charge.

javascript :icon('

Attachment: Untitled 1.mov (804kB)
This file has been downloaded 1482 times

You are so dead!!!

Joeychemist - 21-12-2004 at 20:22

You have been told to stop triple posting under two names and yet you continue to do so without even apologizing to the moderator that let you live. You’re wasting forum space. Please stop! :mad:

You talk about us not believing you, well you’re dumb right we don’t believe you. Sure you can make DPPP but you’re stories contradict each other.exp;
quote:

Originally posted by Hideki Matsumoto
...with a bright orange flash

quote:

Originally posted by Hideki Matsumoto
...it is not very bright

See what I mean. And while were are talking about you’re credibility here why don’t you show us those pictures of the 1” piece of steel that you’re DPPP supposedly “cut through like butter”?
and why not shoe use the other pics you promised us? as I see it from you’re last posts you have no problems taking pictuer from you're last experiment. So go get the piece of steel, take a picture and show it to use. WTF is wrong. :mad:

Any idiot can follow someone else’s instructions and make DPPP, and any idiot can blow-bag about what he dose and doesn’t do with these explosives. Hideki you are not a credible person in my book.

[Edited on 22-12-2004 by Joeychemist]

oooh anger!! over what?

Hideki Matsumoto - 21-12-2004 at 20:27

hey there, want more proof! ?
Pictures of the 1" metal plate coming very shortly ..
I used a shaped film canister full of hardpacked DPPP to do that by the way. So not very much... I unfortunatly didn't have video shot at the time... sorry..

[Edited on 22-12-2004 by Hideki Matsumoto]

I am posting under two names? what?

Hideki Matsumoto - 21-12-2004 at 20:33

I am on a LAN that is why i have same IP adress as Dr.Boom... Thank you it is called a router dumb shit!
fellow who is in the same building as i am is helping me with the video and pict work...

:mad:

Compair this with the det video above

Hideki Matsumoto - 21-12-2004 at 20:57

this is exactly the same amount of DPPP I used in the above video but this is Trimeric AP (TriAcetone Peroxide)
not that in small amounts it doesn't detonate rather poofm (delfagrate violently)

Attachment: APsmall.MOV (3kB)
This file has been downloaded 1368 times

WTF!

Joeychemist - 21-12-2004 at 21:09

You tard you just don’t get it do you, Use the F**KING EDIT BUTTON AND STOP QAUDRUPLE POSTING!!! :mad:

Fine I believe you that you can make DPPP, Do you want a parade or something.

I don’t believe you cut a 1” piece of steel with only 50g of thought, so show me that and I will shut my mouth good and tight, but not until you show actual proof.

I suggest you nicely apologies to the mods, and politely ask them to clean up you’re mess of useless posts.

Hideki Matsumoto - 21-12-2004 at 21:18

Quote:

Originally posted by Joeychemist
You tard you just don’t get it do you, Use the F**KING EDIT BUTTON AND STOP QAUDRUPLE POSTING!!! :mad:

Fine I believe you that you can make DPPP, Do you want a parade or something.

Wasn't asking for a parade flamer...
Wait and i'll show you the picture now shut up!
YOu are acting like you think my DPPP synth and shit is bogus... i wish to prove myself That EVERYTHING I SAID WAS TRUE!!

Blast looked like this for a film canister full of DPPP

Hideki Matsumoto - 21-12-2004 at 21:40

I am starting to get tired of flamers on this site.
Here is a low res picture of the metal panel close up.. it is also not 1in but 3/4" sorry for the inaccuracy.. I don't use imperial mesurements, I am in metric country.. As I said again this was a shaped charge taped to the plate and detonated... this is the result. This hole is actally pretty small (1.3cm) in compairison to the gigantic blast gouge that the charge made. The explosion from this was truly immense and could be felt 300ft away!

blastmetal.jpg - 71kB

So it wasn't 1" thick

Joeychemist - 21-12-2004 at 22:07

Quote:

Originally posted by Hideki MatsumotoI tried an AP 50g charge of equal weight and size against a 50g DPPP charge and I have to say the results were awe striking!! The AP detonated with a bright orange flash and loud sharp crack that we all know and love.The charge was placed on a piece of 1" thick metal sheet and the blast from the AP charge was strong enough to put a dinger in the sheeting. However the DPPP charge cut right through the sheeting as though it was butter. there was also very little flash during detonation. weird stuff....

