RDX again - Archive File

[megalomania]

stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 07-21-2001 04:46 PM
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on this page : http://huizen.dds.nl/~arcticus/synthesis.htm the guy says :

"A final word: the actual equation is 1Hexamine + 4 Nitric Acid ==> 1RDX + 3formaldehyde. So, if we calculate the actual ratios, we find: (mass-ratio)
1.8 Nitric Acid + 1.0 Hexamine ==> 1.59 RDX. Of course, we want to keep the reaction going, so we don't allow the nitric acid concentration to drop below 80% (advised to use an initial concentration of at least 95% fuming). So, we get 100gr hexamine, requires 180 grams of nitric acid (=120 ml) and produces c*159 grams of RDX where c is the yield-ratio. But, the minimum conc should be around 80%, so we don't use 120 ml of nitric acid, but 120/(1-0,8) = 600ml of nitric acid! So, you can use actually twice the amount of hexamine than the books instruct you to use. Wow, that just saved you twice your amount of precious nitric acid! (But if you do decide to use 50 gr, keep in mind that after the reaction the nitric acid concentration is 90% instead of 80%)."

So, if I put 100 g of hexa in 180g of my 95%nitric acid (distilled H2SO4/NaNO3) while stirring vigorously then i heat the solution to 50-60°C for 10 min, i will get 159 g of RDX ???

is this equation right ? and why this fucking Anarchist Crapbook say 50 g in 550 mL !!!!!!??????? and why Megalomania use 75 g in 335 mL ???

Who can I believe ? what's is the real equation ? (in mass ratio)

any reply is more than appreciated...



Tony Montana
Frequent Poster
Posts: 145
From: Australia
Registered: JUN 2001
posted 07-21-2001 06:58 PM
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Trust Megas recipe!!!!!!!

[mandate]

Gone in the blink of an eye. :p

NBK

[kingspaz]

mandate, what is the point of that post? i advice people not to email him as he seems a little *too* forward by posting his email address and that.

[grittysoap]

don't believe any of the fucking high explosive synthesis in the terrorist's handbook.
I had a bad experience with the synthesis of nitroglycerin by that bastard jolly roger a few years ago....the heat rose way to high when I was dripping in the glycerin I had to run away very fucking fast I don't remember what the sythesis was but it was a load of shite

[Mendeleev]

I am trying to dream of make RDX :eek:. It seems deceptively simple. Slowly dissovle hexamine in nitric acid, heat to 55 Celsius, for ten minutes, dump into cold water with baking soda, filter, wash with aceton. Great, except it seems the problem everyone including me is having is getting very concentrated nitric acid :mad:. I do not have the cash or time to set up a complex vacuum distillation with sulfuric acid process, so my only option is pretty much to make concentrated nitric acid using the potassium nitrate + sulfuric acid distillation method. All I want to know is, will the acid from the KNO3 process be conentrated enough to get a semi-decent yield of RDX :confused:?

Thanks :)

[Unknown]

I'm not going to say anything about searching because I am a new poster myself, so I will give you some help. Refer to the "Concentrating HNO3 - Archive File" in the "special project 1: nitric acid" section. There are also numerous other rdx thread that go over concentrating HNO3.
What I will tell you is that you are damn lucky that NBK is on vacation, you still have a fighting chance depending on how forgiving the Mods feel.

[Microtek]

I have written a report on the product of atmospheric distillation ( of dilute HNO3 + conc H2SO4 but the same will go for XNO3 + H2SO4 ). The thread is called " Quantitative report on HNO3 distillation " and it should answer your question ( even though it didn't get a single response ).

[SantasL.Helper]

OK, i tried making RDX using the synth described on AlenG's site: AlenG (http://www.angelfire.com/linux/alengg/main.html)
(synth is on the bottom of the page)

I used my own distilled nitric acid (no vacuum was used during distilling) of which i do not know the concentration and HDN. Quantities: 20 ml nitric, 4,5 gram HDN


I'd put the orange/yellow coloured nitric acid in an erlenmeyer and started to slowly add HDN, keeping the temperature between 25 and 30 degrees celcius. When comming to the end of the addition, the colour of the nitric acid went from orange/yellow, to colourless. The mixture did not go white/cloudy as said on the site. I could also see white coloured gasses (smelled like NOx) forming during the addition.

After heating the mixture etc, i added the mix to water and white crystals formed very quickly. I filtered these, disolved them in aceton, filtered again, and added to water. Again i saw white crystals. Now i asume these are RDX crystals.

They look a bit like HMTD (not like AP, verrrrry fine crystals), white coloured.

Now, excluding detonating it, is there another way of finding out this is RDX and not something else??

[Sonny Jim]

Leave it out dry for a while. RDX is not hygroscopic, while HDN is. If your powder becomes clumped and damp, then you probably have HDN still, because your HNO3 was not strong enough. If not, then I would say you have RDX.

[SantasL.Helper]

How hygroscopic is HDN? Just as bad as AN? Will be totally dissolved in a lill pool of water if you let it sit in the open for a couple of days?

Anyone know another way of indicating?

[blindreeper]

From my experiences HDN left out for a day will become a little pool of sludge! So it is probably worse than AN. Did most of the product desolve in the acetone? Because HDN is insoluble in acetone I think, pretty sure though. If msot of it did dissolve it should be RDX and the residue (crap left in the filter) may be unreacted HDN. Good luck for your sake I hope its RDX

[SantasL.Helper]

Yes i disolved it in aceton aswell, filtered the stuff that didn't dissolve. So it should practically be RDX... Sounds good.

[Mendeleev]

On AlenG's site, it says to first make hexamine dinitrate then add that to 95% or greater nitric acid to get RDX. I thought you could just add hexamine directly to 98% nitric acid and get RDX. Can you?

[blindreeper]

You certainly can use straight hexamine, however using hexamine dinitrate increases yeilds because it already has two NO2 groups attached to it I *think*

[SantasL.Helper]

Question, i lit the ?rdx? and i saw the most beatiful lill flame i've ever seen. Very bright orange, almost white fast burning little flame. Made a "sishhhhh" sound.

This normal?? Should the RDX even burn?

[Microtek]

Yes, it should. But really, if you performed the standard process for RDX synthesis ( that is, by adding hexamine or hexamine dinitrate to highly concentrated HNO3 and regulate temperature as described ), there are only two possible outcomes. Either your acid is not concentrated enough and you will get hexamine dinitrate which is very soluble in warm water, or the acid is sufficiently concentrated and you will get RDX in yields which are dependent on concentration, reaction time, etc. RDX is completely insoluble in water, so separating the two is a simple thing.
RDX is not hugely soluble in acetone ( especially water containing acetone ) so I suggest you use water to remove HDN instead.

