Sciencemadness Discussion Board - RDX synthesis. Safe ir not?

Uh Oh, Ledgard again!

What happens with this author?

Smoker Root - 29-7-2019 at 11:20

There are plenty of topics about RDX synthesis, just use the search engine and you will find whatever you need.

Of course there is, but I am looking for an especific answer, I think this can be a Nice synthesis(as most of the ones of the book are) but I just want to be sure

underground - 29-7-2019 at 11:32

Just try out a small batch to see your yields and if they would be satisfactory, go for full scale.

twelti - 29-7-2019 at 12:00

Uh Oh, Ledgard again!

What happens with this author?

Do a search in this forum, on Ledgard. He is apparently an unreliable source.

Smoker Root - 29-7-2019 at 13:27

Uh Oh, Ledgard again!

What happens with this author?

Do a search in this forum, on Ledgard. He is apparently an unreliable source.

I have researched a bit on this guy, and it defenetly haS a bad reputation. But the synthesis seems fairly easy, that is what majes my head go boom. If not there is what it looks like to be a reliable synthesis from a video in bitchute, Aldo I am not sure. I still linda prefer Ledgar stuff. Looks more profesional and it looks kinda right, but please, please give me a confirmaron that this could not actually develop a quick runaway reaction

[Edited on 29-7-2019 by Smoker Root]

Smoker Root - 29-7-2019 at 13:53

Just try out a small batch to see your yields and if they would be satisfactory, go for full scale.

I am too fearful of god and I don't want to risk it

James Ikanov - 29-7-2019 at 14:29

I am hardly a chemical expert but I have seen a variety of similar procedures for RDX. The general opinion that I have read of them is that they produce poor yields and that they generally do not adequately nitrate the hexamine, leading to the creation of HDN or similar. Most people usually end up making HDN and then renitrating it from what I know. There is a very similar process for TNT that is equally a headache.

I believe there is a less involved process involving acetic anhydride that produces much better yields, but that the problem is that acetic anhydride is very difficult to produce or acquire. If you absolutely must have RDX then there is a (to me) very complex and seemingly dangerous synthesis for acetic anhydride elswhere on the board.

I do not know much about RDX; I was interested in it early on but now my interest lies mostly in finding a potent explosive that requires less headache and dangerous acids and such. If you really want a "high horse power" explosive, perhaps look up the TEX synthesis on this board and try that? it is relatively simple and roughly comparable in power to RDX anyway, if not better.

XeonTheMGPony - 29-7-2019 at 16:22

Uh Oh, Ledgard again!

What happens with this author?

Miserable failure and lots of wasted time and chemicals, if lucky.

underground - 29-7-2019 at 16:24

TEX ? From where do you plan to get glyoxal and formamide ? Nitroesters are much easier and not a headache to synth.

XeonTheMGPony - 29-7-2019 at 16:29

Quote: Originally posted by James Ikanov

I am hardly a chemical expert but I have seen a variety of similar procedures for RDX. The general opinion that I have read of them is that they produce poor yields and that they generally do not adequately nitrate the hexamine, leading to the creation of HDN or similar. Most people usually end up making HDN and then renitrating it from what I know. There is a very similar process for TNT that is equally a headache.

I believe there is a less involved process involving acetic anhydride that produces much better yields, but that the problem is that acetic anhydride is very difficult to produce or acquire. If you absolutely must have RDX then there is a (to me) very complex and seemingly dangerous synthesis for acetic anhydride elswhere on the board.

I do not know much about RDX; I was interested in it early on but now my interest lies mostly in finding a potent explosive that requires less headache and dangerous acids and such. If you really want a "high horse power" explosive, perhaps look up the TEX synthesis on this board and try that? it is relatively simple and roughly comparable in power to RDX anyway, if not better.

I made RDX, it is a bit of a pain but not that much, I went with the HDN route.

Wasn't all that impressed with it, going to make more by previous method, and run more tests.

Insensitivity really is not a big deal for the style of systems I am making, but if I can get better results with compounded materials then why not.

James Ikanov - 29-7-2019 at 21:53

TEX ? From where do you plan to get glyoxal and formamide ? Nitroesters are much easier and not a headache to synth.

They are fairly easy to acquire, last time I shopped around. There's a synthesis published on this very website using the relatively commonly available 40% glyoxal.

