RDX via nitrate/sulfuric acid

[Hinckleyforpresident]

I have searched and searched for this topic for quite some time, it shocks me that I have been unable to find any report of the synthesis of one of the most famous and powerful explosives around from a nitrate/sulfuric acid nitration mix. So I figured I'd start a thread on it.

Recently (today in fact!), I obtained 1.5 lbs of hexamine from my local camping store. I really really want to try RDX, the only problem is that obtaining nitric acid is very difficult for me (and I hate distilling).

So I got to thinking, perhaps one could make RDX from ammonium nitrate, sulfuric acid, and hexamine. A couple months ago I attempted this on a very small scale, but I had a runaway which made me skiddish of the method.

Here is the method I plan on trying at daybreak tomorrow:

-240 g (3 mol) NH4NO3 are dissolved in 156 ml (3 mol, 288g) H2SO4.
-Slowly to this 112 g hexamine is added.
-This is allowed to react for ½ hour (Honestly just a guess, I'd have to test and tweak the time).
-This is then poured into 1500ml of ice water and filtered. The filtrate is washed several times with bicarbonate solution and water.
-This is then recrystallized and dried.

Theoretical yield: 222 g RDX

I was going to cut this down by five to ten times for tomorrow.

Has anybody tried this? Am I crazy to want to attempt this? Will this accidentally make mostly hexamine dinitrate or another lesser explosive?

[totenkov]

Nope. I don't think this will work. RDX requires 99-100% nitric acid with as much nitrogen dioxides removed as possible which you probably already know. One way of making RDX is to first make Hexamethylenetetramine Dinitrate and then nitrate it with a nitrate salt to get RDX. Use this method to make
Hexamethylenetetramine Dinitrate:

5g of hexamethylenetetramine, (hexamine)
65mL of 15% hydrochloric acid,
10g of ammonium nitrate,
A 150mL beaker,
A filter funnel,
A filter paper,
A glass rod,
A fridge.

1) Pour the hydrochloric acid into the beaker and add the ammonium nitrate.
2) Stir the solution with the glass rod until all the ammonium nitrate has dissolved.
3) Cool the solution to 5*C in the fridge.
4) Add the hexamethylenetetramine. Stir it with the glass rod until it has all dissolved. A white crystalline precipitate should form.
5) Quickly filter out the precipitate.
6) Leave it in a warm, dry place to dry fully.

Now from this you make RDX via the nitrate salt method. Using Hexamethylenetetramine Dinitrate you can use concentrations of HNO3 as low as 92-93% Which can be onbtain by distilling.

Hope this helps (This is the way I make RDX, synth of hexamethylenetetramine Dinitrate taken from Mr. Cool's page.

[The_Duke]

Gosh, I wonder why we never thought of that :rolleyes:

Luckily for us Hinckley's here to amaze all with his mad k3wl chem skillz :p

And he wonders why he had a runaway rxn the first time he tried...

[Hinckleyforpresident]

I'm sorry Duke.... I searched and was unable to find anything about it. I hoped that wasn't to good to be true. Sadly, I suppose it is. I was afraid that this was WAY to simple, way to 1 + 1.

Luckily anybody in the future who hopes as I did will now find this thread.

[fiknet]

IIRC any bit of H2SO4 in your nitrating mix will start destroying your product.

[Charles Owlen Picket]

There are SPECIFIC REASONS for the ruination of RDX precursors via the introduction of mixed acids in a nitration. This is the nitration of an amine. I suggest you do some study on this issue, it's old as the hills and well researched. It will provide some insights into the nitration process. However, one cannot produce RDX with a mixed acid nitration. Attempting to do so wastes materials.

So you don't think I'm ragging on you with no positive intent, here is a hint: 1. (this is not a nitric ester so the nitration mechanism is different) 2. The resultant RDX has +3 formaldehyde, +1 ammonia, from the hexamethylenetetramine (or dinitro) starting material. There is actually more than one reason why H2SO4 cannot be utilized in the nitration.

----> Now most importantly..... If you want a fast, simple RDX-type material; consider "R-SALT" !

[Boomer]

This may be an equally stupid idea: But once you have the nitrosamine, anyone tried to oxidize it to RDX, say via H2O2? I'm no chemist, but I distantly remember it's possible to get nitro- from nitroso-. Forgot if it was on a carbon or nitrogen though.

And don't suggest this for TNT, would be too good to be true, upping the OB by making nitro- into -nitrate.

