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Author Topic:   Acetic Anhydride
dlwdaw
Frequent Poster
posted September 13, 1999 07:13 PM     Click Here to See the Profile for dlwdaw   Click Here to Email dlwdaw     
how could I make Acetic Anhydride. could i distill Acetic acid(vineger is 4% acetic acid I would have to have a shitload of it.). and would acetic acid evaporate before or after the water in it. if it would go before. then i could use a distilling apparatus, would plastic be able to handle pure Acetic acid.

if anybody has a file tell me and I will email you and you can reply to it.

thanks in advance

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nbk2000
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posted September 13, 1999 10:44 PM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     
You'll never get anhydride by distilling vineger.You have to pass ketene gas through the glacial acetic acid to make anhydride. I can send you the process if you e-mail me your e-mail address. Send it to "nbk2k@yahoo.com"

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



*Igenx*
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posted September 13, 1999 10:59 PM     Click Here to See the Profile for *Igenx*   Click Here to Email *Igenx*     
I thought that acetic acid decomposes apon heating? The chem book I was loking at a couple days ago said so, but I don't know if it was accurate (or if I remember it corectly)


megalomania
Administrator
posted September 14, 1999 05:42 AM     Click Here to See the Profile for megalomania   Click Here to Email megalomania     
There is about a dozen different ways of making acetic anhydride and the ketene is very dangerous. Ketene is extremely toxic, unless you have the equipment for it, you will probably die. Other methods abound, but making it from acetic acid is more along the lines of availability. There are quite a few steps, however. Phosphorus, chlorine, sodium hydroxide, and vinegar are needed. All can be gotton too. The ketene method would be nice IF the instructions are clear, concise, accurate, and feasible. Why don't you post the data, please

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nbk2000
Moderator
posted September 14, 1999 02:52 PM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     
Ask and ye shall recieve.

ACETIC ANHYDRIDE MFG.

Acetic anhydride is a common industrial chemical. It is used for
synthetic polyester manufacturer. It is a highly dehydrated acetic acid
compound. lt is dehydrated by the addition of ketane gas to acetic acid.
The acetic acid produced by the "E" process as a by product is fortified to
it's original anhydride form by the addition of this ketane gas after
filtering out the product from the reaction liquid. Acetic acid is also
readily available from photo developers as a common photography chemical.
Acetone is available from hardware stores or paint stores as a common
solvent. This process reacts the acetone by heat into the necessary ketane
gas and it is subsequently absorbed by acetic acid to form the acetic
anhydride product. This is attractive due to the ability to recycle the
chemicals for other batches.
CAUTION: Acetic anhydride is a caustic dangerous chemical. It's
vapors are harmful and should be avoided. All contact should be avoided. It
is also highly flammable and should be used with the utmost caution. Wear
appropriate protective clothing.

PROCESS-

Acetic anhydride is produced by absorption of ketane vapors in
acetic acid. Acetone is injected into a chrome/iron alloy pipe through one
end equipped with a feed valve and assembly. This pipe is previously purged
with argon or nitrogen. The pipe is heated to 650 to 670 degrees C. This
heating can be done by electric heat with a thermostat or by a coal or gas
fired oven. The injection of acetone into the reaction tube is begun when
the proper temperature is reached. The other end of the pipe is attached
to a stainless steel 3/8" tubing. This tubing is placed through a two hole
stopper in a gallon jar placed in a salted ice bath. This is to collect all
unreacted acetone. In the other hole in the stopper on this bottle is
placed a second stainless steel tubing. This goes to another gallon jar
through a two hole stopper. In this jar is placed the acetic acid. The
second hole in this stopper is placed in line for venting purposes. This
line is placed outside or in a safe place for the poisonous fumes to go.
Acetone is injected slowly into the chrome/iron pipe @ 650 to 670
degrees C. This will react approximately 15-25% of the acetone into
ketane. The vapors from the reactor is directed into the first bottle. The
unreacted acetone will collect here. The ketane vapor will continue through
the tubing to the next jar. The ketane vapors are absorbed here by the
glacial acetic acid. These vapors are absorbed until the density of the
liquid is 1.08 @ 20 degrees C. This is checked by a hydrometer placed in
the glacial acetic acid. At the time this specific gravity is reached the
material in the second jar is acetic anhydride. If glacial acetic acid is
used from previous "E" process filtering then the acetic anhydride will
need to be filtered to remove the remaining type "B" R.D.X.
CAUTION: Acetone is highly flammable. Great care is needed to
ensure total absence of air in the reactor prior to injection of acetone.
Failure to do this can result in an explosion. The whole reaction should be
done with very good ventilation.

Hope this is informative.

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



nbk2000
Moderator
posted September 14, 1999 02:55 PM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     

Take 2.

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



nbk2000
Moderator
posted September 14, 1999 02:58 PM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     
Fuck it. Here's the link to go get it. http://www.50megs.com/nbk2000/weaponsandtactics/anhydride.jpg

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



nbk2000
Moderator
posted September 14, 1999 03:02 PM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     
You'll have to type in the link into your browser'cause my server doesn't allow linking from the forum apparently. Sorry about that.

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



sharky
Frequent Poster
posted September 14, 1999 10:01 PM     Click Here to See the Profile for sharky   Click Here to Email sharky     
In mega's method for concentrating acetic acid, at what temperature does the sulfuric acid and sodium acetate mixture break down?

Also, could this "glacial" acetic acid be used in the manufacture of RDX or does it have to be pure anhydrous?

nbk2000
Moderator
posted September 15, 1999 01:47 AM     Click Here to See the Profile for nbk2000   Click Here to Email nbk2000     
Anhydrous.

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"The knowledge that they fear is a weapon to be used against them." www.50megs.com/nbk2000



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