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

Printable Version  
 Pages:  1    3  ..  12
Author: Subject: RDX synthesis
trinitrotoluene
Hazard to Others
***




Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline

Mood: paranoid

[*] posted on 18-10-2002 at 11:34
RDX synthesis


Even though meglomainia's site is gone i still saved some of his method.

melting point
205 °C boiling point
--- RDX molecular mass
222.12 g/mol density
1.82 g/mL
class (ABC) sensitivity
low chemical formula
C3H6N6O6 explosive velocity
8500 m/s estimated cost
$?.00/g


RDX, or cyclonite, is a very insensitive high explosive compound. The actual chemical name is cyclotrimethylenetrinitramine, although the chemical names hexahydro-1,3,5-trinitro-1,3,5-triazine; Hexogen; trimethylenetrinitramine; sym-trimethylenetrinitramine ;Hexolite; 1,3,5-trinitrohexahydro-p-triazine; 1,3,5-trinitrohexahydro-s-triazine; cyclotrimrthylene-trinitramine; 1,3,5-triaza-1,3,5-trinitrocyclohexane; trinitrohexahydrotriazine; and T4 are also used. RDX itself stands for Royal Demolition eXplosive and comes from Great Britain, cyclonite is the American usage, Hexogen is for Germans, and T4 is Italian. RDX is a very powerful military explosive that can be stored for long periods of time and handled safely. RDX is usually mixed with other explosives and plasticizers to make a variety of useful compositions for military and civilian use, C-4 and Semtex are two such compounds. It seems so much RDX is made that most scientific books give industrial schematics for thousands of pounds instead of lab preparations. The laboratory methods here are not as efficient as in industry, but are fine. The first method uses methenamine, or hexamethylenetetramine, which can be purchased as heating tablets or synthesized in the lab. The second makes use of acetic anhydride, forbidden by the DEA, but it can be synthesized as well. CHEMICALS APPARATUS
acetic anhydride 500-mL beaker
acetone 1000-mL beaker
ammonium nitrate graduated cylinder
methenamine stirrer/stirring rod
nitric acid thermometer
paraformaldehyde
sodium bicarbonate
water


Put 335 mL of 100% nitric acid in a 500-mL beaker, cool the acid to below 30 °C by setting the beaker in a salt-ice bath. The nitric acid must be as concentrated as possible, it must also be free of nitrogen oxides. Slowly add 75 g of methenamine in small portions to the acid while stirring. The temperature must be kept between 20 °C to 30 °C during the addition. Once all of the methenamine has dissolved, slowly heat it to 55 °C while stirring, hold it to between 50-55 °C for 5 minutes, keep stirring. Now cool the mix to 20 °C then let it sit for 15 minutes. After standing, it is gradually diluted with three or four times its volume of cool water, this should precipitate the RDX from solution. Depending on how the gods of chemistry feel about your reaction it may take from minutes to hours to fully precipitate all of the RDX. Decant most of the liquid then add 1 L of 5% sodium bicarbonate solution to neutralize the remaining acid. Filter the mixture to collect the crystals of RDX that should have formed. Wash them with cold water, then with hot 5% sodium bicarbonate solution, and again with water. The RDX can be dried at room temperature or in an oven. Further purification can be accomplished by recrystallizing from acetone. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.






TNT
View user's profile View All Posts By User This user has MSN Messenger
Polverone
Now celebrating 18 years of madness
*********




Posts: 3164
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline

Mood: Waiting for spring

thumbdown.gif posted on 18-10-2002 at 11:53
Sorry


Neither the E&W Forum nor Megalomania's web page have disappeared. It's noble of you to want to save the information he'd collected, but the information isn't in need of saving. Even if it were in need of saving, this wouldn't be the exact place to post it. Sciencemadness isn't primarily an explosives-oriented site. Discussions about energetic materials that shed new light on them are welcome, but we don't need another forum to rehash "how to make explosive X" questions.

And honestly, that's not even a very good writeup about RDX. It doesn't tell you about the reactions involved. It has no molecular diagrams. It doesn't cite any sources. The acetic anhydride preparation suggested (on Mega's page) is abominable: it requires acetyl chloride for synthesis, which in turn requires phosphorus trichloride. Sure, you can buy phosphorus trichloride or acetyl choride, but in that case you might as well buy acetic anhydride to begin with!
View user's profile Visit user's homepage View All Posts By User
MrsBackFire
Unregistered




Posts: N/A
Registered: N/A
Member Is Offline


[*] posted on 26-10-2002 at 03:51
RDX


trinitrotoluene, shut off your braindead copied descriptions and use your TNT for table-fireworks ! :D
PrimoPyro
on fire
***




Posts: 122
Registered: 7-8-2002
Member Is Offline

Mood: No Mood

thumbdown.gif posted on 26-10-2002 at 03:56
Flaming


Unless that was some weird personal inside joke between the two of you, that was highly uncalled for, and NOT cool.

