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2verud
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[*] posted on 11-9-2009 at 08:57


Does anyone know the runaway temperature for this nitration (meglomania recipe)? I allways like to know stuff like that before i start:)
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[*] posted on 26-9-2009 at 11:18


Quote: Originally posted by 2verud  
(meglomania recipe)?

Recipes are for cooks and k3wls---the correct term 'synthesis' is preferred here. . .or 'synthetic method'.
If you're nitrating hexamine directly the temp shouldn't exceed 30*C.
A few minutes after the addition of hexamine to HNO3 the temp may be cautiously raised to 55*C, but this is probably unnecessary. . .
You should have several litres of drowning water close to hand for safety anyway.
If the reaction even looks like it's getting out of hand, drown it straightaway.
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[*] posted on 15-10-2009 at 15:13


Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205
as a dehydration agent . In 100ml HNO3 1.42gr/ml density, by 0cº temperature, in course of 10 minutes was slowly added 100 gramms of P205, then all P2O5 was added, mixute was heat to 50cº to dissolve deposition, after temperature of reaction solution place at 0cº, 10g of hexamine was slowly added in solution, temperature of solution was near 5cº. Solution was keep in 30 minutes, and add to 500 ml cold water with ice. This mixture was filtered, deposition washed 3 times by 100ml of water and dry out. 13,9 gramms of RDX with 204.4cº melting poing was obtained, i have a photos of product and another.

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[*] posted on 1-11-2009 at 17:55
filaments


i followed rdx recipes and ended up with weird stuff.

i mixed h2so4 and nh4no3 to make nitric acid. the result is yellow fuminn nitric.
(btw, what is the equation for the reaction? and where is the other product of this mix)
I mixed hexamine with this fuming nitric with slight oxides. not all of it dissolved. I let it in 50 degree bath for a few minutes ( vapors might got out of the apparatus).
when i come back, there are short white fibers and no liquid. i dont think it's rdx, nor R-salt, nor hemamine dinitrate. it doesnt look like a crystal. what is it?
it melts pretty fast, dissolves really easily in water, doesnt deflagrate.

thx
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[*] posted on 1-11-2009 at 21:43


haha, oh wow.
Stop doing this chemistry. Dude seriously, just a few posts up the temperature was advised to never rise above 30*C.

It sounds like you need a whole lot of more basic (and safe) schooling in chemistry before you even think about using conc. acids.

And never ask for help with a 'cook' synthesis on this site ever. Read the FAQ ffs.




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[*] posted on 2-11-2009 at 05:16


Good for you, it is a very good thing that it isnt RDX.
It is allmost new years day thats when the retards start getting a horny feeling around loud noises.

Can you at least describe what you have done?

[Edited on 2-11-2009 by User]




What a fine day for chemistry this is.
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[*] posted on 3-11-2009 at 22:13


Quote: Originally posted by dr0ne  

...
i mixed h2so4 and nh4no3 to make nitric acid. the result is yellow fuminn nitric.
(btw, what is the equation for the reaction? and where is the other product of this mix)
thx


H2SO4 + 2NH4NO3 -> 2HNO3 + (NH4)2SO4, so your additional product is ammonium sulfate. Presumably. But I don't know that it makes sense to talk about these as separate products (prior to distillation/separation or what have you) since what you've really created is an acidic soup with a lot of these ions floating around.
However, there's not much anyone can do unless you at least provide quantities of the things you mixed together.
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hissingnoise
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[*] posted on 4-11-2009 at 04:46


Hexamine is decomposed by H2SO4---time for some serious reading, before you do yourself an injury!
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[*] posted on 4-11-2009 at 08:01


Quote: Originally posted by dr0ne  
there are short white fibers and no liquid. i dont think it's rdx, nor R-salt, nor hemamine dinitrate. it doesnt look like a crystal. what is it?
it melts pretty fast, dissolves really easily in water, doesnt deflagrate.


