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Author: Subject: RDX synthesis
KABOOOM(pyrojustforfun)
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[*] posted on 26-1-2003 at 18:46


last night I did an experiment to see if HOONO(peroxynitrous acid) can react with HMTA to get RDX. I pourd 175 ml hydrochloric acid (unknown concentration) and 48.5 ml 45% H2O2in a beaker put it in a ice bath and let it cool under 5°C. I had measured 39g of NaNO2 it was in two film can one containig 18 g another 21 g. I slowly added the NaNO2 it started fizzing, the NaNO2 had big lumps one fell down and a violent reaction happend I was shocked and in response I spilled most of the (18 g) NaNO2 :o a very dense brown fume rushed out that made me run a way.
after few minutes I turned back temp was around 40°C. I waited untill the temp decreased to 5°C I then added all the hexamine almost at once (no temperature rise) then I added the rest (most) of the remaining NaNO2 this time more carefully and with continuous stirring. it wasn't very hard to control the temperature when I added some crashed ice to the solution.
the next morning I decided to filter it there were some precipitates at bottom and some fluffy crystals with bubbles at surface.
now it's drying on a filter paper. and I've washed it a lot. I'll crystalize it by hot aceton and then do some tests to see whether it's RDX or R salt
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Madog
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[*] posted on 27-1-2003 at 19:27


awsome, i sugest disolveing the NaNO2 then adding to the HCl slowly, i have had that happen more than once



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KABOOOM(pyrojustforfun)
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thumbup.gif posted on 30-1-2003 at 20:17
good news


it deflagrates but some of it remains melted. so RDX probably exists in my batch
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[*] posted on 1-2-2003 at 07:53


Rhadon>> Yes Mg(ClO4)2 is strong drying agent (a little danger, I think) for some purposes, but not for drain out the water from H2SO4. H2SO4 as stronger acid displace perchloric acid from its salt. Resulting perchloric acid is high concentrated, thus reactive and unstable.
OK, let's stop this tide and back to the topic




The cyanides are good to digesting!
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KABOOOM(pyrojustforfun)
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[*] posted on 9-2-2003 at 18:35


the substance didn't detonate with 0.5 g HMTD (it's probably mostly R salt)
<b>another idea</b>
doese any body know how oximes react with HNO<sub>2</sub> ? I know that some hydoxylamino compounds form nitramino compounds .but I'm not sure if the same reaction happens for oximes. if so formoxime (made from formaldehyde & hydroxylamine) probably forms H<sub>2</sub>C=N-NO<sub>2</sub> which polymerizes into RDX and (-H<sub>2</sub>C-N(NO<sub>2</sub>-)<sub>n</sub>;) polymers.
Edit: I thought I had edited this post before. oximes can't make nitramines that way but some hydroxylamino comopunds form nitrosohydroxylamino derivatives

[Edited on 1-12-2003 by KABOOOM(pyrojustforfun)]
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Madog
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[*] posted on 11-2-2003 at 17:25


what were your yields like?



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Nick F
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[*] posted on 12-2-2003 at 06:41
W-Process


Does anyone have any information on this? I've been told it was invented by some guy called Wolfram...
It involves the nitration of potassium methyleneamidosulphonate, formed from the potassium salt of sulphamic acid (limescale remover) and formaldehyde.
I tried that first reaction, but got no ppte. I don't know if this is normal, but since I had literally no information to work with I decided to give up until I found some. Which I have not been able to do.
If a ppte had formed then I would have tried to nitrate it, but I didn't bother trying to get any further since I had no idea if anything had happened!
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[*] posted on 12-2-2003 at 11:38
an article


Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate
W. P. Binnie, H. L. Cohen, George F Wright;
J. Am. Chem. Soc.; 1950; 72(10); 4457-4459.

Quote:

[...]

It has been shown previously that, while Cyclonite prepared from hexamethylenetetramine is always contaminated with 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane (HMX), this impurity is absent when the starting material contains a single preformed 1,3,5-triazacyclohexane ring. If, then, the condensation product of formaldehyde and potassium sulfamate were actually trimeric, and composed such a ring system, the Cyclonite produced from it ought to show by its high melting point (204-205 degrees Celsius) that it contained none of the tetramer, HMX. This was found to be the case when the crude product obtained from treatment of the salt with nitric acid and sulfur trioxide was purified by crystallization from nitric acid under conditions where the tetramer, HMX, would not have escaped detection if it had been present.

