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Author: Subject: HMX via nitrolysis of DPT
Nitrosio
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[*] posted on 6-12-2020 at 00:31




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[*] posted on 20-1-2021 at 11:24
HMX second run


Another nitrolysis run was attempted of the DPT.
This time recrystallized pure ammonium nitrate was used and the amount reduced and stirring time was longer.

12 grams of ammonium nitrate was added to 35 ml of white fuming nitric acid with very slight NO2 contamination. The mixture was stirred in an ice-bath whereupon the ammonium nitrate dissolved giving a clear solution.

Once the temperature reached 5 degrees, slow addition of 4.40g of solid DPT was begun. Each addition caused the mixture to turn cloudy light yellow before slowly clearing up again. Complete addition took around 20 mins as the temperature was monitored and kept between 6-8°C.

Once complete, the nitrolysis mixture was removed from the ice bath and brought up to room temperature (25-26°C) with a warm water bath. It was held here with stirring for 40 minutes and an light amber brown solution resulted.

This was then poured into 200ml of crushed ice/distilled water mixture whereupon the desired HMX precipitated out as a fine white powder. It was then washed with 100ml ice cold water and placed in a desiccator to dry overnight. Will update with yield when dry.



[Edited on 20-1-2021 by greenlight]

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[Edited on 20-1-2021 by greenlight]




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[*] posted on 20-1-2021 at 12:12


Nice. How much HMX did you recover ? (yields)

[Edited on 20-1-2021 by underground]
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[*] posted on 21-1-2021 at 10:16


Final dried yield is 2.87g which corresponds to a 65% yield which is not too bad. If worked out with the molecular weights in mind, final yield should be over 6 grams, which means it is within the 45-50% area again.


[Edited on 21-1-2021 by greenlight]

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[Edited on 21-1-2021 by greenlight]




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[*] posted on 21-1-2021 at 11:09


Nice greenlight. You have done a great job so far.
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[*] posted on 22-1-2021 at 05:26


Your work was excellent and exemplary. thank you
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[*] posted on 22-1-2021 at 10:03


Thanks guys.

I'm quite happy there is a method to obtain HMX without trying to find restricted precursors like acetic anhydride. Still want to do a melting point and plate test though.





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[*] posted on 22-1-2021 at 12:26


Can we use fuming nitric acid instead of white fuming nitric?
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[*] posted on 27-1-2021 at 23:42


Using red fuming nitric acid during RDX nitrolysis is a no no because of thermal runaway. Off the top of my head I'm not sure about HMX but to be on the safe side I would just use white fuming nitric.

By the time I got around to the second nitrolysis run, the clear acid had turned light yellow despite being stored in a fridge but i used it and had no issues.


[Edited on 28-1-2021 by greenlight]




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[*] posted on 13-5-2021 at 08:19


You did a great job, thank you.
But are we sure the product is pure hmx? I suspected it to be MNX
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[*] posted on 15-5-2021 at 12:17


Quote: Originally posted by greenlight  
Using red fuming nitric acid during RDX nitrolysis is a no no because of thermal runaway. Off the top of my head I'm not sure about HMX but to be on the safe side I would just use white fuming nitric.

By the time I got around to the second nitrolysis run, the clear acid had turned light yellow despite being stored in a fridge but i used it and had no issues.


[Edited on 28-1-2021 by greenlight]


I made RDX, using RFNA (it was yellow, as a matter of fact). But I used hexamine dinitrate, not hexamine.




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[*] posted on 15-5-2021 at 12:33


Quote: Originally posted by AndraDoria 13  
You did a great job, thank you.
But are we sure the product is pure hmx? I suspected it to be MNX


Looks like a melting point test is in order then considering I don't have any super advanced equipment like an FTIR or NMR.




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[*] posted on 15-5-2021 at 12:35


Quote: Originally posted by caterpillar  
Quote: Originally posted by greenlight  
Using red fuming nitric acid during RDX nitrolysis is a no no because of thermal runaway. Off the top of my head I'm not sure about HMX but to be on the safe side I would just use white fuming nitric.

By the time I got around to the second nitrolysis run, the clear acid had turned light yellow despite being stored in a fridge but i used it and had no issues.


[Edited on 28-1-2021 by greenlight]


I made RDX, using RFNA (it was yellow, as a matter of fact). But I used hexamine dinitrate, not hexamine.


That is very interesting, I have always heard that white acid must be used, maybe it is a myth after all.




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[*] posted on 15-5-2021 at 23:41


Quote: Originally posted by greenlight  
Quote: Originally posted by caterpillar  
Quote: Originally posted by greenlight  
Using red fuming nitric acid during RDX nitrolysis is a no no because of thermal runaway. Off the top of my head I'm not sure about HMX but to be on the safe side I would just use white fuming nitric.

By the time I got around to the second nitrolysis run, the clear acid had turned light yellow despite being stored in a fridge but i used it and had no issues.


[Edited on 28-1-2021 by greenlight]


I made RDX, using RFNA (it was yellow, as a matter of fact). But I used hexamine dinitrate, not hexamine.


That is very interesting, I have always heard that white acid must be used, maybe it is a myth after all.


Try this: 5.15.1.3 Nitrolysis of hexamine with ammonium nitrate – nitric acid (CH2)6N4 + 2 NH4NO3 + 4 HNO3 2 RDX + 6 H2O (Eq. 5.24)
This method is known as the K-process after its discoverer K¨offler.201 Like method 5.15.1.2 it uses ammonium nitrate to compensate for the nitrogen deficiency in hexamine and works to Equation (5.24) where two moles of RDX are produced per mole of hexamine. As observed
with method 5.15.1.2, the addition of ammonium nitrate to nitric acid appears to prevent dangerous oxidation reactions from occurring. In fact, this nitrolysis reaction only occurs at elevated temperature and so a constant temperature of 80 ◦C is usually maintained throughout the reaction. Yields of approximately 90 % are attainable based on one mole of hexamine producing two moles of RDX. And hexamine dinitrate is always better than hexamine.




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