I did a mix of 105 g NH4NO3 and 75 g Hexamine like someone (maybe Lagen) said it's usefull to add ammonoium nitrate in the hexamine...

After that, I followed EXACTLY the Megalomania's synthesis and my homemade nitric acid has a density of 1.51 (100%)

After adding more than the half of the mix, The temperature rised and I wasn't be able of stop it (the erlenmeyer was in a big ice bath with lot of ammonium nitrate in it...)
The temperature rised to 40°C and here, I dumped the solution in water, the reaction was lousy...

WHAT THE FUCK HAPPENDED ????????????
is the ammonium nitrate in the hexamine who fucked up my synthesis ?

thanx...

I don't think 40 degrees is any cause for alarm and I don't think it was the NH4NO3. Was your HNO3 free of nitric oxides? I think they can cause this to happen but I am not sure. Try adding the Hex more slowly. That's the only advice I can give.



------------------
AAARRRRRHHH! My beautiful eyes! It burns!
The goggles do nothing!AAARRRRRHHH!

I produce my own nitric acid by distillation of NaNO3 and H2SO4, he is a little yellow but not red, do you think there are some NOx int it ?

Megalomania said the mixture must be keep between 20-30°C and mine came at 40°C and red fumes were given off...

any reply is more than appreciated...

If your nitric acid is yellow, it definitely contain some NO2 disolved in it. You can 'kill' the NO2 by adding some urea (wich will decrease the concentration of the acid) or with a steam of air conducted in the acid.
The temperature of the reaction MUST be around 55 degrees C; Mr. Cool saids that 70 degrees is a good temp. with NH4NO3/hexamine/nitric acid method.
Add your hexamine/AN mix slowly. If you'll do so, the temperature should not be over 25 degrees after the addition of hexamine/AN in the acid. Then, slowly heat the mixture to 55 degrees C minimum, and hold the mix at this temp. for 30 mins. The resulted mix should precipitate out the RDX in cold water...

------------------
Damn, I got a nitro-headache again...

http://move.to/pyromania

Normally the acid's NOx content is related to it's color, it starts at a greenish then turns to a yellowish then turns orange and slowly goes to red. here is a pic of some NOx vapors flowing through my condenser.

http://www.geocities.com/pyro2000us/dsc_039.jpg

------------------
visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

Yellow nitric = small amounts of NO_x present. The amount of urea (46% N fertilizer) added is around 2% by volume to the acid. Also, the acid can be a little less concentrated, as low as 90% will do, but anything lower will cause unwanted by-reactions to take over forming hexamine dinitrate, etc.

------------------
Visit my website (in development): http://codemason.cjb.net

Pyro, try holding the camera still next time, huh?

------------------
"I have begun evil, I shall end evil. That is the end that awaits me."

Go here (http://briefcase.yahoo.com/nbk2ooo) to download the NBK2000 files and videos.

It was the camera's fault, the damn thing takes so friggin long to take a picture that without a tripod it s nearly impossible to take a quality picture, when I uploaded my pics to the forum ftp I only uploaded a few out of like 50 total pics. that's why I want a reliable cheap digital camera. with film everything works but with digital everything is shit. Don't buy any IXLA cameras.

------------------
visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

So, you think ALL that NOx are the fault of my run away reaction ?

(for purpose only : I bought some urea to my supplier and this stuff is 99.5% pure...)

see ya !

You said that the temperature of the reactants raised so much that NO2 appeared. So, next time you have to :
-add some urea to your yellow nitric acid
-add hexamine/AN mix slower, for god sake !

------------------
Damn, I got a nitro-headache again...

http://move.to/pyromania

ok, I will add some urea to my nitric acid but I added the hexamine/AN slowy and sudden, the temp rises a lot !

thanx for all !

According to Urbañski the K method ( HNO3 with AN ) is cunducted in higher temperatures. The nitration lasts 30 min in 80 degreses.
The amounts of substances:
480-500kg urotropine
4800kg ammonium nitrate
8600kg HNO3 99%

From that amount we should get 1000kg of RDX.