You said no such thing in you're previous posts about it being a shaped charge. What material did you use for the liner of you're shaped charge?

I still suggest you appologise for all these posts as Mr.Chemoleo has already warned you about the double posting. I would think it in you're best interests to heed his advice.

Axt - 21-12-2004 at 22:17

We are sick of your bullshit.

Lets see what you have said so far in your short history here, and how it has changed after they were contested:

1) "1" plate" turns into "3/4" plate" (take a decent photo).
2) "50g charge" turns into a "shaped charge".
3) "Multiple trees" change into two little 3" shrubs, (3' from a bonfire!) Oh, but I guess being in a metric country you got that confused as well.
4) "200g charge" turns into "250g".
5) "Windows around the neighbourhood" turns into your "neighbours".
6) "Wood crate" turns into "wood/metal crate".
7) "1' deep crater" <- wasnt contested, but its complete bullshit. I do notice you always give measurements in inches, where did you say you live again?.
8) "Bright orange flash" turns into "not very bright".

Your either incredibly bloody stupid, or you think everone else is. Then you have the nerve to say "I am starting to get tired of flamers on this site", well, get use to it.

[Edited on 22-12-2004 by Axt]

Sorry you can't read well... or interpret things well .. TO BAD!

Hideki Matsumoto - 21-12-2004 at 23:11

1) "1" plate" turns into "3/4" plate" (take a decent photo). That was from a 300 Mb movie I am not posting the movie. its 0.75" thick sorry... I though it was 1" my mistake.

2) "~50g charge" turns into a "shaped charge".
yes ~50g shaped charge... ie) film canister shapened / bottom punched in to form a cone.. DPPP was pressed under high pressure slowly and moistend with distilled water.. wile compressing the water in the DPPP is forced out.

3) "Multiple trees" change into two little 3" shrubs, (3' from a bonfire!) Oh, but I guess being in a metric country you got that confused as well. ---2 trees and some shrubs got nailed yes... so what...

4) "200g charge" turns into "250g". --- so what 50g woopdy doo. I couldn't remember exact amount.. either or.javascript :icon(' :mad:

5) "Windows around the neighbourhood" turns into your "neighbours". never said this... Windows around the neighbourhood were rattled... neighbours broken yes... i said that.

6) "Wood crate" turns into "wood/metal crate". duh that one was explained dumb ass..... Metal lined wood .. READ THE FUCKING POST!!

7) "1' deep crater" <- wasnt contested, but its complete bullshit. I do notice you always give measurements in inches, where did you say you live again?. So what ... it was about 1 foot... 25cm or so

8) "Bright orange flash" turns into "not very bright".
Breif orange flash, not as bright as a deflagration.. some of the other isomers of Acetone peroxide give a much brighter orange flash.
:mad:

[Edited on 22-12-2004 by Hideki Matsumoto]

After getting e-mail from Dr.Boom and Matsumoto-san

Cato.exp - 21-12-2004 at 23:41

Both Dr. Boom and Matsumoto-san are on to SOMETHING BIG, so I wouldn't be flaming them if I were you axe and others.. They though this place was acceptable for what they were doing (sharing ideas) I guess they are wrong...

You're kidding right???

Joeychemist - 21-12-2004 at 23:48

You're jokeing right Cato.exp, (AKA, DR.boom and hidiki Matsumoto). You just joined two minutes ago. Like we wouldn't catch that one.

Axt is right, You are incredably stupid. You fool.

[Edited on 22-12-2004 by Joeychemist]

Axt - 22-12-2004 at 00:12

This isn't even up for debate. Do I really have to explain why you cant have a bonfire 3' from small trees? Do I really have to explain why 250g APAN in a bonfire won't drive a crater 1' into the ground. I sincerely hope you are banned.

