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DubaiAmateurRocketry
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[*] posted on 1-1-2014 at 09:27


We've been talking of tetrazoles and tetrazines a lot, now what about 4 member or 8 membered nitrogenous rings? diazete dioxide and its derivatives seems good. Also what about other nitrogen hydride cations other than NH4+ and N2H5+ ? Diazene and triazene seems more dense than NH4, N2H5. Can they be protonated to form salts? I also found that hydrazoid acid can be protonated too.

[Edited on 1-1-2014 by DubaiAmateurRocketry]
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[*] posted on 2-1-2014 at 17:29


I want to make NTO, however to start from less steps, I want to start from 2,4-dihydro-3H-1,2,4triazol-3-one. However the 2,4-dihydro is not availible as a commercial product but 2,1 dihydro is..

http://www.chemdoor.com/yp/show_2747_46371.html

Their structure is striking similar except with 1 NH group in on position 4 rather than position 1.

So will I get the exact same final product if I nitrated it ? Will it change to 2,4 form ? Would be happy to know. Thanks !
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[*] posted on 2-1-2014 at 18:38


How do we know how dangerous casting ETN is? The only accidents I know of from ETN heat explosion where when it was rapidly heated (hot plate or glass w/ flame)

Has ETN ever detonated from slow heating by something like a water bath? It may become more sensitive when molten, but if it is undisturbed, I don't see how it would explode for no reason? Is melting 50g of ETN more prone to explosion than 1g melting under the same conditions (water bath).

Because I think a cast of ETN and RDX would have amazing brisance over TNT based casts.
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[*] posted on 2-1-2014 at 19:01


Never never cast ETN. Why would you even handle anything with sensitivity under 20cm of HD50?

ETN is very badly reputed in this form, see some member's severe injuries from ETN.

Lost almost 2 hand/ scared all over for life from ETN

[Video] Lost hand with few grams of sensitive explosive

Few miligram of ETN, and that is what can happen to you.

Sthe person above had just few miligrams... and that happened to him. If 1 piece was toward his eyes he could have been blind..So..... Just Don't... Cast it and you will be on the news.


[Edited on 3-1-2014 by DubaiAmateurRocketry]
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DubaiAmateurRocketry
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[*] posted on 2-1-2014 at 19:16


Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]
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[*] posted on 2-1-2014 at 19:41


google "HMX synthesis" you'll find quiet easily.


That is not the response I was looking for Dubai, the fact of the matter is, ETN can no doubt detonate when subject to thermal shock. Just as NG can.

"Cast and you will be on the news" I've casted ETN before, in a straw in a hot water bath. I may do some tests w/ molten ETN, test friction and shock sensitivity.

My question is, is ETN more prone to detonate when it is molten in large amounts?


I think I would be leaving too powerful of a composition by never trying cast ETN in reasonable amounts (10-50g taking great care of course to not expose it to thermal shock but slow melting and solidifying away from where it would cause damage if it did explode.

How about cast ETN/RDX compositions? 75/25 RDX/ETN at cast density would probably surpass pressed HMX or even HMX plastique in terms of brisance.




Dubia:

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc... I think that is what you're looking for. If you do try it report how it works, and then video detonation.




[Edited on 3-1-2014 by Turner]

[Edited on 3-1-2014 by Turner]
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[*] posted on 2-1-2014 at 20:07


Also look, this guy was very professional with everything he did and took extraordinary safety precautions, 13g Cast ETN: http://www.youtube.com/watch?v=m496k0l1XIk

Because, when doing burn tests with ETN it always melts way before deflagrating, has it ever popped when exposed to open flame?

I would only ever dare cast ETN that has been recrystalized and absolutely no left over acid.



That video is quiet violent, I wonder if the Nitrocellulose coating on the fuse burned down too fast? Once when I was testing out some Visco fuse I ordered, it looked like the NC deflagrated down the fuse very fast while the core burned, maybe not. I've used that fuse 5-8 times w/ no problem though

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[*] posted on 2-1-2014 at 20:19


alright then try casting it behind a blast shiled. or at least fune hood + faceshield + thick lab coat.

and dont try too much. cast it in water, so if it explodes its less fatal. ETN is sensitive.

thx for hmx synthesis ive seen that. is there any.other ? this one is spending too mich acetic anhydride. I remember there are less step methods with slightly less yield.
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[*] posted on 2-1-2014 at 20:26


You could also gain excellent brisance by just using liquid, unadulterated NG, but it also has complexities in handling and a longer storied history of accidents. This is why EM researchers spent so much time getting extremely powerful materials that come nearly insensitive to use as base charges. At some point you have to trust the Tradition of our predecessors and not get too headstrong for the sublime things that you are warned against.
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[*] posted on 2-1-2014 at 20:35


Quote: Originally posted by DubaiAmateurRocketry  
thx for hmx synthesis ive seen that. is there any.other ? this one is spending too mich acetic anhydride. I remember there are less step methods with slightly less yield.