Smoker Root - 29-7-2019 at 23:15

Quote: Originally posted by XeonTheMGPony

Quote: Originally posted by James Ikanov

Can you send me the paper you are following?

Microtek - 30-7-2019 at 00:25

I would say that for a beginner, RDX is one of the safest, most simple synthesis to do. I would not go with such a large excess of nitric acid to begin with, and as you say use HDN as the substrate instead of hexamine. There are many variations on the synthesis, and I suggest you look for some of the topics here on SM where they have been discussed.
Regarding the safety of the procedure, it is safe in the sense that it will not explode. If you do something exceptionally stupid, you can oxidize your hexamine instead of nitrating it, and this will liberate a lot of NOx. The part of the referenced procedure where the reaction mixture is added to 70% HNO3 is there to oxidize unwanted linear nitramines. This is usually accomplished by raising the temperature for a while at the end of the reaction.
Ledgard has a bad reputation around here because some of his procedures are demonstrably false, while most of them are untested (by him) and copy-pasted directly from the patent literature. Patents are useful, but you need to be able to read between the lines to avoid potential pitfalls.

caterpillar - 30-7-2019 at 10:56

Use HDN instead of hexamine. Hexamine is the base and its neutralization by HNO3 is an exothermic process. And you save some HNO3- part of it already presents in HDN. The second stage is exothermic and emits NOx. Do it at fresh air and use some heat resistant glass. You may read about dear Jared here: search for "the worst book ever written". When the process has been complete you may use diluted HNO3 to prepare more HDN.

Smoker Root - 31-7-2019 at 04:22

Quote: Originally posted by Microtek

I would say that for a beginner, RDX is one of the safest, most simple synthesis to do. I would not go with such a large excess of nitric acid to begin with, and as you say use HDN as the substrate instead of hexamine. There are many variations on the synthesis, and I suggest you look for some of the topics here on SM where they have been discussed.
Regarding the safety of the procedure, it is safe in the sense that it will not explode. If you do something exceptionally stupid, you can oxidize your hexamine instead of nitrating it, and this will liberate a lot of NOx. The part of the referenced procedure where the reaction mixture is added to 70% HNO3 is there to oxidize unwanted linear nitramines. This is usually accomplished by raising the temperature for a while at the end of the reaction.
Ledgard has a bad reputation around here because some of his procedures are demonstrably false, while most of them are untested (by him) and copy-pasted directly from the patent literature. Patents are useful, but you need to be able to read between the lines to avoid potential pitfalls.

Should I use the same quantity of HDN as of hexamine? And should I boild the reaction mixture at (Say) 70C instead of adding the mixture to it?

Smoker Root - 31-7-2019 at 05:01

Use HDN instead of hexamine. Hexamine is the base and its neutralization by HNO3 is an exothermic process. And you save some HNO3- part of it already presents in HDN. The second stage is exothermic and emits NOx. Do it at fresh air and use some heat resistant glass. You may read about dear Jared here: search for "the worst book ever written". When the process has been complete you may use diluted HNO3 to prepare more HDN.

As I asked before, I use the same amount of HDN that of hexamine? And how could I avoid Nox fumes? Could I just heat it as someone sujest?

underground - 31-7-2019 at 08:58

As I asked before, I use the same amount of HDN that of hexamine? And how could I avoid Nox fumes? Could I just heat it as someone sujest?

You should add the same moles of HDN to hexamine. Hexamine has 140,186 g/mol. HDN has 140,186 + 2x 63,01 = 266,206 g/mol. So 266,206/140,186= 1.8989. So you have to multiplty your original weigh of HE with the number above to find your HDN quantity

caterpillar - 31-7-2019 at 13:06

As I asked before, I use the same amount of HDN that of hexamine? And how could I avoid Nox fumes? Could I just heat it as someone sujest?

OK, mate. The calculation is very simple. Originally you need to use 14 gr of hexamine and 14x11=155 gr of nitric acid. If you use HDN you have to to take 27 gr of HDN +(155 -13) gr of HNO3 (13 gr already presents in HDN). The next stage has two purposes- to get rid of linear nitramines and to get well-formed crystals of RDX. Oxidization of linear impurities is an exothermic process and you CANNOT avoid the generation of NOx.

