Anthony
March 17th, 2003, 07:20 PM
shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 19, 2001 05:21 PM
--------------------------------------------------------------------------------
This method was worked out by Ebele,and known as the "E-method"in Germany.The same method was also invented indepenently by Ross and Schiessler in Canada in 1940.In this process paraformaldehyde and ammonium nitrate indergo dehydration under the influence of acetic anhydride with the formation of cyclonite according to the equation;
3CH2O+3NH4NO3+6(CH3CO)2---->(CH2N*NO2)3+
12CH3COOH
The studies of Wright and Winkler led to the conclusion that this method involves two essential steps.
THe first is the synthesis of hexamethylenetetramine in acetic anhydride from paraformaldehyde ans ammonium nitrate:
6CH2O+3NH4NO3+3(CH3CO)2O-->C6H12N4+4HNO3+6CH3COOK
THe second step is the known nitrolysis:
C6H12N4+4HNO3-->(CH2N*NO2)3+NH4NO3+3CH2O
The advantage of this method lies in the fact that the preparation of cyclonite is accomplished without using hexamine and nitric acid so that the dangers of nitration are avioded.On the other hand acetic anhydride is required,which is rather expensive.
This method is safe on condition that it is conducted as described below,by adding the reactants to the previously warmed acetic anhydride.Otherwise,the exothemic nature of the reaction may cause an explosion.It is therefore inadmissible to mix the reactants and heat up the mixture,since this causes too violent a reaction.Addition of boron fluoride to the mixture promotes the initiation of reaction and increase its saftey.
It appears that apart from cyclonite,octogen,a N-acetyl derivative and a number of nitromines,mainly chain compound,less stable than cyclonite,are also formed by thid method,in side reactions.Hence the cyclonite obtained has a relatively low melting point(190-195.c)and may be less stable than that prepared by other methods.The conduct of the reaction in the presence of boron fluride reduces the number of by-products formed.
Manufacture at Bobingen was on the following lines.A reactor of aluminium or stainless steel(capacity 1.2m3)is filled with acetic anhydride and then 0.4%of BF3 is added.Acetic anhydride is warmed to 60-65.c and at this temperature ammonium nitrate and paraformaldehyde are added gradully.Due to the high temperature and the presence of boron fluride the reaction starts at once and heat is evolved.The heating is then turned off and the temperature maintained by cooling,within the range 60-65.c.The addition of the reactants requires approximately 6hr,after which the contents of the reactor are cooled to 20.c.The precipitated cyclonite is separated from the solution on a vacuum filter.The by-products remain in the spent liquor.
160kg of cyclonite are obtained from each reactor.The output from a number of reatore,amounting to about 800kg,is stabilized by boiling in an autoclave at 140.c
The spent acid is distilled in order to separate acetic acid.The paste containing cyclonite and by-products that accumulate on the bottom of the retort is removed continously,through a syphon overflow.The greater part of this mass(about 80%) is dissolved in acetic anhydride and returned to the reactor while the residue(about 20%) is mixed with ammonium nitrate to make cheap explosives.
Acetic anhydride is prepared from distilled acetic acid by the ketene method with ethyl phosphate as a catalyst.The water from the first cyclonite wash on the vacuum filter contains on average 20% of acetic acid with is recovered by extration with ethyl acetate.Thr yield of cyclonite on a p;lant 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
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted February 19, 2001 07:06 PM
--------------------------------------------------------------------------------
hey, you're doin' great jobs here.....
is there anyway you post the whole thing in zip/pdf/gif whatever somewhere....
since the idea of save us starts to get me lamer
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 20, 2001 07:08 AM
--------------------------------------------------------------------------------
I like this method...
Maybe it's more easy...
Anyway the problem is with getting the Acetic Anhydride!!!!
Obtaining it from Acetic Acid is pain.
As you said it's expensive too.
Paraformaline you can get it by boiling the formaline (37% formaldehyde) to evaborate the water...then leave it to cool down.
shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 20, 2001 08:58 PM
--------------------------------------------------------------------------------
I am currently copying the book for a member,and hopefully he,she,or they can find a way to publish the book on the net.I cannot as I dont know fuck all about computers.
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 21, 2001 01:29 AM
--------------------------------------------------------------------------------
Shady could you email me the book when you finish it?
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 24, 2001 01:31 AM
--------------------------------------------------------------------------------
Which method is the best?
Faster, Easier, Less $, Gives more RDX
Foxtrot83
Frequent Poster
Posts: 70
From: USA
Registered: OCT 2000
posted February 24, 2001 01:38 AM
--------------------------------------------------------------------------------
What book is shady mutha copying from?
Also, can someone tell me what the hell is this damn sprinks.about.com shit that keeps on popping up when i click anything on the forum?