[SantasL.Helper]

A ok then... YAY!! I'VE MADE RDXXXXX!!!! :p

[Microtek]

BTW, if your acid is strong enough, the best economy is achieved by using 10 grams of HDN to 20 mL HNO3 and letting it react for 25-50 minutes after the last addition of HDN ( including the time it takes to heat to 55 C ). The yield is 74% of theory or more importantly, 0.31 g RDX per mL HNO3. I have not tested the melting point of the product, but performance is equal to other batches made with more conservative HNO3 expenditure.
Concerning HNO3 concentration, I can say that I make mine by distilling a mix of 1 volume of 62% HNO3 and 1 volume of 90 % H2SO4, mixing the product ( which titrates as 88 % ) with an equal volume of 96 % H2SO4 and distilling again. Distillation is carried out in a retort without water cooling or reduced pressure, but with very gentle heating via hotplate and sandbath. The product is heated to 40-50 C and dried air is bubbled through until almost all the yellow colour has disappeared ( this can take more than 10 min ). A pinch of urea is added with swirling, and the acid then titrates as 96 % and is completely colourless when cool.

[Mendeleev]

In the enormous 10 page PETN thread, there was a discussion about how PETN can be made with either a large quantity of very pure nitric acid, or a balanced quantities of 98% H2SO4 and roughly 60-70% HNO3. Well you should be able to do the same for RDX right, since the sulfuric acid simply acts as a dehydrating agent, to concentrate the acid to get better yields right?

[Microtek]

No. This has been discussed many times; sulfuric acid destroys both intermediaries in the reaction and rdx itself. No product will be collected.

[SantasL.Helper]

i had a runnaway reaction yesterday with RDX using red fuming nitric. I was looking at the beaker that was standing in the icebath as the temp went a lill too hight (33 degrees) and i saw the red fumes collecting downwards in the icebath instead of going up my fumehood. So i thought, hmmm thats strange, probably because of the gasses cooling, so i checked the temperature. Then as i stood on a bit higher level i could see that a. my mix was bubling and smoking NO2 (faster and faster) and b. that when looking at my thermometer i could see the temp shooting up to 45-50-60. Dumped it all in ice water and collected the RDX, so nothing REALLY bad did actually happen.

Question:
I was using red fuming nitric acid:
How can i other then adding the HDN to the acid very slowly avoid a runnaway reaction?
And b. how can i best avoid getting killed by NO2?, i mean after being bussy a while i couldn't detect the smell of NO2 anymore (due to the sensors in my nose getting paralised)

[Dave Angel]

I've been doing a bit of reading on RDX and I think it was mentioned somewhere that the process with red nitric acid must be kept very cool compared to the white nitric process which is heated to 50-55C.

Hope you didn't breath in too much NOx - nasty stuff... I use a half face respirator with filters that are supposed to keep out organics, but seem to block NOx and NH3 aswell, as I mentioned in the NC thread in the watercooler.

Also, I have a couple of questions:

Does anyone know if it's possible to use glacial acetic acid and a nitrate salt to nitrate hexamine? This was just a thought that crossed my mind, I have no idea if / how well it would work, but it may be worth investigating if it can't be disproved theoretically.

The other question is has anyone tried using sulphuric acid to break down unprecipitated RDX and other organics before attempting acid recovery? I've read Mr Cools horror story about acid recovery, but I wonder if treatment with H2SO4 first might make the difference.

[MrMagnum]

Please let me underline that NOx is a really dangerous stuff as it stays for a long period of time within the lungs. The first toxic signs and symptoms occur 24 to 48 hours after the inhalation.

You inhale NOx, think that everything's allright and two days later...suddenly...!

Be careful with NOx!!

[SantasL.Helper]

Might be a dumb question, but why will a reaction run away in the first place and why will it happen faster when there is too much NO2 in your nitric acid? I'd say a runnaway is caused when the heat produced goes up, causing the speed of the reaction to go up creating a kind of snowball effect, dunno if i'm right though. But why does this happen way faster when using red fuming nitric acid?

[mongo blongo]

Yes you are right. As I understand it the NOx also acts as an oxidizing agent that will attack the intermediate products and subsequently many other side reactions will occur, releasing a lot of heat (at higher temps,decomposing remaining HNO3 to more NOx) which will add to the "snowball effect".

[Eyes Only]

There is a route to RDX by reacting hexamine dissolved in acetic acid with ammonium nitrate (or ammonia) dissolved in 100% nitric acid (the Bachman method as used at Holston AAP in Tennessee). This produces the so called Bachman RDX which contains up to 10% HMX - ( opposed to Woolwich RDX which is 100% pure)

Yo don't want o go messing with HMX - it comes in differet crysatalline forms abd iuf you are unlucky enough to generate a beta/gamma hybrid, you could find yourself in serious trouble (i.e. bits missing or dead).

Ever wondered what happens to all that hexamine that doesn't become RDX? Ever wondered where all that NOx comes from? Beware of linear nitramines - they make sweating gelignite look user friendly.

Eyes Only

[SantasL.Helper]

Damn, i've now multiple times made RDX by nitrating HDN but this is going to strange. I've made it with above 90% nitric couple of times but last time i did it with even 77%!!! Every time i ended up with the same insoluable in water and soluable in aceton product that burns with that o so beautiful flame and is capable of detonation. So wtf is going on!? Why am i able to make RDX (which i seriously assume it is) by nitrating HDN with even 77% nitric?

[PhoeniX_KEA]

Can RDX be made in the following mannar?
GENERAL DESCRIPTION
Formaldehyde and ammonia yield methenamine, or hexamethylenetetramine.
(from HEXAMINE) Nitration of methenamine gives the explosive cyclonite, or RDX.

[SantasL.Helper]

Depending on how you're going to use your nitric acid and how strong your acid is, yes

[Mendeleev]

Yeah, to make RDX hexamine is nitrated. Hexamine is made from paraformaldehyde and ammonia, not formaldehyde, or will formaldehyde work as well?

[Not_Osama]

I like to store my HDX or any highly hygroscopic explosives in pill bottles, they are almost always airtight and there are no screw threads to accidentally detonate the more sensitive ones...my cousin lost his thumb and middle finger when some black powder detonated that way.

[Ollie Snowie]

Formaldehyde will work, as paraformaldehyde is just a polymer of formaldehyde made by mixing formaldehyde with concentrated sulphuric acid. It is easier to store and handle than straight formaldehyde because formaldehyde is a gas at room temperature (liquid "formalin" is an aqueous solution of formaldehyde).
I've never seen anything posted about RDX being hygroscopic, but I wouldn't know because I've never made RDX. Never heard of HDX and nothing except this thread comes up in a search - was that a typo? Is so, was it RDX or HDN? HDN must be kept away from water because it will decompose. It doesn't seem very useful except as an intermediate stage in making RDX.
I think most of the stuff about sensitive explosives in non screw threaded bottles and hygroscopic stuff sealed up was fairly obvoius and not really relevant to RDX.

[SantasL.Helper]

Heh, my HDN seems to have some colour changing. It went from normal white christals to something nearly the colour of potassium bichromate. I'd say this is caused by it decomposing right?

[Mumble]

Going from white to orange/red is a pretty good sign of decomposition. It's also a pretty drastic change. Perhaps there was some photosensitive dye added at some point. Perhaps there is some impurity that is decomposing.

How long has this batch of crystals been being stored? Are there any odd conditions like being stored in direct sunlight or in a damp place? Was anything spilt or left over in the container?

If any of the compounds I have being stored demonstrated that much of a color change because of what I assumed to be decomposition I would get rid of it as soon as humanly possible. Expecially if I didn't know what products were being formed. You obviously don't know this.