[...]

Experimental:

Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate. -- A solution of potassium sulfamate, prepared in the cold from sulfamic acid and aqueous alkali, was filtered, chilled to 0 degrees Celsius and treated with 75 mL (1 mol) of 37% aqueous formaldehyde solution. The temperature rose to 20 degrees Celsius, was recooled and neutralized to pH 5 with 20-30 mL of 35% aqueous potassium hydroxide. The precipitate (64.5 g) thus formed was filtered off from the chilled slurry. A second identical crop (8.5 g) was obtained by slight dilution of the filtrate. The air-dried material thus represents 50% of the theoretical yield.

[analysis and crystallographic information omitted]

1,3,5-Trinitro-1,3,5-triazacyclohexane (RDX)
A. From Phosphorus Pentoxide. -- Into a 200 mL three-necked flask equipped with a wide sweep powerful stirrer was placed 34.4 mL (0.8 mol) of absolute nitric acid. The stirred acid, maintained at 0 degrees Celsius was treated with 28.4 g (0.2 mol) of phosphorus pentoxide over two minutes. This mixture was chilled and stirred while 29.4 g (0.066 mol) of tripotassium 1,3,5-triazacyclohexane-1,3,5-trisulfonate was added over thirty-five minutes so as to maintain a reaction temperature of 25-30 degrees Celsius. After one hundred fifty minutes more at this temperature the whole was raked into ice (reverse dilution causes decomposition), filtered and washed with dilute ammonia. The vacuum-dried RDX (m.p. 195-197 degrees Celsius) weighed 12.4 g, or 84% of theoretical. This was heated cautiously with 50 mL of 60% nitric acid until by-product decomposition was complete after two minutes, then diluted with 50 mL of water, cooled and filtered. The product, washed with 3% ammonia and vacuum dried weighed 11.8 g. and melted at 204.3-204.7 degrees Celsius.

B. From Sulfur Trioxide. -- The yield was essentially the same as that shown above when 0.01 mol of tripotassium triazacyclohexanetrisulfonate was added to a solution of 0.0225 mol of stabilized liquid sulfur trioxide in 0.11 mol of absolute nitric acid, but the crude (198-201 degrees C) and the refined (204.5-204.8 degrees C) melting points were slightly better. However the violence of solution of sulfur trioxide in nitric acid (even at -40 degrees Celsius) recommends the procedure with phosphorus pentoxide for laboratory use.
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[*] posted on 12-2-2003 at 12:17


Thanks :).
I managed to find a patent for it on espacenet.net earlier today, where they used ammonium methyleneamidosulphonate instead, but it seems that the only reason is that ammonium salts are cheaper than potassium salts.
Obviously I just wasn't looking in the right places for info.
I'm surprised no nasty linear compounds form too, this is a definite advantage.
Well, more experimenting will be done soon...
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[*] posted on 12-2-2003 at 16:21


Is there a way to get phosphorus pentoxide from some chemical supplier whithout raising questions ? As a dessicator, maybe ?
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[*] posted on 13-2-2003 at 04:17


It's worth a try. Say you collect butterflies or beetles or something, and that you need to put some P2O5 in the display case to keep it very dry, otherwise their colours can fade or they can rot etc.
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[*] posted on 18-2-2003 at 23:08
stodgy descriptions


eh,

to the best of my belief, it exist 14 different methods of RDX-synthesis.
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cool.gif posted on 19-3-2003 at 07:28


When HNO3 of lower % than 90% is used, you get not only:
*no RDX
*more risks of runnaway paradoxally the more dangerous is between 70 and 90% HNO3!
*Hexamine dinitrate and aside while heating methylamine nitrate
*You may have some intermediary products like:
-mononitrotriazine, dinitrotriazine, dinitronitrosotriazine and nitrate salts of the above all those should display moderate and intermediary explosive properties between hexamine dinitrate, trinitrosotriazine and RDX!!!

Mg(ClO4)2 would dehydrate the HNO3 to a higher content, but traces of dissolved perchlorate in a nitration reaction that has to be heated ... is a major danger! Also ever tried to heat hexamine diperchlorate that might form in minor quantity?It is very vigorous like NC when it burns with a blueish flame!

