Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
Author: Subject: RDX Synthesis
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 12-8-2012 at 19:52
RDX Synthesis


Hello everyone.
I am new here ... so go easy on me.
I was wondering if anyone has tried using Butyric Anhydride instead of Acetic Anhydride in the E Process as BuAn is used as a bee repelant etc and is NOT a controled chemical like AcAn.
As far as I understand ... the anhydride is only used to remove H2O. BuAn + H2O is an exo rxn... so temp will have to be monitored.
Any thoughts or am I out to lunch ?
Thanks

[Edited on 13-8-2012 by Motherload]
View user's profile View All Posts By User
hissingnoise
International Hazard
*****




Posts: 3939
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 13-8-2012 at 04:40


If Ac<sub>2</sub>O could be substituted by BA, I think we'd all be doing it . . .
View user's profile View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 13-8-2012 at 06:42


But has anyone tried it or has data suggesting otherwise.
View user's profile View All Posts By User
quicksilver
International Hazard
*****




Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline

Mood: ~-=SWINGS=-~

[*] posted on 13-8-2012 at 13:54


Quote: Originally posted by hissingnoise  
If Ac<sub>2</sub>O could be substituted by BA, I think we'd all be doing it . . .



That's it in a nutshell.

Bachmann worked with a number of substitutions - but they didn't pay off. In plant-level production most all companies used either straight nitration or nitration of the hexamine di-nitrate.

Aside from issues of economy and lab-level experimentation; it's a very inexpensive product. Ammonia, formaldehyde (or para) [for one's hexamine] & nitric acid. Dollar for Dollar, in relation to precursor, that's a great deal cheaper than PETN.

To answer the question directly:if it could be done less expensively, it would have. There have been some experimentation with differing formats (gas, etc) but it all gets back to the Law of Parsimony. :)


[Edited on 13-8-2012 by quicksilver]




View user's profile View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 13-8-2012 at 20:43


No worries.
Just a thought.
I have access to AcAn@ $50/liter.
I don't really need a substitute ... BuAn is just a bit cheaper.
Esp for all you brothers residing in the US .... More attainable.
Regardless ... Just an idea. Even if it is a less yield method.
Thanks for the input.
View user's profile View All Posts By User
Ral123
International Hazard
*****




Posts: 735
Registered: 31-12-2011
Member Is Offline

Mood: No Mood

[*] posted on 14-8-2012 at 08:08


Omg you blew my mind quiksilver, hexogen cheaper then petn? I thought petn more sensitive, much worse storage stability and still requires not much less initiating impulse then rdx to go high order, has at least to be cheaper. Simple ng-like nitration. And rdx is perfectly sensitive to very small amounts of azide so I don't see advantage of petn for caps. Yields for petn I suppose are like one part wfna-one part product unlike rdx 10 parts wfna-1 part product.
View user's profile View All Posts By User
quicksilver
International Hazard
*****




Posts: 1820
Registered: 7-9-2005
Location: Inches from the keyboard....
Member Is Offline

Mood: ~-=SWINGS=-~

[*] posted on 14-8-2012 at 14:22


PentaErythritol comes in various grades. One is for the paint and vinyl production business another is a reagent grade. Both are substantially more expensive that those materials used as precursors for RDX. BOTH PETN and RDX if neutral (acid removed / 7 pH) have a typical shelf life of twenty years.
This means that the material must be re-crystallized at least once and a stabilizer and anti-acid used within production. For these figures to be met there are specific levels of testing & production techniques that must be met. NATO has differing procedures that US/EU industry. The precursor cost for PETN is much higher in cost than those of RDX. This is one reason why PETN is used in small weight applications (but not the only reason).

Industrial information, levels & standards are often found in application specific production techniques.
PETN
MW=336.1
MP=144.3 density (@ 20 degrees)=1.76

RDX
MW=222.1
MP (type A) 202-204 (type B)192-193

See Jacqueline Akhavan's various texts for in-depth information. Issues such as VoD are very close. However since one is a nitric ester and the other a nitrioamine the recovery & configuration issues can be unique





[Edited on 14-8-2012 by quicksilver]




View user's profile View All Posts By User
Fulmen
International Hazard
*****




Posts: 1572
Registered: 24-9-2005
Member Is Offline

Mood: Bored

[*] posted on 14-8-2012 at 16:00


Quote: Originally posted by quicksilver  
Bachmann worked with a number of substitutions - but they didn't pay off.


