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Production of o-chlorobenzyl dimethyl phosphonate

A technology for the production of dimethyl o-chlorobenzylphosphonate, which is applied in the field of preparation of pesticide intermediates, can solve the problems affecting the development and application of new pesticides with high efficiency and low toxicity, the inability to realize the industrial production of epoxiconazole, and the production process of epoxiconazole Complexity and other issues, to achieve the effect of improving yield and performance indicators, easy operation, and low production cost

Inactive Publication Date: 2005-10-12
泰州市天成化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process of epoxiconazole is complicated, the production route is long, and many raw materials are used. Among them, a new main raw material that plays a key role in its performance index, dimethyl o-chlorobenzyl phosphonate, cannot be produced in China, and has not been seen abroad. According to related reports, therefore, the industrial production of epoxiconazole has not been realized in China so far, which affects the development and application of new pesticides with high efficiency and low toxicity

Method used

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  • Production of o-chlorobenzyl dimethyl phosphonate

Examples

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Effect test

Embodiment 1

[0017] Example 1: Take 470kg of o-chlorobenzyl chloride, 270kg of trimethyl phosphite, 250kg of chlorinated benzene, and 10kg of soda ash, and put them into a 1000L reactor and mix them thoroughly. The feed is normal pressure and 20°C; heat the above raw materials to 95 ℃, react at normal pressure for 80h; then collect low-boiling substances (chlorinated benzene as a solvent) under normal pressure. With the decrease of low-boiling substances, the temperature in the kettle will increase, and auxiliary heating can also be carried out to the kettle. When the temperature is 165℃, vacuum up to -0.06Mpa, continue to extract low boilers; then the reactor is evacuated to -0.05MPa, heated to 195℃, and crude distillation is carried out for 8h; then transfer to the kettle, vacuum -0.05MPa, and heat to 220℃, rectify for 8h; finally, the finished product obtained by rectification is filled (in barrels), and the yield of the finished product is more than 1.3 times the weight of o-chlorobenzyl c...

Embodiment 2

[0018] Example 2: Take 1004 kg of o-chlorobenzyl chloride, 500 kg of trimethyl phosphite, 480 kg of chlorinated benzene, and 16 kg of soda ash, and put them into a 2000L reactor and mix them thoroughly. The feed is normal pressure and 22°C; heat the above raw materials to 150 ℃, react under normal pressure for 25h; then collect low-boiling substances (chlorinated benzene as a solvent) under normal pressure, when the temperature in the kettle is 165℃, vacuumize to -0.06Mpa, continue to extract low-boiling substances; The reaction kettle is evacuated to -0.08MPa, heated to 210°C, and crude distillation is carried out for 2h; then transferred to the kettle, evacuated -0.08MPa, heated to 250°C, and rectified for 2h; finally the finished product obtained by the rectification is filled (in barrels) ), the yield of the finished product is more than 1.3 times the weight of o-chlorobenzyl chloride, and then the reaction kettle is restored to normal pressure and reduced to normal temperatur...

Embodiment 3

[0019] Example 3: Take 2090 kg of o-chlorobenzyl chloride, 1450 kg of trimethyl phosphite, 1400 kg of chlorinated benzene, and 60 kg of soda ash, put them into a 5000L reactor, mix them thoroughly, and heat the above raw materials to 120 at normal pressure. ℃, react at normal pressure for 50h; then collect low-boiling substances (chlorinated benzene as a solvent) under normal pressure. When the temperature in the kettle is 165℃, vacuumize to -0.06Mpa and continue to extract low-boiling substances; The reaction kettle is evacuated to -0.06MPa, heated to 200°C, and crude distillation is carried out for 5h; then transferred to the kettle, evacuated -0.06MPa, heated to 230°C, and rectified for 5h; finally the finished product obtained by the rectification is filled (in barrels) ), the yield of the finished product is more than 1.3 times the weight of o-chlorobenzyl chloride, and then the reactor is restored to normal pressure and reduced to normal temperature, and the residue is disch...

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Abstract

Production of chlorobenzyl dimethyl ester phosphate is carried out by taking chlorochlor, trimethyl phosphite, benzyl chloride and soda as material, commissioning and synthesizing reacting, separating low boiler, coarse distilling, refining distilling, loading, and obtaining chlorobenzyl dimethyl ester phosphate with purity 70-99.9%. It controls temperature, pressure and time in production, it can be used for insecticide and bactericide. Its advantages include low cost, simple operation, high output, and industrial production.

Description

Technical field [0001] The invention relates to a preparation method of pesticide intermediates, in particular to a production process of dimethyl o-chlorobenzylphosphonate, which is an important raw material of epoxiconazole as a fungicide and pesticide intermediate. Background technique [0002] Epiconazole is an intermediate of a new type of pesticide with high efficiency and low toxicity developed successfully in Germany and the United Kingdom in recent years, and a variety of fungicides and insecticides can be derived from this product as a carrier. At present, some domestic enterprises and research institutes are also actively conducting research in this area. The production process of epoxiconazole is complicated, the production route is long, and the raw materials used are many. Among them, a new main raw material, dimethyl o-chlorobenzylphosphonate, which plays a key role in its performance indicators, cannot be produced in China or seen abroad. According to related repo...

Claims

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Application Information

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IPC IPC(8): C07F9/42
Inventor 申厚宝王泉民尤小雯申立斌
Owner 泰州市天成化工有限公司
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