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View Full Version : RDX "E" procedure - mistake ?


BLASTER
August 18th, 2001, 06:53 PM
Hi guys.
Because I found good source of cheap acetic acid anhydride and paraformaldehyde, decise to make cyclonite with E process. First done some calculations for determination approximate ammounts of chemicals needed to buy. And at this point I found some strange thing. Look below.

...plant scale is 63-65%calculated as formaldehyde on a laboratory scale a yield of up to 80% may be obtained.
To produce 100kg of cyclonite requires
630-635 kg of paraformaldehyde
1800 kg of ammonium nitrate
5000-5100 kg of acetic anhydride containing about 19 kg of boron fluoride.
According to the German data the product contains;
93.4% of cyclonite
6.0% of octogen
0.5% of the acetyl derivitive...

From equation 3CH2O+3NH4NO3+6(CH3CO)2---->(CH2N*NO2)3+12CH3COOH
I've got this ideal results:

40.6g paraformaldehyde
108.1g AN
275.8g acetic acid anhydride
for 100g of cyclonite

If I account with 63% yield and some losses, plant result are still too far from mine and looks really poor. Is there some mistake in original text (100kg - 1000kg)? 7430g of input chemicals to make 100g of cyclonite? It's joke or something?

Regards

BLASTER

Lagen
August 18th, 2001, 07:37 PM
Hi Blaster aka HMX! Yes it should be 1000kg of cyclonite. But if you are Czech you should know that... All the Czech sources state the correct figure.

Tony Montana
August 18th, 2001, 11:13 PM
Good cheap Acetic Anhydride sounds good! where would you get this?

BLASTER
August 19th, 2001, 08:01 AM
Hi Tony
Take a trip to Europe and you can got it.

stanfield
August 19th, 2001, 04:01 PM
I did a search about paraformaldehyde :
one guy said that it can be made by boiling down formaldehyde and the other one said he got nothing with this method...


so, is there a way to produce paraformaldehyde ? (I want a PRECISE recipe with all steps...)

any replies are more than welcome !

stanfield
August 19th, 2001, 04:03 PM
I forgot to said that I live in France, so, BLASTER, if you live in Europe too, tell me where you get your paraformaldehyde...

thanx !

Lagen
August 19th, 2001, 09:35 PM
Hmmm... Cheap good acetic anhydride somewhere near me? Lemme guess... It's this one (http://www.lachema-nera.cz/katalog_pdf/chem_a.pdf)! (On page 4, the "pure" grade.) I know a few dealers for it, the average price is $4.10/liter tax incl.

BLASTER
August 20th, 2001, 02:59 PM
Lagen, try here http://www.vltava2000.cz/ipl/
1000ml for only 166 CZK (incl. tax)

Lagen
August 20th, 2001, 03:12 PM
I was thinking rather about the one from ML Chemica (http://www.mlchemica.cz/), it's 137.50 for 900 ml. BLASTER, have you already ordered anything from Vltava? Do they make any trouble? I heard they require a copy of ID sent to them first.

nbk2000
August 20th, 2001, 04:15 PM
Paraformaldehyde is used as a disinfectant/deodorant in chemical camping toilets. $8US/pound. Try looking in stores that sell RV or camping supplies. It's a granular powder.

------------------
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Go here (http://members.nbci.com/angelo_444/dload.html) to download the NBK2000 website PDF.

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Lagen
August 20th, 2001, 04:34 PM
Thanks for quoting the price, NBK. Now I am sure, that using paraformaldehyde for RDX synthesis is a bit costly. I don't know about other people's sources, but for me the equivalent amount of hexamine would be 3 times cheaper.

Mr Cool
August 20th, 2001, 05:27 PM
But the yields when using the hexamine/HNO3 method are shite.
And $8 for a pound isn't too bad for paraformaldehyde!

Lagen
August 20th, 2001, 06:22 PM
The yield is bad when using the direct nitrolysis method (or "N-nitration"). But I'm using the K-method and the yield is in the range 60-70% theory. There is another problem with the paraformaldehyde and that's moisture content. Lab grade para contains about 5% water and the technical grade you are talking about usually above 10%. This cannot be removed by any means - the water is chemically bound within the polymer.

[This message has been edited by Lagen (edited August 20, 2001).]

BLASTER
August 22nd, 2001, 02:10 PM
To: Lagen
Can you send me your email address?

10fingers
August 22nd, 2001, 08:29 PM
*

[This message has been edited by 10fingers (edited October 25, 2001).]

cutefix
August 23rd, 2001, 02:31 AM
The common way of recovering nitric acid in RDX production is to treat it with ammonia in order to form ammonium nitrate.
How about adding equivalent percentage of phosphorus pentoxide in the reaction mixture in order to compensate for the moisture of the paraformaldehyde.In the nitration of these nitramines you have to do it in an anhydrous environment,that is why you have to use utmost pure nitric acid.

Dhzugasvili
August 27th, 2001, 03:24 PM
To Blaster:

First of all (1) what was your yield in grams with the E process? I have tried this and also got a shit yield, and I think it has to do with adition/ or lack of boron trifluoride, but MOST IMPORTANTLY regulating the temp. I did the reaction as specified by mega, heated AN with ACetic Anhydride to 90degC and then removed from heat and began adding paraformaldehyde keeping temp between 80 and 90 deg C. This was probably where my fuckup was.
2) Today I made RDX from 100ml of 99% nitric acid homemade from distillation without vacuum and got a fucking amazing yield. When about 40g of hexamine was added I stopped, heated to 55degC for 10 min and put in twice vol of cold water and got about 30g RDX estimate have not weighed yet.

BLASTER
August 28th, 2001, 02:48 PM
Here is detailed procedure for E process, taken from some swedish textfile, not yet tested.

Tillverkningsprocedur:

1. Väg upp 7.6 g paraformaldehyd och 21 g torrt ammoniumnitrat.

2. Upphetta 52 ml ättiksyraanhydrid i en trehalsad reaktor utrustad med
termometer, omrörningsmagnet och pulvertratt till 80øC. Man kan
eventuellt koppla till en Liebig kylare för att kondensera gaser som
bildas. Till detta tillsätter man ammoniumnitratet.

3. Gör under tiden i ordning ett kylbad av is/snö och vatten.

4. Sätt reaktorn ovanför kylbadet på en magnetomrörare. När temperaturen
nått 70 C tillsätts lite paraformaldehyd. Temperaturen kan nu sjunka
några grader. För att motverka detta skall man försiktigt blåsa på
reaktorn med en värmepistol (man kan också flytta över reakton i en
värmemantel) tills dess att temperaturen stigit till 70øC igen. Var dock
försiktig här. Värmen kan stiga mycket fort om reaktionen kommer igång,
så kyl så fort temperaturen stiger över 70øC. Försök nu att hålla
temperaturen mellan 60 och 70øC. Sjunker den under 65øC och ingen mer
värme tillförs kommer reaktionen sakta stanna av.
OBS! Använder du värmepistol måste du se till att du har en kylare på
reaktorn! Gaserna som bildas är mycket brandfarliga!

5. När allt paraformaldehyd är tillsatt skall temperaturen hållas i
intervallet i ytterligare 20 min med magnetomröraren påslagen. Låt den
svalna till rumstemperatur och filtrera bildat RDX. Denna tvättas med
åtskilliga mängder kallt och varmt vatten. När tvättvattnet är neutralt
är du klar. Även här är det vettigt att begagna sig av sugfiltrering!
Utbytet bör ligga på 8-9g