What is changed with the AN method ?
Do I need to heat the mixture longer ?

in brief, what's the difference with hexamine method and AN/hexa method ?

any reply is more than appreciated...

The main difference between the AN/hexamine and hexamine (SH) method is that with the first method you'll get two moles of RDX reported to one mole of hexamine, and with the second (SH) - one mole of RDX .
There is also the temperature factor. With SH method it should be around 55 degrees, and with AN/hexamine - 70-80 degrees C. Also the concentrations : the SH method require 98 % HNO3, otherwise it won't work. You'll get only hexamine dinitrate instead of RDX with a lower concentration of HNO3 (in the best case). But if you use ammonium nitrate, the minimum concentration can be around 95 % (what a release, huh http://theforum.virtualave.net/ubb/smilies/wink.gif )

C6H12N4 + 4 HNO3 --> C3H6N6O6 + 3 CH2O + NH4NO3

And with ammonium nitrate:

C6H12N4 + 4 HNO3 + 2 NH4NO3 --> 2 C3H6N6O6 + 6 H2O


HNIW, do you have Urbanski's books ?


------------------
Damn, I got a nitro-headache again...

http://move.to/pyromania

Urbañski book's yea I've read 3 parts a few times. But this books consist only of synthesis no practical usage. Urbañski was a scientist from my country so I've got them in polish.
Now back to the topic. K method is usually used because of smaller amount of hexamine needed for RDX. Because hexamine needs to be pure for RDX manufacture that's why this method may be usefull. Nowadays this method isn't used, because hexamine is much cheaper then for example 50 years ago. So the K method becomes more expensive because it needs additional heat ( the nitration mixture is pumped with hexamine and AN through heated pipes ) and finally it is much more dangerous.

so, I have to slowy add my hexa/AN mix to my WHITE nitric acid (95% min.) then, I have to heat the beaker/erlenmeyer to 70-80°C for 30 min, is it right ?

thanx for all !

In my opinion don't give a shit with this method, use hexamine and nitric acid ( 98-99% ) it is a good method, I conducted it many times.

Lower acid concentrations work for the destructive nitration of hexamine, I have heard you can even get away with using 85%, yields are just shocking. Anything lower than 85%, however, and all you will be left with is hexamine dinitrate.

------------------
Visit my website (in development): http://codemason.cjb.net

If those figures from Urbanski are correct, then your hexamine consumption is lower, but the HNO3 consumption is a lot higher. I would recommend reacting hexamine dinitrate with nitric acid ( at 20-30 C then heating to 55 C for 5 min ).

HNIW, I will give a shit with this method http://theforum.virtualave.net/ubb/smilies/smile.gif
why ? simply because more RDX is produced and then, more funny explosions too...

What will I have to do and what won't I have to do with hexa/AN ?

How can I difference hexamine dinitrate and RDX ?

thanx...

found nothing... sorry !

Stanfield I use RDX rarely because I have to "play" with nitric acid. Normally I just go to the shop and buy 60kg of AN ( 2$ per 10kg ). To set it of I use about 3-4g RDX and from one nitration I'm getting about 500g of RDX so I can make 100 blasting caps. RDX is ok but for plastic explosives or blasting caps. Even in demolitions I don't use RDX, even for boosters to saletroles I use pressed TNT. RDX is rather good for army, the production on larger scale is rather complicated.

thanks, that's very interesting http://theforum.virtualave.net/ubb/smilies/smile.gif

"(if at this point the RDX does not crystallize out you will need to dump it into water to precipitate it)"
===> effectively, I see that the nitric acid must be free of nitrogen oxide...

Could you explain to me why, when I add urea and bubble air through acid, this last stay yellow !!!

I added 10 g of urea in my 480 mL of HNO3...nothing append, the color is the same before and after the addition of urea !

help me plz !

10fingers: In your reference to Lagens procedure shouldn't it be 861 grams HNO3? Otherwise it is certainly a great improvement! Also, you can strike the 'supposedly' from the HDN to RDX reaction - it is confirmed. You perform the nitration as you would with hexamine, simply substituting HDN. You may need more than half the amount of nitric, but the yield is considerably better.

