inspector071
Hazard to Self
Posts: 69
Registered: 20-2-2012
Member Is Offline
Mood: No Mood
|
|
Acquiring chemicals for energetic syntheses
I've been a lurker for a while, and have been performing chemistry experiments for quite a few years. I've recently become interested in the energetic
materials. I started off by making some black powder, and now I'm making my way through the timeline into more modern energetics. Some of the ones
I've made recently are nitrocellulose and picric acid. My nitric acid was made from KNO3 and concentrated sulfuric and seemed to turn out quite
nicely, with only a faint yellow tint. I synthesized the picric acid from acetylsalicylic acid, but didn't start out with much and lost a lot of the
final picric acid from filtering. Is acetylsalicylic acid the preferred reagent for household synthesis of picric acid? If not, where can phenol be
acquired?
As soon as I distill some more nitric acid, I plan to create RDX. I bought some >99% hexamine heating tablets to try and nitrate.
I would also like to make some styphnic acid/lead styphnate but I don't know where resorcinol can be found.
Tetryl and pentaerythritol tetranitrate are also down on my list for energetics to synthesize but I cannot find a source for N,N-dimethylaniline or
pentaerythritol.
As an individual, what are the best methods for acquiring phenol, resorcinol, N,N-dimethylaniline, and pentaerythritol?
|
|
|
Ral123
National Hazard
Posts: 735
Registered: 31-12-2011
Member Is Offline
Mood: No Mood
|
|
Is there a real practical reason for an individual to make tetryl? Every time I think of making it I give up to the idea of just mixing rdx and
tnt(also very inpractical). I don't think there's a convenient way of getting pentaeritiritol. I have opportunity to purchase but it will cost almost
as much a the fuming nitric acid.
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Open for the spoon.
TNP is easily prepared from ASA in the home lab. It is a great and cheap substrate and is available globally. What more could you ask for. Who needs
phenol? Follow a good procedure (try Rosco's ASA >TNP wright up) and you will get great yields and good purity with a single recrystallization.
Who needs pentaerythritol? I hear that erythritol is a great sugar replacement though. It is many people's sugar alcohol of choice.
Resorcinol is discussed to death here. It can be synthesized. I hope you used the forum search engine. If you didn't you missed a lot. Resorcinol can
be purchased online as well, IIRC.
Good luck and don't advance to quickly. These experiments you plan have a great capacity to cause suffering and loss.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
inspector071
Hazard to Self
Posts: 69
Registered: 20-2-2012
Member Is Offline
Mood: No Mood
|
|
Thanks for the responses. I just thought I would attempt to make tetyrl, but you're right: it doesn't seem very practical to make. And while I have
easy access to toluene, the TNT synthesis is rather involved.
Is ASA preferred over SA to make TNP? Both are easy to get. Half a pound of SA seems to run about $14. I believe I found Rosco's procedure you
mentioned. Is it TNP from ASA and NaNO3 you are referring to?
Good point about the pentaerythritol vs erythritol. I'll order some of that and make some ETN instead.
It's been a while since I've been involved with a forum regularly, however I did search for each of my compounds but did not find much on a source of
resorcinol. It is of course available on chemical supply sites and it seems to be in acne/skin treatment in rather low concentrations, but I can't yet
find a source of small and pure amounts.
I am starting off slowly, partly because I can only distill so much nitric acid in a day with my 500 mL retort. Now I need to start thinking about
primaries. Silver acetylide sounds promising, and I still have a can of CaC2 from my days of playing around with carbide lamps. I read up on a method
of purifying sterling silver, though I might just be better off getting silver nitrate online somewhere. Will silver acetylide be sufficient for
detonating picric acid, RDX, and ETN?
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
Read this forum. Here is at least one discussions on Ag2C2. I was able to get phenol (and resorcinol) in a special shop. I bought there something
useful like H2O2, phenol and resorcinol. As for me, picric acide can be obtained very easy and you have no need in distillation. Read this forum, I
explained how it could be done in the most simple way. Usually mixed acide can be replaced by H2SO4+KNO3 (NaNO3). I made gun cotton using Ca(NO3)2.
Situation with RDX is worse: H2SO4 destroys it and therefore conc HNO3 is a must.
Women are more perilous sometimes, than any hi explosive.
|
|
|
Pulverulescent
National Hazard
Posts: 793
Registered: 31-1-2008
Member Is Offline
Mood: Torn between two monikers ─ "hissingnoise" and the present incarnation!
|
|
Styphnic acid is less powerful that TNT!