[al93535]

I made RDX using this method:
50 ml distilled white nitric acid
6 grams Hexamine
in an ice bath I dissolved Hex into the HNO3 slowly, it made a hissing noise
keeping the solution at about 20 degrees
after it all dissolved it was placed in a hot water bath to raise temperature to 55 degrees
stirred while keeping at 55 for 12 minutes
When solution reached 55 degrees it began bubbling
as solution cooled to 25 degrees a stir caused some RDX to precipitate in the acid
poured into 175 ml water and instant precipitation
Final dry yield: 3.1562 grams
Has anyone else seen the bubbling after it reached 55? decomposing? Any ideas?
EDIT: Ahh I bet it was producing formaldehyde?

[Microtek]

When you heat the mix after having added the hexamine, you are decomposing unstable linear nitramines which are undesirable in the finished product. Among the decomposition products are assorted gaseous species which cause the bubbling.
Your method is hugely inefficient. If you use thoroughly dried hexamine dinitrate instead of straight hexamine, you can get away with adding 25 grams of HDN to 50 mL HNO3 and still achieve a yield of 74 %.
That is, 15.5 g RDX from 50 mL HNO3. Of course you also need a little low conc. HNO3 for making the HDN but that is almost negligible.
If you decide to try my method, you should pay particular attention to drying the HDN. I suggest washing the filtered HDN once with alcohol and once with acetone, quickly air drying in a place with low humidity and then storing it in an airtight box with some kind of dessicant ( CaCl2, AN, etc ).

[Boomer]

That sounds good, my HDN with the same method was not perfectly dry, and I got 12g. :(

I know RDX is more brisant than NG, and easier to use (no headache, can be pressed or plastified ...).
BUT with that amount of high conc HNO3 I can make MUCH more NG than RDX. Best yield up to now was 108ml neutralised NG (120ml acidic) from 125ml HNO3 and 60ml glycerine. That is 580% of my / 450% of your RDX yield per ml of NA! BTW this is 93% of theory.

If I want a solid HE with 8260m/s VoD, I make MHN. The yield is again easily 90% of theory, giving 65g (instead of 15g) of a stuff that has more energy than RDX at 95% of its brisance. :D

[al93535]

Microtek,

I believe thats what I will do next. And I will make sure to use the acetone/alcohol washing. I will post my results after converting to RDX. However if I use HDN instead of hexamine, do I still follow the exact same procedure, besides the increase in HDN vs. hex? Thanks for the information. :D

[Mendeleev]

Why are the yields for RDX so bad? Nitroglycerine and picric acid nearly double in amount while RDX nearly halves in amount. Will the procedure involving acetic anhydride improve yields, if so by how much?

[Microtek]

Al93535: Yes, the method is exactly the same; 20-30 C during addition, 50-55 C for 5 min, then allowing it to cool. You should then wait until 30 minutes has elapsed from the end of the addition before you dilute it with water.

Mendeleev: In my experience the process using Ac2O, AN and paraformaldehyde does not give very good yields. Whether it is worthwhile will of course depend on what is easier to obtain: HNO3 or acetic anhydride.

Boomer: I agree that the nitric esters are very hard to beat from a yield/performance perspective, but RDX and HMX have their uses. RDX is a useful alternative to PETN or MHN as a high melting HE for use in thermoplastic PBXs ( eg, my polyethylene/RDX (15/85); PETN melts at the processing temperature for polyethylene and cast explosives do not have the chemical or mechanical resistance of that PBX ).
HMX obviously has the advantage of VOD, though I haven't used it much yet as I haven't found a good way to prepare uniform liners for shaped charges.
Regarding NG, I don't really like to use it as an explosive in itself, instead I incorporate it in composites as energetic plasticizer or oxygen donor.

[al93535]

I tried making RDX from HDN to improve my yield and got no RDX! :mad:
I did everything just as I did before with hexamine, except I used an ice bath to cool it down after heating it to 55 degrees. My HDN was completely dry. The only thing I can think of is last time I let the solution cool down by sitting in the air, giving it extra time. This time it sat for 15 minutes after cooling to 20 in the ice bath. Any ideas? :confused: I used 50 ml distilled HNO3, 18.5 grams HDN. I added the HDN rather quickly because not much heat was generated. After it dissolved it was heated to 55 for 12 minutes, cooled in ice bath, sat for 15 minutes and added to 200 ml water. I let the solution sit for 30 minutes with no precipitate.
EDIT: Boomer: What is MHN?
EDIT: Pdb: Thanks alot, I wasn't quite sure.

[pdb]

MHN stands for mannitol hexanitrate...

[Microtek]

Al93535: Don't use an icebath and don't hold it at 55 C for so long. As I said, 5 minutes at 55 C and let it cool on its own until at least 30 minutes has passed since the end of addition. You should also stir it ( or at least swirl frequently ) for the entire duration of the synthesis. That is until you have quenched the reaction in water.

[al93535]

Thanks Microtek,
I did my synthesis before I read your earlier post, and didn't wait long enough. I will make some more HDN and try again. I make sure to stir through the whole procedure. And why do you only heat for 5 minutes? Does the longer heating reduce yield? I read on here, someone heated for 10 minutes, then another one for 12 and got a higher yield. Thanks again,

[Microtek]

I can't say for certain whether a longer heating period will have any effect on yield. It is probable that yield will be increased if the nitration time at 20-30 C was not long enough in the first place, due to the increased reaction rate at elevated temperature. Then again, decomposition may play a role in prolonged heating. The purpose of heating is to decompose unstable linear nitramines, which can be done in 5 minutes according to the litterature so in my opinion, any more than that is superflous.
At any rate, it is a good idea to change only one parameter at a time when optimizing or debugging any kind of procedure, not just in chemistry.
It will save you some headaches if some of those parameters act in opposite ways.

[Maniak]

the process of making RDX using acetic anhydride is the better way for who have some anhydride - but not with paraformaldehyde, it gives very bad yields and poor quality. I use only the method with HNO3,Ac2O,HDN and AN and there are results:
700ml acetic anhydride
165g amonium nitrate
90ml fuming HNO3 (cca 95%, quite bad quality)
250g dry HDN
yield: 280-310g RDX, m.p.193°C, stabilised by boiling with water for 30min.

[Mendeleev]

Wow, that is an incredible yield! Thank you very much for the information, Maniak. I will get working on my anhydride still. RDX is melt castable right? If so does anyone have experience in casting RDX, the high temperature would make it much more difficult than TNT, thus my inquiry. Furthermore, how significant would the gains be in performance of cast RDX?

[mongo blongo]

RDX is not cast (melted) on it's own. It is mixed with a castable explosive like TNT (to make comp B) or Erithritoltetranitrate with low melting points and then cast. The gains are mainly increased VOD, good for shaped charges and EFP's.

[Microtek]

I don't think 300 g RDX from 700 mL Ac2O is really good. I would rather use 1000 mL HNO3 to get the same amount of RDX and then use the Ac2O for HMX. Although, if you have access to P2O5 as well, then there is a method that is much better in my opinion ( you still need the anhydride ).

[palpy]

Microtek: Yes, that's true for the US and other countries, where Ac2O is banned, but if you can obtain it for some $4/litre... ;))

[Mendeleev]

The point is, he got an increased mass of RDX from HDN, compared to other members who got nearly half the mass of RDX from HDN. Furthermore he used 90 mL of HNO3 for 250g HDN. Also, I think the Ac2O can be recycled with greater ease than the spent nitric. Or am I wrong?

