Sciencemadness Discussion Board - RDX synthesis

RDX synthesis

Pages: 1 2 3

trinitrotoluene - 18-10-2002 at 11:34

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.

Sorry

Polverone - 18-10-2002 at 11:53

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!

RDX

MrsBackFire - 26-10-2002 at 03:51

trinitrotoluene, shut off your braindead copied descriptions and use your TNT for table-fireworks !

Flaming

PrimoPyro - 26-10-2002 at 03:56

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

Cyclonite Synth.

hissingnoise - 28-12-2002 at 07:52

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.

Cyclonite Synth.

hissingnoise - 28-12-2002 at 09:03

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.

hissingnoise - 28-12-2002 at 09:06

Ooops; missed a (t) in undoubtably.
When the subject is explosive, accuracy is essential.

hissingnoise - 28-12-2002 at 09:08

Don't know where the repeat came from.

/Oops/ ?

BrAiNFeVeR - 28-12-2002 at 11:40

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 ...

Madog - 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.

kingspaz - 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.

trinitrotoluene - 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?

Hexamine dinitrate

hissingnoise - 29-12-2002 at 08:29

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

trinitrotoluene - 29-12-2002 at 13:45

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

im ok

Madog - 29-12-2002 at 17:19

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.

lucifer - 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%

Madog - 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

kingspaz - 31-12-2002 at 02:02

you do know that R-salt is carcinogenic?

Madog - 1-1-2003 at 12:26

yes, its very carcinogenic, and i am going to do my best to protect myself.

Nick F - 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...

Ramiel - 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...

osamafon - 7-1-2003 at 06:12

can I dry 60% HNO3 to 99% with anhydrous Mg(ClO4)2 ?

Praetorian - 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?

Rhadon - 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.

Madog - 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.

KABOOOM(pyrojustforfun) - 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

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

Madog - 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

good news

KABOOOM(pyrojustforfun) - 30-1-2003 at 20:17

it deflagrates but some of it remains melted. so RDX probably exists in my batch

Praetorian - 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

KABOOOM(pyrojustforfun) - 9-2-2003 at 18:35

the substance didn't detonate with 0.5 g HMTD (it's probably mostly R salt)
another idea
doese any body know how oximes react with HNO2 ? 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 H2C=N-NO2 which polymerizes into RDX and (-H2C-N(NO2-)n

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)]

Madog - 11-2-2003 at 17:25

what were your yields like?

W-Process

Nick F - 12-2-2003 at 06:41

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!

an article

Polverone - 12-2-2003 at 11:38

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.

Nick F - 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...

a_bab - 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 ?

Nick F - 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.

stodgy descriptions

Krypton - 18-2-2003 at 23:08

eh,

to the best of my belief, it exist 14 different methods of RDX-synthesis.

PHILOU Zrealone - 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.

Could someone

Boob Raider - 1-4-2003 at 21:16

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)

Ok this makes me question

Boob Raider - 1-4-2003 at 21:33

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)

PHILOU Zrealone - 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:

Microtek - 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.

Krypton - 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.

Madog - 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.

Theoretic - 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.

Theoretic - 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:

KABOOOM(pyrojustforfun) - 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

KABOOOM(pyrojustforfun) - 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 NaNO2 & 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

HighPress

SAM4CH - 20-2-2009 at 05:48

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..

edmo - 10-8-2009 at 02:51

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

2verud - 11-9-2009 at 08:57

Does anyone know the runaway temperature for this nitration (meglomania recipe)? I allways like to know stuff like that before i start

hissingnoise - 26-9-2009 at 11:18

Quote: Originally posted by 2verud

(meglomania recipe)?

Recipes are for cooks and k3wls---the correct term 'synthesis' is preferred here. . .or 'synthetic method'.
If you're nitrating hexamine directly the temp shouldn't exceed 30*C.
A few minutes after the addition of hexamine to HNO3 the temp may be cautiously raised to 55*C, but this is probably unnecessary. . .
You should have several litres of drowning water close to hand for safety anyway.
If the reaction even looks like it's getting out of hand, drown it straightaway.

