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Method for preparing cyhalothrin

A technology of cyhalothrin and chlorocyanyl trifluoride, which is applied in the field of preparation of pyrethroids, can solve the problems of reduced raw powder yield, low purity, black color, etc., and achieves reduced production costs, simple separation, and high yield. high effect

Inactive Publication Date: 2012-08-08
JIANGSU HUANGMA AGROCHEM
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] But the cyhalothrin crude oil prepared by the existing method has low purity (usually<90%), poor color (in dark black), and the trifluoromethrin obtained after carrying out the next step differential isomerization with this cyhalothrin crude oil The yield of cypermethrin former powder is not high (<80%), and color and luster is black, and purity is low (<90%), does not reach the quality requirement of commodity, needs recrystallization to remove organic impurity, has reduced former powder further like this again. The yield, while increasing the amount of waste mother liquor treatment, increased treatment costs

Method used

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  • Method for preparing cyhalothrin

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Embodiment 1

[0019] The method for preparing cyhalothrin of the present embodiment has the following steps:

[0020] ① Prepare a mixed solution. 200kg purity is 99% ether aldehyde (1kmol), the concentration of 235.2kg is 25% sodium cyanide aqueous solution (1.2kmol), the toluene solvent of 800kg, the 2,2-dimethylaminopyridine of 200g mixes and obtains mixed solution .

[0021] ② Preparation of crude product containing cyhalothrin. By trifluorochlorocyanoyl chloride, step 1. ether aldehyde and sodium cyanide in the mixed solution as reactants, by step 1. 2,2-dimethylaminopyridine in the mixed solution is a catalyst, by step 1. the toluene in the mixed solution Carry out the following chemical reaction of generating cyhalothrin for the solvent: the 269kg purity that the preparation example gained is 97% chlorocyanoyl chloride (1kmol) dropwise in the above-mentioned mixed solution in 4h at the temperature of 17 ℃, then in Stirring at 20°C for 8 hours gave a crude product containing cyhalot...

Embodiment 2～ Embodiment 7

[0024] Each embodiment is basically the same as Embodiment 1, and the differences are shown in Table 1.

[0025] Table 1

[0026]

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Abstract

The invention discloses a method for preparing cyhalothrin, which comprises the following steps: (1) preparing a mixed solution as follows: mixing ether aldehyde, sodium cyanide water solution, organic solvent and aminopyridine or derivatives thereof as a catalyst to obtain the mixed solution; (2) preparing a crude product containing cyhalothrin: dropwise adding cyanuryl chloride to the mixed solution obtained in step (1) at the temperature of 0 DEG C-40 DEG C, and stirring after dropwise adding to obtain the crude product containing cyhalothrin; and (3) refining: layering the crude product containing cyhalothrin obtained in step (2), washing the oil layer with water, and removing the organic solvent to obtain the crude oil of the cyhalothrin. The method of the invention can obtain the crude oil of the cyhalothrin with high purity, good color and luster and high yield, has simple separation, does not need recrystallization, avoids the generation of discarded mother solution, and reduces the production cost.

Description

technical field [0001] The invention relates to a method for preparing pyrethroids, in particular to a method for preparing cyhalothrin. Background technique [0002] Cyhalothrin, also known as Kungfu permethrin, its chemical formula is C 23 h 19 CIF 3 NO 3 , the chemical name is cyano(3-phenoxyphenyl)methyl 3-(2-chloro-3,3,3-fluoro-1 propenyl)-2,2-dimethylcyclopropylcarboxylate. It can be used not only as a single insecticide, but also in combination with other types of insecticides and acaricides. Its main features are high efficiency, low pollution, low drug resistance, and low cost of use. [0003] But the cyhalothrin crude oil prepared by the existing method has low purity (usually<90%), poor color (in dark black), and the trifluoromethrin obtained after carrying out the next step differential isomerization with this cyhalothrin crude oil The yield of cypermethrin former powder is not high (<80%), and color and luster is black, and purity is low (<90%), d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/39C07C253/00
Inventor 宦志东
Owner JIANGSU HUANGMA AGROCHEM
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