[Maniak]

yes, my yield is about 74% of theory (theoretical yield is about 410g RDX from 250g HDN). I agree with Palpy, in some countries it is easy to buy the anhydride or it is easier then making fuming NA.
But I´m not sure that you can recycle anhydride, you can only take 20% of spent anhydride (acetic acid) and add it to next reaction to improve next yield. It´s much difficult (for me) to recycle an acetic acid to an anhydride by keten process.

[Mendeleev]

I recently was reading several articles on www.howstuffworks.com , a crappy website for 3rd greater, but it came on a google search about bunker buster bombs and the new moab (massive ordnance air burst), which has 18,000 lbs of HE, that's around 8000 kg, however I was surprised to find out that bunker busters and moab use tritonal, a mix of 80% TNT and 20% Aluminum powder, having a relative brisance of 118% that of TNT. This surprised me because bunker busters need to have as much power as possible, and TNT isn't exactly the best way to go with RDX and HMX on the table. I had always figured RDX and HMX were the explosives of choice for bunker busters and shaped charges so I was little thrown off. Does anyone know why they use tritonal as opposed to RDX or HMX :confused:? Oh, and they have a video of moab detonating, nothing impressive because it detonates in the desert with nothing to compare the blast size with, but still. Furthermore, I read about the hellfire missile on the Apache helicopter being able to blow apart the the entire frame of a T-72 tank, as opposed to just penetrating it, as well as destroying the M1 Abrams, which is nearly freakin' impenetrable. I was wondering if anyone knew what explosive the hellfire uses, because I have not been able to find any information about it on google. I would have assumed HMX, but due to these recent findings I am not sure, and what about tank artillery shells?

[Maniak]

Mendeleev: I read that there is some PBXN-5 in hellfire missiles - it is pressed explosive with 95%HMX and 5%viton A polymer.
I think TNT is used because it is much cheaper and it´s not so brisant. For bunker bustering it isn´t so important to have huge brisance, but much energy (from Al).

[Mendeleev]

How is it possible that RDX is more expensive than TNT? TNT is made from toluene, something that has to be extracted from crude oil, while hexamine is made from the extremely cheap formaldehyde and ammonia, which are both made from the most widely available atmospheric gases, ammonia from nitrogen and hydrogen, formaldehyde from hydrogen and carbon monoxide. Hydrogen is produced from electrolyzing water, the most abundant natural resource on the plant, and nitrogen is the most abundant gas in the atmosphere, while carbon monoxide is also very common. TNT requires an assload more nitric and sulfuric acids, divided into three nitrations. So generally TNT is based on oil drilling as well as requiring a lot more acids, how can it be cheaper?

[Microtek]

You basically said it yourself. Toluene is availible from crude oil, so it doesn't need to be synthesized. In RDX manufacture, you have to manufacture the precursors in several steps, each of which require a different process ( which means they often take place on different factories ). Each of the manufacturers need to make a living and also recover the money it cost to build the factory, so some 10-100 % of the purchasing/manufacturing costs will be added at each step. On top of this the nitric acid is not easy to recover in RDX production, whereas the waste acids can be used directly in the lower nitrations in the TNT procedure. In this way almost all the HNO3 is used.

[Jetex Kid]

Adding aluminum in any quantity to any CHNO explosive lowers its detonation velocity and brisance.

RDX is 43% oxygen and TNT is 42%. 20% aluminum consumes roughly an equal amount of oxygen. The remaining oxygen can then be consumed almost completely by efficiently combining with hydrogen, even though TNT has scant hydrogen.

Thus, there is little energy difference in combustion chemistry in these two 80/20 mixtures. The biggest difference occurs because RDX has a positive heat of formation (+100 cal/g) while TNT’s Hf is –50 cal/g. This is a 150 cal/g difference in the neighborhood of 2,000 cal/g (under 10%). If one wants 10% more energy, it would be most cheaply done by increasing the charge weight by 10%.

Plus, TNT is its own binder and RDX isn’t.

Regarding the T-72 and the Hellfire, the key is not “what,” but “how much.” The Hellfire has a large warhead. The old Composition B explosives are about as effective as PBXs, but lack the shelf life.

[Mendeleev]

Jetex Kid: So you're saying that aluminum doesn't increase the power?

Microtek: I always though extracting toluene from crude oil was more expensive. Was I wrong? My thinking was that the three starting materials for hexamine are basically water, N2, and CO. The first available in any country with a coast, the second in any country with air, and the third in any country with air pollution, thus any country. Crude oil on the other hand is a limited resource, requiring 500 million years to form in the quantities we use it today, and it is being consumed at a rate of 3 billion gallons a day, and furthermore requires deap sea drilling and much war with the middle east. Anyone hear the letterman joke (or at least I think it was Letterman)? "President Bush announced yesterday that reconstruction in Iraq would be divided into three zones: leaded, unleaded, and premium."

[Jetex Kid]

Jetex Kid: So you're saying that aluminum doesn't increase the power?

Exactly. It increases the energy and decreases the peak power. The pressure-time curve has more area with aluminum, but the peak is lower. The practical consequence is that unaluminized explosives generate higher energy fragments than the corresponding aluminized explosive. By the time the pressure of the aluminized explosive is greater than the unaluminized, the fragments have separated from each other so that gases leak through them rather than propelling them.

My main point was that as an oxidizer of aluminum, TNT is about 90% as good as RDX, because their O2 content is so similar.

[Microtek]

Mendeleev: I just had a look around, and I found a web site with some bulk prices for chemicals. I couldn't find hexamine, but I did find both formaldehyde and ammonia as well as toluene.

Now, one ton of hexamine requires 0.485 ton ammonia ( 100 % ) and 1.285 ton formaldehyde ( 100 % ). At a price of 170 £/ton for ammonia and 300 £/ton for formaldehyde, that works out to 468 £/ton for hexamine ( assumine 100 % yield ). In comparison, toluene costs 170 £/ton.
On top of this, one ton of hexamine gives 1.585 ton RDX if 100 % yield could be achieved, while one ton of toluene gives 2.465 tons of TNT ( also at 100 % yield ).
Considering that TNT manufacture is also much more efficient than RDX manufacture, TNT really is a lot cheaper than RDX.

[nbk2000]

Depending on the configuration, the Hellfire can have between 30 and 100 pounds of HE. That's a lot of explosive to blow a tank apart, which explains why they usually get blown apart in the process. :)

[Dave Angel]

With regards to the E process, I have read that it is best to use low molecular weight paraformaldehydes, owing to their better solubility in the liquid reactants.

I realise there is often some confusion between paraformaldehyde (the chain polymer, average n = 8) and trioxane (the cyclic trimer of formaldehyde). There is also a third form, polyoxymethylene, with chain lengths greater than 100. The confusion often lies in all three types being called paraformaldehyde.

Does anyone know if trioxane would make a good substitute for the low molecular weight paraformaldehyde in this synthesis, or is there something about it's cyclic structure which makes it too stable or otherwise unsuitable?

