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Technique for preparing trichloromethyl chloroformate

A technology of trichloromethyl chloroformate and methyl chloroformate is applied in the field of new technology for preparing trichloromethyl chloroformate, and can solve the problems of low yield, incomplete conversion of methyl chloroformate, incomplete illumination and the like

Inactive Publication Date: 2007-12-12
梁建忠
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing trichloromethyl chloroformate also uses methyl chloroformate as a raw material, and under the light of a lamp (fluorescent lamp), a tube with several rows of small holes is passed into the material for light chlorination. This process is due to incomplete light. The yield is low, and methyl chloroformate cannot be completely converted into trichloromethyl chloroformate, which still has an impact on the following synthesis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] First put 1000 kg of methyl chloroformate into the reaction kettle, add 900L of toluene, turn on the jacket cooling water, connect the jet pump and the chlorine system, start the jet pump, adjust the flow of chlorine to keep the reaction temperature not exceeding 60°C, and then The reduction reaction of chlorine gas is also close to complete. When 2245 kilograms of chlorine gas measured are passed through, the temperature suddenly drops to 39 ° C, which is the end of the reaction. It is properly heated to 65 ° C to obtain the toluene solution of the product trichloromethyl chloroformate. Its content is 69.65%.

Embodiment 2

[0010] First put 1000 kg of methyl chloroformate into the reaction kettle, add 1350L of toluene, turn on the jacket cooling water, connect the jet pump and the chlorine system, start the jet pump, adjust the flow of chlorine to keep the reaction temperature not exceeding 65°C, and then The reduction reaction of chlorine gas is also close to complete. When 2356 kilograms of chlorine gas measured are passed through, the temperature suddenly drops to 42°C, which is the end of the reaction. Properly heat to 65°C to obtain the toluene solution of the product trichloromethyl chloroformate. Its content is 62.56%.

[0011] Implementation three

[0012] First put 750 kg of methyl chloroformate into the reaction kettle, add 1350 L of toluene, turn on the jacket cooling water, connect the jet pump and the chlorine system, start the jet pump, adjust the flow of chlorine gas to keep the reaction temperature not exceeding 62 °C, and then The reduction reaction of chlorine gas is also close...

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Abstract

The invention relates to a method for preparing intermediate compound diphosgene for pesticide and medicine. It comprises following steps: taking methyl chloroformate as raw material, toluene as disslovant, injecting chlorine gas into pump with sepecial glass injecting pump, the proportion among methyl chloroformate, chlorine and toluene is: 1: 3.05- 3.5: 1- 2, stopping injecting chlorine gas when the reaction temperature reduces rapidly, heating to remove chlorine gas and getting product. The product content is between 50%- 70%.

Description

technical field [0001] The invention relates to a preparation process of trichloromethyl chloroformate (commonly known as: Shuangguang) which is an intermediate of pesticide and medicine Background technique [0002] Existing trichloromethyl chloroformate also uses methyl chloroformate as a raw material, and under the light of a lamp (fluorescent lamp), a tube with several rows of small holes is passed into the material for light chlorination. This process is due to incomplete light. The yield is low, and methyl chloroformate can not be completely converted into trichloromethyl chloroformate, which still has an impact on the following synthesis. Contents of the invention [0003] Purpose of the present invention is exactly in order to overcome above defect, and illumination is complete, has increased chlorine and methyl chloroformate effective collision, thereby makes methyl chloroformate can react completely. [0004] Technical solution of the present invention: [0005...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C71/00A01N37/02A61K31/19
Inventor 梁建忠
Owner 梁建忠
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