Stanfield: The acid doesn't need to be completely free of NOx. Bubbling dry air through it until the vapours are white rather than brown is usually good enough. NOx is not the only thing that can colour the acid yellow; remember that any protein containing matter that is contacted by nitric is turned bright yellow....

Yeah and Uncle Fester even points out some of the glaring errors in KIPE in the book.

------------------
Visit my website (in development): http://codemason.cjb.net

Well in my experience the HDN to RDX process gives about 2 g RDX from about 2 g HDN which has come from about 1 g hexamine. Thats about 1 mol RDX from 1 mol hexamine which is all you can expect from the simple nitration as I understand it.
Would one of you by any chance be able to upload this "uncle fester" text to ctrl_c's ftp?

I downloaded it from someones page here on the Forum, but I can't recall which one at the moment. If I think of it I'll let you know.
Please post the exact procedure you are referring to for HDN to RDX.

The procedure ( which may not be optimized ) goes like this:

- 30 grams of 100% nitric acid, reasonably free from NOx, is brought to 20 C in a beaker.
- 10 grams of HDN is added slowly, keeping the temp between 20 and 30 C.
- When the addition is complete, temp is raised to 55 C and held between 50 and 55 C for 5 min.
- The mixture is cooled to 20-30 C and allowed to stand for 15 min ( don't let it stand longer; it seems to start to break down, reducing yield if left for longer )
- 80 mL cool water is added gradually to precipitate the RDX. If the acid is concentrated enough, yield should be around 8 grams.

I finally found a source of paraformaldehyde for E-process...
My question is :
If you follow exactly the megalomania's synthesis (68g of para), what's the theoritical yield in grams ? what's the equation of the reaction ?

thanx !

Someboby tried to make very pure RDX without conc. HNO3 from CTMNA, 55-65% HNO3 and 30-50%H2O2??? Yeild may be 90-95%. One my friend says that he tried it and all was fine...
I cannot to check it because I cannot to obtain NaNO2 now. If you want try to make it I can give more detailed description.
Also do somebody knows about brisance measuring by Cast's method (not formula but practical method)?
I could not understand why this value better for CTMNA than octogene (4.7 and 4.2 mm - from "Chemistry and technology of HE" by Orlova. 3-d edition 1981. L.)... Is it at the same density?

I'm planning on making some imaginary RDX and I'm wandering if yellow, white fuming nitric acid needs urea, and how much would go into 345ml of this acid I think someone posted that it's 6% volume of the acid but my acid according to someone doesn't have that much nitrogen oxides. I will follow mega's procedure and I will use 345ml because he says to use 335 ml of 100% acid and I have 97%, so the extra ten make up for that.

------------------
"Friends don't let friends play with
Nitrogen Triiodide"

I'll admit that I haven't got round to doing this myself yet, but no one else seems ot be running forward with answers so I'll try to help. I'd add a small amoutn of urea, leave it for a bit and add more if necessary, judging on the amount (if any) change.

Personally, I'd try the air method first - set the beaker in front of a fan so that the air blows accross the top the beaker. This should work, or maybe *gentle* bubble are into the HNO3 with an aquarium air pump?

Thanks man, I'll take a go at it tommorrow, and I swear if I have a run away reaction I'm gonna... go on a cursing spree and try again http://theforum.virtualave.net/ubb/smilies/wink.gif

------------------
"Friends don't let friends play with
Nitrogen Triiodide"

(Contents of Dream)
Well, yesterday I tried like I said, I followed mega's procedure, I put the 345ml nitric acid in the beaker. I wasn't sure how much urea to put in the acid, so I put in 10g, I went away measuring out the hexamine and when I came back the acid was perfectly clear and I was happy. I put the beaker in an ice bath and very slowly added the hexamine, 75g, every time I added some it made a fizzing sound and a lot of white fumes come up, the same happened when I was adding the urea. The temperature was kept at 25C the during the addition, once all of it dissolved I heated it gently and slowly on a hotplate to 55C, kept it there for five minutes, I cooled it to 20C and waited 15min then poured it in a gallon glass jug that had 4 times its volume of cool water and immediatly I could see the solution turn milky white and I let it sit there overnight. Today I filtered it, washed it, dried it, and now I just weighed it... Guess what... a measly 10.7 grams!!!