Like cutefix (in another thread), I have noted that suppliers tend not to list the chain length or melting point of their paraformaldehyde. Being able to use trioxane would remove this problem, though I have a feeling trioxane may be more expensive, typically.

[al93535]

Ok HDN really does increase the yield of RDX. I nitrated 6 grams hexamine and got back about 3.1 grams RDX, using 50 ml hno3. When I used 15 grams of HDN in 50 ml hno3 I got 11 grams!! I would recomend making hexamine into HDN first! I'll be using only HDN from now on.

[al93535]

Hmmm, I was unable to edit my last post. I see some people say to use 25 grams HDN in 50 ml HNO3, others say 10, and yet others use different amounts. Does anyone know the most HDN you can use? Or even the best amounts, ratio? I have searched around and I just see all these different ratios. any Ideas? Microtek said 25 grams to 50 ml would be good, I think I will try that now.
Edit: How many of you recrystalize your RDX? Is it really worth it?

[apathyboy]

Mendeleev: also, remember that refineries arent just extracting the toluene from crude oil and then throwing the rest away. Almost all oil products are essentially byproducts of gasoline and kerosene manufacture that people have found a use for. Im pretty sure that manufacturers worry more about a glut of those types of chemicals on the market rather than a shortage

[SantasL.Helper]

WTF is going on!?! I had like a nice amount of RDX in my filter. Then i decided to purify it by dissolving it in about 120 ml acetone, and adding that to 700 ml's of water.

Now after filtering, it looks like i lost HALF or at least a quarter of my RDX yield!! :confused: :( :mad: What the hell happened!?!??!?

[kingspaz]

You could have had 1/4 impurities. Good job you purified it!

[aikon]

...Then i decided to purify it by dissolving it in about 120 ml acetone, and adding that to 700 ml's of water.
Now after filtering, it looks like i lost HALF or at least a quarter of my RDX yield!! :confused: :( :mad: What the hell happened!?!??!?

I don't know about your exact ratios you used but for recrystallizing I use 10 g of acetone for 1 g of RDX. After heating the acetone/RDX in the waterbath it's cooled down and the first purified crystals appear. There is still RDX dissolved in the acetone left behind so it's boiled down to half it's previous volume and packed in ice again and another crop of crystals form.
You should repeat the process several times to get out all of the dissolved RDX.

[akinrog]

This surprised me because bunker busters need to have as much power as possible, and TNT isn't exactly the best way to go with RDX and HMX on the table. I had always figured RDX and HMX were the explosives of choice for bunker busters and shaped charges so I was little thrown off. Does anyone know why they use tritonal as opposed to RDX or HMX :confused:?

A few years ago, I had translated a document for a defense contractor. The reason for why military munitions use TNT is TNT is castable. While RDX and HMX are very powerful they are not suitable for loading into munitions. (Assume that you fill the shell with RDX/HMX mechanically. You have to compact/press the charge in order to preclude air voids, etc. which implies a more complicated process unlike casting.) In the translated text, the guys at the munition factory was melting a slurry of explosives (I don't remember the composition) and casting them into shells. After casting they were insterting probes (containing temperature sensors) into the molten charge to place them in furnaces to allow slow cooling of the cast explosive to prevent formation of cracks. The temperature sensor probes are connected to a system controlling the furnace temperature. HTH.

[SantasL.Helper]

I don't know about your exact ratios you used but for recrystallizing I use 10 g of acetone for 1 g of RDX. After heating the acetone/RDX in the waterbath it's cooled down and the first purified crystals appear. There is still RDX dissolved in the acetone left behind so it's boiled down to half it's previous volume and packed in ice again and another crop of crystals form.
You should repeat the process several times to get out all of the dissolved RDX.


ah ok, i added it to water, so pretty possible a lot of RDX was still dissolved in the acetone. Will do that next time, thanks!

[The_Rsert]

50g Hexamine to 550 gramm or ml nitric acid?
Because:

http://www.google.de/search?q=cache:fqbeAamBaZ0J:www.flashdance.cx/txt/Explosivt/BOMB__TXT+make+RDX+HNO3&hl=de

"...To make R.D.X. place 550 grams of the nitric
acid produced by the above procedure in a 1000 ml. beaker in a salted bath.
50 grams of hexamine, (methenamine)..."

[Boomer]

Just had a look at that page, and a good laugh. Read yourself:

... red gas called nitrogen trioxide ... TRI-oxide? At least he didn't say it's blue ...
Unlike potassium chlorate, sodium chlorate won't explode spontaneously when mixed with phosphorus ... you sure it won't ?
Mix Potassium chlorate 75%, Sulfur 12.5% ... useful in making a pipe bomb ... yeah, chlorate + sulphur is fine, especially in a pipe ... :p
Astrolite is (...) the world's most powerful non-nuclear explosive ... you can't kill that lie ...

And finally the 'generic bomb', the apex of stupidity: Aquire a glass container. Put in a few drops of gasoline. Add a few drops of potassium permanganate. To detonate just throw against a hard object. (...) the same as a half stick of dynamite! :rolleyes:

LOOK HERE FOR INFO if you want to survive!

And BTW converting the hexa to HDN first saves you a LOT of nitric. Instead of 550g/360ml you need 100ml of 99% nitric, plus 50ml of 70% for the HDN. This is one third of the amount needed for the hexamine process, plus the mothod is safer!

[The_Rsert]

Uuups!
Astrolite? Most poweful non-nuclear explosiv? -Hahahha, muhahahaa!
The site is almost pure shit!
I'm sorry!

[Myrol]

Hello guys! To do a special performance test I want to make some RDX (around 25g) and mix it with 25% Aluminium to compare THIS explosion with other aluminized explosives like Ammonal, APANAl or ANNMAl. Yesterday I fired one 31g APANAl shaped Charge and one 30g APANAl shaped charge with a 20g APAl LSC beside him. Ok, perhaps I made my cones to bad but the effect of a High-velocity Jetimpact wasn't very visible. I think the standoff was to short...or something like that it doesn't matter now. The Explosion from the 31g APANAl Filmcanister was awesome! First I thought this stuff works like ordinary APAN, no no no.....I was f***ing surprised. We felt a hard Blastwave, an eardeafening Bang and I saw even in good Sunlight a luminious orange-yellow flash! I can say without problems it has the same power like ANNM, really! Next weekend its time to make sure it wasn't a over-exaguration from me but I dont think so! Without Aluminium...my APAN has never such a power and I'm absolutely sure that ANNM is stronger as APAN...but with APANAl....I dont know... ;) we'll see. To RDX: What for Yields are typical if I Nitrate 50g dry HDN with 100ml 99% Nitric Acid? You guy's change the ratios very often how I see. Someone used 90ml HNO3 and 250g HDN?? Is this true? In Germany RDX is called "Hexogen" so my target is "Hexal" 75/25. If I fire it on a massive Brickstone and do it also with the same amount APANAl or APANNMAl under the same circumstates, it should be ok to test the performance this way, right? Perhaps PLX is also a nice Idea!

