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Ethoprophos product and method for preparing ethoprophos

A technology of profenaphos and its products, which is applied in the field of pesticides, can solve the problems of low purity, strong odor, and large environmental pollution, and achieves the effects of simple process operation and mild reaction conditions.

Active Publication Date: 2013-04-24
JIANGSU FENGSHAN GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process of profenphos technical, there are always problems such as high residual amount of thiol in the product, low purity, strong odor, large environmental pollution and high cost.

Method used

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  • Ethoprophos product and method for preparing ethoprophos
  • Ethoprophos product and method for preparing ethoprophos

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Put 600g of phosphorus oxychloride into a 1000ml three-necked reaction bottle, install a stirring, rectifying tower, dropping funnel, and thermometer, then lower the temperature to below 2 degrees Celsius, and slowly add 100g dropwise under slight negative pressure and vigorous stirring Absolute ethanol, control the reaction temperature below 3 degrees Celsius. After the ethanol was added dropwise, the insulation was continued for 12 hours, and after rectification and recovery of phosphorus oxychloride, 336 g of dichloro compounds with a content of more than 99% by weight were obtained at a temperature not higher than 100 degrees Celsius.

Embodiment 2

[0037] Put 600g of phosphorus oxychloride into a 1000ml three-necked reaction bottle, install a stirring, rectifying tower, dropping funnel, and thermometer, then lower the temperature to below 0 degrees Celsius, and slowly add 100g dropwise under slight negative pressure and vigorous stirring Absolute ethanol, control the reaction temperature below 10 degrees Celsius. After the ethanol was added dropwise, the insulation was continued for 6 hours, and after phosphorus oxychloride was recovered by rectification, 317g of dichloro compounds with a content of more than 99% by weight were obtained at a temperature not higher than 80 degrees Celsius.

Embodiment 3

[0039] After adding 60ml of toluene into a 250ml three-necked bottle, add 7g of sodium hydroxide and 0.38g of additives in turn, raise the temperature to 65 degrees Celsius, slowly add 25g of propanethiol dropwise, keep warm for three hours, then lower the temperature to 0~5 degrees Celsius, dropwise add Dichloro compound 10g, naturally warming up to room temperature, insulation for 5 hours. After adding 5% hydrochloric acid aqueous solution to adjust the pH to 6, after stirring for 30 minutes, the water layer was separated, and the organic layer was washed to neutral with water. The solvent was removed under vacuum. Obtained 14 g of protonphos products with a small amount of remaining propanethiol, the content of which was greater than 98% by weight.

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PUM

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Abstract

The invention discloses an ethoprophos product and a method for preparing ethoprophos. The method for preparing ethoprophos comprises the following steps of: contacting phosphorus oxychloride with ethanol to generate o-ethyl phosphonic dichloride; and contacting o-ethyl phosphonic dichloride with propanethiol in presence of an aromatic hydrocarbon solvent, an assistant and alkali to obtain ethoprophos, wherein proportion of volume of the aromatic hydrocarbon solvent to weight of propanethiol is 800ml: 50-200g. The content of ethoprophos in the ethoprophos product prepared by the method can reach over 98wt%.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a profenphos product and a method for preparing it. Background technique [0002] Ethoprophos, also known as ethoprophos, is an organic ester insecticide developed by the French Mobile Chemical Company. It is mainly used to prevent and control nematodes in peanuts, tobacco and other crops, especially for rice gall ants. . In the production process of profenphos technical, there are always problems such as high residual amount of thiol in the product, low purity, strong odor, large environmental pollution and high cost. [0003] Therefore, the process for preparing high-purity prolinephos remains to be further studied. Contents of the invention [0004] The inventor finds: at present, the purity of the proparaphos products of the prior art is usually 90-92% by weight, and the present production technology is also difficult to obtain the proparaphos products with a purity of more than...

Claims

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Application Information

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IPC IPC(8): C07F9/17
Inventor 林辉殷凤山
Owner JIANGSU FENGSHAN GROUP
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