[Charles Owlen Picket]

You can bring R-salt to RDX via a direct mix acid nitration IIPC. But the yield drops to much lower than 50%. Let's say that for some reason you could never acquire high strength HNO3 and the only way would be a mixed acid nitration with solid nitrates; with R-salt as a starting point, you could use mixed acids. At least this was some of the material discoursed by Bachman.

[Rbick]

I really really want to try RDX, the only problem is that obtaining nitric acid is very difficult for me (and I hate distilling).


There is an alternative method to making RDX without the use of any concentrated acids. This is known as the "E-method", after the dude Ebele who invented it. This method was used extensively during WWII in which a Dr. Bachman began using large amounts of acetic anhydride instead of Nitric Acid to make large amounts of RDX safely. The reactants are: Acetic Anhydride, paraformaldehyde, and Ammonium Nitrate. On the web, it claims that yields of 80% have been achieved through this method in the laboratory, although only 60-70% elsewhere. This is still a great yield! The reactants are fairly easy to obtain, and I calculated the cost to be about 50 USD for decent amounts of anhydride and the paraformaldehyde. You just have to look around a bit.

The reaction is pretty straight forward, the byproducts being acetic acid and RDX:

3 CH2O + 3 NH4NO3 + 6 (CH3CO)2O -> (CH2N-NO2)3 + 12 CH3COOH

The instructions on this method can be seen on Megas site. I havn't heard anyone talk about this method nor have I tested it myself. But it is cheap, and fairly easy to obtain the needed supplies. However, acetic anhydride is an irritant and flammable, so be careful. I think its used to make methanphetamines too, which could attract unwanted attention. Just do your research so you'll have a good excuse to have it in your possession. I'll have to give this a try :)

[Hinckleyforpresident]

@Rbick

I bit the bullet and vacuum distilled some nitric acid. I must say, it's a hell of a lot faster with vacuum.

Acetic anhydride is also a rather tricky chem to acquire, since acetic anhydride + morphine --> heroin. However, if one can find it, AA seems to be cheaper when it's purchased than nitric acid.

[Rbick]

I have actually found several sources that supply acetic anhydride for 18 dollars per 500mL. Although AA is the main component in this reaction, the product and yield may be worth the cost for one not able to obtain concentrated acids, or doesn't want to deal with them. It took a bit of searching, but they are out there. The fact that it can be used to make drugs is definitely a downer. As if buying chemicals that could potentially be used to synthesize explosives wasn't bad enough, now there is this to deal with...

Because of its use for the synthesis of heroin by the diacetylation of morphine, acetic anhydride (known as 'AA' in clandestine chemistry circles) is listed as a DEA List II Precursor,[4] and restricted in many other countries.

There is also another aspect I didn't mention. Other sites state that the use of Boron Triflouride is needed as a catalyst to cut down on unwanted byproducts. I'm not sure what the byproducts would be, but it also mentioned that the yield would increase by quite a bit. BF3 is hard to find and extremely expensive. Apparently BF3 is not essential, but does help with the yield. And like other RDX synthesis methods, if the byproduct is HMX, that wouldn't bother me too much :D

[fiknet]

I have actually found several sources that supply acetic anhydride for 18 dollars per 500mL.

Oh you'll have no problem ordering it, but most companies have no qualms about taking your money first then handing your details to the appropriate law enforcement, the nice ones normally just refuse to sell it and end it there.

[Rbick]

No offense intended but; Do you have any examples or proof that they do indeed do this? I'm assuming that if they have it for sale, it isn't inteded for a trap to get you arrested. I have no doubts that the feds will AT LEAST put your name on a list of some kind, and I can only imagine the lists that I am on already... Perhaps you just need a really good excuse to have some, such as making asprin ;)

[fiknet]

Well here's something that's a similar case about some muslim guy.

"A NSW Supreme Court jury last year convicted him of acting in preparation for terrorism by seeking prices for chemicals capable of making explosives."

"He's accused of sending a fax headed 'Eagle Flyer' in October last year, requesting a list of chemical prices from the company Deltrex Chemicals."

This guy simply requested a list of prices for some chemicals (I think a few were Urea, Glycerine, Nitric acid... not a smart order, also doesn't help that he is a muslim) in with his company name which they looked up and was found to be false and they handed the information over to the police.