[piro_raj]

In normal nitration you can use 70% HNO3 instead of concentrated nitric acid, but you need to add more 98% H2SO4, which absorbs water (the product is not so good, but it works).
I think that in the production of RDX you could also use 70% HNO3 and a chemical that absorbs water. H2SO4 is not good, as we all know, because decomposes the product and acetic anhydride is very hard to obtain, so I thought about AlCl3 or CaCl2. Both are powerful water absorbers and are not reactive to mess the reaction and also easy to obtain or make. Would it work? This parasitic reaction is possible: 3HNO3 + AlCl3 --> 3HCl + Al(NO3)3 if HNO3 is stronger acid than HCl. There are also other chemicals that absorb water and could be as good or even better for this purpose. AlCl3 and CaCl2 could be also good for other nitrations as a total or partial replacement of H2SO4.
Another way is to use 98% H2SO4 and ammonium nitrate in large excess.
Reaction: H2SO4 + 2NH4NO3 --> 2HNO3 + (NH4)2SO4
In the mixture there would be no H2SO4 and almost no water after the reaction(only HNO3, (NH4)2SO4 and NH4NO3). This mixture could be used for hexamine nitration in order to make RDX. The presence of ammonium nitrate in the mixture is appreciated, because it helps the nitration (the K process). Has anyone tried this?
More than 90% HNO3 is expensive for me ($63 for 500ml). For $63 I can buy 10 l of 69% HNO3 or 10 l of 98% H2SO4. If one of the two above procedures have ten times smaller yield than the original procedure I can make the same amount of RDX at the same price.

[tom haggen]

Why exactly is RDX only castable with TNT? Is it because RDX has a very high melting point?

[Microtek]

RDX decomposes quite rapidly when it reaches the melting point ( around 200 C ).

[Myrol]

RDX is fascinating me for a long time, but the Yields with so much anhydrous HNO3 are quite dissapointing me!

The only process with good yields is perhaps the Bachmann-process but with just 500ml Acetic Anhydride in stock I think I can't make so much RDX until I get more of it! So I "wasted" some time to think a little deeper about the K-method wich produces two moles of RDX per each mole Hexamine two moles AN and 4 moles HNO3.

I think a big problem is the rapid dissolution of the HNO3 by the formation of three moles Water per every mole RDX, so why not using a dessicant in the process wich doesn't attack RDX. Sulfates are forbidden, I think even the Sulfat-Ion in an acidic medium will destroy most of the RDX to give poor yields.

Chlorides such as MgCl2 or CaCl2 could be destroyed also by the HNO3 to form HCl.....also bad! So my last thought: Calcium Nitrate wich bonds 4 moles Crystalwater per each mole CN. If the equatation for the process is right, I've used the stochiometric ratio of CN to absorb all the water wich is formed in the process.

The Educt's are as follows: Hexamine-Dinitrate no excess, Nitric Acid 200% Excess, Calcium Nitrate stochiometric, Ammonium Nitrate 100% excess.

so summed together my method works this way:

Dissolve 12g anhydrous Ammonium Nitrate and 4,5g Calcium Nitrate in 9ml white Nitric Acid wich will form a very thick mud.

Then add slowly 10g Hexamine-Dinitrate and maintain the Temperature at 15°C until all of the HDN is in the Flask.

Add another load of 4,5g Calcium Nitrate to the mix and heat everything for 30min. to 80°C (352Kelvin).

Let it cool down and add 50ml cold Water, 99% of the RDX will precipipate out.

Ummm, can this be a real method? Remember that 3/4 of the reactands are solid. Could be improved via using 5,3g Hexamine and 18ml HNO3 but that wouldn't be then more the nice deal of reducing the necessary amount white Nitric Acid wich we're all looking for, right? I try this after I#ve made some fresh HDN and some new anhydrous Nitric Acid. I can't wait to get my own RDX. I don't know why but I like RDX MUCH more than PETN, even if they are both nearly as same as powerful and PETN has much better yields....who know's :confused:

[Myrol]

RDX is fascinating me for a long time, but the Yields with so much anhydrous HNO3 are quite dissapointing me!

The only process with good yields is perhaps the Bachmann-process but with just 500ml Acetic Anhydride in stock I think I can't make so much RDX until I get more of it! So I "wasted" some time to think a little deeper about the K-method wich produces two moles of RDX per each mole Hexamine two moles AN and 4 moles HNO3.

I think a big problem is the rapid dissolution of the HNO3 by the formation of three moles Water per every mole RDX, so why not using a dessicant in the process wich doesn't attack RDX. Sulfates are forbidden, I think even the Sulfat-Ion in an acidic medium will destroy most of the RDX to give poor yields.

Chlorides such as MgCl2 or CaCl2 could be destroyed also by the HNO3 to form HCl.....also bad! So my last thought: Calcium Nitrate wich bonds 4 moles Crystalwater per each mole CN. If the equatation for the process is right, I've used the stochiometric ratio of CN to absorb all the water wich is formed in the process.

The Educt's are as follows: Hexamine-Dinitrate no excess, Nitric Acid 200% Excess, Calcium Nitrate stochiometric, Ammonium Nitrate 100% excess.

so summed together my method works this way:

Dissolve 12g anhydrous Ammonium Nitrate and 4,5g Calcium Nitrate in 9ml white Nitric Acid wich will form a very thick mud.

Then add slowly 10g Hexamine-Dinitrate and maintain the Temperature at 15°C until all of the HDN is in the Flask.

Add another load of 4,5g Calcium Nitrate to the mix and heat everything for 30min. to 80°C (352Kelvin).

Let it cool down and add 50ml cold Water, 99% of the RDX will precipipate out.

Ummm, can this be a real method? Remember that 3/4 of the reactands are solid. Could be improved via using 5,3g Hexamine and 18ml HNO3 but that wouldn't be then more the nice deal of reducing the necessary amount white Nitric Acid wich we're all looking for, right? I try this after I#ve made some fresh HDN and some new anhydrous Nitric Acid. I can't wait to get my own RDX. I don't know why but I like RDX MUCH more than PETN, even if they are both nearly as same as powerful and PETN has much better yields....who know's :confused:

[Myrol]

RDX is fascinating me for a long time, but the Yields with so much anhydrous HNO3 are quite dissapointing me!

The only process with good yields is perhaps the Bachmann-process but with just 500ml Acetic Anhydride in stock I think I can't make so much RDX until I get more of it! So I "wasted" some time to think a little deeper about the K-method wich produces two moles of RDX per each mole Hexamine two moles AN and 4 moles HNO3.

I think a big problem is the rapid dissolution of the HNO3 by the formation of three moles Water per every mole RDX, so why not using a dessicant in the process wich doesn't attack RDX. Sulfates are forbidden, I think even the Sulfat-Ion in an acidic medium will destroy most of the RDX to give poor yields.

Chlorides such as MgCl2 or CaCl2 could be destroyed also by the HNO3 to form HCl.....also bad! So my last thought: Calcium Nitrate wich bonds 4 moles Crystalwater per each mole CN. If the equatation for the process is right, I've used the stochiometric ratio of CN to absorb all the water wich is formed in the process.

The Educt's are as follows: Hexamine-Dinitrate no excess, Nitric Acid 200% Excess, Calcium Nitrate stochiometric, Ammonium Nitrate 100% excess.

so summed together my method works this way:

Dissolve 12g anhydrous Ammonium Nitrate and 4,5g Calcium Nitrate in 9ml white Nitric Acid wich will form a very thick mud.

