| Pages:
1
..
4
5
6
7
8
..
37 |
shadeT
Hazard to Self
Posts: 56
Registered: 3-8-2003
Member Is Offline
Mood: No Mood
|
|
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]
|
|
|
J_O_H_N_Q
Harmless
Posts: 21
Registered: 25-9-2003
Member Is Offline
Mood: No Mood
|
|
Isophorone?
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
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
Isophorone has a different structure than regular phorone so it cannot be used.
|
|
|
Dr. BOOM
Banned
Posts: 14
Registered: 15-12-2004
Member Is Offline
Mood: No Mood
|
|
successful synthasis of DPPP explosive
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.
|
|
|
Joeychemist
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
Too much heat
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
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
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 .
|
|
|
Joeychemist
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
Please stay out off this,unless you wish to help
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
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
| 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 .
|
|
|
Dr. BOOM
Banned
Posts: 14
Registered: 15-12-2004
Member Is Offline
Mood: No Mood
|
|
just made DPPP... quite a bit different than AP
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 
|
|
|
Dr. BOOM
Banned
Posts: 14
Registered: 15-12-2004
Member Is Offline
Mood: No Mood
|
|
Alright, I got a better yeild with lower heat!
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.
|
|
|
Joeychemist
Hazard to Others
Posts: 275
Registered: 16-9-2004
Location: Canada
Member Is Offline
Mood: Sedated
|
|
Sorry
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
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
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
Alchimiste Belge Notoire
Posts: 110
Registered: 2-8-2003
Location: Belgium
Member Is Offline
Mood: No Mood
|
|
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
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
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]
|
|
|
Hideki Matsumoto
Banned
Posts: 32
Registered: 16-12-2004
Member Is Offline
Mood: No Mood
|
|
Well, look at the link below!
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?
|
|
|
chemoleo
Biochemicus Energeticus
Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline
Mood: crystalline
|
|
Very interesting!
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]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
|
|
|
sylla
Alchimiste Belge Notoire
Posts: 110
Registered: 2-8-2003
Location: Belgium
Member Is Offline
Mood: No Mood
|
|
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]
|
|
|
Hideki Matsumoto
Banned
Posts: 32
Registered: 16-12-2004
Member Is Offline
Mood: No Mood
|
|
What i used to make this stuff with.
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.
|
|
|
Hideki Matsumoto
Banned
Posts: 32
Registered: 16-12-2004
Member Is Offline
Mood: No Mood
|
|
You can either slowly add the peroxide or fudge it.
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
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
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
Biochemicus Energeticus
Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline
Mood: crystalline
|
|
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?
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
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 .
|
|
|
Dr. BOOM
Banned
Posts: 14
Registered: 15-12-2004
Member Is Offline
Mood: No Mood
|
|
DDDP reaction
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.
|
|
|
Hideki Matsumoto
Banned
Posts: 32
Registered: 16-12-2004
Member Is Offline
Mood: No Mood
|
|
yup 90% yeild ... not 70%
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
Hazard to Others
Posts: 306
Registered: 29-4-2004
Member Is Offline
Mood: No Mood
|
|
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!
|
|
|
| Pages:
1
..
4
5
6
7
8
..
37 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