Have you seen this one.

Attachment: cyclic and linear nitramines.pdf (726kB)
This file has been downloaded 454 times

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[*] posted on 2-1-2014 at 20:48


Quote: Originally posted by DubaiAmateurRocketry  
Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]


Here's a cut from Chemistry and Technology of Exp. Vol3 (page 110)

pg110_CATOEv3.png - 33kB
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[*] posted on 2-1-2014 at 21:58



thank you roxfeller

what are other nitrogen-oxide anions other than NO2 N3O4 NO2 NO NO3

[Edited on 3-1-2014 by DubaiAmateurRocketry]
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[*] posted on 6-1-2014 at 20:15


I kinda suppose the answer to be 'no', but do you suppose that the paraformaldehyde from campa-chem could ever be washed clean enough to be suitable for the rdx synthesis?
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[*] posted on 12-1-2014 at 01:53


What's wrong with blue RDX ??
Try washing with MeOH.

They only sell the Eco friendly crap here now.
Can trioxane be used instead of paraformaldehyde ?




"Chance favours the prepared mind"
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[*] posted on 12-1-2014 at 02:03
Can DEGDN really be co-nitrated ?


Diethylene glycol dinitrate(DEGDN) is low in sensitivity therefore I would like to have a mixture of trimethylolethane trinitrate(TMETN) with DEGDN to decrease the sensitivity of TMETN.

however on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

Megalomania's guide on DEGDN specified very clearly, that DEGDN can not be nitrated like others, it will decompose in acids. So it is carried out in a inert solvent, such as dichlorofluoromethane.

However on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

DEGDN is co-nitrated with TMETN without any solvent. Will DEGDN decompose ?
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[*] posted on 12-1-2014 at 05:19


Quote: Originally posted by DubaiAmateurRocketry  
Diethylene glycol dinitrate(DEGDN) is low in sensitivity therefore I would like to have a mixture of trimethylolethane trinitrate(TMETN) with DEGDN to decrease the sensitivity of TMETN.

however on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

Megalomania's guide on DEGDN specified very clearly, that DEGDN can not be nitrated like others, it will decompose in acids. So it is carried out in a inert solvent, such as dichlorofluoromethane.

However on this page.

http://web.mit.edu/semenko/Public/Military%20Manuals/RogueSc...

DEGDN is co-nitrated with TMETN without any solvent. Will DEGDN decompose ?


DAR,

this is copy-pasta from Military explosive (TM 9-1300-214)

"-DEGDN can be manufactured with a yield of approximately 85 percent of the theoretical by adding diethylene glycol to mixed acid containing approximately 50.3 percent nitric acid, 44.7 percent sulfuric acid, and 5.0 percent water. The temperature of the mixture is kept at 10° to 15°C. The spent acid is very unstable and fumes off if heated or allowed to stand for a few hours. The separated DEGDN is purified by washing with successive portions of water, dilute sodium carbonate solution, and water until neutral. The purity of the product is dependent mainly on the purity of the diethylene glycol used in the manufacturing process.

-DEGDN is so insensitive that mixing with another nitrated compound is required to produce a useful explosive. DEGDN alone, however, does explode in the pendulum friction test. The explosion temperature test value for DEGN is 237°C"

this is also a patent US1936020 for the nitration of diethylene glycol.

Dany.
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[*] posted on 12-1-2014 at 08:46


Short question from me:

from the wikipedia article on Ammonium sulfate:

In November 2009, a ban on ammonium sulfate, ammonium nitrate and calcium ammonium nitrate fertilizers was imposed in the former Malakand Division—comprising the Upper Dir, Lower Dir, Swat, Chitral and Malakand districts of the North West Frontier Province (NWFP) of Pakistan, by the NWFP government, following reports that they were used by militants to make explosives. In January 2010, these substances were also banned in Afghanistan for the same reason.