Also after a bit of searching and relevant to America is this document I found which gets straight to the point.

http://www.deadiversion.usdoj.gov/pubs/manuals/chem/appendix/app_e.htm

"Appendix E-1: Suspicious Orders Task Force

*
* Suspicious Orders Identification Criteria All Levels / All Chemicals
*
* Distributor (Non-retail) of Regulated OTC Products
Wholesale Drug Distribution Indicators

Appendix E-2: Factors Which May Suggest a Suspicious Transaction

Appendix E-3: Suspicious Order Reporting System for Use in Automated Tracking Systems"

The following criteria are provided in order to assist the industry in identifying suspicious orders.

"New customer or unfamiliar representative or established customer who begins ordering listed chemicals.*

Customers who don't seem to know industry practice or who fail to provide reasons for an order at variance with accepted legitimate industry practice."

So I guess my point would be to use your wits and act like a responsible member of society and unless you have a good opportunity where you know you won't get caught stay away from listed chemicals.

As for the reason why they have these chemicals there , it's not that they are a trap just that lots of highly regarded research institutions use these chemicals and have the appropriate licenses, so when the Head of Science at University of Such and Such orders 5 Liters of acetic anhydride along with some morphine and pseudoephedrine they don't bat an eyelid because they are an established scientific institution that has demonstrated that they need these chemicals for genuine research however when Mr Joe Bloggs tries to order some they say hang on this guy doesn't even have a company let alone an established research firm and he wants some Acetic Anyhydride that could make 'shitloads' of Heroin.

[Charles Owlen Picket]

You actually don't need the morphine. Codeine will function just fine....that's the issue. The real gateway is the AA. However if you ordered a small sample like 500ml or some shit like that you most likely would not get a knock on the door; but you would get on the "A-team" list. And from then on you would be looked at for other issues. From that point on they would consider dealing with you. Get enough attention and someone would make a "snitch-proposal" to you or some other serious nightmare. No way in Hell I would be buying that or Red P or anything else that said "drug-cook"......it just ain't worth it.

[Rbick]

I see, that is a good example.

The muslim dude failed in what I call the "social engineering" portion of his attempt. And the fact hes a muslim doesn't support his attempt either :rolleyes: I have actually contacted several companies via phone for samples of products and have actually purchased a few. I found the key is to remain professional and precise with your order. They usually do inquire as to why, so I always do my research and provide a reason.

I think it is rather silly he requested those things all at once from one company.

*RING RING* -Hello, this is Deltrex Chemicals, you're leading supplier in fine chemicals and reagents, how may we help you?

-(with heavy accent)Yes, hello, this is Mohammed with the Jihad company. We would like to order some Sulfuric Acid, some Nitric Acid, some Pentaerythritol and a pack of gum please.

-Ok, and in what quantities?

-Alot. Can we pick them up in our personal vehicle?

-No sir, these are hazardous materials and require a class D HAZMAT license.

-Oh, ok... I guess I just want to know how much they are... Death to the infadels!

Ok I doubt it was that bad, but it might as well have been :p. Anyway, there are companies out there, mostly in Texas where laws on this sort of thing are very "lose" who don't require the person ordering to be part of an institution. Its a money transaction, a shipment, and no questions asked. Of course this doesn't prevent the feds from tracking it, but unless you're making rediculous orders and a lot of them, it shouldn't be a problem.

Anyway, back on topic. I looked up synthesis for AA as a way to aquire it through other means than just ordering some. The processes are usually quite complex, but can be found by searching "Acetic Anhydride Synthesis" in google. I'll have to go with Charles on this, it probably isn't worth it. As I said before, a few of us here are probably already on enough lists as it is. Although this process would be cool to experiment with, and if one had the access to AA without arising suspicion, it would probably be a great idea. In my case, I'll probably just stick with the HNO3 distillation apparatus...

[Charles Owlen Picket]

Frankly, I can't underline enough the reasons why not to do something of this nature (acquiring materials that can be used for drugs, etc). Most people on this forum are either "Walter Mitty" types or young people who are a bit wild but both are basically harmless. Why raise an eyebrow from the authorities? Why paint one's self as something that you are not?

Personally, I love my country, have served my country, would not do anything to harm my country or others who have not harmed me. I have some interests that could be painted as out of the mainstream but not to the point of being anything but a bit eccentric. That's fine and it's true. I don't need headaches from over zealous bureaucrats attempting to pump up their stats.

[Emil]

The worst thing about it all is not knowing who or what is watching you.

We don't know for sure what gets you on a "list" or what would get you a visit from the people themself, as they are the only ones who know.
Overall it's just a area or science to stay far far away from.

It's like dipping your foot in the bath water before you have tested it with your finger... by the time you realise it's too hot, you've already been burned.