Microtek - 1-8-2019 at 11:14

My highest yield has been 0,31 g of RDX per ml of HNO3. I don't recall the exact details, and I dont have my lab journal with me (and I didn't analyse the product, so there may have been impurities), but it should give you an indication of what you can get out of the reaction.

caterpillar - 1-8-2019 at 12:16

Quote: Originally posted by Microtek

My highest yield has been 0,31 g of RDX per ml of HNO3. I don't recall the exact details, and I dont have my lab journal with me (and I didn't analyse the product, so there may have been impurities), but it should give you an indication of what you can get out of the reaction.

What did you use, hexamine or HDN? For hexamine, your yield is too hi, for HDN normal.

Smoker Root - 2-8-2019 at 06:05

Thanks you to everybody helping me. I want to have a long lasting love with this compounds(and with my finguers) so I want to be 100% sure I am doing this right. So for finishing nitrating it would be better yo heat it in a water bath(50C) for 5min and then ley it cool to room temp for 20min and the precipitate it. This is better since it does not generate NOx due too water in the 70% acid. I also notice that is a too much excess of acid, but I don't care a Lot. Si long story short this is what I Will do:

-Use HDN
-Have a bucket un case of a runaway reaction(Si i can dump the mixture if it things get más)
-Nitrate with heat(maybe), basically heat at 50C for 5 min un a hot waterbath, and if not oxidice with acid but in a well ventilated área
-Use HDN with NO ACETONE to prevent run away reactions

So that is basically it, I can't think of something else to add. Can somebody

markx - 2-8-2019 at 11:52

Thanks you to everybody helping me. I want to have a long lasting love with this compounds(and with my finguers) so I want to be 100% sure I am doing this right. So for finishing nitrating it would be better yo heat it in a water bath(50C) for 5min and then ley it cool to room temp for 20min and the precipitate it. This is better since it does not generate NOx due too water in the 70% acid. I also notice that is a too much excess of acid, but I don't care a Lot. Si long story short this is what I Will do:

-Use HDN
-Have a bucket un case of a runaway reaction(Si i can dump the mixture if it things get más)
-Nitrate with heat(maybe), basically heat at 50C for 5 min un a hot waterbath, and if not oxidice with acid but in a well ventilated área
-Use HDN with NO ACETONE to prevent run away reactions

So that is basically it, I can't think of something else to add. Can somebody

So, I understand that this shall be your first plunge into the realm of high energetics?
I do not know how much of a chemistry related background you have, but In light of that being your first attempt, I would suggest to keep everything very simple....start from the very basic "raw" nitration of pure hexamine to establish a baseline. The process is very well researched in practice and well documented. There shall be ample time to improve upon yield and other parameters once you get a feel for the process.

Please study the chapter related to cyclic nitramines...there is a lot of good and reliable information contained:
https://archive.org/details/Chemistry_and_Technology_of_Explosives_vol_3_Urbanski/page/n87

1) work with small quantities
2) keep a quench bath ready
3) do not attempt to nitrate with heat. You need good cooling to keep the nitration mixture below 25C. The process tends to be rather exothermic.
4) do not heat the undiluted reaction mixture to decompose the linear impurities. This has do be done with a diluted (around 55% NA) mixture.
5) for simplicity and safety sake omit the linear impurity decomposition stage and go straight to precipitation after nitration. The direct nitration route of hexamine with WFNA tends to produce quite pure product with rather negligible impurities, so the decomposition step is optional. Which can not be said about the synthesis routes involving acetic anhydride and ammonium nitrate (Bachmann process)
6) read and study numerous sources before attempting practice. Always keep a certain "mistrust" towards the sources...even the reputable ones. Not seldom does it happen that what is written in books turns out to be "mildly incorrect" in practice.

twelti - 2-8-2019 at 12:06

Smoker root: I'm just wondering where you are getting white fuming nitric acid. It is difficult to buy, at least for me. Since you are just starting out, will you be able to make it? It is not too hard I guess, but could be dangerous for a novice. This is one reason I am interested in alternatives (ETN, PETN, and DAUN etc.).

XeonTheMGPony - 3-8-2019 at 04:36

Smoker root: I'm just wondering where you are getting white fuming nitric acid. It is difficult to buy, at least for me. Since you are just starting out, will you be able to make it? It is not too hard I guess, but could be dangerous for a novice. This is one reason I am interested in alternatives (ETN, PETN, and DAUN etc.).

