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Nemo_Tenetur
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[*] posted on 2-4-2024 at 06:57


Anyone here with carbodihydrazide synthesis experience? I require a larger quantity as precursor for different energetic materials and I don´t want to buy it because I´m a cheapskate. Fisher scientific sell it for 450 Euro per 500 gram, that´s a ripp off.

There are different routes, phosgene as precursor is out of question. Cyanuric acid and Propylene carbonate are mentioned in patents as better yielding and purer product than urea, but the latter is unbeatable cheap (about 100 euro / 50 euro per kilo versus less than 2 euro per kilo for fertilizer grade).

The yield ist not decisive for me, but the purity (or more precise, the ease of purification) of the final product. The available information is pretty sparse about purity and purification with respect to the different routes. So input and comments about the different routes are welcome. I have enough glassware, fume hood, two stage vacuum pump etc. and 80% hydrazine hydrate in stock.
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dettoo456
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[*] posted on 2-4-2024 at 07:25


The propylene carbonate route may yield propyl carbazate impurities, so an excess of N2H4 and long rxn time would be required. But I’d say that’d be easiest method. Dry Hydrazine Sulfate & NaOH can be refluxed in n-propanol or isopropanol to extract the Hydrazine, then that propanol solution can be decanted and refluxed with propylene carbonate while distilling off the excess solvent. I haven’t heard of the cyanuric acid route though.

I also know a Russian supplier who has carbohydrazide for 2400₽/kg, but I don’t know how sanctions are where you live, and their payment provider isn’t very secure. I’ve had to cancel a debit card due to fraud payments after a purchase from them in the past, even though my order arrived fine to me in the US - it was Red P that cleared customs too :D . I’ll send the info via U2U if you’re interested.
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Nemo_Tenetur
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[*] posted on 2-4-2024 at 09:22


Thank you for fast reply and information. There are plenty sanctions here in the EU and try to import something from Russia at present time is like asking for trouble, at least will raise a big red flag.

Additionaly, there are so much overhead costs and paperwork associated with such a transaction that I´ll avoid it whenever possible. About 20 years ago I´ve bought an exotic amine from TCI in Japan. I´ve paid additional 550 Euro for air freight, tax, hazmat fee, ATLAS fee etc.
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underground
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[*] posted on 2-4-2024 at 13:13


Quote: Originally posted by Nemo_Tenetur  
Anyone here with carbodihydrazide synthesis experience? I require a larger quantity as precursor for different energetic materials and I don´t want to buy it because I´m a cheapskate.


What do you have into your mind. You can buy it from ali for a relative good price
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Nemo_Tenetur
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[*] posted on 4-4-2024 at 14:05


I have no experience with ali (baba or express?) and I´m not sure if such a parcel with white powder (hazmat) will raise a red flag at the EU border. Do they ship in compliance with dangerous goods regulations?
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Trashcanman
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[*] posted on 4-4-2024 at 15:09


Quote: Originally posted by Nemo_Tenetur  
I have no experience with ali (baba or express?) and I´m not sure if such a parcel with white powder (hazmat) will raise a red flag at the EU border. Do they ship in compliance with dangerous goods regulations?


A few years ago I bought 3 americium ionization chambers from aliexpress.
Those things have radiation warnings on them and I think those packages were opened after crossing the EU border because the packages looked as if someone cut them open and sealed them again. I don't know what will happen if some overmotivated customs officer opens a parcel with white powder that was sent from china xD.

But that's just my two cents :)




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Yorty2040
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[*] posted on 15-4-2024 at 17:47


What adhesives resist 95% NM/5% Ethylenediamine PLX?
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dettoo456
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[*] posted on 15-4-2024 at 20:14


What do you mean by adhesives? Are you trying to gelatinize PLX with a polymer? If so, that might cause some issues since NM could simply dissolve a wide range of polymers and ethylenediamine is a fairly aggressive base that could attack esters & olefins.
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Yorty2040
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[*] posted on 15-4-2024 at 21:16


I might need to glue the blasting cap in place, and need a glue that can withstand contact with PLX. If there is no such glue, I'll need to get creative with solder, which will present its own issues.
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dettoo456
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[*] posted on 16-4-2024 at 11:25


Sorry, I don’t think there’d be a clear answer to that query.

You’ll probably just need to test on a small scale to figure out the best glue or somehow mount a fitting with plastic screws to hold a detonator in place.
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dettoo456
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[*] posted on 16-4-2024 at 11:28


This inert version of a binary mix (https://inertproducts.com/product/texpak-binary-explosive-se...) uses a custom molded case to partially surround the detonator.

So you might be able to just tape your cap directly to the bottle of PLX and achieve full detonation.
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Yorty2040
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[*] posted on 29-4-2024 at 17:37


Has anyone done any work on the nitration of hydantoin? The dinitramine looks like it might make an interesting energetic.