NH2-OH is hell expensive and to think to use it and then use HNO2 to make RDX is a little bit useless if you have acces to R-salt and H2O2 or to HNO3 conc and hexamine.
:):(:D;):cool::mad::o:P




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[*] posted on 1-4-2003 at 21:16
Could someone


briefly explain me why H2SO4 doesn't work in hexamine nitration. Is acetic anhydride serving as a H2O scvanger or is acetyl nitrate formed which nitrates the hexamine.
Also is acetic anhydride required in order to nitrate other compounds with =NH (eg. Uric acid, has 4 =NH groups)
I came accross this old book of organic synthesis. Acetone cyanohydrin nitrate is a powerful nitrating agent and nitrates quite a variety of compounds containing =NH group. How does one nitrate Acetone cyanohydrin (Btw, it is also an explosive)




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[*] posted on 1-4-2003 at 21:33
Ok this makes me question


Why can't something like methyl nitrate, isopropyl nitrate or isobutyl nitrate be used to nitrate "stuff", what makes acetone cyanohydrin different than a standard tert alcohol.
Sorry ... all this is not directly related ... but I am only on a quest to synth cyclonite (like most of us)




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PHILOU Zrealone
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smile.gif posted on 7-4-2003 at 03:07


It seems that in normal -CH2-NH-CH2- nitration strong mineral acids destroys the resulting nitramine!Sole exception to this are nitroureas and nitroguanidines!

The use of Ac2O both help by catching H2O and by generating AcONO2 (powerful nitrating agent)!

Uric acid provides very poorly stable nitro derivatives (very fast hydrolysed and low power except for the pernitrostuff that is hard to get owing to previous remark).

Nitrate ester have been used as nitrating media with strong mineral acids, but only for aromatic compounds!There is no real benefit vs metal nitrate/H2SO4 and it is even more troubles since nitrate ester are explosives and needs a previous isolation step!

:cool::cool::cool:




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[*] posted on 7-4-2003 at 22:22


Another exception: DAPT can be nitrated to diacetyl-dinitro tetrazocine with HNO3 + H2SO4 in a promising route to HMX.
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[*] posted on 13-4-2003 at 13:55


Other cheap synthesis ways for hexogen or octogen when for instance octogen oxidised from
1,3,5,7-tetranitroso-1,3,5,7-tetrazacyclooctane
without the presence of H2SO4 with their destoying attributes.




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[*] posted on 14-4-2003 at 10:39


you disolve the binders in toluene or white gas and mix in the RDX.

detonate it with a cap, the binders do desensitise it.




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shocked.gif posted on 25-12-2003 at 03:43


Would someone please provide an equation for the nitration of hexamine to form RDX, there seems too little nitrogen in the heamine molecule for it to convert to RDX, and it seems unlikely that the nitrogen in nitric acid is reduced on the spot from +5 to -3 oxidation state by the extra carbons... ...it works nevertheless, but it's still interesting.
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shocked.gif posted on 26-12-2003 at 04:46


Adiabatic:
If that's so, then a byproduct of RDX synthesis is trimethanolamine - (CH2OH)3N. Very interesting it is why it is never mentioned, it should make a valuable precursor... :cool:
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[*] posted on 30-12-2003 at 20:51


either the file is corrupted or winzip 9.0 beta is old for this (though win ace couldn't open it either) plz attack it again or give the Pat NO



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KABOOOM(pyrojustforfun)
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[*] posted on 31-12-2003 at 15:05


first time? I think it was swedish informania but most of what I learned about it was on E & W. for peaple like me who have NaNO<sub>2</sub> & hexamine in Kg quantity it's a wonderful explosive as it's very easy to make and is quite safe in term of sensitivity.
in that folly experiment I did, the run away reaction caused most of the peroxide to decompose anyway I'm not sure if HOONO is made that way. it would easily reform into nitric acid and even if it could form nitramine by reacting with amines (which now I think is veeery doubtful) the product would be some polymethylene nitramines but not RDX also the hydrogen peroxide could peroxidize/oxidise the formaldehyde ....there are many other possiblities as well




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[*] posted on 20-2-2009 at 05:48
HighPress


Dose any one have this article:

"High Pressure Pressing Technique for Solvated Cyclotrimethylenetrinitramine (RDX) and Cyclotetramethylenetetranitramine (HMX) Pellets"

Corporate Author : NAVAL WEAPONS CENTER CHINA LAKE CA

I need it as Pdf file free.. it is very important for my works..
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[*] posted on 10-8-2009 at 02:51


bwah ha ha. i heard it was super easy via Hexamine to HDN and then to RDX.
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