I did everything right except having 100% acid, as you know I had 97% and the urea probably made it a bit less concentrated.
I guess I wasted a lot of time distilling.
I have 100ml nitric acid left, I'm gonna try PETN tommorrow with that acid and 25g pentaerythritol, it should be more forgiving of my 97% acid, it's not as anal a reaction as RDX.

Next time I try RDX I'm going to try the reaction with NH4NO3, I can then use my 97% nitric, and I get more RDX.

I'm going to mix my 10.7g RDX with some really nifty silicone putty that the hospital gave me for physical therapy after I cut my tendons with a knife...
One day, not this last summer but the one before that, I was playing with my spudgun and I was going to cut a potato in half, so I put the potato in my left hand and holding my M-16 bayonet in the other started pushing down, the bayonet is thick and sharp even though it's not supposed to be sharp as a bayonet, instead of slowly cutting through it, the potato split and the bayonet shot right through and hit my fingers, it didn't hurt, and I put my hands to my side and my friend was just staring at my hand, so I looked and could see my tendons, bone, and everything in my left index and middle finger, and my hand quickly filled with blood... my fingers and tendons got stitched up and I had to there a couple times a week to be able to move my fingers and they gave me this cool putty I had to squeeze that has really great properties. Fun to play with and great for plastique. So go cut up your hand and get some. That summer I made explosives single handed.( I had to wear this gay contraption with pullies and rubber bands) And I have a Z shaped scar on each finger from where doctors(butchers) made incisions. If I would have cut my hand the other way I could hav had the SS symbol on my two fingers.

(Sorry to tell you my life story)
------------------
"Friends don't let friends play with
Nitrogen Triiodide"

[This message has been edited by CyclonitePyro (edited 12-13-2001).]

Well I can point to two things you should have done differently:
- Use hexamine dinitrate in stead of hexamine. ( same stochiometric amount ).
- Don't let the solution stand longer than prescribed at any point in the process.

this may be a stupid question but here it goes:

can i nitrate hexamine dinitrate with crappy HNO3 or a H2SO4/KNO3 mix to RDX?

if so then you could make hexamine dinitrate by doing the procedure for r-salt but only use KNO3 instead of KNO2 then you could nitrate it to rdx and you wouldn't need any 98-100% white HNO3. am i right?

edit: there must be a flaw here, sounds too easy.

------------------
"To live is to suffer, to survive... well thats to find meaning into suffering." -DMX

[This message has been edited by Madog555 (edited December 15, 2001).]

i think H2SO4 stops the formation of RDX.

Sulfuric acid decomposes rdx and hmx. Sodium hydroxide also decomposes rdx but not hmx ( at least in moderate concentrations ). According to Urbanski rdx decomposed in sulfuric acid is a nitronium ion source, and the solution can be used to nitrate aromatics.

<font face="Verdana, Arial" size="2">can i nitrate hexamine dinitrate with crappy HNO3 or a H2SO4/KNO3 mix to RDX?</font>There has been an incredible amount of discussion on this before, that's what the Search button is for! For the former question, usually, yes, but it depends on how "crappy" the nitric is. And the latter, NO, sulfuric acid decomposes fragile intermediates. The only reason one would want to use the hexamine dinitrate to RDX method is very minorly increased yields.
<font face="Verdana, Arial" size="2">if so then you could make hexamine dinitrate by doing the procedure for r-salt but only use KNO3 instead of KNO2 then you could nitrate it to rdx and you wouldn't need any 98-100% white HNO3. am i right?</font>First of all HNO₂ will form if an aqeous solution of KNO₂ has a low pH (hence the use of the HCl). The same will NOT happen for KNO₃! Secondly, hexamine dinitrate is an ionic compound of protonated (basic) hexamine and NO₃ anions, basically ammonium nitrate with hexamine instead of ammonia, whereas R-Salt is like RDX with NO groups instead of NO₂. There is a vast difference. Thirdly, 98% white nitric acid (100% white is impossible, or at least extremely unstable) is not required. 90% will do adequately, you can get away with even as low as 85%, with diminished yields.