There are papers about the use of 5,5-dimethyl dinitrohydantoin as a nitration agent for arenes, but the synthesis involves the use of triflic anhydride, which is a bit pricey.

I reckon that the nitrate salt of hydantoin, plus acetic anhydride, ammonium nitrate, and fuming nitric acid, might form the dinitramine, but I can't find any references for the dinitration of unsubstituted hydantoin.
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dettoo456
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[*] posted on 30-4-2024 at 07:47


Mononitration at the 1 position likely wouldn’t be too difficult but the dinitration would definitely prove harder due to how bulky those carbonyls are. And the product (either mono or dinitramine) probably wouldn’t be too stable. Nitrourea compounds and related nitroamides are not known for their fantastic hydrolytic stability; they tend to hydrolyze very quickly even at rt and in neutral conditions. Plus, pure hydantoin isn’t very commercially available. BCDMH is, but it’s still expensive on its own. And Ac2O is hard to get as well.

A better use for hydantoin could be through di-oxidation (if possible) and subsequent oxidation to just the dinitroimidazolidine. But hydroxylamine is expensive too.
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Yorty2040
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[*] posted on 30-4-2024 at 13:36


I think hydantoin can be made from glycine hydrochloride and potassium cyanate, via the Urech hydantoin synthesis. But if the product of the dinitration hydrolyzes rapidly in water that would be a problem. Do you think MeCl2 could extract the product from the nitration mixture?
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dettoo456
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[*] posted on 1-5-2024 at 17:20


DCM will dissolve nitric acid very readily, though I don’t know how soluble the hydantoin is in DCM either. And it’s not that it might hydrolyze in a water solution, but likely in trace amounts of water and/or acid. It doesn’t seem like a very good EM candidate from a price, stability, or ease of manufacturing perspective.

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dettoo456
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[*] posted on 9-5-2024 at 07:13


Although there doesn’t seem to be much info on it, the detonation velocity (from the few sources I’ve seen) of TEGDN is around 2000m/s. This seems extremely low considering that EGDN is 6600m/s and DEGDN shouldn’t be much lower than that.

Does anyone know why TEGDN is apparently so weak? Apart from its low OB%, it doesn’t make sense to me.

https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8154001/
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clearly_not_atara
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[*] posted on 9-5-2024 at 10:08


Extending the oxyethylene chain not only decreases the oxygen balance but also the density.



[Edited on 04-20-1969 by clearly_not_atara]
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dettoo456
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[*] posted on 15-5-2024 at 07:39


Has anyone noticed some papers describing odd synthesis methods for EMs? The paper linked below describes using a 1:1 molar ratio of AN to Erythritol in an excess of H2SO4 to prepare ETN, but there should be at least a 4:1 ratio of AN to Erythritol, to properly convert all of the AN to HNO3 in-situ and all hydroxyl groups to nitrates, correct?

[Edited on 15-5-2024 by dettoo456]

IMG_1764.png - 311kB

Attachment: freye2020.pdf (3MB)
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[Edited on 15-5-2024 by dettoo456]
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Yorty2040
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[*] posted on 17-5-2024 at 09:05


Anybody have a good synthesis of 2-imidazolidinone? The wiki says ethylene glycol and urea, but it doesn't say how it's done. Is it as simple as mixing them and boiling off the water, or is an acidic or basic catalyst required?

Most of the literature is for the ethylenediamine+ethyl carbonate procedure, which is less accessible to the amateur.
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EF2000
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[*] posted on 17-5-2024 at 09:30


Quote: Originally posted by Yorty2040  
Anybody have a good synthesis of 2-imidazolidinone? The wiki says ethylene glycol and urea, but it doesn't say how it's done. Is it as simple as mixing them and boiling off the water, or is an acidic or basic catalyst required?

Most of the literature is for the ethylenediamine+ethyl carbonate procedure, which is less accessible to the amateur.

2-imidazolidinone is also called 1,3-ethyleneurea, right? So, it appear that this article is what you are looking for: Ethyleneurea. II. Syntheses From Ethylene Glycol or Ethanolamine and Urea (or Carbon Dioxide and Ammonia) by Carl E. Schweitzer.

Attachment: schweitzer1950.pdf (440kB)
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Wroom wroom
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Yorty2040
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[*] posted on 17-5-2024 at 18:03


Thank you! Unfortunately that synth looks like a PITA with the high pressures and temperatures, but it's still a good find.

BTW, is ammonium hydroxide basic enough to deprotonate ethylenedinitramine and form a salt, or will only alkaline metals do? I can't find a good literature value for EDNA's pKa in water or I'd answer myself.

[Edited on 18-5-2024 by Yorty2040]
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