Just got a 91% yield of ETN after recrystallisation with 99% isoproypl alochol and I ve used 20g of erythrithol and dissolved it in 60ml of 98% conc
sulfuric, while keeping everything cool in an normal water bath, than when everything was dissolved I put the etn-sulfuric acid soulution in a
dropping funnel and dripped everything dropwise without cooling to the red fuming nitric acid, the temperture rised up to I guess close 40 after
everything was added, than everything was heated to 45C with a hot water bath (it was the same cooling water from the beginning) and was stirred for
30 min. No runaway happend and it was stirred the whole time. Than after the time was over I just cooled everything down with and salt-ice bath to 10C
and during this time ETN crystals started to percipitate. And at 10C I started to crash everything in an ice bath and filter it. I didnt meassure the
crude yield but after recrystallisation in 55C hot Isopropyl alcohol I let the solution cool down to 10C and crashed everything again in a 10% urea
solution and filter the recrystallised ETN. In the end I got 45,65g of ETN. Is this yield good? I am a beginner in engergetics I just synthesize the
ETN by a literature I found online here: https://yadda.icm.edu.pl/baztech/element/bwmeta1.element.baz...
So I was just wondering if this what I got was a average yield or not Microtek - 26-5-2025 at 12:59
91% is a decent yield for nitric esters. However, be aware that ETN is a very sensitive energetic, and 45 grams will easily kill you if it goes off at
the wrong time.Sir_Gawain - 26-5-2025 at 14:01
That’s interesting, I tried the dissolve-in-sulfuric-acid-first method and got an abysmal yield. Perhaps because I used 68% nitric acid and kept it
around 10°C. How much RFNA did you use?dettoo456 - 26-5-2025 at 16:39
@Sir_Gawain If he followed the prep method he linked, the molar ratio of HNO3 to Erythritol was very large; 3.4 moles HNO3 per OH-. That volume was
probably what kept the exotherm in check. Even then though, it is odd that such high yields were achieved at 40C instead of the normal chilled temps.
The excess of water in your synth is probably just what killed the yields.
Maybe if a molar excess of 2 or less HNO3:OH dissolved in DCM was used, the reverse addition scheme (H2SO4 & Erythritol to HNO3) could work. Or
simpler, as ETN isnt soluble in DCM afaik, DCM could be added to the mixture after nitration, and the excess HNO3 could be extracted and recycled,
granting enough H2SO4 was present to sequester water generated in the nitration. Sir_Gawain - 26-5-2025 at 21:00
Since nitric acid is nearly always the most expensive and difficult to obtain, shouldn’t the yield be based on it instead of erythritol?Laboratory of Liptakov - 27-5-2025 at 11:26
The article that started this thread looks like it was created using artificial intelligence. The error in the title and the other information looks
like it was put together from several sources. Including an unrealistically high yield. Especially for a beginner.....nitropyrotech - 27-5-2025 at 11:44
@Laboratory of Liptakov Hmm idk I just searched for some random ETN synthesis in the internet and found this article at my first attempt I got pretty
low yield I dont really remember it but it was like in the 70% range or so but that was because I didnt kept the temp, soon I ll just improved my
yield quickly by just letting everything stir at constantly at 45C, but I really got this big 91% yield, Idk how but it wasnt the weight of the remain
water I checked the weight after drying for a week or so flat on paper, I also tested it in some of my blasting caps and the ETN works just fine nitropyrotech - 27-5-2025 at 11:48
That’s interesting, I tried the dissolve-in-sulfuric-acid-first method and got an abysmal yield. Perhaps because I used 68% nitric acid and kept it
around 10°C. How much RFNA did you use?
I used regular RFNA I distilled my own from cheap Ammonium nitrate and melt sufluric acid drain cleaner, for my batch I used 96ml of RFNA Laboratory of Liptakov - 27-5-2025 at 12:31
nitropyrotech...Thanks for explain. Interesting.....