Everything you have said is total and complete bullshit. Try fitting 50g into a film canister and you will see that. Common kodak film canisters have a volume of 32ml, now taking into account the volume taken by the shaped charge cone we can see the stupidity in your claim.

You are far too deep in you own shit to talk your way out of this.

BTW, I did see your post before you edited it, real mature.

[Edited on 22-12-2004 by Axt]

what the?

Dr. BOOM - 22-12-2004 at 01:50

( Edit by Chemoleo: AND YOU STOP POSTING FROM TWO USERNAMES! GROW UP!)

Hey Chemoleo, great advice but as far as i know I have 1 username, last time i checked. Your 1 user name per IP address is seriously screwed because anyone can mask an IP address or use a LAN system.
Common now Chemoleo, you took basic computing and networking, right?

I have asked Hideki to stop screwing with the forum and leaving multiple posts....yes it is annoying! If he doesn't just boot his f&*ing user name--- but if you bann his IP you will kick me off as well and because we are not the same person then you will have kicked me for no reason. i have not double posted, nor have I done anything to warrent that type of action.

HIDEKI STOP YOUR MULTIPLE POSTS NOW!
-------------
All future information regarding my finding with the mysterious DPPP synth are will no longer be shared.
It is nothing but a joke to you guys, oh well, be ignorent all you want.. the patient explains everything. Look it up and tell me I'm full of shit. i dare you.

[Edited on 22-12-2004 by Dr. BOOM]

[Edited on 22-12-2004 by Dr. BOOM]

vulture - 22-12-2004 at 02:29

I've had it with this Bullshit.

For now, Dr. Boom and Cato exp are banned because they are the same person.

Furthermore, if mister Hideki double posts AGAIN he is banned too! There are boundaries to patience and reason.

The info might or might not be true, but that is now irrelevant as this person killed his own credebility in a very thorough way.

PainKilla - 22-12-2004 at 03:29

I still believe him, whether it is actually DPPP or something else however is yet to be determined..... I shall post some results when I get around to making it. There is snow on ground and cold....and I hate the cold. However, it may serve as good cooling so I shall see, and hopefully be able to get a movie or at least pictures. I will also compare with something stronger than AP since it is "so strong."

Joeychemist - 22-12-2004 at 03:32

If you still belive him, check out his other lies if the had an accident thread.

[Edited on 22-12-2004 by Joeychemist]

Let's bring this back on track.

chemoleo - 22-12-2004 at 09:30

It started off so interesting - and I just don't believe he'd make up everything - despite some exaggerations.
Let's bring this back on topic, and forget the flaming/exaggerations etc for now.

What's important for us to find out whether this method of heating the HCl/acetone first, then adding H2O2 to the chilled chlorophorone, actually does yield crystals.
Did anyone succeed in it?

If so, it's Christmas time, and I hope someone finds the will to follow this up, in a more thorough way! There is lies no shame in not succeeding, at least not in our 'profession'!

Merry Christmas!

[Edited on 23-12-2004 by chemoleo]

How about you unban Dr.boom asshole

Hideki Matsumoto - 22-12-2004 at 10:05

I HAVE HAD IT WITH THIS SITES BULLSHIT
javascript :icon(' :mad:

Man you guys are assholes... As i said Dr.Boom is on a LAN.. i guess they don't have those in UK do they?

Just more evidence that this site has issues with their pride and ego... As soon as i posted the movies you guys got pissed offf ... I don't get it.. Oh and if you guys mail me threatning emails again ... i'll be forced to take action against this site...
By the way What i said wasn't BS at all.... You seem to be the BS around here, banning won't slove the problem ... get your ego under controll...

Edit by Chemoleo:
You've made your point, shown what you could, so let someone else try to verify it. Just like what is done in proper science. If it works for others, too, then the better!
Don't you think it's rather unlikely that there are 4 individuals, all from the 'same LAN', all having made DPPP successfully, and yet not knowing each other, but magically registering all around the same time, always in support of each other? This is why you suffer a lack of credibilty. So please, let someone else do it according to your descriptions, and wait to see your preparation of DPPP hopefully verified. There is no point in insisting in the same thing over and over again.

[Edited on 23-12-2004 by chemoleo]

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