I personally find one of the greatest feelings is knowing that you definitely haven't raised any eyebrows. This gives a feeling of acomplishment, knowing that you have started from complete scratch, with basic OTC materials, and have exited with your specific material.

For example, fuming Nitric acid - To most of us, Impossible to buy. That's why being able to produce it is the greatest gift of all. Leave the watched chemicals to the uneducated, the desperate, and the damn right stupid ;)

[Charles Owlen Picket]

Ya' know.....this opens up the subject of what is a watched chemical at this point in time. The reason why I say that is that so many materials have been added to various lists that from a somewhat paranoid perspective you could make a case that virtually anything could get you on a list. The reporting agenda is stronger than the chemical itself. If someone wants to drop a dime due to acetone purchase; it would suffice as a watched chemical.

The CPSC has made a great many chemicals restricted but not watched per se'. But as soon as you cross the line to actually getting a list chemical tied up with a restricted one you certainly will get some attention.

One way of knowing if you actually are on a list is if you ever bought anything from any company that was involved with the big CPSC pyro issues. If you ever got "The Letter", it goes without saying; you're on a list. If you ever applied for any fed license, etc. But really, all in all, it's not that big of a deal. I know that I am on one or two lists. I just don't want to get on eight or ten of them.

That's the basic reason for not chasing down some AA. I would love to have about a gallon but that's still too much. I think they top out at 500ml. Shit, that's about 2-3 labs. Just enough to learn what you are doing inefficiently.

[Rbick]

Yes the AA is a bad idea. I did some more research and any place you can get it from requires you to fill out a "Form of Intent" describing what you plan to do with it. I wonder if they would be more happy about finding that it was for RDX instead of meth :D

The best route I can think of without using concentrated nitric acid in starting with nitrosomine (R-salt, mentioned earlier by Charles) which can be made via reacting nitrous acid with hexamine. Nitrous acid can be made by dissolving a nitrite in concentrated HCl in an aqueous solution. For example, NaNO2 is dissolved in water and mixed with HCl. The positive H ion of HCl disassociates in water and a double replacement reaction takes place, with NaCl (table salt) and HNO2 (nitrous acid) being formed. This is then mixed with hexamine to give you the nitrosomine, which is the same as RDX except with NO groups instead of NO2. PH must be kept at 1 or the dinitroso will form instead of the trinitroso, which is not what you want. VoD is around 7800 m/sec at 1.4 g/cm3 or something. And its carcinogenic! YAY. More detailed synthesis info is available through an easy search on the forum.

There is also this file from sciencemadness (http://www.sciencemadness.org/talk/viewthread.php?action=attachment&tid=3453&pid=59793), which is quite helpful

This apparently can be oxidized into RDX quite easily. I've seen methods with and without HNO3, and even one involving hydrogen peroxide. Nitrites are fairly easy to find and cheap.

I wouldn't be too complacent with being on "the list". Even if you haven't ordered nitric acid before, it pays to be cautious. Buying simple nitrates such as AN is now being watched closely, and nitrates are a must for distilling Nitric Acid, obviously. Be careful out there ;)

EDIT: Here is a good paper on the carcinogenic properties of nitrosamines: http://lpi.oregonstate.edu/f-w00/nitrosamine.html From what I can tell, as long as you don't eat it or accidentally ingest it through absorption through the skin, you should be ok. Just wear protective gear while handling and wash well when done :)

[Masonjar Chemist]

Rbick, would you mind letting us in on your source of nitrites? I have been on the look out for them for over a year and still have had no luck. The decomposition of nitrates arent really working for me either, so any help is much appreciated. Oh, and please pm me if you are worried about keeping it a secret, thanks.

[ChippedHammer]

Well here's something that's a similar case about some muslim guy.

He attempted to buy 20L of nitric and sulfuric acids (in 2.5L bottles) and about a gallon glycerine. No wonder why they forwarded his order to the feds.

Having a raghead name didn't help his cause.

He also tried and failed to buy sulfuric acid by attempting to bullshit his way through a order of supposed 'battery acid', that company I think ended up ignoring him instead of contacting the feds.

[Rbick]

In response to Masonjar: It is well known that nitrites such as potassium and sodium nitrite are used in preserving foods. That should help you narrow down your search. Also, there are several online sources that supply reagent grade nitrites.

What methods are you using to decompose your nitrates to nitrites? Simply heating KNO3 will probably yield you very low amounts, as the decomposition temp. of the N-O bond to make it a nitrite is close to that of the other bonds, which will leave you with very little and impure nitrite.