phantasy - 15-10-2009 at 15:13

Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205
as a dehydration agent . In 100ml HNO3 1.42gr/ml density, by 0cº temperature, in course of 10 minutes was slowly added 100 gramms of P205, then all P2O5 was added, mixute was heat to 50cº to dissolve deposition, after temperature of reaction solution place at 0cº, 10g of hexamine was slowly added in solution, temperature of solution was near 5cº. Solution was keep in 30 minutes, and add to 500 ml cold water with ice. This mixture was filtered, deposition washed 3 times by 100ml of water and dry out. 13,9 gramms of RDX with 204.4cº melting poing was obtained, i have a photos of product and another.

filaments

dr0ne - 1-11-2009 at 17:55

i followed rdx recipes and ended up with weird stuff.

i mixed h2so4 and nh4no3 to make nitric acid. the result is yellow fuminn nitric.
(btw, what is the equation for the reaction? and where is the other product of this mix)
I mixed hexamine with this fuming nitric with slight oxides. not all of it dissolved. I let it in 50 degree bath for a few minutes ( vapors might got out of the apparatus).
when i come back, there are short white fibers and no liquid. i dont think it's rdx, nor R-salt, nor hemamine dinitrate. it doesnt look like a crystal. what is it?
it melts pretty fast, dissolves really easily in water, doesnt deflagrate.

thx

Ramiel - 1-11-2009 at 21:43

haha, oh wow.
Stop doing this chemistry. Dude seriously, just a few posts up the temperature was advised to never rise above 30*C.

It sounds like you need a whole lot of more basic (and safe) schooling in chemistry before you even think about using conc. acids.

And never ask for help with a 'cook' synthesis on this site ever. Read the FAQ ffs.

User - 2-11-2009 at 05:16

Good for you, it is a very good thing that it isnt RDX.
It is allmost new years day thats when the retards start getting a horny feeling around loud noises.

Can you at least describe what you have done?

[Edited on 2-11-2009 by User]

bbartlog - 3-11-2009 at 22:13

Quote: Originally posted by dr0ne

...
i mixed h2so4 and nh4no3 to make nitric acid. the result is yellow fuminn nitric.
(btw, what is the equation for the reaction? and where is the other product of this mix)
thx

H2SO4 + 2NH4NO3 -> 2HNO3 + (NH4)2SO4, so your additional product is ammonium sulfate. Presumably. But I don't know that it makes sense to talk about these as separate products (prior to distillation/separation or what have you) since what you've really created is an acidic soup with a lot of these ions floating around.
However, there's not much anyone can do unless you at least provide quantities of the things you mixed together.

hissingnoise - 4-11-2009 at 04:46

Hexamine is decomposed by H2SO4---time for some serious reading, before you do yourself an injury!

bbartlog - 4-11-2009 at 08:01

Quote: Originally posted by dr0ne

there are short white fibers and no liquid. i dont think it's rdx, nor R-salt, nor hemamine dinitrate. it doesnt look like a crystal. what is it?
it melts pretty fast, dissolves really easily in water, doesnt deflagrate.

If hissingnoise is correct then maybe you had the ingredients to make some sort of primitive formaldehyde polymer, which might behave like this. Hexamine should hydrolyze to formaldehyde plus ammonia; the ammonia would react with the acid to form (even more) ammonium sulfate and/or ammonium bisulfate, leaving the formaldehyde to possibly form long chains. Though in the case of industrial polymers of this type (e.g. Delrin) the product is not exactly water soluble, we can assume you wouldn't have had anything more than contaminated medium-chain-length gunk.
On the other hand, it does seem a little weird that conditions that would hydrolyze one condensation product (hexamine) would also encourage the formation of another; formaldehyde polymers are supposed to be attacked by acid. Things might be very sensitive to the amount of water actually present in your mix.

hissingnoise - 4-11-2009 at 12:56

Most, or all of the formaldehyde will be oxidised by nitric acid as it forms!
Some small amounts of resins may form, in addition.

quicksilver - 5-11-2009 at 10:13

I have seen the use of WNA (1.52) used for a simple nitration on hexamine dinitate and the yield was fairly better (about 80%; don't really remember) and some of the German methods joins the synthesis of the hexamine with [what we would see as a ] nitration. That, I believe is a "plant method" and may produce the highest yield for given precursors. If we search "H2SO4, RDX" you'll get two whopper threads on it from awhile back. So the "hexamine" is IN the lab with the active nitration.
There has been a great deal of discussion as to why a "classic" mixed acid route is not used with cyclonite. Aside from all that acidic anhydride is just too damn tough to get because of all the cooks.

