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megalomania
February 28th, 2003, 01:26 PM
^Baphomet^
A new voice
Posts: 31
From: amman,jordan
Registered: OCT 2000
posted December 18, 2000 06:46 PM
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ok here what i`ve done ...
260 ml of aceteic anhydride(from a chemical suply house)was placed in a 1 litre beaker ,105 gm NH4NO3(this one also was pure)was added while stirring ,then when i got the desired tempreture (using a a hot plate and a thermometer )wich is 90C i`ve started to add 38gm of paraformaldehyde(made by evaporating the formaldehyde solution)in a small protions (1/2-1 gram at a time )_.....
well the result was not quit what i was expecting ...here is what happen
-THE NH4NO3 DIDNT DISSOLVE .
-I WAS TOLD THAT WHEN I ADD THE PARAFPRMALDEHYDE THERE WILL BE A FOAMING ...WELL I KEPT ON ADDING AND THERE WASNT ANY SIGN OF A REACTON UNTILL THERE WAS HALF OF THE PARA HAS BEEN ADDED ,THEN .......I GOT A GOD SIZE CLOUD OF GASES AND THERE WAS A HELL SIZE BALL OF FOAMING ,SO I STOPPED THE ADDITION UNTILL THE FOAMING WENT DOWN (AND TILL I COULD SEE WITH MA FUCKED EYES WHAT I WAS GONNA DO WITH THE REST OF THE REACTION), SO WHEN I STARTED TO ADD THE PARA AGAIN ...THERE WASNT ANY SIGN OF A REACTION IN THE SOLUTION AND THE 2ND TIME ADDED PARA IT STAYED AT THE BOTTOM OF THE BEAKER.......SO PLZ GUYS ( ESPECIALY MEGA &PHILOU) I NEED GUIDENESS
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{6@pH0m3t}
do what thou wilt shall be the whole of the law...

[This message has been edited by ^Baphomet^ (edited December 18, 2000).]

[This message has been edited by ^Baphomet^ (edited December 18, 2000).]


jin
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Posts: 111
From: uk
Registered: SEP 2000
posted December 18, 2000 09:26 PM
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maybe there could be water in the ammonium nitrate fucking the acetic anhydride up or you could try useing liquid formaldehyde if you can not get the paraformaldehyde,i thought the temp you should use was 80 c.btw i read somewhere you can use phosphoric acid as a catalyst,not sure about this you better ask someone else.
[This message has been edited by jin (edited December 18, 2000).]


Detonator
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Posts: 132
From:
Registered: NOV 2000
posted December 19, 2000 03:49 AM
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That is exactly the same thing i did guys and i had the same results...!!
So I'm interested to know what is wrong...


Detonator
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From:
Registered: NOV 2000
posted December 20, 2000 12:45 PM
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MMM I hope someone will help us out!!!!


^Baphomet^
A new voice
Posts: 31
From: amman,jordan
Registered: OCT 2000
posted December 20, 2000 03:12 PM
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me too ..................
hello guys ....can any one here ma calling????
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{6@pH0m3t}
do what thou wilt shall be the whole of the law...


BoB-
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From:
Registered: SEP 2000
posted December 20, 2000 04:25 PM
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it would be great if you mentioned *what* your talking about.


^Baphomet^
A new voice
Posts: 31
From: amman,jordan
Registered: OCT 2000
posted December 20, 2000 05:42 PM
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iam talking about the topic smarty.....
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{6@pH0m3t}
do what thou wilt shall be the whole of the law...


Lost
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Posts: 89
From:
Registered: SEP 2000
posted December 20, 2000 05:44 PM
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He means what are you trying to make
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-Lost
<a href="http://www.noneinc.org" target="_blank">http://www.noneinc.org</a>


Detonator
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Posts: 132
From:
Registered: NOV 2000
posted December 21, 2000 03:40 AM
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It's making RDX!!!!!!!!!!!
Why no one answer? did anyone make RDX this way???