Why did they ban the sulfate?
it must be a big PITA to make AN from the sulfate and maybe KNO3 or something, AN is much more soluble.
What's the Warlords use for it?

[Edited on 12-1-2014 by dangerous amateur]
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[*] posted on 12-1-2014 at 09:01


In war time every substance become precious for people doing explosives/energetic materials. Maybe it is difficult to make ammonium nitrate form the sulfate, but Al-Qaeda terrorist have mastered how to extract KNO3 form sheep and other animals excrement to make black powder. the KNO3 may be used to make ammonium nitrate when combined with the ammonium sulfate. Maybe they should ban sheep in Afghanistan :D. It is impossible to stop making explosive since many of the materials used for their fabrication has a dual uses and many of these chemical is simple to synthesized. So even you ban a large amount of chemical you still not able to stop bomb manufacturing.

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[*] posted on 12-1-2014 at 09:12


Quote: Originally posted by Dany  
So even you ban a large amount of chemical you still not able to stop bomb manufacturing.

Dany.


No doubt about that.

But I'm still wondering. If I was so poor as these guys I would have had other troubles than making nitrates out of shit...
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[*] posted on 12-1-2014 at 10:06


I wonder if someone can perform an exchange type reaction with ammonium sulfate (or other NH4+ ion containing salt) and a nitrate salt like Potassium Nitrate or sodium nitrate in Large amounts.

if someone had 200 lbs of ammonium sulfate fertilizer, and 200 lbs of sodium nitrate fertilizer, they could theoretically have that amount of ammonium nitrate.
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[*] posted on 12-1-2014 at 10:11


Dany,

Ahh that patent is very helpful, thanks a lot.

Quote: Originally posted by Dany  

-DEGDN is so insensitive that mixing with another nitrated compound is required to produce a useful explosive. DEGDN alone, however, does explode in the pendulum friction test. The explosion temperature test value for DEGN is 237°C"


where did you find that ? I wish i can see any sensitivity of DEGDN mixtures with another high explosive such as BTTN or NG
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[*] posted on 13-1-2014 at 20:07


Quote: Originally posted by DubaiAmateurRocketry  
Where can I find a full synthesis of HMX starting from Hexamine ? The one that uses paraformaldehyde and Acetic anhydride ? Is there any paper on perfecting this method ? And also RDX ?

[Edited on 3-1-2014 by DubaiAmateurRocketry]


I just noticed this while reading the Urbanski text (vol 3 pp 117):

Quote:

This observation also appears to explain why an excess of paraformaldehyde should have a harmful influence on the yield of cyclonite. In particular, Winkler noticed that the addition of formaldehyde to a hexamine solution in aqueous acetic acid causes the decomposition of hexamine which proceeds at a rate depending on the ratio of formaldehyde to hexamine.


Are you really intending to add paraformaldehyde and Ac2O to a hexamine/nitric acid process?

As far as blue RDX, the blue will probably come out when all is done for purification, but the cyclic polymerization can sometimes be finnicky. Hence the oft quoted low yields, the waste acid is full of linear nitramines that never polymerized. I'm hoping that impurities after washing won't hinder this polymerization.
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[*] posted on 13-1-2014 at 20:16


Quote: Originally posted by Turner  
I wonder if someone can perform an exchange type reaction with ammonium sulfate (or other NH4+ ion containing salt) and a nitrate salt like Potassium Nitrate or sodium nitrate in Large amounts.

if someone had 200 lbs of ammonium sulfate fertilizer, and 200 lbs of sodium nitrate fertilizer, they could theoretically have that amount of ammonium nitrate.


This is getting a bit taboo for the forum. Lab work can be scaled up (the essence of chemical engineering) but why are you hypothesizing 200 lbs of AN (I don't think your stoich works out), and why here? That's alot of solution to be sloshing around and drying.
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[*] posted on 31-1-2014 at 05:51


Does hydroxylammonium-5-amino-tetrazolate exist ? Any papers/ information of it ?

How to I obtain ammonium nitrate form a solution ? I have around 100ml of water dissolving around 5 gram of AN and it did not precipitate even when I put it in my fridge(around 5 degree C)



[Edited on 31-1-2014 by DubaiAmateurRocketry]
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[*] posted on 31-1-2014 at 15:31


You will need to evaporate all the water, boil the solution down, and then put it in an oven to evaporate the rest, you will end up with dry ammonium nitrate.
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