In fact IF acidic anhydride were available, there are fairly simple methods the synthesize HMX with limited lab expense.

[Edited on 5-11-2009 by quicksilver]

Leander - 11-11-2009 at 05:25

Quote: Originally posted by phantasy

Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205

as a dehydration agent .

I've wondered for quite some time now, whether it's possible to prepare RDX using HNO3/P2O5 as a nitrating agent. I really don't believe this k3wl I quoted, since those yields are not even achievable with 97% HNO3.

In my search for references regarding this method a basically found none. In Urbanski there are some experiments done with nitrocellulose using HNO3/H3PO4/P2O5 mixtures with good results. For the rest of the 100+ nitrations described P2O5 isn't mentioned. Also, urbanski says that H3PO4 is in fact strong enough to protonate, forming the nitronium ion.

Further, regarding the safety of such an experiment, i'm worried about nitric oxides. Books like the mercks index tell me that N2O4 is made in the lab using the same P2O% and HNO3! Unless I keep the temperature below 0oC most of it will instantly form NO2, since the equilibrium shifts to the right. The only solution for this is to use exactly enough P2O5 to react with all the water, leaving the nitric acid unharmed.

Any ideas?

[Edited on 11-11-2009 by Leander]

hissingnoise - 11-11-2009 at 05:46

Yields of 70% have been claimed for the nitrolysis using 100% HNO3, but typically it is around 65%---yields are higher using Ac2O/CH2O/AN, obviously but you'll have to synthesise Ac2O, yourself. . .

Microtek - 13-11-2009 at 10:04

HNO3 and P2O5 does not form N2O4 but rather N2O5, nitric anhydride. N2O5 is an excellent and fairly mild nitrating agent which is used in many experimental nitrolysis operations.

AndersHoveland - 23-1-2012 at 13:40

Here is a possible route that could potentially be used to selectively oxidize R-salt to RDX,

Quote:

A modified electrode comprising a film of mixed-valent ruthenium oxides with cyano cross-links on glassy carbon mediates the oxidation of N-nitrosamines. The oxidations are two-electron processes. Using N-nitrosodi-n-propylamine as a model compound, the mechanism of the oxidation was shown to involve a coupled protonation of the oxidized form of the mediating film. Bulk-scale controlled-potential electrolysis of N-nitrosamines yielded the corresponding N-nitramine; gas chromatography—mass spectrometry did not show any evidence of side reactions.
"Oxidation of N-nitrosamines at a ruthenium-based modified electrode in aqueous solutions", Waldemar Gorski, James A. Cox

see the thread about R-salt: C.T.M.T.N.A. (R-salt)
Its preparation does not require concentrated acids, even 15% conc. HCl is sufficient.

There are several threads about "glassy carbon" anodes in the technochemistry section of this forum.
http://www.sciencemadness.org/talk/viewthread.php?tid=15345
http://www.sciencemadness.org/talk/viewthread.php?tid=17370

[Edited on 23-1-2012 by AndersHoveland]

caterpillar - 1-2-2012 at 03:44

My first experiment produced only red fume. Conc HNO3 is not a problem, if you have a glass distillation apparat. According to russian- it is not actualy a book- it is something without hard cover for students something like "laboratory manual on syntesys of nitrocompaunds", excuse me my poor translation. There was a simple process described: 1 gr of hexamine per 20 gr of conc HNO3. A simple (and efficient) modification: to use not hexamine, but its dinitrate. I think anyone may recalculate how much of dinitrate can be used (and weihgt of HNO3- dinitrate puts some HNO3, so one may decrease amount of conc HNO3). This process didn't produces red fumes. Final stage is oxidation of unstable linear nitroamines. I do not remember details. reacting micture must be dissolved and some nitrous acid must be added (salt, of course). During this process liquid will boil and produce toxic gases- CH20 and NO2. Final concentration of nitric acid must be 70% if I'm correct. During oxidation RDX will precipitate. Wash it and use as you wish. I made it once and got some sow-white crystals.

quicksilver - 1-2-2012 at 10:02

The original patent from Britain proposed a 1:7 ratio of (1.5 HNO3). Ratios are similar w/ the hexamine di-nitrate ratio is not quoted to be less however the yields may be greater than 60%. It may have been Bachmann who determined that 90% acid was the lowest that could support an RDX synthesis (see PATR)

Attachment: RDX_from_Hexamine_and_Nitric_Acid_-_GB_Patent_0145791.pdf (261kB)
This file has been downloaded 1507 times

dann2 - 1-2-2012 at 11:45

Quote: Originally posted by caterpillar

My first experiment as you wish. I made it once and got some sow-white crystals.