10fingers
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Posts: 421
From: USA
Registered: SEP 2000
posted December 21, 2000 09:08 AM
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deleting post.
[This message has been edited by 10fingers (edited March 19, 2001).]


^Baphomet^
A new voice
Posts: 31
From: amman,jordan
Registered: OCT 2000
posted December 21, 2000 11:14 AM
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no......the ammoniun nitrate i used was kept in an airtight container and i also put one of those (silicagel) bag to keep the ammonium nitrate out of moisture and my paraformaldehyde was extremly dry IAM SURE ...

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{6@pH0m3t}
do what thou wilt shall be the whole of the law...


Detonator
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Posts: 132
From:
Registered: NOV 2000
posted December 31, 2000 02:15 AM
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^Baphomet^
Here is the deal,
When you add the para formaline (should be dried) keep stiring...wait then add another portion then wait...now the temp should not exceed 70c so you should have cold water.
If it reaches 70 and more you should put it in the water (or ice) until it gets back to 60c then you add another portion and so on.
watch out the toxic fumes...
after you finish add the water and tara you have your crystals for sure... ;-)
This is for your happy new year...


Mr Cool
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Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted January 02, 2001 11:08 AM
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Just make sure everything is completely anhydrous (and get good ventilation! Acetic anhydride and paraformaldehyde are NASTY substances. Carcinogenic, amongst other things) Other than that I'm not sure what might be wrong. Was the formaldehyde solution a pure chemical reagent, or was it sold as a preservative or something? If it was sold as a preservative, it might contain other things. Make sure you stir very well throughout the reaction, and don't add more stuff until the previous addition has reacted/dissolved.
If I were you I'd use the hexamethylenetetramine / nitric acid / ammonium nitrate reaction. I always get good results with this, although it does contain slightly less octogen (HMX) in the finished product.


PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted January 11, 2001 04:06 AM
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Paraformaldehyde + NH4NO3 + acetic anhydride giving RDX... right but I think to remember you need some anhydrous HNO3 in catalytic quantity to initiate the reaction... for sure acetyl nitrate is an intermediate reactant.You also have to heat the mix between 70-80C not exceeding the last one because of runaway reaction.Anhydrous media is needed because the more diluted the more the risk of runaway is big.
BTW: I do think the quantity you have made is too big for a first trial....dont forget scaling up factors:
cooling will be less effective; so will agitation and thus you may have hot spots of runaway... speed of reaction is multiplied by two each 10C so does the heat release; that means heat increases the speed in those spots and speed increase the heat in the very same place...accelerating ring of reaction leading to exponential instability!
You will not have the time to react efficiently in such a case and 150g RDX is not something I would see explode from 1 meter nor be in the same room.
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o )"


Detonator
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Registered: NOV 2000
posted January 11, 2001 06:41 AM
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PHILOU, it worked without HNO3 it yields about 30grams do you think with the HNO3 it would be better???


PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted January 11, 2001 08:26 AM
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Yes! Your yield is exceptionnaly low as compared to the reactants involved! This process should give you close to 100% conversion based on the paraformaldehyde involved when done correctly of course.Normal process with HNO3 (100%) and hexamine dry give something like 40% yield.
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o )"


Detonator
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Registered: NOV 2000
posted January 11, 2001 08:37 AM
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so where can i get anhydrous HNO3??
You know making HNO3 is pain thats why it's better not to do it...
It takes time and the yiel in labs is not enough...

So what about anhydrous HNO3?


PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted January 11, 2001 11:04 AM
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I already explained a process that might help getting 100% HNO3 by mixing it with plaster....plaster is CaSO4 anhydrous. When it comes in contact with water, it heats and take water as cristallisation water to make gypsum CaSO4.xH2O (unsoluble solid that can be filtered with fiberglass paper). Several processes will allow you to get concentrated HNO3. Better do several ones than a big one since HNO3 boils at 80C and the reaction release a lot of heat; also some of the HNO3 will be lost by capilarity between the cristal grains -except if you have a vaccuum scruber filter what may diminish the loss !
Better also start from the commercial 70% HNO3 because less concentrated ones will lead you to an excessive number of runs.
Once done keep the HNO3 in a wel closed vessel- resistant to HNO3!!!!
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o )"


Detonator
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Registered: NOV 2000
posted January 12, 2001 08:32 AM
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PHILOU You said that the yield shoud be somthing like 100% based on the paraformaldehyde involved, in the process thats in Meag's site. it says that you should use 38g (as i remember) of paraformaldehyde...I've got about 30g RDX it's means the yield is about 80% and this is good?