I'm sure this is true, but that doesn't answer the question whether it's feasible. What's considered an economic dead end for commercial production might well be simpler or more convenient in small scale.
View user's profile View All Posts By User
Ral123
International Hazard
*****




Posts: 735
Registered: 31-12-2011
Member Is Offline

Mood: No Mood

[*] posted on 14-8-2012 at 20:00


I guess I'll agree then, I thought semtex was a cheapoo with that petn and those 20% inerts and C4 was the original stuff. Having dealt with etn, that hexogen like shelf life is kinda difficult to imagine.
View user's profile View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 14-8-2012 at 20:41


Quoting Fulmen Post >
"I'm sure this is true, but that doesn't answer the question whether it's feasible. What's considered an economic dead end for commercial production might well be simpler or more convenient in small scale."


Exactly my point ... I am not trying to make the synthesis more efficient ... just more ... how do I put it ... doable with somewhat readily available and less "watched" precursors.
I am going to try it ... as soon as I secure some BuAn.
I was looking at Propanoic Anhydride but thats even worse than AcAn as it's used for Fentanyl synthesis.
So BuAn ... liquid medium and a good dehydrating agent.
Although stinks like a mofo from what I have heard ... but ... I love the great outdoors ... anything in the name of science.
Thanks for the input.
View user's profile View All Posts By User
shannon dove
Hazard to Self
**




Posts: 77
Registered: 30-11-2011
Member Is Offline

Mood: No Mood

[*] posted on 15-8-2012 at 10:00


I have read some of the hundreds of post about rdx and nitric acid.
There was discussion about why sulphuric acid will not work. I suppose this means sulphur trioxide too. So why does phosphorus pentoxide work and sulphur trioxide does not? Are not they both acid anhydrides?
If red fuming acid is used, does it not work at all, or is the yield just really bad? I mean if the acid had 1% NO2 in it, would it still make a very small yield? Does urea have to be used to clear up the acid, or can just using dry air do a good job of removing NO2?
View user's profile View All Posts By User
Ral123
International Hazard
*****




Posts: 735
Registered: 31-12-2011
Member Is Offline

Mood: No Mood

[*] posted on 15-8-2012 at 11:25


In ordinary nitrating mixture the H2SO4 is in the form of true acid, the HNO3 is more oxidising and nitrating I think. With P2O5, the HNO3 will be the true acid, I suspect the P2O5 will dehydrate well and enable more efficient rdx production. They sell P2O5 here-about a kilo at the price of 2l wfna. I think with hdn you can use HNO3 with more NO2 impurities and still get decent yield.
View user's profile View All Posts By User
shannon dove
Hazard to Self
**




Posts: 77
Registered: 30-11-2011
Member Is Offline

Mood: No Mood

[*] posted on 15-8-2012 at 12:00


I did search first. What are calories per gram rdx?
I think nitro glycerine is about 1.5 and black powder is about 0.75 and for reference sugar is 4 (not including oxidizer) and gasoline about 10 ( not including oxidizer) .
Do those numbers sound right?
Yes, I know the calories is not an indicater of explosive effectiveness, but it is nice to know.
View user's profile View All Posts By User
shannon dove
Hazard to Self
**




Posts: 77
Registered: 30-11-2011
Member Is Offline

Mood: No Mood

[*] posted on 15-8-2012 at 12:08


I meant to say Cal/gram rdx using only its own oxygen, not combustion in the open air, although that would be interesting to know too.
View user's profile View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 8-5-2013 at 08:34


Well I have only access to 70% HNO3 but I have phosphorous pentaoxide and I am interested in making rdx will anyone please tell me the method which use only 70%HNO3 and phosphorous pentaoxide.



Girls break promises like a small child breaks pencil tips so don't trust girl bcoz no girl=no tension
View user's profile View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 8-5-2013 at 10:51


I don't believe mixing P2O5 and 70% HNO3 is a good idea.
The reaction is endothermic enough with 100% HNO3 .... 30% extra water will definately be very violent.