Not very white then I guess?

[Edited on 1-2-2012 by dann2]

caterpillar - 1-2-2012 at 15:24

What makes you think so? Definitely white. It was many years ago, I cannot tell you precisily. These crystals burned with such hissing sound. BTW, you may try K process- treatment of hexamine with HNO3+NH4NO3. It promices higher yield than the simple nitrolisys. WARNING: this process requires temperature at 80 Celsius. I think, it is the best way to get as much RDX as possible (per 1 gr of conc HNO3, which is the most problematic component). Mixture of HNO3 + NH4NO3, heated up to 80 Celsius and hexamine dinitrate. It is only my proposition, of course.

AndersHoveland - 1-2-2012 at 16:39

Quote: Originally posted by KABOOOM(pyrojustforfun)

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

a very dense brown fume rushed out that made me run a way.

Peroxynitrous acid (which only transiently forms in solution) is a very strong and reactive oxidizer. It would easily attack the methylene groups also, and the result would probably be mostly a variety of undesirable oxidation products. The decomposition of peroxynitrous acid proceeds through hydroxyl radicals and nitronium cations, so it can act as both an oxidizing and nitrating agent (even in dilute solution).

Also, at such high concentrations, there is likely to be significant side reactions between the hydrochloric acid and hydrogen peroxide. Such mixtures could potentially chlorinate organic compounds.

Quote: Originally posted by KABOOOM(pyrojustforfun)

doese any body know how oximes react with HNO2 ? 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 H2C=N-NO2 which polymerizes into RDX and (-H2C-N(NO2-)n) polymers.
Edit: I thought I had edited this post before. oximes can't make nitramines that way but some hydroxylamino comopunds form nitrosohydroxylamino derivatives

Oximes can be oxidized by either nitrous acid or nitrogen dioxide, and the resulting product will depend on whether the oxime is of a ketone or aldehyde.

Oximes of ketones are oxidized to "pseudonitrosoles", with a structure such as
(CH3)2C(-NO2)-NO
The nitroso (-NO) groups tend to dimerize, so the structure could also be represented as
(CH3)2C(-NO2)-N(-O)-ON-C(-NO2)(CH3)2
Further oxidation results in geminal nitro groups,
for example (CH3)2C(NO2)2
which tend not to be thermally stable, and gradually decompose in storage.

Oximes that are adjacent to another ketone group,
for example CH3-C(=NOH)-C(=O)-CH3
are oxidized by nitrous acid to di-ketones,
R-C(=O)-C(=O)-R
"Less familiar reactions of oximes", Jeremiah P. Freeman, Chem. Rev., 1973, 73 (4), pp 283–292
(the "R" group would likely also be vulnerable to oxidation if it was a methyl group, because of additional tautomerization, but not if it was a tert-butyl or phenyl group)

(organic amines can also be oxidized by hydrogen peroxide, first to hydroxylamine derivitives, and then to oximes)

The literature seems to be conflicting.
Apparently, some oximes can be converted back to their original aldehyde, in 100% yields, by oxidation with NO2.
"Quantitative Regeneration of Carbonyl Compounds from. Oximes and hydrazones by Gaseous Nitrogen Dioxide", J. Mokhtari, Iran University of Science and Technology, Tehran (Iran) This paper specifically mentioned oxidation of benzaldehyde oxime to benzaldehyde using N2O4, with 100% yield.
Whereas in the Ponzio reaction (1906), the conversion of m-nitrobenzaldoxime to m-nitrophenyldinitromethane with dinitrogen tetroxide, is possible.
"Reinvestigation of the ponzio reaction for the preparation of gem-dinitro compounds", P.J. Honey, R. W. Millar

But I suppose what you would really be interested in is the oxidation of formaldoxime CH2=NOH with nitrous acid. I do not really know, but perhaps the below will be helpful:

"results indicate that the rearrangement from nitrosomethane to more stable trans-formaldoxime" , EXPLORING THE POTENTIAL ENERGY SURFACE OF THE CATALYZED ISOMERIZATION OF NITROSOMETHANE TO FORMALDOXIME by GUO-MING LIANG

from a patent: "The trimer is a high melting solid (m.p. 145-156 C)"

In the reaction in water, there apparently exists an equilibrium between the trimer and monomer. The formaldoxime monomer stays as the monomer in dilute solution but when formaldoxime monomer reaches 15-20 weight percent, the trimer will startto form. The rate and extent of the trimer formation seem to depend on temperature/pH/time. The higher the pH, the more the amount of monomer which forms."

this suggests that the main reaction of formaldoxime with NO2 might be formation of trinitromethane, rather than nitromethane. Although, this would mean most of it would be tied up in the trimer, and there would only be a small ammount of the CH2=NOH (with a double bond on the carbon) in equilibrium in water, and that double bond is rquired for NO2 to be able to oxidize hydrogens off.

Bot0nist - 1-2-2012 at 16:48

Quote: Originally posted by caterpillar

What makes you think so? Definitely white. It was many years ago, I cannot tell you precisily. These crystals burned with such hissing sound. BTW, you may try K process- treatment of hexamine with HNO3+NH4NO3. It promices higher yield than the simple nitrolisys. WARNING: this process requires temperature at 80 Celsius. I think, it is the best way to get as much RDX as possible (per 1 gr of conc HNO3, which is the most problematic component). Mixture of HNO3 + NH4NO3, heated up to 80 Celsius and hexamine dinitrate. It is only my proposition, of course.

He was only making fun because you said "sow-white" instead of "snow-white" crystals. Sow = mother pig. Just A typo. I know English probably isn't your first tongue. I think your typing is very good considering this.

caterpillar - 1-2-2012 at 19:02

Well, I can confirm your proposition- English isn't my mother's tongue. Well, take a piece of info:

(CH2)6N4 + 2 NH4NO3 + 4 HNO3 --> 2 RDX + 6 H2O (5.24)

This method is known as the K-process after its discoverer Koffler.
It uses ammonium nitrate to compensate for the nitrogen deficiency in hexamine and works to Equation (5.24) where two moles of RDX are produced per mole of hexamine. As observed with method 5.15.1.2, the addition of ammonium nitrate to nitric acid appears to prevent dangerous oxidation reactions from occurring. In fact, this nitrolysis reaction only occurs at elevated temperature and so a constant temperature of 80 C is usually maintained throughout the reaction. Yields of approximately 90% are attainable based on one mole of hexamine producing two moles of RDX.

I can only add that I'd use hexamine dinitrate instead of pure hexamine. Description of K method was taken from a nice and useful book, written by Agrawal and Hodgson- Organic chemisrty of explosives.

ksj_6808 - 15-8-2012 at 01:57

This is interesting...
So you can supposably get a 90% yield on cyclonite production by dissolving phosphorus pentoxide in the 95+% nitric acid, according to the patent...Now when i first heard "Phosphorus Pentoxide" i thought i could just go and buy it somewhere or at least do a simple reduction reaction to acquire it. Well thats just not really feasable. However heres how to make the p205...Pee in a cup, i suppose a 20oz and let it sit uncovered for 7 days, then take two tablespoons of finley ground charcoal and two tablespoons of finely ground cinnamon and mix them together, now put them in the urine and stirr it, then do a classic distillation except the receiver flask should be filled with water and the exit tube from the condenser in the water and you will start to see white phosphorus form in the bottom of the flask, dont remove it from the water or it will burst into flames...Now put your white phosphorus into a reaction vessle, preferably a beaker filled with oxygen gas with some type of lid, put a small hole in the lid, now take some tweezers and place the phosphorus in the middle of the beaker and take a copper rod and heat it with a torch, now reach through the hole with the rod and touch the WP and it will burst into flames and produce phophorus pentoxide, now scrape it up, seal it and use it for your next cyclonite synth!!!

