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Rosco Bodine
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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 .
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Joeychemist
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Distill the solution first.
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.
 . 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.
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Hideki Matsumoto
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70-90% of the volume becomes DPPP,yes
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.
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Hideki Matsumoto
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Tried a DPPP charge today against an AP charge
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....
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Joeychemist
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Higher Vod
| 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).
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Hideki Matsumoto
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crystal size influencing devol?
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.
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Rosco Bodine
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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"
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Smoer
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H2O2 concentration
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
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The_Davster
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It should work just add more. Calculate to get the volume of 30% you would need.
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Joeychemist
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superduper explosive
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.
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Smoer
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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.
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Rosco Bodine
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| 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.
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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. |
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Axt
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| 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.
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Hideki Matsumoto
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oh the picture I have !!!
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]
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Joeychemist
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| Quote: | | Originally posted by Rosco Bodine but there you may have compatability problems . What makes you think a plastic composition would result ?
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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??
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Axt
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| Quote: | Originally posted by Hideki Matsumoto
Ok you don't beleive me...
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I dont believe, nor disbelieve you. Since you <i>are</i> 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
<br><br>
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The_Davster
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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.
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Joeychemist
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Maybe heat longer
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.
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PainKilla
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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?
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Hideki Matsumoto
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I agree about adding steps !!
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]
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PainKilla
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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?
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Hideki Matsumoto
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right on Painkilla!
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?
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$0meb0dy
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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]
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PainKilla
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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 :/.
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The_Davster
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Fish tank tubing works fine, although it will become coloured white on the inside. I use it for bubbling chlorine all the time.
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