Improved process for synthesizing omethoate

A technology of omethoate and process, which is applied in the field of improved process of synthesizing omethoate, can solve problems such as increasing side reactions, reducing yield, and large heat release of the system, and achieves the effect of improving the purity of crude oil and improving the overall process

Active Publication Date: 2018-12-14
兰博尔开封科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional process of this reaction, water needs to be added, and the reaction is carried out at 65°C. The entire process environment is particularly conducive to the dissolution of ammonium chloride in the crude ester system, thus resulting in a large amount of exothermic heat in the system, difficulties for employees to operate the temperature, and increased The progress of the side reaction increases the chance of meeting the main by-products to a greater extent and reduces the yield of this step
For example, Omethoate crude oil needs to be desolventized, and Omethoate will be hydrolyzed in the process, resulting in a reduction in the yield and content of Omethoate crude oil

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] An improved process for synthesizing Omethoate, comprising the following steps:

[0040] (1) Preparation of Thionate Crude Ester

[0041] Put 900kg of methyl chloroacetate, 500L of ammonium sulfophosphate, and 2.5kg of triethylamine into the reaction kettle in sequence, turn on the stirring and steam valve, close the steam valve when the temperature rises to 45°C, keep it at 45°C for 3 hours, and open it after the heat preservation is over The cooling water valve is used to cool the material, and when the temperature drops to 30°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride, and the filtrate thrown out is the crude oxathion ester; the centrifuged ammonium chloride is dried and then processed sales of by-products;

[0042] (2) Preparation of oxathion refined ester

[0043] Use 3A molecular sieves to carry out tertiary drying of the crude oxathion esters, the weight ratio of molecular sieves to the crude oxathi...

Embodiment 2

[0054] An improved process for synthesizing Omethoate, comprising the following steps:

[0055] (1) Preparation of Thionate Crude Ester

[0056] Put 1200kg of methyl chloroacetate, 900L of ammonium sulfophosphate, and 3.5kg of triethylamine into the reaction kettle in sequence, turn on the stirring and steam valve, close the steam valve when the temperature rises to 55°C, keep it at 55°C for 3 hours, and open it after the heat preservation is over The cooling water valve is used to cool the material, and when the temperature drops to 30°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride, and the filtrate thrown out is the crude oxathion ester; the centrifuged ammonium chloride is dried and then processed sales of by-products;

[0057] (2) Preparation of oxathion refined ester

[0058] Use 3A molecular sieves to carry out tertiary drying of the crude oxathion esters, the weight ratio of molecular sieves to the crude oxa...

Embodiment 3

[0069] An improved process for synthesizing Omethoate, comprising the following steps:

[0070] (1) Preparation of Thionate Crude Ester

[0071] Put 1000kg of methyl chloroacetate, 700L of ammonium sulfophosphate, and 4kg of triethylamine into the reaction kettle in sequence, turn on the stirring and steam valve, close the steam valve when the temperature rises to 50°C, keep it at 50°C for 3 hours, and open it to cool down after the heat preservation is over The water valve is used to cool down the material, and when the temperature drops to 30°C, the material is discharged, and the material is subjected to centrifugal separation of ammonium chloride, and the filtrate thrown out is the crude phosphorothioate; the centrifuged ammonium chloride is dried and then subjected to secondary Production and sales;

[0072] (2) Preparation of oxathion refined ester

[0073] Use 3A molecular sieves to carry out tertiary drying of the crude oxathion esters, the weight ratio of molecular ...

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PUM

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Abstract

The invention discloses an improved process for synthesizing omethoate. In the process of preparation of omethoate by using a post aminolysis method, coarse prepared omethoate crude oil is first dried, and then desolvation is conducted so as to obtain omethoate crude oil. Through improvement of multiple processes, improvement of the reaction environment, improvement of the progress of a main reaction and reduction of hydrolysis are achieved to the greatest extent, the reaction yield is improved, and the post-treatment of salt-containing compounds is more convenient. By using the process, the yield of refined ester of oxygen sulfur phosphorus ester can be increased to 86% or above, and the purity is also increased to 90% or above; the purity of ammonium chloride can reach 99% or above, andthe ammonium chloride can be directly sold as a by-product first-grade product; the total yield of the omethoate crude oil can be increased to 79% or above, the purity of the crude oil is also improved, the overall process is greatly improved, and the social and economic benefits are huge.

Description

technical field [0001] The invention relates to an improved process for synthesizing omethoate, which belongs to the technical field of organic compound synthesis. Background technique [0002] Organic synthesis is a common reaction, but due to the self-reaction of organic compound synthesis, some problems will appear in the process of organic synthesis. For example, there are many side reactions in the solid-liquid organic synthesis reaction, the most common of which is the generation of salt-containing by-products, and the occurrence of side reactions has more or less a certain impact on the main reaction, for example: affecting the main reaction The process affects the content, yield and so on of the main product. If the organic compound is hydrolyzed, the content and yield of the product will be adversely affected. [0003] Omethoate is a highly efficient systemic insecticide and acaricide, widely used in rice, cotton, fruit trees, wheat, sorghum, sugar cane and other ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/165
CPCC07F9/1651
Inventor 常书浩霍二福董光霞刘沛敬李晓琼孙宝臣乔晓会刘宏勋汤肖倩李红金
Owner 兰博尔开封科技有限公司
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