Then add slowly 10g Hexamine-Dinitrate and maintain the Temperature at 15°C until all of the HDN is in the Flask.

Add another load of 4,5g Calcium Nitrate to the mix and heat everything for 30min. to 80°C (352Kelvin).

Let it cool down and add 50ml cold Water, 99% of the RDX will precipipate out.

Ummm, can this be a real method? Remember that 3/4 of the reactands are solid. Could be improved via using 5,3g Hexamine and 18ml HNO3 but that wouldn't be then more the nice deal of reducing the necessary amount white Nitric Acid wich we're all looking for, right? I try this after I#ve made some fresh HDN and some new anhydrous Nitric Acid. I can't wait to get my own RDX. I don't know why but I like RDX MUCH more than PETN, even if they are both nearly as same as powerful and PETN has much better yields....who know's :confused:

[simply RED]

I do not think this will work because of the Ca+ ions being negative catalyst of the reaction.

Have you tried it?

[simply RED]

I do not think this will work because of the Ca+ ions being negative catalyst of the reaction.

Have you tried it?

[simply RED]

I do not think this will work because of the Ca+ ions being negative catalyst of the reaction.

Have you tried it?

[Boomer]

What about a water trap, without contact to the actual batch? Working over sulfuric or CaCl2, at lower temp for a longer time? I think about this for some time, might as well try it...

If you go up to 80C, even a dean-stark might work (perhaps under slightly reduced pressure?).

[Boomer]

What about a water trap, without contact to the actual batch? Working over sulfuric or CaCl2, at lower temp for a longer time? I think about this for some time, might as well try it...

If you go up to 80C, even a dean-stark might work (perhaps under slightly reduced pressure?).

[Boomer]

What about a water trap, without contact to the actual batch? Working over sulfuric or CaCl2, at lower temp for a longer time? I think about this for some time, might as well try it...

If you go up to 80C, even a dean-stark might work (perhaps under slightly reduced pressure?).

[Jetex Kid]

Re: Myrol and K-Process Improved

A German factory was producing RDX at the end of WWII using magnesium nitrate trihydrate as a desiccant. I can't cite the source but think it was Urbanski. The Mg nitrate hexahydrate is precipitated by cooling the mixture. At 120C to 140C the hexahydrate reverts to trihydrate.

About a year ago a forum member described an accident in which he tried to distill strong nitric acid that contained the remains of RDX manufacture. The remains started to oxidize and the forum member became concerned about losing his life.

Using Mg nitrate as a desiccant, perhaps the remains would contribute meaningfully to the next batch of RDX.

Also, US Patent 5,012,019 is about using Mg nitrate as a desiccant in TNT manufacture.

[Jetex Kid]

Re: Myrol and K-Process Improved

A German factory was producing RDX at the end of WWII using magnesium nitrate trihydrate as a desiccant. I can't cite the source but think it was Urbanski. The Mg nitrate hexahydrate is precipitated by cooling the mixture. At 120C to 140C the hexahydrate reverts to trihydrate.

About a year ago a forum member described an accident in which he tried to distill strong nitric acid that contained the remains of RDX manufacture. The remains started to oxidize and the forum member became concerned about losing his life.

Using Mg nitrate as a desiccant, perhaps the remains would contribute meaningfully to the next batch of RDX.

Also, US Patent 5,012,019 is about using Mg nitrate as a desiccant in TNT manufacture.

[Jetex Kid]

Re: Myrol and K-Process Improved

A German factory was producing RDX at the end of WWII using magnesium nitrate trihydrate as a desiccant. I can't cite the source but think it was Urbanski. The Mg nitrate hexahydrate is precipitated by cooling the mixture. At 120C to 140C the hexahydrate reverts to trihydrate.

About a year ago a forum member described an accident in which he tried to distill strong nitric acid that contained the remains of RDX manufacture. The remains started to oxidize and the forum member became concerned about losing his life.

Using Mg nitrate as a desiccant, perhaps the remains would contribute meaningfully to the next batch of RDX.

Also, US Patent 5,012,019 is about using Mg nitrate as a desiccant in TNT manufacture.

[Boomer]

Does anybody know whether a very long reaction time will destroy the RDX already formed, or whether in the contrary the "remains" will keep forming RDX with each molecule of water being removed by dessication?

I know this works for nitrate esters, you can keep a batch of NG or MHN in the freezer for a week without lowering the yield, add more sulfuric later and increase yield even more.

The reason I ask is: With an RDX batch running over sulfuric or CaCl2, it will take long for the water to get trapped in the dessicant (without contact), slowly concentrating the remaining HNO3. If this 'waiting time' lowers yield by destroying RDX which has already formed (instead of forming more RDX by making the nitric stronger), there is no use in me trying!

Can one of the chemists here give a hint?

[Boomer]

Does anybody know whether a very long reaction time will destroy the RDX already formed, or whether in the contrary the "remains" will keep forming RDX with each molecule of water being removed by dessication?

I know this works for nitrate esters, you can keep a batch of NG or MHN in the freezer for a week without lowering the yield, add more sulfuric later and increase yield even more.

The reason I ask is: With an RDX batch running over sulfuric or CaCl2, it will take long for the water to get trapped in the dessicant (without contact), slowly concentrating the remaining HNO3. If this 'waiting time' lowers yield by destroying RDX which has already formed (instead of forming more RDX by making the nitric stronger), there is no use in me trying!

Can one of the chemists here give a hint?

[Boomer]

Does anybody know whether a very long reaction time will destroy the RDX already formed, or whether in the contrary the "remains" will keep forming RDX with each molecule of water being removed by dessication?

I know this works for nitrate esters, you can keep a batch of NG or MHN in the freezer for a week without lowering the yield, add more sulfuric later and increase yield even more.

The reason I ask is: With an RDX batch running over sulfuric or CaCl2, it will take long for the water to get trapped in the dessicant (without contact), slowly concentrating the remaining HNO3. If this 'waiting time' lowers yield by destroying RDX which has already formed (instead of forming more RDX by making the nitric stronger), there is no use in me trying!

Can one of the chemists here give a hint?

[VasiaPupkin]

Nitric acid is slowly decompose RDX in prolonged standing (practically more than 1-2hours).

[VasiaPupkin]

Nitric acid is slowly decompose RDX in prolonged standing (practically more than 1-2hours).

[VasiaPupkin]

Nitric acid is slowly decompose RDX in prolonged standing (practically more than 1-2hours).

