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Author: Subject: ETN synthesis without H2SO4
Mikhail01
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[*] posted on 29-12-2019 at 13:22
ETN synthesis without H2SO4


Have any of you tried nitrating erythritol with only 100% HNO3?
Some nitrations have to be performed without H2SO4, such as RDX... and as far as i know it is possible to nitrate certain polyols like mannitol, glycerine with great yield (using only WFNA)... can the same be applied to erythritol, and if so, do any of you have some experience or a synthesis?
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Pyro_cat
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[*] posted on 30-12-2019 at 19:51


From what I have read I think I remember that the H2SO4 is needed to pull out the water.

Is 100% nitric acid is that even possible outside a high end lab ?

Distilling nitric is not something I have experimented with yet.

See what happens if I get back into mastering nitrocellulose.
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Vosoryx
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[*] posted on 30-12-2019 at 19:57


if you can get WFNA. but i cant think of a way to WFNA without using H2SO4 in the first place.



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Mikhail01
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[*] posted on 31-12-2019 at 15:11


Quote: Originally posted by Pyro_cat  
From what I have read I think I remember that the H2SO4 is needed to pull out the water.

Is 100% nitric acid is that even possible outside a high end lab ?

You can distill the weak nitric acid to pretty close to 100% with the help of some concentrated H2SO4. I think you could make RDX even with less than 99% concentrated nitric acid but with great loss of yield...

Quote: Originally posted by Vosoryx  
if you can get WFNA. but i cant think of a way to WFNA without using H2SO4 in the first place.

Yes, the whole process has to involve H2SO4 either directly or indirectly, i was just curious about if someone has ever tried synthesizing ETN with only WFNA, i was curious about the possible yields...

I don't really want this thread to turn into an argument about costs or ease of acquiring reagents. Yes, i know you can obtain sulfuric acid relatively easily nowadays, but i'd like to add that even though you need H2SO4 to distill the weak HNO3 you can recycle it (with a bit of loss of sulfuric acid) so in the end, if one had a cheap source of HNO3 (Birkeland-Eyde process comes to mind, which might be even cheaper than buying actual lab grade HNO3 for some people, although time consuming-) and a proper distillation apparatus you could -almost- forget about the valuable sulfuric acid. It should be noted that sulfuric acid will likely be forbidden or strictly regulated in coming years, specially in the EU, and making nitric acid is easier than making sulfuric acid (you only need air, water and energy).

Looks like no one has tried it, so i will probably do it myself in the not so far future and report back, for the sake of it.

[Edited on 31-12-2019 by Mikhail01]
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underground
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[*] posted on 31-12-2019 at 16:24


It is actually working. I have seen a patent (don't remember which one exactly) that PETN has been made with FNA with almost 100% yields, so i am pretty sure it is working for ETN too. I would though make PETN or RDX with FNA.

[Edited on 1-1-2020 by underground]
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Microtek
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[*] posted on 2-1-2020 at 05:22


Whenever I have made PETN, I have always used WFNA (and no sulfuric). The yields are better, and the product is easier to purify (and it is more economical since the sulfuric that was used to concentrate the nitric in the first place can be reconcentrated and reused indefinitely). I'm sure that a similar process could be used for ETN.
Nitric acid can be concentrated using Mg(NO3)2 instead of sulfuric for breaking the azeotrope, though I don't think it is practical on the lab scale.
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