^Baphomet^
A new voice
Posts: 31
From: amman,jordan
Registered: OCT 2000
posted January 16, 2001 05:47 AM
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thx guyz
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{6@pH0m3t}
do what thou wilt shall be the whole of the law...


PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted January 18, 2001 08:05 AM
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38g paraformaldehyde (-CH2-O-)3 is a trimer or polymer of CH2=O (12+2+16=30g/mole); you thus have 38/30 moles of CH2=O that has to turn into a trimer of CH2=N-NO2 (12+2+14+14+16+16=74g/mole).
Assuming the transformation process is 100% effective then you would have each mole of CH2=O turned in a mole of CH2=N-NO2...what means for 1.2666 mol of (38g)CH2=O you should get 1.2666mol of CH2=N-NO2 what is 1.2666mol*74g/mol= 93.7333g.
Now if you judge 30g of RDX as beeing an exceptional yield, I don't understand you!
It is close to 33% yield and not 80%!!!!
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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o )"


PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted January 18, 2001 08:13 AM
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I understand the misunderstanding here...
yield based on the paraformaldehyde means:
the number of grams of RDX really obtained divided by the hypothetical number of grams you should get if the process is 100% effective (this last one comes from the CH2=O reactant weighted initially).
Yield is not the number of g of RDX / by the number of g of paraformaldehyde...you must always compare apples with apples.
Following this erroneous concept, I should have had a yield of 93.73/38= 246.6% and by definition a yield is comprised between 0 and 100% otherwise we have found the way to produce matter and why anti-matter exists :-) :-p

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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o )"


pete
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Posts: 56
From: u.k
Registered: JAN 2001
posted February 09, 2001 06:33 PM
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Mr Cool, could u give me a full description of the Ammonium nitrate/nitric acid/hexamine process please as i just can't seem to get good yields, Thanks!!!


Mr Cool
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From: None of your bloody business!
Registered: DEC 2000
posted February 10, 2001 07:01 AM
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Put 18 parts by weight of HNO3 (95% or better) into a suitably sized flask. Cool it to 10*C. Then, add 1 part by weight of hexamine, and 10 parts of ammonium nitrate, while keeping the temperature below 15*C. Stir it at this temp. for 10 minutes, and then slowly raise the temp. to 75-80*C. I do this over a period of 30 minutes, and then hold the mixture at this temp. for a further 30 minutes (just a idea: put a reflux column in a one holed stopper, and a thermometer in the other hole, and put this into the neck of the flask. This will allow you to read the temperature, and the reflux column should reduce wastage of HNO3 at this temp. It will also reduce the amount of fumes that are released, which would be good, and it should recycle more of the formaldehyde produced back into the reaction flask where it can react with the ammonium nitrate. I've never tried this though.)
I then cool it by putting the flask into a bowl of ice/water, and cool it down to 10*C and filter it. The solid collected will be mainly RDX, and should be purified in the usual way.
It might also be a good idea to get the remaining acid as cold as possible to precipitate out any more RDX, which can be purified and used, and unreacted AN or hexamine which can be filtered out. Then, you could recycle the left over acid by distilling it, and concentrating it by distilling it with conc. H2SO4 if necessary. This would make the reaction quite efficient.


pete
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Posts: 56
From: u.k
Registered: JAN 2001
posted February 10, 2001 10:17 AM
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Thanks Mr cool, I will give this process a go, if the yeilds are good then this will make a good process for the production of RDX. I have used the NA/hexamine process before to make RDX put the yeilds were bad, the little i did get was very powerful however.