ghost711 - 22-9-2003 at 23:59
Dunno if you guys are doing this or not..but this is how its really done...real white and sparkly stuff.. enjoy 
EXAMPLE 2
10.6 Grams of acetonitrile and a catalytic amount (0.5 gram) of concentrated sulfuric acid were mixed and heated to gentle reflux of the nitrile in a
glass flask provided with a dropping funnel, magnetic agitator and reflux condenser. A solution of 11.5 grams of formaldehyde as trioxane in 10.6
grams of acetonitrile was added to the flask contents during about 30 minutes at such a rate as to maintain the reflux. When the addition was about
one-third complete, the triazine compound began to separate as a white solid; and when the addition was complete, the slurry was quite heavy with
solids, and if allowed to cool, the slurry became a very viscous semisolid. After the addition of the acetonitrile-trioxane solution was complete, the
slurry was added slowly portionwise to about 10 volumes of 99% nitric acid, which was agitated in a glass flask cooled in an ice bath. The agitated
reaction mixture was held for an additional 15 minutes with ice bath cooling, allowed to warm to ambient temperature for 15 minutes and then heated to
about 60.degree.C. for 60 minutes. The reaction mixture was then allowed to cool to room temperature and drowned into five volumes of ice water. The
precipitated RDX was filtered off, washed with water and dried. The RDX was thus obtained in high purity and 31% theory yield, based on the
acetonitrile.
[Edited on 24-9-2003 by ghost711]
Nick F - 23-9-2003 at 05:26
It's good to know other methods, but yields are normally twice that using the much simpler HDN/HNO3 route!
(I know comparing yields is a bit silly, since they are based on different chems... but it still seems like a lower yielding way of doing it to me)
vulture - 23-9-2003 at 06:08
Not to mention that acetonitrile is a very toxic chemical, which also tends to polymerize violently if no stabilizer has been added.
BASF - 23-9-2003 at 08:50
Hmm...i´m wondering what happens if one does this cyclization with acetaldehyde and then nitrate it(Ac2O/HNO3/methylenechloride ??).
Maybe it would have interesting properties....
I´d suppose it would have a density of ~1.6, and Vod~7500m/s.
BASF - 23-9-2003 at 08:59
BTW, the patent initially referred to seems to be US 3,937,703.
considering...
ghost711 - 23-9-2003 at 15:47
I havent really seen this method discussed other than the old: "get some hexamine and nitrate it" one so flagrantly thrown around the web.
Also, despite the initial shock of only a 31% yield...it can be improved to around 50-60% with continued tweaking of the formaldehyde/acetonitrile
ratios along with the amount of HNO3 in the nitration step. Acetonitrile is also not as expensive and fiendish as proposed. The cyanide is quite
safely tied up in its chemical structure..and- the cost of 4L worth only runs you around $60 (shipped). It is also quite common (and available) as a
chromatography solvent.
BTW- Ive got a few quick questions as well- I have always just distilled pure nitric out of 40% HNO3/H2SO4. I came across the method with the
KNO3/H2SO4 and coldfinger setup..is the nitric as pure as indicated? At least 95-98%??
Finally- does anyone know the patent # for the HDN(HMX)/HNO3 route??
madscientist - 23-9-2003 at 16:21
The synthesis you posted was very unique and interesting. Thanks for sharing.
KABOOOM(pyrojustforfun) - 25-9-2003 at 21:00
another way to get let's say trimethylRDX could be nitrating the condensation product of CH3CHO & NH3.