If hissingnoise is correct then maybe you had the ingredients to make some sort of primitive formaldehyde polymer, which might behave like this. Hexamine should hydrolyze to formaldehyde plus ammonia; the ammonia would react with the acid to form (even more) ammonium sulfate and/or ammonium bisulfate, leaving the formaldehyde to possibly form long chains. Though in the case of industrial polymers of this type (e.g. Delrin) the product is not exactly water soluble, we can assume you wouldn't have had anything more than contaminated medium-chain-length gunk.
On the other hand, it does seem a little weird that conditions that would hydrolyze one condensation product (hexamine) would also encourage the formation of another; formaldehyde polymers are supposed to be attacked by acid. Things might be very sensitive to the amount of water actually present in your mix.
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[*] posted on 4-11-2009 at 12:56


Most, or all of the formaldehyde will be oxidised by nitric acid as it forms!
Some small amounts of resins may form, in addition.
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[*] posted on 5-11-2009 at 10:13



I have seen the use of WNA (1.52) used for a simple nitration on hexamine dinitate and the yield was fairly better (about 80%; don't really remember) and some of the German methods joins the synthesis of the hexamine with [what we would see as a ] nitration. That, I believe is a "plant method" and may produce the highest yield for given precursors. If we search "H2SO4, RDX" you'll get two whopper threads on it from awhile back. So the "hexamine" is IN the lab with the active nitration.
There has been a great deal of discussion as to why a "classic" mixed acid route is not used with cyclonite. Aside from all that acidic anhydride is just too damn tough to get because of all the cooks.

In fact IF acidic anhydride were available, there are fairly simple methods the synthesize HMX with limited lab expense.

[Edited on 5-11-2009 by quicksilver]
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[*] posted on 11-11-2009 at 05:25


Quote: Originally posted by phantasy  
Hello guys! I'm have near 90% yeild of RDX, using 70% HNO3 with P205

as a dehydration agent .


I've wondered for quite some time now, whether it's possible to prepare RDX using HNO3/P2O5 as a nitrating agent. I really don't believe this k3wl I quoted, since those yields are not even achievable with 97% HNO3. :(

In my search for references regarding this method a basically found none. In Urbanski there are some experiments done with nitrocellulose using HNO3/H3PO4/P2O5 mixtures with good results. For the rest of the 100+ nitrations described P2O5 isn't mentioned. Also, urbanski says that H3PO4 is in fact strong enough to protonate, forming the nitronium ion.

Further, regarding the safety of such an experiment, i'm worried about nitric oxides. Books like the mercks index tell me that N2O4 is made in the lab using the same P2O% and HNO3! Unless I keep the temperature below 0oC most of it will instantly form NO2, since the equilibrium shifts to the right. The only solution for this is to use exactly enough P2O5 to react with all the water, leaving the nitric acid unharmed.

Any ideas?











[Edited on 11-11-2009 by Leander]
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[*] posted on 11-11-2009 at 05:46


Yields of 70% have been claimed for the nitrolysis using 100% HNO3, but typically it is around 65%---yields are higher using Ac2O/CH2O/AN, obviously but you'll have to synthesise Ac2O, yourself. . .
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[*] posted on 13-11-2009 at 10:04


HNO3 and P2O5 does not form N2O4 but rather N2O5, nitric anhydride. N2O5 is an excellent and fairly mild nitrating agent which is used in many experimental nitrolysis operations.
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[*] posted on 23-1-2012 at 13:40


Here is a possible route that could potentially be used to selectively oxidize R-salt to RDX,

Quote:

A modified electrode comprising a film of mixed-valent ruthenium oxides with cyano cross-links on glassy carbon mediates the oxidation of N-nitrosamines. The oxidations are two-electron processes. Using N-nitrosodi-n-propylamine as a model compound, the mechanism of the oxidation was shown to involve a coupled protonation of the oxidized form of the mediating film. Bulk-scale controlled-potential electrolysis of N-nitrosamines yielded the corresponding N-nitramine; gas chromatography—mass spectrometry did not show any evidence of side reactions.
"Oxidation of N-nitrosamines at a ruthenium-based modified electrode in aqueous solutions", Waldemar Gorski, James A. Cox


see the thread about R-salt: C.T.M.T.N.A. (R-salt)
Its preparation does not require concentrated acids, even 15% conc. HCl is sufficient.