"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
View user's profile View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 23-5-2013 at 21:04


Has anyone attempted the AcAn NH4NO3 and paraformaldehyde method ?
Synthesis of megalomania's page describe toxic and flammable fume evolution ..... Can anyone tell me .....
1). What they might be ?
(Concerned mostly due to odour if any and would also like to know the waste products .... Don't want my neighbours thinking someone is "cooking" crack)
2). What intensity of fuming ?
(Would an average kitchen hood fan suffice for say synthesis of a 100 gms of product ?)




"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
View user's profile View All Posts By User
Nitro-esteban
Harmless
*




Posts: 39
Registered: 10-4-2013
Location: Fifth dimension
Member Is Offline

Mood: inert

[*] posted on 15-6-2013 at 15:38


I think RDX can be made by the folowing process:
NH3 + HCl = NH4Cl.
NH4Cl + 2CH2O = CH3NH2*HCl + HCOOH.
CH3NH2*HCl + NaOH = NaCl + H2O + CH3NH2.
3CH3NH2 + 3CH2O = C6N3H15 + 3H2O.
C6N3H15 + 3 HNO3 = N6C3O6H6 + 3CH3OH.
View user's profile Visit user's homepage View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 15-6-2013 at 16:22


Quote: Originally posted by Nitro-esteban  
I think RDX can be made by the folowing process:
...

C6N3H15 + 3 HNO3 = N6C3O6H6 + 3CH3OH.

Nice try, but I don't think so. That methyl group is not going to just hydrolyze off. The methylene (-CH2-) groups are much more vulnerable to anything here.




I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
View user's profile Visit user's homepage View All Posts By User
Nitro-esteban
Harmless
*




Posts: 39
Registered: 10-4-2013
Location: Fifth dimension
Member Is Offline

Mood: inert

[*] posted on 16-6-2013 at 08:05


I think that it will work because I have done similar things. What worries me is that methanol vapor can react with nitric acid vapor to form methyl nitrate which is dangerous and could detonate the RDX.
View user's profile Visit user's homepage View All Posts By User
Motherload
Hazard to Others
***




Posts: 245
Registered: 12-8-2012
Location: Sewer
Member Is Offline

Mood: Shitty

[*] posted on 16-6-2013 at 11:21


I will have to agree with Anders on that.

I am getting the impression no one has attempted the AcAn synth.

Here is another query.
The E-method generates 6 mols of water for every mol of RDX.
In megalomania's method approx 1/2 mol of RDX is formed and only approx 2.5 moles of AcAn are used
AcAn can only use up its equivalent in mols of water.
So is the glacial Acetic Acid formed dehydrating/removing the residual 1/2 mole of water ??





"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
View user's profile View All Posts By User
Nitro-esteban
Harmless
*




Posts: 39
Registered: 10-4-2013
Location: Fifth dimension
Member Is Offline

Mood: inert

[*] posted on 17-6-2013 at 14:15


I tried it out and nothing happened. Does any one have any ideas on how to get rid of those methyl groups?
Sorry for my stupidity:(
View user's profile Visit user's homepage View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 18-6-2013 at 03:48


I wonder what would happen if acetamide was condensed with formaldehyde, then nitrated. Then it would be acetyl groups.

Surely there must be acetyl groups stuck on as an intermediate in the RDX reaction, with all that acetic anhydride? Presumably the acetyl groups are hydrolyzed off?

There was a thread about using acetamide before, but perhaps if the reaction was modified, RDX would result? Or perhaps it really was RDX they made, but they failed to recognize it as such.
http://www.sciencemadness.org/talk/viewthread.php?tid=18243
View user's profile Visit user's homepage View All Posts By User
Nitro-esteban
Harmless
*




Posts: 39
Registered: 10-4-2013
Location: Fifth dimension
Member Is Offline

Mood: inert

[*] posted on 18-6-2013 at 13:06


Thats what I was thinking, but I dont have acetamide. Think it will work with formamide?
View user's profile Visit user's homepage View All Posts By User

  Go To Top