ksj_6808 - 15-8-2012 at 02:17

This is even more interesting...
YOU DONT HAVE TO USE NITRIC AT ALL!!! Well kinda, what you have to have is nitrogen pentoxide, nope couldn't find that one for sale either....however you can make it as well. Nitrogen Pentoxide or "dinitrogen pentoxide" is the anhydride of nitric acid and can do the nitration job much better than just plain ol nitric, it's made by the dehydration of nitric acid with phosphorus pentoxide...Hexamine is dissolved in a little chloroform, then another beaker of chloroform has some nitrogen pentoxide, then the hexamine/chloroform solution is slowly added to the chloroform/nitrogen pentoxide solution, the nitrogen pentoxide is the nitrator in the reaction therefore precipitating pure RDX crystals!! See here's why this reaction is quite a bit more effecient than the traditional nitric/hexamine reaction...The main byproducts of this reaction are RDX, Formaldehyde, and the lower oxides of nitrogen, the formaldehyde which is the main portion of the byproducts besides RDX is insoluble in chloroform and after the hexamine is converted to RDX it comes out of the solution, you can then filter off the rdx and reuse the solution by adding more nitrogen pentoxide and hexamine to the solution, it's a continuous manufacturing solution, yields are supposed to be about 89%. Honestly it would probably be easier with the original phosphorus pentoxide method since you have to use p205 to reduce nitric acid and that just takes an extra couple of steps, both yields are about the same. Two advantages of this procedure over the first one...I imagine nitrogen pentoxide would store better than fuming acid and the fact that you can continually produce the RDX unlike the other solution where you have to put in a fresh batch of nitric. The only downsides are it's probably a bitch to make and supposedly nitrogen pentoxide is an unstable oxidizer so...

Motherload - 20-7-2013 at 22:19

Can one use a mixed acid nitrolysis of hexamine with nitrate salt and excess H3PO4 ?
I found a local chem supply for 85% H3PO4.

Or can one do a nitration of Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate with H2SO4 and nitrate salt ?

[Edited on 21-7-2013 by Motherload]

I like surprising quirky procedures. I think this is interesting.

franklyn - 22-7-2013 at 21:09

Motherload - 23-7-2013 at 11:12

Does 68% HNO3 suffice for the above reaction ?

Pulverulescent - 23-7-2013 at 11:26

I'd doubt it, Motherlode ─ I'd guess >90%!
Do you have a lot of that old HMTD lying around?

Motherload - 23-7-2013 at 13:07

Yeah it's fermenting in my wine cellar.
Well if one has to use WFNA ..... Why bother with the shitty >30% yield ?
Not to mention the need for me to wear a diaper when handling organic peroxides !!

Any input on my previous questions regarding mixed acid nitrations ?

Quote: Originally posted by Motherload

Can one use a mixed acid nitrolysis of hexamine with nitrate salt and excess H3PO4 ?
I found a local chem supply for 85% H3PO4.

Or can one do a nitration of Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate with H2SO4 and nitrate salt ?]

[Edited on 24-7-2013 by Motherload]

Rosco Bodine - 23-7-2013 at 21:08

There were some experiments done by Boomer looking at limiting ratios of acid to hexamine dinitrate for predictability of good yields.

http://www.sciencemadness.org/talk/viewthread.php?tid=4701&a...

Some discussion of reaction conditions and times and additives effect is found in the same thread.

is this correct

Vikascoder - 24-7-2013 at 01:03

Quote: Originally posted by phantasy

Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205
as a dehydration agent . In 100ml HNO3 1.42gr/ml density, by 0cº temperature, in course of 10 minutes was slowly added 100 gramms of P205, then all P2O5 was added, mixute was heat to 50cº to dissolve deposition, after temperature of reaction solution place at 0cº, 10g of hexamine was slowly added in solution, temperature of solution was near 5cº. Solution was keep in 30 minutes, and add to 500 ml cold water with ice. This mixture was filtered, deposition washed 3 times by 100ml of water and dry out. 13,9 gramms of RDX with 204.4cº melting poing was obtained, i have a photos of product and another.

Well the process I have ever found for making RDX uses HNO3 of >90% concentration and he have made RDX with HNO3 of 70% concentration only is this data correct can RDX BE MADE WITH 70% HNO3 ONLY

VladimirLem - 24-7-2013 at 08:06

Quote: Originally posted by Vikascoder

Well the process I have ever found for making RDX uses HNO3 of >90% concentration and he have made RDX with HNO3 of 70% concentration only is this data correct can RDX BE MADE WITH 70% HNO3 ONLY

Its correct, but he used some extreme stong dehydrating agent (P2O5) to that 70% HNO3