There are several threads about "glassy carbon" anodes in the technochemistry section of this forum.
http://www.sciencemadness.org/talk/viewthread.php?tid=15345
http://www.sciencemadness.org/talk/viewthread.php?tid=17370

[Edited on 23-1-2012 by AndersHoveland]
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[*] posted on 1-2-2012 at 03:44


My first experiment produced only red fume. Conc HNO3 is not a problem, if you have a glass distillation apparat. According to russian- it is not actualy a book- it is something without hard cover for students something like "laboratory manual on syntesys of nitrocompaunds", excuse me my poor translation. There was a simple process described: 1 gr of hexamine per 20 gr of conc HNO3. A simple (and efficient) modification: to use not hexamine, but its dinitrate. I think anyone may recalculate how much of dinitrate can be used (and weihgt of HNO3- dinitrate puts some HNO3, so one may decrease amount of conc HNO3). This process didn't produces red fumes. Final stage is oxidation of unstable linear nitroamines. I do not remember details. reacting micture must be dissolved and some nitrous acid must be added (salt, of course). During this process liquid will boil and produce toxic gases- CH20 and NO2. Final concentration of nitric acid must be 70% if I'm correct. During oxidation RDX will precipitate. Wash it and use as you wish. I made it once and got some sow-white crystals.



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[*] posted on 1-2-2012 at 10:02


The original patent from Britain proposed a 1:7 ratio of (1.5 HNO3). Ratios are similar w/ the hexamine di-nitrate ratio is not quoted to be less however the yields may be greater than 60%. It may have been Bachmann who determined that 90% acid was the lowest that could support an RDX synthesis (see PATR)

Attachment: RDX_from_Hexamine_and_Nitric_Acid_-_GB_Patent_0145791.pdf (261kB)
This file has been downloaded 1115 times





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[*] posted on 1-2-2012 at 11:45


Quote: Originally posted by caterpillar  
My first experiment as you wish. I made it once and got some sow-white crystals.


Not very white then I guess?



[Edited on 1-2-2012 by dann2]
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[*] posted on 1-2-2012 at 15:24


What makes you think so? Definitely white. It was many years ago, I cannot tell you precisily. These crystals burned with such hissing sound. BTW, you may try K process- treatment of hexamine with HNO3+NH4NO3. It promices higher yield than the simple nitrolisys. WARNING: this process requires temperature at 80 Celsius. I think, it is the best way to get as much RDX as possible (per 1 gr of conc HNO3, which is the most problematic component). Mixture of HNO3 + NH4NO3, heated up to 80 Celsius and hexamine dinitrate. It is only my proposition, of course.



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[*] posted on 1-2-2012 at 16:39


Quote: Originally posted by KABOOOM(pyrojustforfun)  
last night I did an experiment to see if HOONO(peroxynitrous acid) can react with HMTA to get RDX. I pourd 175 ml hydrochloric acid (unknown concentration) and 48.5 ml 45% H<sub>2</sub>O<sub>2</sub>in a beaker put it in a ice bath and let it cool under 5°C. I had measured 39g of NaNO<sub>2</sub> it was in two film can one containig 18 g another 21 g. I slowly added the NaNO<sub>2</sub> it started fizzing, the NaNO<sub>2</sub> had big lumps one fell down and a violent reaction happend I was shocked and in response I spilled most of the (18 g) NaNO<sub>2</sub> :o a very dense brown fume rushed out that made me run a way.


Peroxynitrous acid (which only transiently forms in solution) is a very strong and reactive oxidizer. It would easily attack the methylene groups also, and the result would probably be mostly a variety of undesirable oxidation products. The decomposition of peroxynitrous acid proceeds through hydroxyl radicals and nitronium cations, so it can act as both an oxidizing and nitrating agent (even in dilute solution).

Also, at such high concentrations, there is likely to be significant side reactions between the hydrochloric acid and hydrogen peroxide. Such mixtures could potentially chlorinate organic compounds.


Quote: Originally posted by KABOOOM(pyrojustforfun)  
doese any body know how oximes react with HNO<sub>2</sub> ? I know that some hydoxylamino compounds form nitramino compounds .but I'm not sure if the same reaction happens for oximes. if so formoxime (made from formaldehyde & hydroxylamine) probably forms H2C=N-NO2 which polymerizes into RDX and (-H2C-N(NO2-)n) polymers.
Edit: I thought I had edited this post before. oximes can't make nitramines that way but some hydroxylamino comopunds form nitrosohydroxylamino derivatives



Oximes can be oxidized by either nitrous acid or nitrogen dioxide, and the resulting product will depend on whether the oxime is of a ketone or aldehyde.