Flaming is not a part of this board. The members here do not wish to have this bullitin board cluttered with mean and derogotory comments like this.

This board is for science, and science has no room for namecalling.

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




Posts: 3940
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 28-12-2002 at 07:52
Cyclonite Synth.


When I made cyclonite many moons ago, I used red(dissolved no2)hno3 70%, concentrated by distillation from h2so4. As hexamine was added it made a "hissing noise" and the acid became colourless. The hexamine dissolved as it went in. I waited a minute before drowning. I love the way it melts into globules when flame is applied and its deflagration is so gentle. Maybe that's why it took 21 years for it to be recognised as the explosive it undoubably is.
View user's profile View All Posts By User
hissingnoise
International Hazard
*****




Posts: 3940
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 28-12-2002 at 09:03
Cyclonite Synth.


When I made cyclonite many moons ago, I used red(dissolved no2)hno3 70%, concentrated by distillation from h2so4. As hexamine was added it made a "hissing noise" and the acid became colourless. The hexamine dissolved as it went in. I waited a minute before drowning. I love the way it melts into globules when flame is applied and its deflagration is so gentle. Maybe that's why it took 21 years for it to be recognised as the explosive it undoubably is.
View user's profile View All Posts By User
hissingnoise
International Hazard
*****




Posts: 3940
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 28-12-2002 at 09:06


Ooops; missed a (t) in undoubtably.
When the subject is explosive, accuracy is essential.
View user's profile View All Posts By User
hissingnoise
International Hazard
*****




Posts: 3940
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 28-12-2002 at 09:08


Don't know where the repeat came from.
View user's profile View All Posts By User
BrAiNFeVeR
Harmless
*




Posts: 42
Registered: 23-5-2002
Location: Belgium
Member Is Offline

Mood: busy

[*] posted on 28-12-2002 at 11:40
/Oops/ ?


And just like that you created more then half of the amount of posts under your name (7 at the time), which are all pretty useless if I may say so ...

And what you where making there is most likely hexaminedinitrate ...




Visit my site => http://brainfever.2ya.com
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 28-12-2002 at 14:52


i tried to nitrate a gram of hexamine the other night, it proved to be a slight disaster and unsucessful. i used Mr Cools method on his site. about 1.2g of AN + 8ml of white HNO3 about 90%. then i added a gram of hexamine to this slowly while stirring. it was in an ice bath and a tilted it towrds me as i stirred it. all of a sudden a drop of HNO3 shot out from stirring right into my right eye! ouch, i ran to the sink and started to wash it. it hurt. then i moved to the other sink and washed it more with sodium bicarb for probaly 15 min. my vision was kinda blurred and it felt like i had something caught in my eye. i finished the nitration and drowned it. got absolutely nothing. damnit! oh well, i got my PETN to play with.



Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
kingspaz
Hazard to Self
**




Posts: 55
Registered: 23-7-2002
Location: UK
Member Is Offline

Mood: No Mood

[*] posted on 28-12-2002 at 16:16


madog, you should go the hospital and say you got acid in your eye when recharging your car battery or somthing. they will put a dye in your eye and check it out for damage.



the unexamined life is not worth living to a human
View user's profile View All Posts By User
trinitrotoluene
Hazard to Others
***




Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline

Mood: paranoid

thumbdown.gif posted on 28-12-2002 at 23:24


Dude safety is number 1 you should always wear safety goggles even if your handleing dilutted strong acids. Was you wearing goggles when you got the HNO3 in your eye?



TNT
View user's profile View All Posts By User This user has MSN Messenger
hissingnoise
International Hazard
*****




Posts: 3940
Registered: 26-12-2002
Member Is Offline

Mood: Pulverulescent!

[*] posted on 29-12-2002 at 08:29
Hexamine dinitrate


Brainfever, you must know that the di-salt is very soluble in water and does not precipitate when drowned.
Lighten up!




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




Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline

Mood: paranoid

thumbdown.gif posted on 29-12-2002 at 13:45


blah this thread is going nowhere. I 've should had never started this when I was a newbe.



