Method for preparing bifenthrin

A technology of bifenthrin and bifenthrin, applied in the field of bifenthrin preparation, can solve problems such as difficult large-scale industrial production, difficult treatment of three wastes, high carcinogenicity, etc., and achieve easy treatment of three wastes, environmental friendliness, Remove the effect of poison

Inactive Publication Date: 2011-05-25
GENCHEM & GENPHARM CHANGZHOU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the existing production process of bifenthrin, a large amount of expensive acid-binding agent pyridine is used. Due to the unfavorable factors such as high carcinogenicity of pyridine, difficulty in recycling, and difficulty in the treatment of three wastes, it is difficult to form large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Put 500kg of measured Kung Fu acid, 0.5kg of N,N-dimethylformamide, and 500kg of toluene into the reactor, put 246kg of measured thionyl chloride into the high level tank, and open the tail gas absorption device to absorb HCl and SO 2 , Slowly add thionyl chloride dropwise in the kettle not exceeding 0°C. After the dropwise addition, keep the temperature in the kettle not exceeding 15°C for 20 hours. After the reaction, recover the toluene under reduced pressure until there is no distillation. spare.

[0035] 250kg of biphenyl alcohol and 250kg of toluene were put into the reactor, and aqueous sodium hydroxide solution (50.5kg of sodium hydroxide, 202kg of water) was sucked into the elevated tank, the temperature was lowered to 3°C, and 204kg of aqueous sodium hydroxide solution and kung fu acid chloride were slowly added dropwise at the same time. And control the pH value of the system to 8. After the dropwise addition, keep it warm at 3°C ​​for 5 hours. After the reac...

Embodiment 2

[0037] Put 500kg of measured Kung Fu acid, 1kg of N,N-dimethylformamide, and 1000kg of toluene into the reactor, put 260kg of measured thionyl chloride into the high level tank, and open the tail gas absorption device to absorb HCl and SO 2 , Slowly add thionyl chloride dropwise in the kettle at no more than 3°C. After the dropwise addition, keep the temperature in the kettle at no more than 1°C for 20 hours. After the reaction, recover the toluene under reduced pressure until there is no evaporation. spare.

[0038] Drop into biphenyl alcohol 250kg, toluene 1000kg in the reaction kettle, draw in sodium hydroxide aqueous solution (sodium hydroxide 60kg, water 400kg) in the elevated tank, cool down to 5 ℃, slowly add dropwise sodium hydroxide aqueous solution and 250kg of kung fu acid chloride at the same time, and Control the pH value of the system to 8. After the dropwise addition, keep it warm at 5°C for 6 hours. After the reaction is over, separate the water phase and recov...

Embodiment 3

[0040] Put 500kg of Kung Fu acid, 25kg of N, N-dimethylformamide, and 2500kg of toluene into the reaction kettle, put 490kg of thionyl chloride into the high level tank, and open the tail gas absorption device to absorb HCl and SO 2 , Slowly add thionyl chloride dropwise in the kettle at no more than 4°C. After the dropwise addition, keep the temperature in the kettle at no more than 20°C for 24 hours. spare.

[0041] Drop into 250kg of biphenyl alcohol, 2500kg of toluene in the reaction kettle, draw in aqueous sodium hydroxide solution (85kg of sodium hydroxide, 1020kg of water) in the head tank, cool down to 5 ℃, slowly add aqueous sodium hydroxide solution and 305kg of kung fu acid chloride dropwise at the same time, and Control the pH value of the system to 9. After the dropwise addition, keep it warm at 4°C for 6 hours. After the reaction is over, separate the water phase and recover the toluene under reduced pressure. Dried, whirlwind crushed, and dried to obtain 522 kg...

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PUM

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Abstract

The invention discloses a method for preparing bifenthrin, which comprises the following steps: adding lambda cyhalthrin acid, inert organic solvents and catalysts into a reaction kettle, dripping thionyl chloride under the condition between -5 DEG C and 30 DEG C, carrying out reaction for 0 to 72h at the temperature between -5 DEG C and 30 DEG C, and then, recovering the inert organic solvents through vacuum distillation to prepare and obtain lambda cyhalthrin acyl chloride; adding 2-methyl-3-biphenylmethanol and the inert organic solvents into the other one reaction kettle, controlling the pH value between 7 and 12 at the -5 DEG C to 30 DEG C, dripping the lambda cyhalthrin acyl chloride and acid-binding agent water solution at the same time, carrying out reaction for 0 to 24h at 0 DEG C to 5 DEG C, recovering the inert organic solvents through phase separation and pressure reduction to prepare crude products, adding recrystallization agents, recrystallizing the crude products, and preparing and obtaining the required bifenthrin. The method disclosed by the invention has the advantages of simple production process, low cost, milder operation condition and little three wastes, the reaction rate is higher than 97 percent, the product purity is higher than 98 percent, and the method is applicable to industrialized production.

Description

technical field [0001] The invention relates to a method for preparing pesticide raw materials, in particular to a method for preparing bifenthrin. Background technique [0002] At present, countries all over the world have become more and more aware of the necessity of upgrading the structure of pesticide products, and at the same time are fully promoting the development of new pesticides with high efficiency, safety and good environmental compatibility. Pyrethroid pesticides are a new generation of insecticides developed on the basis of simulating the active ingredients of natural pyrethrins and their chemical structures. The characteristics of low animal toxicity have become the ideal species advocated by countries all over the world to replace highly toxic and high residual organophosphorus pesticides. [0003] Bifenthrin is a synthetic pyrethroid insecticide, which is a cyano-free pyrethroid. It is mainly used to prevent cotton, vegetables, fruit trees, tobacco, tea tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/743C07C67/14
Inventor 王玉琴詹玉俊
Owner GENCHEM & GENPHARM CHANGZHOU CO LTD
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