------------------
~Semper Fi~
Foxtrot83
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 19, 2001 05:21 PM
--------------------------------------------------------------------------------
This method was worked out by Ebele,and known as the "E-method"in Germany.The same method was also invented indepenently by Ross and Schiessler in Canada in 1940.In this process paraformaldehyde and ammonium nitrate indergo dehydration under the influence of acetic anhydride with the formation of cyclonite according to the equation;
3CH2O+3NH4NO3+6(CH3CO)2---->(CH2N*NO2)3+
12CH3COOH
The studies of Wright and Winkler led to the conclusion that this method involves two essential steps.
THe first is the synthesis of hexamethylenetetramine in acetic anhydride from paraformaldehyde ans ammonium nitrate:
6CH2O+3NH4NO3+3(CH3CO)2O-->C6H12N4+4HNO3+6CH3COOK
THe second step is the known nitrolysis:
C6H12N4+4HNO3-->(CH2N*NO2)3+NH4NO3+3CH2O
The advantage of this method lies in the fact that the preparation of cyclonite is accomplished without using hexamine and nitric acid so that the dangers of nitration are avioded.On the other hand acetic anhydride is required,which is rather expensive.
This method is safe on condition that it is conducted as described below,by adding the reactants to the previously warmed acetic anhydride.Otherwise,the exothemic nature of the reaction may cause an explosion.It is therefore inadmissible to mix the reactants and heat up the mixture,since this causes too violent a reaction.Addition of boron fluoride to the mixture promotes the initiation of reaction and increase its saftey.
It appears that apart from cyclonite,octogen,a N-acetyl derivative and a number of nitromines,mainly chain compound,less stable than cyclonite,are also formed by thid method,in side reactions.Hence the cyclonite obtained has a relatively low melting point(190-195.c)and may be less stable than that prepared by other methods.The conduct of the reaction in the presence of boron fluride reduces the number of by-products formed.
Manufacture at Bobingen was on the following lines.A reactor of aluminium or stainless steel(capacity 1.2m3)is filled with acetic anhydride and then 0.4%of BF3 is added.Acetic anhydride is warmed to 60-65.c and at this temperature ammonium nitrate and paraformaldehyde are added gradully.Due to the high temperature and the presence of boron fluride the reaction starts at once and heat is evolved.The heating is then turned off and the temperature maintained by cooling,within the range 60-65.c.The addition of the reactants requires approximately 6hr,after which the contents of the reactor are cooled to 20.c.The precipitated cyclonite is separated from the solution on a vacuum filter.The by-products remain in the spent liquor.
160kg of cyclonite are obtained from each reactor.The output from a number of reatore,amounting to about 800kg,is stabilized by boiling in an autoclave at 140.c
The spent acid is distilled in order to separate acetic acid.The paste containing cyclonite and by-products that accumulate on the bottom of the retort is removed continously,through a syphon overflow.The greater part of this mass(about 80%) is dissolved in acetic anhydride and returned to the reactor while the residue(about 20%) is mixed with ammonium nitrate to make cheap explosives.
Acetic anhydride is prepared from distilled acetic acid by the ketene method with ethyl phosphate as a catalyst.The water from the first cyclonite wash on the vacuum filter contains on average 20% of acetic acid with is recovered by extration with ethyl acetate.Thr yield of cyclonite on a p;lant 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
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted February 19, 2001 07:06 PM
--------------------------------------------------------------------------------
hey, you're doin' great jobs here.....
is there anyway you post the whole thing in zip/pdf/gif whatever somewhere....
since the idea of save us starts to get me lamer
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 20, 2001 07:08 AM
--------------------------------------------------------------------------------
I like this method...
Maybe it's more easy...
Anyway the problem is with getting the Acetic Anhydride!!!!
Obtaining it from Acetic Acid is pain.
As you said it's expensive too.
Paraformaline you can get it by boiling the formaline (37% formaldehyde) to evaborate the water...then leave it to cool down.
shady mutha
Frequent Poster
Posts: 149
From: australia
Registered: SEP 2000
posted February 20, 2001 08:58 PM
--------------------------------------------------------------------------------
I am currently copying the book for a member,and hopefully he,she,or they can find a way to publish the book on the net.I cannot as I dont know fuck all about computers.
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 21, 2001 01:29 AM
--------------------------------------------------------------------------------
Shady could you email me the book when you finish it?
Detonator
Frequent Poster
Posts: 132
From:
Registered: NOV 2000
posted February 24, 2001 01:31 AM
--------------------------------------------------------------------------------
Which method is the best?
Faster, Easier, Less $, Gives more RDX
Foxtrot83
Frequent Poster
Posts: 70
From: USA
Registered: OCT 2000
posted February 24, 2001 01:38 AM
--------------------------------------------------------------------------------
What book is shady mutha copying from?
Also, can someone tell me what the hell is this damn sprinks.about.com shit that keeps on popping up when i click anything on the forum?
------------------
~Semper Fi~
Foxtrot83