TNT
View user's profile View All Posts By User This user has MSN Messenger
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 29-12-2002 at 17:19
im ok


my vision is fine now, all is good.

tnt, lets make this topic go somewhere.

who else here has made RDX and by what method? i would really like to hear about it. has anyone seen that method involveing HMTD? i think im gona make R-salt in the next couple days, and probaly oxidise it to RDX. has anyone here done that? the method from mr cools page for oxidation of R-salt to RDX is gone. i would like to get it again.




Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
lucifer
Harmless
*




Posts: 21
Registered: 23-11-2002
Member Is Offline

Mood: No Mood

[*] posted on 30-12-2002 at 03:09


I’ve made rdx with distilled 99% HNO3 and with methenamine,
The Yeild wasn’t bad, 74% (29,7gr rdx out of 25gr methenamine).

I,ve changed the nitration time in meglomainia’s method, to get a better yeild.
(info from urbanski).



Slowly ad 25gr methenamine to the HNO3, which went quite easy keeping the temperature under 30degr C
After that put the solution in a water bath of 60 degr C, letting the temperature of the solution rise to 55 degr C Keep it at this temperature for 12 minutes.
Then cool it down in a ice bad to 20 degr C
During this phase some rdx becomes visible in the solution.
Let it stand for 10 min.
Then add to the solution 400 ml of ice water
A lot more of rdx will precipitatet out of the solution.
Let this solution stand for 5 minutes
After filtering neutralised the rdx with 400 ml 5% sodium bicarbonate solution.

The yeild after completely drying was 29.7 gr which is if I am ride about 74%


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




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 30-12-2002 at 18:44


ok, awsome, thats good to hear. i dont have alot of HNO3. i should make more. i think i will try to make R-salt tomarrow. then ill try oxidiseing it to RDX



Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
kingspaz
Hazard to Self
**




Posts: 55
Registered: 23-7-2002
Location: UK
Member Is Offline

Mood: No Mood

[*] posted on 31-12-2002 at 02:02


you do know that R-salt is carcinogenic?



the unexamined life is not worth living to a human
View user's profile View All Posts By User
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 1-1-2003 at 12:26


yes, its very carcinogenic, and i am going to do my best to protect myself.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
Nick F
National Hazard
****




Posts: 439
Registered: 7-9-2002
Member Is Offline

Mood: No Mood

[*] posted on 1-1-2003 at 13:41


Actually most people I've spoken to seem to think that R-Salt would not be very carcinogenic, and is probably less toxic than RDX itself. I can't remember why they were of this opinion, it had something to do with the decomposition products / metabolites being different to those of the more carcinogenic nitrosamines.
But they had no figures or references to support this, it was just their opinion, so stay cautious...
View user's profile View All Posts By User
Ramiel
Vicious like a ferret
****




Posts: 484
Registered: 19-8-2002
Location: Room at the Back, Australia
Member Is Offline

Mood: Semi-demented

[*] posted on 2-1-2003 at 00:46


If I may hazard an opinion, all this talk or carcinogenicy (or whatever) it bunk. Hell, badly done french fries are carcinogenic... the sun is carcinogenic where I live. It's not as if you drop this stuff on your finger and you suddenly get a bubbing, tenticaled cancer weeping from the flesh wound...
View user's profile View All Posts By User This user has MSN Messenger
osamafon
Harmless
*




Posts: 16
Registered: 26-12-2002
Location: x
Member Is Offline

Mood: No Mood

[*] posted on 7-1-2003 at 06:12


can I dry 60% HNO3 to 99% with anhydrous Mg(ClO4)2 ?
View user's profile View All Posts By User
Praetorian
Harmless
*




Posts: 7
Registered: 7-11-2002
Location: Czech republic
Member Is Offline

Mood: No Mood

[*] posted on 19-1-2003 at 10:20


osamafon >>
Actually sad, no. If a chem stuff called anhydrous, it shouldn't be dehydration agent directly (which is potent to dehydrate HNO3). You should try P2O5, H2SO4, acetanhydride... with distillation ( in next step.

Would be somebody so kindly tell me what the R-salt is?




The cyanides are good to digesting!
View user's profile View All Posts By User
Rhadon
Hazard to Others
***




Posts: 169
Registered: 26-5-2002
Location: Germany
Member Is Offline

Mood: No Mood

[*] posted on 19-1-2003 at 10:46


Hmm, actually Mg(ClO4)2 is a strong drying agent which can be used as a substitute for P2O5. I don't know if it can be used here though... perhaps someone else does.
View user's profile View All Posts By User
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 20-1-2003 at 18:28


eh, not to be an ass hole, maybe we should stay on topic

R-salt is RDX but only with NO groups in the place of the NO2 groups, i forget what that is called. but that explains it. it can be oxidised to RDX.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
 Pages:  1    3  ..  12

  Go To Top