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A technology for the preparation of dichloroacetyl chloride, which is applied in the field of preparation of dichloroacetyl chloride, can solve the problems of low yield, long processing time, high pressure, etc., achieve low equipment cost, reduce three wastes, and improve safety Effect
Active Publication Date: 2008-06-11
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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Problems solved by technology
[0002] The synthesis method of dichloroacetyl chloride is currently reported to be oxidized with oxygen as the oxidation source, which requires high pressure and the yield can only reach 89%.
At the same time, the processing time is long, about 15 hours
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example 1
[0013] 1. In a 1000ml tower reactor, put 400g of trichlorethylene, 0.3g of vanadium pentoxide, 0.2g of triphenylphosphine, and 0.6g of ammonium chloride.
[0014] 2. Raise the temperature to 100°C, and pass through dry air at 100°C to react for 11 hours.
[0015] 3. After the reaction was completed, transfer it to a 500ml three-necked flask for atmospheric distillation, collect fractions at 108°C, and obtain 461g of dichloroacetyl chloride, a colorless and transparent liquid product, with a purity of 99%.
[0016] 4. The distillate below 105℃ is mainly trichlorethylene, which can be recycled.
example 2
[0018] 1. In a 1000ml tower reactor, put 400g of trichlorethylene, 0.6g of manganese dioxide, 0.2g of triphenylphosphine, and 0.6g of ammonium chloride.
[0019] 2. Raise the temperature to 100°C, and pass through dry air at 105°C to react for 10 hours.
[0020] 3. After the reaction was completed, transfer it to a 500ml three-neck flask for atmospheric distillation, collect fractions at 106°C, and obtain 462g of dichloroacetyl chloride, a colorless and transparent liquid product, with a purity of 99%.
[0021] 4. The distillate below 105℃ is mainly trichlorethylene, which can be recycled.
example 3
[0023] 1. In a 1000ml tower reactor, put 400g of trichlorethylene, 0.6g of manganese dioxide, 0.2g of triphenylphosphine, and 0.6g of ammonium chloride.
[0024] 2. Raise the temperature to 100°C, and pass through dry air at 110°C to react for 9 hours.
[0025] 3. After the reaction was completed, transfer it to a 500ml three-neck flask for atmospheric distillation, collect fractions at 105°C, and obtain 462g of dichloroacetyl chloride, a colorless and transparent liquid product, with a purity of 99%.
[0026] 4. The distillate below 105℃ is mainly trichlorethylene, which can be recycled.
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Abstract
A technique for preparing dichloracetyl chloride is provided. The invention relates to a technique for preparing dichloracetyl chloride as insecticide, which adopts trichloroethylene as raw material and comprises 1) placing trichloroethylene the tower reactor to charge composite catalyst, wherein the weight ratio of the composite catalyst and trichloroethylene is 0.1-1.0: 100, the raw materials are stirred evenly and heated to 100-110 DEG C and the container is aerated by dry air under the temperature to keep 9-11 h; 2) distilling the obtained product of the step one and processing under normal pressure and collecting fraction at 105-108 DEG C, the colorless transparent liquid product dichloracetyl chloride is obtained. The invention uses dry air as oxidizing source, the reaction yield reaches 93.5% and the content is more than 99% through compressing air and oxidizing, thereby fitting for industrialized energy-saving production, reducing three-waste and improving economic benefit. The invention is simple in technique without special requirement of equipment in the processing procedure and low in equipment cost, which improves the security in the processing procedure greatly.
Description
technical field [0001] The invention relates to a synthesis process of an agricultural insecticide dimefen, in particular to a preparation process of dichloroacetyl chloride as an insecticide. Background technique [0002] The currently reported synthesis method of dichloroacetyl chloride uses oxygen as the oxidation source to oxidize, which requires high pressure, and the yield can only reach 89%. This method produces low oxygen utilization rate, low yield and low content, which directly affects the production cost, and at the same time, the amount of three wastes is relatively large, and the safety factor is not high. [0003] The application number of the State Intellectual Property Office is: 95110365.2, and the title is: "A preparation method of dichloroacetyl chloride". The disclosed one uses trichloroethylene as the main raw material and azodiisobutyl ester as the reaction catalyst. Triethylamine is the technical scheme of reaction initiator. Among them, the additio...
Claims
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