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Smoker Root
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[*] posted on 29-7-2019 at 04:39
RDX synthesis. Safe ir not?


Hi, this is my first post on this amazing forum. I hope se all get along.

So I saw this RDX synthesis on The preparstory manual of explosives, which is a quite solid book un my opinion. However, I wanted to make sure it was Nice before trying it.

This procedure uses an excessive amount of 99% nitric acid to properly carryout the reaction. This excessive
amount of acid can be recovered by treating the reaction mixture (after complete removal of the product) with methylene
chloride to recover the nitric acid. Prior to this action, a small amount of sulfuric acid should be added to the reaction mixture.
Afterwards, the reaction mixture should be extracted with several volumes of methylene chloride. These combined volumes
can then be carefully distilled to recover the nitric acid of 99% purity (see nitric acid, 90% and 99% respectively).
Place 220 grams of 99% nitric acid into a beaker, and then cool to 10 Celsius by means of a cold water bath. When the
temperature of the 99% nitric acid reaches about 10 Celsius, slowly add 20 grams of hexamine while stirring the 99% nitric
acid and maintaining its temperature at about 10 Celsius. After the addition of the hexamine, maintain the reaction mixtures
temperature at 20 Celsius for 40 minutes with constant stirring. Then place 14 grams of 70% nitric acid and 2 grams of sodium
nitrite into a flask and heat to 70 Celsius. When the temperature reaches 70 Celsius, slowly add the reaction mixture while
maintaining the temperature of the 70% nitric acid mixture at 70 Celsius and stirring. After the addition of the reaction mixture,
continue heating at 70 Celsius for about 40 minutes. After which, remove the heat source, and allow the reaction mixture to
cool to room temperature. Then place the reaction mixture into an ice bath, and cool to about 5 Celsius. Finally, add the entire
reaction mixture to 500 milliliters of cold water and then filter-off the precipitated RDX product, wash with 200 milliliters of
water, and then vacuum dry or air-dry.

This synthesis gives me weird feelings. I think it captures the feeling of a normal synthesis, it washes the RDX with water to libérate it from acid for long term storage(Aldo it does not talk about the litmus test) But I find that using hexamine is a bad idea, to many fumes. I prefer using HDN. I don't know if the adition rate and conditions they especify un here are good enough to avoid them. It does not talk about having a bucket of water un case a SIDE reaction happens were you can dump everithing into. It does not talk about a method of heating(Aldo a hot water bath looks to he the best) And also the dilution of the acid, i have heard that any water present in the synthesis can fuck everithing up, and they use 70% nitric acid, si I am not confident. I Will also like to add that a recristalization from hot acetone is posible.

Can somebody tell me if this is safe? Trusty? And worth it? Love you all
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twelti
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[*] posted on 29-7-2019 at 07:25


Uh Oh, Ledgard again!
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[*] posted on 29-7-2019 at 09:50


There are plenty of topics about RDX synthesis, just use the search engine and you will find whatever you need.
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Smoker Root
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[*] posted on 29-7-2019 at 11:08


Quote: Originally posted by twelti  
Uh Oh, Ledgard again!


What happens with this author?
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Smoker Root
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[*] posted on 29-7-2019 at 11:20


Quote: Originally posted by underground  
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
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[*] posted on 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.
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twelti
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[*] posted on 29-7-2019 at 12:00


Quote: Originally posted by Smoker Root  
Quote: Originally posted by twelti  
Uh Oh, Ledgard again!


What happens with this author?

Do a search in this forum, on Ledgard. He is apparently an unreliable source.
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Smoker Root
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[*] posted on 29-7-2019 at 13:27


Quote: Originally posted by twelti  
Quote: Originally posted by Smoker Root  
Quote: Originally posted by twelti  
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]
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[*] posted on 29-7-2019 at 13:53


Quote: Originally posted by underground  
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
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James Ikanov
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[*] posted on 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.




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[*] posted on 29-7-2019 at 16:22


Quote: Originally posted by Smoker Root  
Quote: Originally posted by twelti  
Uh Oh, Ledgard again!


What happens with this author?


Miserable failure and lots of wasted time and chemicals, if lucky.
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[*] posted on 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.
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[*] posted on 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.
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[*] posted on 29-7-2019 at 21:53


Quote: Originally posted by underground  
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.




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[*] posted on 29-7-2019 at 23:15


Quote: Originally posted by XeonTheMGPony  
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.


Can you send me the paper you are following?
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[*] posted on 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.
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[*] posted on 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.



Women are more perilous sometimes, than any hi explosive.
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Smoker Root
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[*] posted on 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?
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[*] posted on 31-7-2019 at 05:01


Quote: Originally posted by caterpillar  
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?
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[*] posted on 31-7-2019 at 08:58


Quote: Originally posted by Smoker Root  
Quote: Originally posted by caterpillar  
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?



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
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[*] posted on 31-7-2019 at 13:06


Quote: Originally posted by Smoker Root  
Quote: Originally posted by caterpillar  
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?


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.




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[*] posted on 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.
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[*] posted on 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.




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[*] posted on 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
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[*] posted on 2-8-2019 at 11:52


Quote: Originally posted by Smoker Root  
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.




Exact science is a figment of imagination.......
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