There are several methods out there, and I saw some a sciencemadness and here on RS. For example, you could mix 2Al + 3KNO3 ---> Al2O3 + 3KNO2

This can also be done with Lead, magnesium, and even carbon. The method involves melting both reactants, then mixing a stirring. Search around and you'll be able to find detailed descriptions. A way to test your end product would be to dissolve it in water and check solubility, as Potassium Nitrite is very soluble in water. Or mixing it with HCl to see if it creates Nitrous Acid, which is blue in color.

ChippedHammer: Thats hilarious. That is ALOT of fricken acids. What the hell was going through his mind? Thankfully, most of us are smarter than that... I hope. Nitrating 3.7L of glycerine would be annoying and time consuming, not to mention dangerous. That would take one huge ass separating funnel :D Still, if he did succeed, even if he broke even in volume of product, some dumb ass terrorist would have about 6kg of NG :eek:

EDIT: Before you guys go off trying to make the nitrosamine so you can have a shot at RDX, read this article (http://www.robac.co.uk/DOC/Nitrosamines_solutions.pdf) as well as the one I have in my last post about the mutagenic and carcinogenic properties of it. If you take proper safety precautions like not letting it touch ANY part of your body, you should be ok. I'm not sure if I'd be willing to take the risk...

[ChippedHammer]

ChippedHammer: Thats hilarious. That is ALOT of fricken acids. What the hell was going through his mind? Thankfully, most of us are smarter than that... I hope. Nitrating 3.7L of glycerine would be annoying and time consuming, not to mention dangerous. That would take one huge ass separating funnel :D Still, if he did succeed, even if he broke even in volume of product, some dumb ass terrorist would have about 6kg of NG :eek:

Even if they got everything they needed it was doubtful that they would make a working device - I doubt they would have gotten close with their jihad joe DIY book they had.

Nitrites are fairly easy to buy, search for the food numbers (E249, E250) in google or find a specialist shop.

[Yafmot]

They shouldve just called the authorities with the idea of letting them go ahead and attempt to make all that NG, while keeping them under suveillance. They'd probably have an accident, medieval dumbshits that they are. And if they did manage to make six kilos, just stick a .50 API through their product. We, in the physical realm, would get a cloud of jihadi atoms, and they'd be up there with Allah and their 72 virgins. (And wait 'till they find out WHY they're virgins! UUGGHH!!!)

===

This is a +1 post on a two month old thread. Don't do it again. - Enkidu

[Sweeper]

Please never told lies about an uric nitrate and the sensitivity against sulfuric acid ! Shit happens, what nitrate you came up to the stuff by mixing it to it ! Nothing will yield RDX or B-Type. My experiences told, HNO3 treated with at least NH4NO4 by adding HMT chauses a yield to zero and adding HMT to HNO3 and H2SO4. Better cool or die ! Never you can exctract an nitrnamine from this
with H2SO4. Acetic anhydride will help to simulate a homemade HNO3 to <99%.

A yield result told me, NH4NO3 is an precipitation inhibitor when adding HMT to HNO3. 5 parts HNO3/one part acetic anhydride can increase the yield by bind the water in the HNO3 and what developed.
In my oppinion, RDX is never get with an nitrate and Su-acid.

[Masonjar Chemist]

Come again? I didn't quite catch what you were trying to say.

I think I understood that sulfuric acid destroys urea nitrate, nitric acid and ammonium nitrate will not produce any yeild (of, I am assuming RDX) when you add HMT to it, you should put your reaction vessel in an ice bath when mixing HMT, H2SO4, and HNO3 unless you want to die and you shouldn't expect any nitramine product from it assuming you do live through the reaction.

Ammonium nitrate prevents precipitates from forming when you add HMT to nitric acid? What is this Su-acid, Sulfuric?

I am amazed at the level you managed to rape the English language, heres good luck to you for being able to stay around long enough to have a chance to improve on it.

[-=HeX=-]

Masonjar: thank you for doing that. I was going to last night but the extent of the rape injured my eyes. You have translated it correctly. And no, sulphuric does not destroy urea nitrate, it is used to make it into nitrourea.

Also, what is so special about RDX? ETN or PETN can of the job as well, just with a bit lower velocity of detonation. Do you all want to make it into shaped charges? Or just for the experience?

[megalomania]

Don't listen to a word that idiot sweeper is spewing out with his bad machine translation. We have no way of knowing what he is talking about since he can't write in English. Either that or he has some sort of typing impediment :)