megalomania
June 1st, 2003, 12:19 AM
Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-19-2001 09:08 PM
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Hello all,
Here is a excerpt from Pat. # 1,280,612 for those who do not want to down load it!
Benzoyl Chloride
Dry bleaching powder (calcium hypochlorite, or other equivalent hypochlorite,) and toluene are mixed in proportions varying according to the extent of chlorination desired. For example, 200 kilograms of toluene are heated, as in a 'steam jacketed iron mixing kettle to a high temperature, say 900 C. Dry bleaching powder is then slowly added to this, the temperature being gradually raised until it approximate'-s the boiling point of toluene. When 200 kilograms of bleaching powder have been added the mixture is held at the high temperature attained, (i. e., to secure the best results, from 1000 C. to 1050 C.) for about one hour, or, until the reaction is effected, with continuous thorough mixing. The escape of toluene vapor during the operation may be prevented by means of a reflux condenser fitted to the mixing vessel.The resulting mixture is then cooled down and allowed to settle and as much oil as possible is siphoned off from the top. The oil left adhering to the line residue is then removed by steam distillation and added to that siphoned off. In this way 200 to 210 kilos of oil are obtained, having a specific gravity of .940 to .960 at 200 C. and containing from 30 to 35 per cent. of benzyl chloride and from 70 to 65 per cent. of toluene. These can then be separated by fractional distillation. A higher percentage of chlorinated product can be obtained by using a greater proportion of the bleaching powder. In this case, however, some benzal chloride and benzo-trichloride will be formed.
Or, if desired, sufficient bleaching powder
may be added to convert all the toluene directly to benzal chloride and benzo-trichloride and the resulting mixture of lime and the chlorides can be converted into benzaldehyde and benzoic acid by boiling with water.
P.S., Please note that the amounts are for commercial quanities, so for lab use, make them as required for your needs. The ratio's are one to one!
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[This message has been edited by Alchemist (edited April 20, 2001).]
nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 04-19-2001 09:33 PM
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I'm sure this is very interesting, but you need to post a lab scale, not industrial scale, sized reaction. You can find one in the organic synthesis series or vogels organic techniques.
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"The knowledge that they fear is a weapon to be used against them"
Go here to download the NBK2000 website PDF.
Go here to download the NBK2000 videos.
Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-20-2001 12:40 PM
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Your VERY correct nbk2000. I am sorry about the error!
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-19-2001 09:08 PM
--------------------------------------------------------------------------------
Hello all,
Here is a excerpt from Pat. # 1,280,612 for those who do not want to down load it!
Benzoyl Chloride
Dry bleaching powder (calcium hypochlorite, or other equivalent hypochlorite,) and toluene are mixed in proportions varying according to the extent of chlorination desired. For example, 200 kilograms of toluene are heated, as in a 'steam jacketed iron mixing kettle to a high temperature, say 900 C. Dry bleaching powder is then slowly added to this, the temperature being gradually raised until it approximate'-s the boiling point of toluene. When 200 kilograms of bleaching powder have been added the mixture is held at the high temperature attained, (i. e., to secure the best results, from 1000 C. to 1050 C.) for about one hour, or, until the reaction is effected, with continuous thorough mixing. The escape of toluene vapor during the operation may be prevented by means of a reflux condenser fitted to the mixing vessel.The resulting mixture is then cooled down and allowed to settle and as much oil as possible is siphoned off from the top. The oil left adhering to the line residue is then removed by steam distillation and added to that siphoned off. In this way 200 to 210 kilos of oil are obtained, having a specific gravity of .940 to .960 at 200 C. and containing from 30 to 35 per cent. of benzyl chloride and from 70 to 65 per cent. of toluene. These can then be separated by fractional distillation. A higher percentage of chlorinated product can be obtained by using a greater proportion of the bleaching powder. In this case, however, some benzal chloride and benzo-trichloride will be formed.
Or, if desired, sufficient bleaching powder
may be added to convert all the toluene directly to benzal chloride and benzo-trichloride and the resulting mixture of lime and the chlorides can be converted into benzaldehyde and benzoic acid by boiling with water.
P.S., Please note that the amounts are for commercial quanities, so for lab use, make them as required for your needs. The ratio's are one to one!
------------------
[This message has been edited by Alchemist (edited April 20, 2001).]
nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 04-19-2001 09:33 PM
--------------------------------------------------------------------------------
I'm sure this is very interesting, but you need to post a lab scale, not industrial scale, sized reaction. You can find one in the organic synthesis series or vogels organic techniques.
------------------
"The knowledge that they fear is a weapon to be used against them"
Go here to download the NBK2000 website PDF.
Go here to download the NBK2000 videos.
Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-20-2001 12:40 PM
--------------------------------------------------------------------------------
Your VERY correct nbk2000. I am sorry about the error!