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Author: Subject: RDX synthesis. Safe ir not?
twelti
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[*] posted on 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.).
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XeonTheMGPony
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[*] posted on 3-8-2019 at 04:36


Quote: Originally posted by twelti  
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.
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[*] posted on 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.
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[*] posted on 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.



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[*] posted on 3-8-2019 at 14:13


Caterpillar have you ever try the method above ?
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[*] posted on 3-8-2019 at 18:34


Quote: Originally posted by underground  
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




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XeonTheMGPony
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[*] posted on 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.
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[*] posted on 4-8-2019 at 05:15


Quote: Originally posted by markx  
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.


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
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[*] posted on 4-8-2019 at 06:14


Quote: Originally posted by caterpillar  
Quote: Originally posted by underground  
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


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.
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[*] posted on 4-8-2019 at 07:45


Quote: Originally posted by Smoker Root  


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

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.




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[*] posted on 4-8-2019 at 17:16


Quote: Originally posted by underground  


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.




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[*] posted on 4-8-2019 at 22:04


Quote: Originally posted by caterpillar  
Quote: Originally posted by underground  


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.




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[*] posted on 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.




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Herr Haber
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[*] posted on 5-8-2019 at 01:51


Quote: Originally posted by Smoker Root  

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]




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[*] posted on 5-8-2019 at 12:58


Quote: Originally posted by caterpillar  
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.


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.
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shocked.gif posted on 5-8-2019 at 13:34
Late to the party


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]
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[*] posted on 5-8-2019 at 21:23


Quote: Originally posted by underground  


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!




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[*] posted on 6-8-2019 at 15:59


Quote: Originally posted by caterpillar  
Quote: Originally posted by underground  


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!


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.
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[*] posted on 6-8-2019 at 16:49


Quote: Originally posted by caterpillar  
Quote: Originally posted by underground  


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!


I for one would be interested in the doc. Especially if DAUN doesn't work out.
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[*] posted on 6-8-2019 at 22:25


https://yadi.sk/i/wRzHgThjGp73lA here is the link. I can only add that urea can be replaced with urea nitrate or even nitrourea. I wish you success.



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