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Author: Subject: New ETN Synthesis
dettoo456
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[*] posted on 6-3-2024 at 09:02


Yes, recryst from slightly basic NH4OH or Urea sol, air dry, and add Diphenylamine, centralite, curcumin, or guaiacol. ETN PBXs will store even better.
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[*] posted on 6-3-2024 at 15:39


Quote: Originally posted by pjig  
Quick question on stabilization of the final product. As literature claims, ETN stores poorly. Even if the materials are washed and stabilized with nitrogen scavenger, how long can this material safely bee stored? I know it’s big brother PETN store's indefinitely once re-crystallized and purified. I guess if stored properly cool location could years be possible for ETN?


ETN actually stores remarkably well. I would suggest two or three recrystalizations and add some urea to your dunk bucket. My suggestion is to use different solvents each time. ETN is soluble in acetone, methanol, and isopropyl alcohol. My suggestion is to recrystalize in acetone first, and then crystalize in methanol or isopropyl alcohol next. The reason for that is acetone gives a 'crunchy' texture to the ETN crystals while methanol and isopropyl give a much finer powder texture, which is safer to handle and use.

I will need to give a third recrystalization to my ETN down the line because I forgot to add urea to the dunk water! But even without that, two recrystalizations, along with the aggressive washing I did should have eliminated just about any acid residue. I still always want to be sure.
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pjig
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[*] posted on 6-3-2024 at 22:57


Excellent ideas. I like it, never heard of this method, but makes sense how you explained it. What amount of urea approximately are you using in your crash water ? What’s your vessel size for this (I assume ice crash bath in a glass bowl or large beaker.) Some have claimed better success with a wide surface area to crash…. Maybe a large cooking glass Pyrex? I’m sure it al depends on the starting materials volumes of course :cool:
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[*] posted on 11-3-2024 at 08:44


Quote: Originally posted by pjig  
Excellent ideas. I like it, never heard of this method, but makes sense how you explained it. What amount of urea approximately are you using in your crash water ? What’s your vessel size for this (I assume ice crash bath in a glass bowl or large beaker.) Some have claimed better success with a wide surface area to crash…. Maybe a large cooking glass Pyrex? I’m sure it al depends on the starting materials volumes of course :cool:


you can use 0.3% by weight of urea in the water you are crashing it into. But I did see in Dugan Boomfax's video (it is on youtube) that he used a 5% urea solution for the crash.

For crashing I use a 2 gallon plastic (HDPE) mop bucket. It has a nice spout at the end to allow for easy pouring. I stir the water to make some nice whirlpool action before dumping the stuff in and stir the stuff before starting to filter. With acetone it will chunk up, but with methanol (and I assume isopropyl) it will be much more powdery.
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pjig
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[*] posted on 15-4-2024 at 07:18


Nice and simple…:cool:
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[*] posted on 29-4-2024 at 13:14


Regarding stabilizing ETN. Has anyone tried crashing out the initial mixed acid into a solution ox NOX scavenger (Urea for example)? Wouldn't it create many side products?
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[*] posted on 29-4-2024 at 13:33


Quote: Originally posted by Nowortimore  
Regarding stabilizing ETN. Has anyone tried crashing out the initial mixed acid into a solution ox NOX scavenger (Urea for example)? Wouldn't it create many side products?

Urea nitrate?
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Sir_Gawain
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[*] posted on 29-4-2024 at 14:10


No, just urea. It absorbs nitrogen oxides and residual acid.



“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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[*] posted on 29-4-2024 at 15:00


Quote: Originally posted by Sir_Gawain  
No, just urea. It absorbs nitrogen oxides and residual acid.

I know, what i mean is urea will react with residual nitric acid to form low solubility urea nitrate side product.
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[*] posted on 30-4-2024 at 03:06


It wouldn't be a huge issue, urea nitrate is s lower power explosive than ETN. Not really sensitive. At the same time it could be removed by regular recrystallization from Acetone. Urea nitrate is sparingly soluble in Acetone.
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DennyDevHE77
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[*] posted on 30-4-2024 at 21:30


Don't you think it would be easier to flush the ETH with water? Because it is cheaper and ETN is not soluble in it, unlike urea nitrate?
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dettoo456
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[*] posted on 1-5-2024 at 17:27


Crashing the nitration mixture into a Urea sol is pointless and wasteful, as the mixed acids could possibly be recovered for later nitrations.

The first recrystallization however, in which Acetone, crude ETN, and bicarbonate are mixed, could be poured into a urea solution with no issues.

After that, any subsequent recrystallizations should involve the pure ETN without urea or cyanamide, or anything other than an organic NOx scavenger like DPA or Centralite. Too large of a proportion of urea or urea nitrate will prompt hygroscopicity during storage in the ETN.
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