It really isn't. I chill (Fridge temp is plenty, it just avoids minor fuming during addition) my sulfuric acid that I had distilled, add it to the KNO3 stir then warm till every thing is dissolved and gently re fluxing, then I pull vacuum and distill it to dryness (Well dry as you can get with slight excess H2SO4)

Lowest temp practical is what gives you the cleanest HNO3, don't force things let it proceed at it's own pace.

A good distillation set is vital for chemistry IMO if you want to be even half assed into it, if you want to go full assed into it then you need allot of gear, but that one simple set is the most impactful to upping ones game.

wessonsmith - 3-8-2019 at 05:33

Quote: Originally posted by XeonTheMGPony

Lowest temp practical is what gives you the cleanest HNO3, don't force things let it proceed at it's own pace.

A good distillation set is vital for chemistry IMO if you want to be even half assed into it, if you want to go full assed into it then you need allot of gear, but that one simple set is the most impactful to upping ones game.

These are two excellent points that Xeon makes.

caterpillar - 3-8-2019 at 13:29

I made RDX (successfully) twice. I used yellow fuming acid, not white. No problem with it. HDN is better than hexamine- the reaction is not very exothermic. The second stage (oxidization of linear nitramines) is obsolete, yeah, but it is very simple and provides one with relatively large crystals. The liquid will boil and emit NOx. To prepare concentrated HNO3 one can use a simple coffee pot- steel is resistant to conc HNO3. Insert a glass tube into the nose of the teapot and plug the gap with wet asbestos. As a matter of fact, the only disadvantage of RDX is the large amount of HNO3, needed for its preparation. But there is a way to use usual mixed acid (40:60 HNO3:H2SO4). Yeah, yeah, it is possible. This route provides one with a mix of RDX and keto-RDX. Urea+HDN+mixed acid, preparation is described at this forum. And mixed acid can be prepared without distillation. Ca(NO3)2 + H2SO4. Very simple.

underground - 3-8-2019 at 14:13

Caterpillar have you ever try the method above ?

caterpillar - 3-8-2019 at 18:34

Caterpillar have you ever try the method above ?

Which one? The method of preparation of RDX+Keto-RDX or mixed acid or both of them? I made mixed acid as I described above and many times, but when I made it I had no idea that it could be used for RDX preparation! I made NC and NG only. Now I have only a few gr of KMnO4 and that's all. Read this: http://www.sciencemadness.org/talk/viewthread.php?tid=28395

XeonTheMGPony - 4-8-2019 at 04:35

Oh word of warning, part of the formation process at the higher temp phase produces a clear gas, this is not decomp and will give you an epic head ache.

The gas production is mentioned in literature, its head ache inducing effect not so much.

Smoker Root - 4-8-2019 at 05:15

Quote: Originally posted by markx

Firstly I hace too thank you for replying and giving a trusty source of info. My experience with high energetics is not extended but not nule in a long shot. I have worked touch powder, nitroglicerine, silver and Mercury fulminante. And Mercury fulminante scared me a Lot fue to Nox fumes and working with Mercury(Aldo I worked with minimal amounts), and especially fue top it's sensitivity. That is why I AM trying to take more care with explosives manufacture.

I ser were you go by avoiding impurities elimimation, since it looks very difficult but I think is completly necesary since an inestable product is incredibly dangerous. I don't attempt to nitrate with heat, but to decompose impurities as many other synthesis sugest. If not which other method you recomend?

And lastly, how could I notice if a runaway reaction is happening?
Thanks you so much

underground - 4-8-2019 at 06:14

Caterpillar have you ever try the method above ?

As you can see i have myself open the above topic, but still nobody have tried it yet. It is well known that H2SO4 decompose hexamine. I am not sure if the related patents are going to work.

markx - 4-8-2019 at 07:45

The runaway reaction is basically a selfpropagating oxidation provoked by nitric acid. It releases heat which speeds up the reaction releasing even more heat....and so forth. The first signs are rising temperature and the evident formation of brown nitric oxides. So keep an eye on temperature when conducting the synthesis.
The “off gassing” step of rdx synthesis (the linear impurity removal step) is a controlled form of a deliberately provoked runaway reaction that consumes the more unstable noncyclic reaction products and leaves the cyclic nitramines relatively untouched.
The “off gassing” procedure was developed not to actually purify the end product, but to purify the waste acid for regeneration in industrial scale operations. The linear sensitive byproducts accumulated into the waste acid and made it inherently dangerous to conduct the regeneration of said acid.

caterpillar - 4-8-2019 at 17:16

As you can see i have myself open the above topic, but still nobody have tried it yet. It is well known that H2SO4 decompose hexamine. I am not sure if the related patents are going to work.