what about following the same synthesis route but replacing formaldehyde with glyoxal? wow, CL-20 ?!<br>6CH<sub>3</sub>CN + 3OHCCHO
<s> ></s>
C<sub>18</sub>H<sub>24</sub>N<sub>6</sub>O<sub>6</sub>
H(acetyl)NIW<br>C<sub>18</sub>H<sub>24</sub>N<sub>6</sub>O<sub>6</sub> +
6HNO<sub>3</sub> <s> ></s>
C<sub>6</sub>H<sub>6</sub>N<sub>12</sub>O<sub>12</sub>(HNIW) + 6CH<sub>3</sub>COOH
putsi minge - 28-9-2003 at 13:49
hello! do you know this process what uses only conc. HNO3 and hexamin,or where can I find it.Thanks
KABOOOM(pyrojustforfun) - 28-9-2003 at 20:59
<b>modified preparation of 1,3,5-triacetylhexahydro-s-triazine</b><br>I think condensing methylene diacetamide (correct name?) with
acetonitrile and formaldehyde in presence of H2SO4 might work.<br>the standard method: 3RCN + 3CH<sub>2</sub>O
<s> ></s>
>(-CH<sub>2</sub>-N(COR)-)<sub>3</sub>><br>suggested method:
2CH<sub>3</sub>CONH<sub>2</sub> + CH<sub>2</sub>O <s> ></s>
(CH<sub>3</sub>CONH)<sub>2</sub>CH<sub>2</sub> +
H<sub>2</sub>O<br>(CH<sub>3</sub>CONH)<sub>2</sub>CH<sub>2</sub> + CH<sub>3</sub>CN
+ 2CH<sub>2</sub>O <s> ></s>
>(-CH<sub>2</sub>N(COCH<sub>3</sub>
-)3> +
H<sub>2</sub>O<br>H<sub>2</sub>SO<sub>4</sub> absorbs the water produced in the last reaction improving the
yield.<br>benefit: the modified method gives 3 times more triacetyl.. based on acetonitrile (in theory)<br><br><b>modified
preparation of RDX</b><br>this reaction tells it
all:<br>C<sub>6</sub>H<sub>12</sub>N<sub>4</sub>H<sub>2</sub>(NO<sub>3</sub><sub>2</sub> + 3CH<sub>3</sub>CN + 4HNO<sub>3</sub>
<s> ></s> 2RDX + NH<sub>4</sub>NO<sub>3</sub> +
3CH<sub>3</sub>COOH<br>nitration of HMTA results in formation of CH<sub>2</sub>O as by product which further condenses
with acetonitrile then nitrolysation of the product occurs forming more RDX.<br><br>to putsi minge: can't you really find one? <a
href="http://roguesci.org/megalomania/explosives.html">megalomania</a> or you may wanna check some personal sites: <a
href="http://www.flashbangboom.homestead.com/home_page.html">Nick F's site</a> <a
href="http://www.angelfire.com/linux/alengg/main.html">ALENGOSVIG1's site</a> <br><b>just do a little
search.</b>
nice
ghost711 - 1-10-2003 at 05:20
very nice kaboom....but to increase production of the triazine during the standard acetonitrile synth- what about adding a little more than a
catalytic amount of sulfuric? ..maybe more triazine compound and even using 70% nitric during the nitrolysis step in 5/1 ratios or even less!! Lets
think cheap/available chems in acceptable ratios...
Nevermore - 1-10-2003 at 05:23
I wish to know if someone measured the yeld of megalomania's method, using acetic anydride and paraformaldehyde, mixed with ammonium nitrate.
Also what plasticizer is better to use, i was thinking about petrolatum, but maybe will come out a bit too oily, maybe mixing with some paraffin...
DBSP - 2-10-2003 at 12:01
Nevermore, yoou are a member of E&W, go there and search!!
Stanfield attempted the method you mentioned several times, he has posted a lot of info on the subject.
Nevermore - 2-10-2003 at 23:10
thank you, i couldn't find much until you told me the name of the user who post the informations..now i found everything i need thanks! i will
just try formaldheide and ammonia method, much more easy than getting para.
Mahlzahn - 21-4-2005 at 07:10
A useful method are too:
(hexamethylentetramin + H2O) + HNO3 (~70%)
->
hexamethylentetramin*2HNO3
(hexamethylentetramin*2HNO3) + HNO3 (<95%)
+H2O
->RDX (C3H6N6O6)
[Edited on 21-4-2005 by Mahlzahn]