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Method for preparing chlorpyrifos by clean technology

A chlorpyrifos and process technology, which is applied in the field of preparation of chlorpyrifos by a clean process, can solve the problems of increasing the difficulty of wastewater treatment, long process flow, and many reaction steps, and achieve environmentally friendly production costs, high reaction yield, and improved purity and yield Effect

Inactive Publication Date: 2013-03-20
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 by clean technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] To a 1000ml three-necked flask equipped with a thermometer and mechanical stirring, add 400g of a mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium and water with a mass concentration of 15%, raise the temperature to 40°C and stir evenly, and then 0.8335 g of 4-dimethylaminopyridine, 0.7586 g of benzyltrimethylammonium chloride, 0.5036 g of 15-crown-5 and 45 ml of O,O-diethylphosphorylthiochloride were added. Add dropwise 30% Na after adding 2 CO 3 Keep the pH value of the solution at 8.5-11. After the pH is stable, raise the temperature to 55° C. and react for 1.5 hours. Stop stirring and let it stand at 60°C for 10 minutes, remove the water layer while it is hot, filter the organic phase with water, wash with water, and dry to obtain the finished product of chlorpyrifos. The content of HPLC analysis is 98.31%, and the yield is 98.12%.

Embodiment 2

[0025] To a 1000ml three-neck flask equipped with a thermometer and mechanical stirring, add 400g of a mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium and water with a mass concentration of 15%, raise the temperature to 30°C and stir evenly, and then 0.8335 g of 4-dimethylaminopyridine, 0.7956 g of trioctylmethylammonium chloride, 0.5036 g of polyether P104 and 45 ml of O,O-diethylphosphorylthiochloride were added. After the addition, 30% KOH solution was added dropwise to maintain the pH value at 8.5-11. After the pH was stable, the temperature was raised to 50°C and reacted for 1.5 h. Stop stirring and let it stand at 60°C for 20 minutes, remove the water layer while it is hot, filter the organic phase with water, wash with water, and dry to obtain the crude product of chlorpyrifos. The content of HPLC analysis is 98.14%, and the yield is 98.03%.

Embodiment 3

[0027] To a 1000ml three-neck flask equipped with a thermometer and mechanical stirring, add 400g of a mixed solution of 3,5,6-trichloropyridin-2-alcohol sodium and water with a mass concentration of 15%, raise the temperature to 30°C and stir evenly, and then 0.8335 g of 4-dimethylaminopyridine, 0.6834 g of tetrabutylammonium chloride and 45 ml of O,O-diethylphosphorylthiochloride were added. After the addition, add 20% NaOH solution dropwise to maintain the pH value at 8.5-11. After the pH is stable, raise the temperature to 55°C and react for 2 hours. Stop stirring and let it stand at 55°C for 15 minutes, remove the water layer while it is hot, filter the organic phase with water, wash with water, and dry to obtain the crude product of chlorpyrifos, the content of HPLC analysis is 98.03%, and the yield is 98.00%.

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Abstract

The present invention discloses a novel method for preparing chlorpyrifos by the clean technology. Sodium 3,5,6-trichloropyridine-2-alkoxide and O,O-diethyl phosphoryl chloride are used as main raw materials. The reactants are added once, water is used as medium, and a highly dispersed system is formed under the action of a composite catalyst for reaction. The reaction time is greatly shortened, and the target product of chlorpyrifos can be obtained by simple separation and purification. The invention is environmental-friendly, and is simple in the synthetic method. The water phase method of chlorpyrifos synthesis can be efficiently conducted through a simple process operation. The product is high in purity, and high in yield. The method is suitable for 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58
Inventor 王红明李健刘善和方红新薛谊
Owner ANHUI COSTAR BIOCHEM CO LTD
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