[Boomer]

Thank you! This means I can forget about that route, it was soooo promising .... :(

[Boomer]

Thank you! This means I can forget about that route, it was soooo promising .... :(

[Boomer]

Thank you! This means I can forget about that route, it was soooo promising .... :(

[aikon]

There are a lot of threads about RDX and the different ways one can
produce it so I don't want to strat a new one. What I'm missing in the discussion is the procedure Uncle Fester gives in his book "Home Workshop Explosive". When it comes to temperature control his directions are different to that in all the other literature and patents. While the Herz patent (UK 145,791) states that you have to keep the temperature between 20°C and 30°C during the addition of hexamine to the nitric acid (1.52 spec.grav.)
Uncle Fester is of the opinion to keep the temperature around -20°C.
(Quote: "The cold temperature slows down the unwanted reaction quite a bit more than the desired reaction producing RDX"). According to the patent one should wait a few minutes after the last addition of hexamine and the mixture should be heated to 55°C for a period of about 5 minutes after wich the mass is again cooled down to the original temperature. After 15 minutes, the mixture is poured in a bucket of ice cold water.
Uncle Fester: "The temperature of the mixture should under no circumstances be allowed to go above 20°C; and it would be best if it were held well below that temperature." "When the last of them has dissolved (the hexamin crystals), wait 5 minutes and then pour the whole batch into a gallon of cold water. The length of time between the end of adding the hexamin, and the point when it all has dissolved is around 15 minutes."
Uncle Fester says nothing about heating to 55°C for 5 minutes. I'm wondering why his method is so different from all other publications. Does anyone know the answer?
He talks about 95g per batch (770ml nitric acid (90% strength), 100g hexamine).
Has anyone tried UF procedure? Is it an acceptable one or is it pure BS?
Any comments aprecciated.

[aikon]

There are a lot of threads about RDX and the different ways one can
produce it so I don't want to strat a new one. What I'm missing in the discussion is the procedure Uncle Fester gives in his book "Home Workshop Explosive". When it comes to temperature control his directions are different to that in all the other literature and patents. While the Herz patent (UK 145,791) states that you have to keep the temperature between 20°C and 30°C during the addition of hexamine to the nitric acid (1.52 spec.grav.)
Uncle Fester is of the opinion to keep the temperature around -20°C.
(Quote: "The cold temperature slows down the unwanted reaction quite a bit more than the desired reaction producing RDX"). According to the patent one should wait a few minutes after the last addition of hexamine and the mixture should be heated to 55°C for a period of about 5 minutes after wich the mass is again cooled down to the original temperature. After 15 minutes, the mixture is poured in a bucket of ice cold water.
Uncle Fester: "The temperature of the mixture should under no circumstances be allowed to go above 20°C; and it would be best if it were held well below that temperature." "When the last of them has dissolved (the hexamin crystals), wait 5 minutes and then pour the whole batch into a gallon of cold water. The length of time between the end of adding the hexamin, and the point when it all has dissolved is around 15 minutes."
Uncle Fester says nothing about heating to 55°C for 5 minutes. I'm wondering why his method is so different from all other publications. Does anyone know the answer?
He talks about 95g per batch (770ml nitric acid (90% strength), 100g hexamine).
Has anyone tried UF procedure? Is it an acceptable one or is it pure BS?
Any comments aprecciated.

[ALENGOSVIG1]

Festers books are sometimes good for a quick read, but they should really be taken with a grain of salt. If his words aren't backed up by other books/patents/info on roguesci and you don't completely understand the dynamics of the reaction, then think twice about proceeding. Or at least proceed with caution...:)

[al93535]

I have tried quite a few different ways to get RDX. I have never received any RDX from any experiment that was not heated. Maybe it was something else I did, but the only way I had any yield, was after heating the beaker to 55 degrees. Has anyone else made RDX without the heating?

[pdb]

See COPAE, which mention a process with 100% HNO3 at 30°C. But, unsurprisingly, the yield is very low.

[aikon]

...I have never received any RDX from any experiment that was not heated...

That's the reason why I wonder about Fester's process. Normally his books are quite well researched especially his drug books. I'd like to know if he has ever made RDX using the "cold process". The book has it's weak points -especially the detonating section- but the nitroglycerin chapter is always a good read and quite accurate. I'll write him an e-mail and ask why he recommends a temperature around -20°C. If I get an answer I'll let you know.

[quicksilver]

That's the reason why I wonder about Fester's process. Normally his books are quite well researched especially his drug books. I'd like to know if he has ever made RDX using the "cold process". The book has it's weak points -especially the detonating section- but the nitroglycerin chapter is always a good read and quite accurate. I'll write him an e-mail and ask why he recommends a temperature around -20°C. If I get an answer I'll let you know.

I thought the same thing re: his works (especially the det issues). It may actually be a mis-print. -20c has not been mentioned in the patents I have read but 20c has! I have never had any trouble when working within limits of below 20c. Therefore I though he may have meant "somewhere below 20 degrees" instead of the absolute of being -20.
The best material I have come accross has been the Los Alamos energetic work at http://www.fas.org/sgp/othergov/doe/lanl/index.html
(sorry about the link; please cut & paste)

[nitrogeno]

the problem of bachmann method is the stability. for more stability (Urbansky Vol I), is necessary add 1% of Borum Fluoride (BF3).

[quicksilver]

That's the reason why I wonder about Fester's process. Normally his books are quite well researched especially his drug books. I'd like to know if he has ever made RDX using the "cold process". The book has it's weak points -especially the detonating section- but the nitroglycerin chapter is always a good read and quite accurate. I'll write him an e-mail and ask why he recommends a temperature around -20°C. If I get an answer I'll let you know.
I could only assume that "-20" was a misprint. He was talking about utilizing a simple ice bath and -20 would be a stretch for that to be reached and continued for any time frame. The book as a whole seemed unique as he seemed to stay w/ nitric esters until RDX. It seems if he were to stray from nitric esters that picric acid would have been a easier choice for a "home workshop" enterprise.
Is his Email in the book? Does he have a web-page?

[tom haggen]

I've browsed through this thread and have yet to see a balanced equation anywhere. I’m just wondering how the hell you guys come up with your numbers when determining the masses of your beginning reagents.

I have a thread in the water cooler with a balanced equation but it seems that even this equation does not even call for enough HNO3. I guess my question is how much excess HNO3 you should use with respect to the balanced equation.

[Chris The Great]

Checked Urbanski for the equation, it says there are two main ones taking place:
(CH2)6N4 + 4HNO3 -> (CH2-N-NO2)3 + 3CH2O + NH4NO3
(CH2)6N4 + 6HNO3 -> (CH2-N-NO2)3 + 6H2O + 3CO2 + 2N2
And a side reaction:
2CH2O + 2HNO3 -> 2HCOOH + H2O + NO + NO2
which I doubt goes very quickly.
It also lists the hydrolysis of hexamine but I don't think that would happen much with the large amount of HNO3 and very low amount of water even near the end of the reaction.

It says that a 4 to 8 fold molar excess of nitric acid is needed over the theoretical. I would think 100% nitric acid would need only the 4 fold excess while less concentrated acid would need larger excesses for the reaction to proceed.

[tom haggen]

In one of your equations your saying that 6 mols of water are being formed?
I find that hard to believe due to the fact that water keeps the reaction from proceeding any further.

[Viper III]

if I am not failed is RDX the same like Hexogen

because i have a recept for this where you need no HNO3

the only problem is that you need "vinegaracidformaldehyd" witsh is very difficult to get it.

furthermore you need paraform and AN...

sorry for my bad english, I am from austria

[Viper III]

is RDX the same like Hexogen ?

[Boomer]

Ever thought why so much excess acid is needed?

BTW over at MSDB we have a discussion going (mostly Rosco, Microtek + me) about improving the HDN method, and several additives (AN, urea nitrate ...). In my last tests I got *reproducable* yields of 80%+ with 2.5-3 ml WFNA per gram of HDN, while with 2ml yield varied between 30 and 60%. Go have a look...