Oximes of ketones are oxidized to "pseudonitrosoles", with a structure such as
(CH3)2C(-NO2)-NO
The nitroso (-NO) groups tend to dimerize, so the structure could also be represented as
(CH3)2C(-NO2)-N(-O)-ON-C(-NO2)(CH3)2
Further oxidation results in geminal nitro groups,
for example (CH3)2C(NO2)2
which tend not to be thermally stable, and gradually decompose in storage.

Oximes that are adjacent to another ketone group,
for example CH3-C(=NOH)-C(=O)-CH3
are oxidized by nitrous acid to di-ketones,
R-C(=O)-C(=O)-R
"Less familiar reactions of oximes", Jeremiah P. Freeman, Chem. Rev., 1973, 73 (4), pp 283–292
(the "R" group would likely also be vulnerable to oxidation if it was a methyl group, because of additional tautomerization, but not if it was a tert-butyl or phenyl group)

(organic amines can also be oxidized by hydrogen peroxide, first to hydroxylamine derivitives, and then to oximes)

The literature seems to be conflicting.
Apparently, some oximes can be converted back to their original aldehyde, in 100% yields, by oxidation with NO2.
"Quantitative Regeneration of Carbonyl Compounds from. Oximes and hydrazones by Gaseous Nitrogen Dioxide", J. Mokhtari, Iran University of Science and Technology, Tehran (Iran) This paper specifically mentioned oxidation of benzaldehyde oxime to benzaldehyde using N2O4, with 100% yield.
Whereas in the Ponzio reaction (1906), the conversion of m-nitrobenzaldoxime to m-nitrophenyldinitromethane with dinitrogen tetroxide, is possible.
"Reinvestigation of the ponzio reaction for the preparation of gem-dinitro compounds", P.J. Honey, R. W. Millar

But I suppose what you would really be interested in is the oxidation of formaldoxime CH2=NOH with nitrous acid. I do not really know, but perhaps the below will be helpful:

"results indicate that the rearrangement from nitrosomethane to more stable trans-formaldoxime" , EXPLORING THE POTENTIAL ENERGY SURFACE OF THE CATALYZED ISOMERIZATION OF NITROSOMETHANE TO FORMALDOXIME by GUO-MING LIANG

from a patent: "The trimer is a high melting solid (m.p. 145-156 C)"

In the reaction in water, there apparently exists an equilibrium between the trimer and monomer. The formaldoxime monomer stays as the monomer in dilute solution but when formaldoxime monomer reaches 15-20 weight percent, the trimer will startto form. The rate and extent of the trimer formation seem to depend on temperature/pH/time. The higher the pH, the more the amount of monomer which forms."

this suggests that the main reaction of formaldoxime with NO2 might be formation of trinitromethane, rather than nitromethane. Although, this would mean most of it would be tied up in the trimer, and there would only be a small ammount of the CH2=NOH (with a double bond on the carbon) in equilibrium in water, and that double bond is rquired for NO2 to be able to oxidize hydrogens off.
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[*] posted on 1-2-2012 at 16:48


Quote: Originally posted by caterpillar  
What makes you think so? Definitely white. It was many years ago, I cannot tell you precisily. These crystals burned with such hissing sound. BTW, you may try K process- treatment of hexamine with HNO3+NH4NO3. It promices higher yield than the simple nitrolisys. WARNING: this process requires temperature at 80 Celsius. I think, it is the best way to get as much RDX as possible (per 1 gr of conc HNO3, which is the most problematic component). Mixture of HNO3 + NH4NO3, heated up to 80 Celsius and hexamine dinitrate. It is only my proposition, of course.



He was only making fun because you said "sow-white" instead of "snow-white" crystals. Sow = mother pig. Just A typo. I know English probably isn't your first tongue. I think your typing is very good considering this.