Its lead salt is a deflagrant used to initiate lead azide as LA needs high temperature for its certain detonation.
Hardly worth the effort, though . . .
P
"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"
A Einstein
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
That's true. Lead stiphnate's ability to initiate secondary hi explosive is low compared with lead azide for example. But, one the other hand,
preparation of styphnic acide is simpler than one of lead azide. If I remember numbers correctly, in one thick russian book was written something like
this: to initiate tetryl one needs 0.4 gr of lead azide or 2 gr of lead styphnate.
Women are more perilous sometimes, than any hi explosive.
|
|
|
inspector071
Hazard to Self
Posts: 69
Registered: 20-2-2012
Member Is Offline
Mood: No Mood
|
|
If I get my hands on some mercury, I can make some fulminate. With the chemicals I currently have, I could also make silver acetylide and lead
picrate. For detonating either RDX or ETN (or a mix of the two), and using picric acid as a booster, what would the preferred primary be?
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
silver acetylide is good enough. using picric acide as a booster to detonate RDX is rather strange idea- RDX is more sensitive. Once I used mercury
fulminate and at nearly killed myself. I think (but my opinion isn't shared with many people here) that TATP is nice primer. Do not make large amount
of primers- 2 gr is more than enough to make one (or two) detonators. If you wanna make silver acetylide, you must bubble acetilene through hot
solution of AgNO3 + some HNO3. To make TATP, use HCl as katalyst.
Women are more perilous sometimes, than any hi explosive.
|
|
|
inspector071
Hazard to Self
Posts: 69
Registered: 20-2-2012
Member Is Offline
Mood: No Mood
|
|
Ah, from all my reading so far I've seen picric acid referred to as a booster, while RDX and ETN are secondaries. I would have assumed RDX is less
sensitive. What are some good sources for making a proper detonator? The only reading material I've scrounged up so far on the subject is the Army's
munitions handbook which explains how to make blasting caps from brass casings. I reload for my firearms so I have plenty of brass on hand. I've also
heard of people using straws and plastic when dealing with picric and its salts. Is fuse to primary to secondary the preferred method, or would a
nichrome hot match work fine for silver acetylide as a primary?
Does anyone do much with DDNP? From what I've read its safer and more stable than a lot of other primaries and it can be made from picric acid. I
guess what I'm really looking for is a guide on primaries. Something like "this amount of primary can detonate this amount of secondary."
|
|
|
freedompyro
holmes1880
Posts: 116
Registered: 16-6-2011
Member Is Offline
Mood: No Mood
|
|
Silver Acetalyde is a suicidal primary... You must be thinking of the double salt Ag2C2.AgNO3.
If you can get a primary to detonate any amount of a secondary the detonation will continue to propagate through an infinite amount of the
secondary... LoL! Btw, Picric Acid is an even more insensitive secondary than RDX and ETN.
I never really understood why people use boosters for cap sensitive explosives. The only thing that needs a booster is something that isn't cap
sensitive like ANFO in a mine hole or a cheddite...
Good luck with Lead Picrate... Have not managed to get it to detonate anything without large amounts. The picrate metal salts and DDNP are very
finicky in their synthesis. Temperatures, agitation, etc... It all matters! You can end up with something that works like a secondary, or if your
lucky you end up with something that works as a primary...
[Edited on 23-2-2012 by freedompyro]
|
|
|
inspector071
Hazard to Self
Posts: 69
Registered: 20-2-2012
Member Is Offline
Mood: No Mood
|
|
Thanks for the tips! So is a double salt just a 1:1 ratio of silver nitrate and silver acetylide, with the nitrate acting as a desensitizer/inhibitor?
I'm aware once the secondary detonates it will continue to propogate, but im wondering if anyone has made a table saying "you need X g of lead picrate
(lead styphnate, mercury fulminate) to detonate RDX (PETN, picric acid, TNT)."
I may not use a booster, it was just a thought to plan out a reliable cap design. What do you feel is the easiest primary to work with for secondaries
like RDX and PETN (or ETN)?
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
A lot comes into factor, like shape, confinement, density, placement design, etc. It is not as black and white as your asking. I like silver acetylide
double salt as it is pretty east to prepare and works great. I also would place around .3g of melt-casted or compressed ETN in first, then the
compressed silver acetylide. Silver acetylide's flame sensitivity is such that a pyrogen layer is usually not needed, IMO.
[Edited on 23-2-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