------------------
Live free or die! | http://codemason.cjb.net

Microtek: Sure that's interesting, but hardly useful. Who would trade a good batch of RDX for some TNT?

------------------
Live free or die! | http://codemason.cjb.net

Well then why did I get such a shity yield with 96% white nitric acid.
The gods of chemistry really hate me I guess?

(Maybe you didn't make a proper sacrifice to the right GmOD. Read my post in the NG thread by stiler to get the joke. NBK2000)

------------------
"Friends don't let friends play with
Nitrogen Triiodide"

[This message has been edited by nbk2000 (edited December 16, 2001).]

Madog555 - in response to your question about nitrating hexamine dinitrate with H2SO4/KNO3 mixture:

Try this out,
Preparation of RDX from Hexamethylenetetramine Dinitrate.
Prepare a solution by combining alternately and proportionately ,27 gram of hexamethylenetetramine dinitrate and 68 grams of 90% H2SO4 at 8-15 C for 30 minutes.Stir it at 15C for 45 minutes.
Pour this mixture into 110 grams of preferably 99+% nitric acid slowly within the 10 minute period,while maintaining temperature at 10C.Then let the temperature rise to 25C and stir for 25 minutes.
Pour it into 10 times its weight of ice and water mixture.This will precipitate crude cyclonite...

Posted by Cutefix originally. He also said a H2SO4/XNO3 mixture could be used, with yields around 30%.

Codemason - metal/ammonium nitrates in a soln. with a low pH will form HNO3, I've made hexamine dinitrate with hexamine, NH4NO3 and HCl.

Mr Cool: There is no problem with forming hexamine dinitrate from hexamine + H₂SO₄ + HNO₃, so why aren't there any methods utilizing these as the starting materials? Because the intermediates are too fragile for use with H₂SO₄. Making RDX this way seems to be a pipe dream to me.

[quote]Codemason - metal/ammonium nitrates in a soln. with a low pH will form HNO3, I've made hexamine dinitrate with hexamine, NH4NO3 and HCl.<hr></blockquote>Well, yes, I forgot about that. I apologize to Madog555. But I doubt HNO₃ actually forms, perhaps the the NO₃^- ions take over the Cl^- of a hydrochloride intermediate?

I suppose there are no commonly heard about methods with H2SO4 because the yields are so shite, but as long as you keep the level of H2SO4 low, the rate of decomposition will be fairly low, and you'll still get some RDX out. Just don't expect more than 10% on a small scale, doing it in a home-made lab!

In the solution of HCl and KNO3 everything disosciates (sp? right word?!) into H3O+, Cl-, NO3- and K+ ions, but I suppose in this case the hexaminium (?) ion forms rather than the hydroxonium. So it has the same effect as a solution of nitric acid and potassium chloride, or in this case hexamine dinitrate and KCl, and the Hex. Din. pptes. out because it's the least soluble combination I guess.
But no, HNO3 molecules don't actually form, since it's in an aqueous soln., it just has the same effect as dil. HNO3.

To a_bab,

you said:

And with ammonium nitrate:

C6H12N4 + 4 HNO3 + 2 NH4NO3 --&gt; 2 C3H6N6O6 + 6 H2O

According to this equation:

140 g of hexamine + 252 g (168 ml/) of NA + 160 g of AM to give theoritically 444 of RDX.

If we ignore the quantity of NA (as I think we will need much more) using the above ratios of hexamine and AM is new to me , the recipe I use is 5 g hexamine + 48 g AM with 57 ml NA. do you think its wise to adjust the ratios according to the above equation ?