the baron of explosives
Harmless
Posts: 1
Registered: 5-5-2011
Member Is Offline
Mood: No Mood
|
|
Needing help in synthetis of PETN
Hi guys im new to this forum and i'm currently reading a book the chemsitry of powder and explosives. I'm am about to do PETN according to the method
in the text seen below: I am wondering if it's quite safe to do and what are the dangerous factors/what can go wrong. I have properly laboraty
equipment at home. Advices are appreciated !
Method:
PETN may be prepared, according to Naoum,109 by adding
100 grams of finely powdered pentaerythrite to 400 cc. of nitric
acid (1.52) while the temperature is maintained between 25° and
30° by efficient cooling. Toward the end of the nitration a certain
amount of the tetranitrate crystallizes out. The separation of the
product is completed by the gradual addition of 400 cc. of con-
centrated sulfuric acid (1.84) while the stirring and cooling are
continued. The mixture is not drowned, but the crude PETN
(85-90% of the theory) is filtered off directly, and washed first
with 50% sulfuric acid and then with water. It still contains
some occluded acid and is purified, according to Naoum, by dis-
solving in hot acetone to which a little ammonium carbonate is
added, and filtering the hot solution into twice its volume of 90%
alcohol by which the PETN is precipitated in fine needles.
Pentaerythrite may also be nitrated satisfactorily, and prob-
ably in better yield, without the use of sulfuric acid and with the
use of nitric acid from which the nitrous acid has been removed.
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
PETN is a pretty sensitive HE that has been discussed at great length on this site. I suggest you; <a
href="http://www.sciencemadness.org/talk/search.php?token=&srchtxt=PETN&srchfield=subject&srchuname=&f[]=all&srchfrom=0&filter
_distinct=yes&searchsubmit=Search">Try here first.</a> A.K.A. utfse
Read all of COPAE, read about nitration and the dangers, look into proper lab technique and risk management in the high explosives manufacturing
industry. I would never call making H.E. at home "safe," though if you do your homework and scale down you may prevent a catastrophe.
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.
|
|
gregxy
Hazard to Others
Posts: 421
Registered: 26-5-2006
Member Is Offline
Mood: No Mood
|
|
Here is a thread on safety.
http://www.sciencemadness.org/talk/viewthread.php?tid=13466#...
|
|
quicksilver
International Hazard
Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline
Mood: ~-=SWINGS=-~
|
|
It's all pretty much been said. However make sure you pull all that acid OUT of the final product. Without it being ph neutral the product becomes
increasingly sensitive and toxic during it's shelf life until a serious issue become irreversible. Re-crystallization is vital. The threads you were
directed to and advice give are a wise course of action.
|
|
detonator
Harmless
Posts: 29
Registered: 12-4-2011
Location: Maoming City, Guangdong Province, China.
Member Is Offline
Mood: No Mood
|
|
Mixture of fuming nitric acid(≥95%) and phosphorous anhydride,Proven to be an efficient Nitrating agent.
|
|
The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
Member Is Offline
Mood: .
|
|
And do not use the 100g scale in that procedure. Start with a gram and work up once you have a feeling for the material and the reaction.
|
|