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Author: Subject: Chloroacetone failure
Lestat
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thumbdown.gif posted on 7-6-2004 at 16:03
Chloroacetone failure


I attemped to make a fairly large batch, about a 1/2 liter, however I added a touch too much KMnO4 to the bottle of HCl I was using to generate the Cl and the reaction got a little too violent and sent a few drops of the HCl/KMnO4 solution down the tube for the chlorine to come out.

This seems to have poisoned the reaction completely, no matter how much Cl I pumped in it just would not do it's thing, is there any way to clean up the acetone or should i flush it? :(




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Organikum
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[*] posted on 7-6-2004 at 18:03


Are you sure what you are doing?

What procedure do you follow? Pumping Cl2 into acetone and wait whats going to happen?




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Lestat
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[*] posted on 7-6-2004 at 18:05


Yep, pumping Cl2 into acetone is the method I have been using.



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[*] posted on 7-6-2004 at 20:04


Thats a bad method.
If reaction kicks in the content of your flask will jump all over you.
Add about 1% HCl to the acetone to get it smooth going. Keep the flask in a waterbath to hold it at about 25°C. The reaction is strongly exothermic.

You will cry your eyes out anyways, you know this?




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Lestat
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[*] posted on 7-6-2004 at 20:08


I am COMPLETELY aware of the tendency for ir to fire out of the reaction vessel, I had a shot-glass full (now wouldn't THAT be nasty if some poor shit drank it) launch itself all over my garage, this ofcourse brought with it some first hand experience of the somewhat lachrymatory nature of the stuff...

Why the HCl?, and is there enything other than MgO to stabilize it, would an alkali metal carbonate do the trick?

Basically, the method i've been using is HCl+KMnO4 in a coke bottle with a rubber tube in to dispense the Cl, put the tube into the bottle of acetone and run the hell away :D


I did indeed produce said fountain of chlorinated acetone the first time I tried it, but ive never had problems since, I'm going to include the HCl next time I try it.
Luckily my neighborhood just doesn't seem to care what comes out of my garage, at least within certain limits :D



[Edited on 8-6-2004 by Lestat]

[Edited on 8-6-2004 by Lestat]

[Edited on 8-6-2004 by Lestat]




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[*] posted on 8-6-2004 at 01:47


First: Your method of Cl2 production is wrong. Right would be dropping HCl on KMnO4, not throwing KMnO4 in HCl.
Second: You would produce a fountain of partially chlorinated acetone the way you tried it and not only you but your whole neighborhood will cry its eyes out - afterwards you get in big trouble.

The HCl which has to be added to the acetone before is plain muriatic acid. The 1% refers to weight. Do a small batch if at all.
Thats not funny.
:mad:

[Edited on 8-6-2004 by Organikum]




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