I wish I could... But now as I wrote I have no chems at all. Try yourself- preparation is very simple.

markx - 4-8-2019 at 22:04

As you can see i have myself open the above topic, but still nobody have tried it yet. It is well known that H2SO4 decompose hexamine. I am not sure if the related patents are going to work.

I wish I could... But now as I wrote I have no chems at all. Try yourself- preparation is very simple.

Mixed acid synthesis routes to cyclic nitramines usually deal with anhydrous acids....I seriously doubt the "conventionally concentrated grades" shall yield a positive result.

caterpillar - 5-8-2019 at 01:21

Quote: Originally posted by markx

Mixed acid synthesis routes to cyclic nitramines usually deal with anhydrous acids....I seriously doubt the "conventionally concentrated grades" shall yield a positive result.

Look, when I found the way to prepare mixed acid without distillation, H2SO4 was available in our shops. Its concentration was 94% approximately. Reaction with anhydrous Ca(NO3)2 definitely extracts some water (the product is CaSO4*0.5H2O). Urea can be replaced with urea nitrate or even nitrourea. I think that above described route to RDX+Keto-RDX should work.

Herr Haber - 5-8-2019 at 01:51

And lastly, how could I notice if a runaway reaction is happening?

Oh... you will

Bubbling, lots of NOx everywhere and that gut feeling yelling at you to do something.
Though not a desirable experience I still recommend seeing it at least once.
Not only because you'll know what to look for when it's unexpected but also for the chemistry involved.
Sure, you're trying to synthesize a compound but if you screw up, understand where you screwed up and what happened after you screwed up you will have gained a LOT of understanding.
There are many reasons why a runaway is happening and if you know them you can avoid it. Probably...

Edit: My first runaway ? Making nitrocellulose. It had worked everytime but that time was an impurity I didnt see in the cellulose.

[Edited on 5-8-2019 by Herr Haber]

underground - 5-8-2019 at 12:58

Quote: Originally posted by markx

Mixed acid synthesis routes to cyclic nitramines usually deal with anhydrous acids....I seriously doubt the "conventionally concentrated grades" shall yield a positive result.

Sounds interesting, we have to give it a try too. It would be really straight forward to make RDX w/o the need of 98%+ NA, also keto-RDX is even better than HMX in performance.

Late to the party

wessonsmith - 5-8-2019 at 13:34

So, this keto-RDX material seems quite impressive and by the looks of it very easy to make, assuming you have the HN0₃ and H₂SO₄

9150 m/s Det Velocity
36.8 Gpa
Det Temp 4,587 K

Who here has made it successfully? Looks like the stuff is also somewhat sensitive, not as sensitive as ETN though.

Is this stuff worth making?

[Edited on 5-8-2019 by wessonsmith]

caterpillar - 5-8-2019 at 21:23

Sounds interesting, we have to give it a try too. It would be really straight forward to make RDX w/o the need of 98%+ NA, also keto-RDX is even better than HMX in performance.

Go ahead, mate, and I wish you success. If you wanna read the original article (that hardly can be obtained now- paid access) let me know and I'll upload it to Google drive. Believe me, I was about to cry, reading it. How many options I missed when I was young and have all necessary chems!

underground - 6-8-2019 at 15:59

Sounds interesting, we have to give it a try too. It would be really straight forward to make RDX w/o the need of 98%+ NA, also keto-RDX is even better than HMX in performance.

I will give it a try for sure in future but at the moment i am so busy. Work and liabilities in life never ends. I am doing some other projects too. I am making an EBW system now for few months but i am doing very little progress each time due to luck of time. I will post a topic when i will finish it. I also have to test some DAUN, so there are plenty of things that i have to do 1st.

twelti - 6-8-2019 at 16:49