Morrow96 - 7-8-2025 at 21:36
So I’ve tried this twice. The first time was a success. Mixed acid method. 20 grams of Pentaerythrotil, 49mL sulfuric drain cleaner, and 68mL nitric
(67%). My second attempt I upped it to 32.5 grams but I didn’t also up the time control and it was a failure. But here’s the thing…it was only a
failure after trying it. The ‘fake’ PETN looked the same and feels the same, it’s just not going off. A TON of iNAP didn’t set it off. When I
burn test it, it takes a little longer to burn. So that’s maybe the tell tail sign of if the synthesis was a success? It’s not burning under a
flame as quick as the first batch that successfully goes off.
Curious what I made if it’s not PETN? And if so, can I put it back in something to get it workin? It’s like 70 grams I’d prefer to not waste it.
CuriousOnlooker - 8-8-2025 at 03:14
Probably a lower nitrate ester, such as pentaerythritol tri-nitrate
dettoo456 - 13-8-2025 at 04:26
PETN seems to be prepared in the easiest fashion either through WFNA, WFNA/H2SO4, or AN/H2SO4.
If you are adding the PE to the mixed acid solution and not yielding what you want, try to instead (on small scale to measure yield first) add the PE
slowly to the chilled H2SO4, then slowly drip in the azeo HNO3 and keep the temp low. Under anhydrous or aggresively dried reaction conditions, the
reaction can be run much hotter. Obviously 'wetter' solutions will be prone to hydrolysis though. CuriousOnlooker is probably correct, in that you may
have some less-nitrated products.
ManyInterests - 13-9-2025 at 00:37
I made PETN twice, once with 90% nitric acid and sulfuric acid (I should not have used sulfuric acid with nitric acid that concentrated) and a second
time with ammonium nitrate and sulfuric acid. I had PETN that detonated both time readily in blasting caps with both iNAP and NHN.
Did you control for temperature? The temperature range for PETN is very particular, you should keep it between 9C to 15C, and once it is all added it
you should let it reach room temperature for around 20 minutes before slowly heating it (hot water bath is safest) to around 40C for a few minutes
before crashing it in cold water.
Also did you recrystalize it? That is very critical. When I made PETN, I removed a LOT of impure crap with just the first recrystalization. I would
suggest at least 3 with hot acetone and adding some sodium bicarbonate or other weak base to the dissolved PETN to remove the acid impurities. Even
with very aggressive washing, the crude PETN can still have a lot of trapped residual acids. Adding urea to the crash water to act as an acid scrubber
is also highly recommended.