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Method for preparing chlorpyrifos

A technology for chlorpyrifos and trichloropyridine, which is applied in the field of preparing chlorpyrifos by cleaning process, can solve the problems of increasing the difficulty of wastewater treatment, long process flow, many reaction steps, etc., and achieves environmentally friendly production cost, high reaction yield, purity and yield. rate increase effect

Inactive Publication Date: 2013-04-10
ANHUI COSTAR BIOCHEM CO LTD
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AI Technical Summary

Problems solved by technology

Wherein the organic solvent and the double solvent method have the following problems: many reaction steps and long process flow
The operation is relatively cumbersome, the yield can only reach 95.5%, and the sodium chloride introduced by this method increases the difficulty of wastewater treatment

Method used

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  • Method for preparing chlorpyrifos

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Embodiment 1

[0018] A method for preparing chlorpyrifos, the specific steps are as follows: 3,5,6-trichloropyridin-2-alcohol sodium is mixed with 4 times the weight of water, and dodecyltrimethylammonium chloride, dodecane Dimethyl betaine, stir evenly, heat up to 40-45°C, add dropwise 1 / 2 of the total weight of O,O-diethylphosphorylthiochloride, and dropwise add sodium hydroxide solution to keep the pH stable at 9.5 -10, the reaction temperature is controlled at 40-45°C during the dropwise addition, and reacted for 2 hours; then the temperature is raised to 55-60°C, and the remaining O,O-diethylphosphoryl thiochloride is added dropwise, and N-formazan is added dropwise at the same time For imidazole, keep warm and continue to react for 0.5-1 h; continue to heat up to 65-70°C, react for 1.5-2 h, stop stirring and let it stand for 30-60 min, remove the water layer by separating while it is hot, wash the organic phase with suction, and separate the water Dried to obtain the finished product ...

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Abstract

The invention discloses a novel method for preparing chlorpyrifos by using 3,5,6-trichloropyridine-2-sodium alkoxide and O,O-diethyl thiophosphoryl chloride as main raw materials. The novel method disclosed by the invention mainly comprises the following steps of: based on water as a medium, adding reactants by times; forming a high dispersion system under the effect of a compound catalyst to carry out reaction, wherein the reaction time is greatly shortened; and carrying out simple separation and purification to obtain the target product chlorpyrifos. The novel method disclosed by the invention is environment-friendly; a synthesis method is simple; water-phase method chlorpyrifos synthesis can be efficiently carried out through simple process operation and the obtained product has high purity and high yield; and therefore, the novel method is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a new method for preparing chlorpyrifos by using 3,5,6-trichloropyridin-2-alcohol sodium and O, O-diethylthiophosphoryl chloride as main raw materials through a clean process. Background technique [0002] Chlorpyrifos, chemical name O, O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate, alias chlorpyrifos, also known as Lesben. Its structural formula is as follows: [0003] [0004] Chlorpyrifos is a broad-spectrum insecticide with high efficiency, low toxicity and low residue. Corn, cotton, sugar cane, tea, fruit trees, flowers, livestock and other crops are included in the recommended pesticide varieties for pollution-free agricultural products. There are broad market and application prospects. [0005] The synthetic method of chlorpyrifos can be divided into organic solvent method, double solvent method and aqueous phase method according to different reaction conditions. Wherein the organic solvent and dual-sol...

Claims

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Application Information

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IPC IPC(8): C07F9/58
Inventor 顾福海李健俞建良方红新
Owner ANHUI COSTAR BIOCHEM CO LTD
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