Without that dehydrating agent it would take aloooot (~days) of time to get RDX and the yield would be extremely low - all in all: that wouldnt work

malford - 7-10-2013 at 09:53

Has anyone else tried this method? P2O5 is available for <$14 for 250g and 70% HNO3 is available for <$20 for a liter. This would be far cheaper than producing or purchasing WFNA.

roXefeller - 8-12-2013 at 15:13

Bump

I didn't want to start a new thread on this when this one is relevant. How do the linear nitramines finish the polymerization into the cyclic trimer? I can work out the nitrification of the hexamine, and the nitronium doing an excellent job and breaking the hexamine into linear nitramines. The addition of urea nitrate and ammonium nitrate have a strong effect empirically on the result. I expect the species resulting from the decomp of byproducts at higher temperatures plays a role also. It was mentioned that the ammonium salt might act as a catalyst (as it does in other reactions). The Bachmann, et al article from 1951 regarding this used a nitrogen tracer and they indicated that a not insignificant portion of the ammonium ion ends up in the final trimer, suggesting that it more likely makes up for the nitrogen imbalance in the hexamine. Would this indicate that a more stoichiometric addition of ammonium nitrate is called for?

roXefeller - 19-12-2013 at 19:45

I found quite a discussion on nitramines in the Agrawal, Hodgson Org Chem of Exp text. It referenced the Bachmann results for increased yields using NH4NO3 as well as pointing out the 3 and 4 nitrogen linear nitramines that form at low temperatures prior to the heterocycle forming. I'm going through the Urbanski text still.

roXefeller - 23-12-2013 at 06:59

Quoting Agrawal:The nitrolysis of hexamine (104) is one of the most complex and widely studied processes in
the history of energetic materials synthesis. There are twelve CH2–N bonds in hexamine (104)
which can undergo scission, and with nitrolysis occurring to varying extents, it is unsurprising
that many different compounds can be produced during these reactions. Many of the possible
compounds are transient intermediates or are too unstable for isolation, as in the case of many
linear methylol nitramines whose existence is known from their reactions in solution or from
the isolation of their acetyl or nitrate ester derivatives. With so many reaction routes available
during the nitrolysis of hexamine it may seem strange that the cyclic nitramines RDX (3) and
HMX (4) can be isolated in such high yields. The reason for this observation is that both RDX
and HMX are very chemically stable and by far the most stable compounds present under
the harsh conditions of the nitrolysis. If fact, studies have shown that various fragments from
the nitrolysis of hexamine can recombine to form either RDX or HMX and so provide a sink
for active methylene and nitrogen containing fragments. Linear methylol nitramines and their
derivatives are unstable under the nitrolysis conditions and at reaction temperatures of 80◦C
they can fragment into smaller molecules which are also capable of forming RDX or HMX. End quote

I was a little disappointed with the Urbanski text. But I found the above quote on rereading Agrawal. It would seem that cyclic trimerization is merely a product of the stability sink. The addition of AN to the mix then adds the necessary nitrogen to the soup that is already leading towards stability in RDX. It does say to use a saturated AN / nitric acid solution as a nitrating medium at a temp between 60-80oC to prevent a hexamine buildup. What is the solubility of AN in nitric acid?

[Edited on 23-12-2013 by roXefeller]

Vikascoder - 30-1-2014 at 02:27

What about the synthesis of rdx using other anhydrides like phthalic anhydride instead of acetic anhydride because phthalic anhydride is easily available. Or the possible way of making acetic anhydride from phthalic anhydride

underground - 30-1-2014 at 05:59

I believe one of the easiest synthesis of rdx would be through the keto-rdx process with just only NA,SA,U and hexamine, and may the NA can be replaced with SA/Nitrate salt. Check this pdf file

[Edited on 30-1-2014 by underground]

Vikascoder - 30-1-2014 at 08:41

Quote: Originally posted by underground

I believe one of the easiest synthesis of rdx would be through the keto-rdx process with just only NA,SA,U and hexamine, and may the NA can be replaced with SA/Nitrate salt. Check this pdf file
[Edited on 30-1-2014 by underground]

In simple words I would like to tell you that rdx can not be made with sulfuric acid based nitrations do some research and then post on sciencemadness threads

[Edited on 30-1-2014 by Vikascoder]

underground - 30-1-2014 at 08:52

With this way, it can...

