| Pages:
1
2 |
Nitrosio
Hazard to Self
Posts: 57
Registered: 31-3-2018
Member Is Offline
Mood: No Mood
|
|
Attachment: DPT2.pdf (116kB)
This file has been downloaded 552 times
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
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]
 
[Edited on 20-1-2021 by greenlight]
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
underground
National Hazard
Posts: 692
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
Nice. How much HMX did you recover ? (yields)
[Edited on 20-1-2021 by underground]
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
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]
[Edited on 21-1-2021 by greenlight]
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
underground
National Hazard
Posts: 692
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
Nice greenlight. You have done a great job so far.
|
|
|
Petn1933
Hazard to Others
Posts: 106
Registered: 16-9-2019
Member Is Offline
|
|
Your work was excellent and exemplary. thank you
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
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.
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
Petn1933
Hazard to Others
Posts: 106
Registered: 16-9-2019
Member Is Offline
|
|
Can we use fuming nitric acid instead of white fuming nitric?
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
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]
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
AndraDoria 13
Harmless
Posts: 2
Registered: 17-4-2019
Member Is Offline
|
|
You did a great job, thank you.
But are we sure the product is pure hmx? I suspected it to be MNX
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
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.
Women are more perilous sometimes, than any hi explosive.
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
Looks like a melting point test is in order then considering I don't have any super advanced equipment like an FTIR or NMR.
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
greenlight
National Hazard
Posts: 705
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
| 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.
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
|
|
|
caterpillar
Hazard to Others
Posts: 472
Registered: 8-1-2012
Member Is Offline
Mood: No Mood
|
|
| 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.
Women are more perilous sometimes, than any hi explosive.
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