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[*] posted on 1-2-2012 at 19:02


Well, I can confirm your proposition- English isn't my mother's tongue. Well, take a piece of info:

(CH2)6N4 + 2 NH4NO3 + 4 HNO3 --> 2 RDX + 6 H2O (5.24)

This method is known as the K-process after its discoverer Koffler.
It uses ammonium nitrate to compensate for the nitrogen deficiency in hexamine and works to Equation (5.24) where two moles of RDX are produced per mole of hexamine. As observed with method 5.15.1.2, the addition of ammonium nitrate to nitric acid appears to prevent dangerous oxidation reactions from occurring. In fact, this nitrolysis reaction only occurs at elevated temperature and so a constant temperature of 80 C is usually maintained throughout the reaction. Yields of approximately 90% are attainable based on one mole of hexamine producing two moles of RDX.

I can only add that I'd use hexamine dinitrate instead of pure hexamine. Description of K method was taken from a nice and useful book, written by Agrawal and Hodgson- Organic chemisrty of explosives.






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[*] posted on 15-8-2012 at 01:57


This is interesting...
So you can supposably get a 90% yield on cyclonite production by dissolving phosphorus pentoxide in the 95+% nitric acid, according to the patent...Now when i first heard "Phosphorus Pentoxide" i thought i could just go and buy it somewhere or at least do a simple reduction reaction to acquire it. Well thats just not really feasable. However heres how to make the p205...Pee in a cup, i suppose a 20oz and let it sit uncovered for 7 days, then take two tablespoons of finley ground charcoal and two tablespoons of finely ground cinnamon and mix them together, now put them in the urine and stirr it, then do a classic distillation except the receiver flask should be filled with water and the exit tube from the condenser in the water and you will start to see white phosphorus form in the bottom of the flask, dont remove it from the water or it will burst into flames...Now put your white phosphorus into a reaction vessle, preferably a beaker filled with oxygen gas with some type of lid, put a small hole in the lid, now take some tweezers and place the phosphorus in the middle of the beaker and take a copper rod and heat it with a torch, now reach through the hole with the rod and touch the WP and it will burst into flames and produce phophorus pentoxide, now scrape it up, seal it and use it for your next cyclonite synth!!!:D
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[*] posted on 15-8-2012 at 02:17


This is even more interesting...
YOU DONT HAVE TO USE NITRIC AT ALL!!! Well kinda, what you have to have is nitrogen pentoxide, nope couldn't find that one for sale either....however you can make it as well. Nitrogen Pentoxide or "dinitrogen pentoxide" is the anhydride of nitric acid and can do the nitration job much better than just plain ol nitric, it's made by the dehydration of nitric acid with phosphorus pentoxide...Hexamine is dissolved in a little chloroform, then another beaker of chloroform has some nitrogen pentoxide, then the hexamine/chloroform solution is slowly added to the chloroform/nitrogen pentoxide solution, the nitrogen pentoxide is the nitrator in the reaction therefore precipitating pure RDX crystals!! See here's why this reaction is quite a bit more effecient than the traditional nitric/hexamine reaction...The main byproducts of this reaction are RDX, Formaldehyde, and the lower oxides of nitrogen, the formaldehyde which is the main portion of the byproducts besides RDX is insoluble in chloroform and after the hexamine is converted to RDX it comes out of the solution, you can then filter off the rdx and reuse the solution by adding more nitrogen pentoxide and hexamine to the solution, it's a continuous manufacturing solution, yields are supposed to be about 89%. Honestly it would probably be easier with the original phosphorus pentoxide method since you have to use p205 to reduce nitric acid and that just takes an extra couple of steps, both yields are about the same. Two advantages of this procedure over the first one...I imagine nitrogen pentoxide would store better than fuming acid and the fact that you can continually produce the RDX unlike the other solution where you have to put in a fresh batch of nitric. The only downsides are it's probably a bitch to make and supposedly nitrogen pentoxide is an unstable oxidizer so...
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[*] posted on 20-7-2013 at 22:19


Can one use a mixed acid nitrolysis of hexamine with nitrate salt and excess H3PO4 ?
I found a local chem supply for 85% H3PO4.

Or can one do a nitration of Tripotassium 1,3,5-Triazacyclohexane-1,3,5-trisulfonate with H2SO4 and nitrate salt ?

[Edited on 21-7-2013 by Motherload]




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