Attachment: Synthesis+of+Keto-RDX+and+its+Characterizations+Calculation.pdf (1.1MB)
This file has been downloaded 980 times

Motherload - 15-3-2014 at 17:51

I was wondering about CH2Cl2 as a solvent during nitrolysis.
Since only anhydrous (covalent) HNO3 is soluble in CH2Cl2 ..... any diluted HNO3 (ionic) should phase separate from the solution due to the generation of H2O when HDN is added. The dilute aqueous layer shouldn't interfere with the HDN and can be later recycled to produce more HDN.
This should keep the nitrolysis mix anhydrous and separate and shouldn't compromise yields.
Any thoughts ?

TheAlchemistPirate - 27-3-2014 at 19:51

Hey im posting this question here because I don't want to make a new thread and it seems relevant enough.
Is nitric acid produced by distilling KNO3 and H2SO4 (not vacuum) going to have more water in it than using maybe magnesium nitrate as it is anhydrous? I haven't really seen any threads on this that came to a conclusive answer.

Turner - 27-3-2014 at 19:56

No use 33ml:30g that is H2SO4:KNO3 for distillation of anhydrous nitric acid, this is a good ratio assuming sulfuric acid concentration is 95%+ and your KNO3 isn't wet obviously.

TheAlchemistPirate - 27-3-2014 at 20:04

I meant anhydrous as in not making water when reacting with acids like sulfuric, I was led to believe that it could happen. But thanks, and sorry if this isn't related to the thread.

[Edited on 28-3-2014 by TheAlchemistPirate]

roXefeller - 28-3-2014 at 12:07

This isn't acid/base neutralization where salt/water is created. This is a double replacement reaction. On that subject, never put a dry base into conc. H2SO4, far too much energy release if not done well. The water that starts out in the reaction is the 5% of H2SO4, and the HNO3 will cling to it azeotropically unless enough excess H2SO4 is present to dehydrate (hence the suggestion of 33:30 which has about 2:1 molar, one mole to react, one to dehydrate). Water will later come from the distillation if the HNO3 starts to decompose at temperature, forming H2O vapor and NOx non-condensibles. So you will generate diluent water.

Vikascoder - 31-3-2014 at 10:00

Well this thread have confused me a lot about the synthesis of rdx will anyone please help me with synthesis of rdx using hexamine dinitrate and concentrated nitric acid 95+% conc and I don't have acetic anhydride

TheAlchemistPirate - 31-3-2014 at 17:21

This guy already showed a way.

Quote: Originally posted by lucifer

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%

Zyklon-A - 31-3-2014 at 17:36

Can we please try and capitalize acronyms? (RDX) I mean, come on, here we are making high explosives. Lets try not to act k3wl. I know TheAlchemistPirate, that you are capitalizing - I'm talking to those who aren't.
http://www.sciencemadness.org/talk/viewthread.php?tid=14999

Quote: Originally posted by watson.fawkes

I suggest two social norms for capitalization. A social norm means that members may urge compliance independently, with requiring an official policy.

All chemical compounds should use proper element capitalization. I know what "naoh" probably refers to, and it's likely not a misspelling of the guy with an ark. Nevertheless, it's still harder to read. My attitude, rarely expressed directly to members who do this, is "If you can't be bothered to hit the shift key, I can't be bothered to care about your question."
All abbreviations should be spelled out in full at least once before they are used, especially in subject lines that open new threads and appear on summary pages and in HTML titles. I suggest the spell-first, abbreviation-in-parentheses-following (SP-AiPF) convention for clarity. SP-AiPF is pretty widespread already. My attitude, similarly mostly silent, is "If you can't be bothered to explain yourself, I can't be bothered to care."

To my mind, these are some of the least burdensome consequences of a general care in writing for many other people to read. There's already a social norm here that members should at least some research before asking a question. How much less work is it to take an extra moment to ask a question legibly?

[Edited on 1-4-2014 by Zyklonb]

Idea for simple RDX synthesis

underground - 1-4-2014 at 00:06

I was wondering if RDX can be made by mixing H2SO4 with an excess of Ammonium Nitrate, so all of H2SO4 is going to react, to form pure HN03, and also the rest AN is also going to help the formation of RDX

DubaiAmateurRocketry - 1-4-2014 at 02:32

^ RDX probably decompose in nitric acid which is whyyyy people use Ac2O and HNO3 for nitration of high yield.

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