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New synthesis method for improving quality of thiophanate methyl

A technology of thiophanate-methyl and synthesis method, which is applied in the field of synthesis to improve the quality of thiophanate-methyl, can solve problems such as inability to increase the content, poor temperature control, unstable quality, etc., to reduce the generation of by-products, The effect of reducing the generation of pollutants and easy temperature control

Inactive Publication Date: 2018-09-11
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing production method of thiophanate-methyl is that acetone, sodium thiocyanate and methyl chloroformate are successively added into the synthesis kettle for reaction, and then the resultant is condensed with o-phenylenediamine. The reaction process The temperature is not well controlled, the safety is not good, the content cannot be increased, the impurity content is high, the purity of thiophanate-methyl is only 95% to 96%, and the quality is unstable; the reaction conversion rate is low, only 88%

Method used

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  • New synthesis method for improving quality of thiophanate methyl

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Comparison scheme
Effect test

Embodiment 1

[0023] like figure 1 Shown, the technical scheme that the present invention adopts is: a kind of new synthetic method that improves the quality of thiophanate-methyl, and described synthetic method specifically comprises the following steps:

[0024] 1). Add ethyl acetate as a solvent to the enamel reaction kettle, then add sodium thiocyanate into the reaction kettle, control the reaction temperature at 59°C, start the mixer to stir, and quickly add methyl chloroformate dropwise to the inside of the reaction kettle Ester, methyl chloroformate and sodium thiocyanate react in the reactor. After the reaction stops, the reaction materials are filtered and centrifuged, and then the centrifugal liquid is subjected to vacuum distillation, and the low boiling point liquid is transferred to the inside of the reactor for circulation. reaction, the high boiling point liquid is methyl isothiocyanate;

[0025] The enamel reaction kettle in the step 1 is connected to the external circulati...

Embodiment 2

[0038] like figure 1 Shown, the technical scheme that the present invention adopts is: a kind of new synthetic method that improves the quality of thiophanate-methyl, and described synthetic method specifically comprises the following steps:

[0039] 1). Add ethyl acetate as a solvent to the enamel reaction kettle, then add sodium thiocyanate into the reaction kettle, control the reaction temperature at 50°C, start the mixer to stir, and quickly add methyl chloroformate dropwise to the inside of the reaction kettle Ester, methyl chloroformate and sodium thiocyanate react in the reactor. After the reaction stops, the reaction materials are filtered and centrifuged, and then the centrifugal liquid is subjected to vacuum distillation, and the low boiling point liquid is transferred to the inside of the reactor for circulation. reaction, the high boiling point liquid is methyl isothiocyanate;

[0040] The enamel reaction kettle in the step 1 is connected to an external circulatio...

Embodiment 3

[0053] like figure 1 Shown, the technical scheme that the present invention adopts is: a kind of new synthetic method that improves the quality of thiophanate-methyl, and described synthetic method specifically comprises the following steps:

[0054] 1). Add ethyl acetate as a solvent to the enamel reaction kettle, then add sodium thiocyanate into the reaction kettle, control the reaction temperature at 45°C, start the mixer to stir, and quickly add methyl chloroformate dropwise to the inside of the reaction kettle Ester, methyl chloroformate and sodium thiocyanate react in the reactor. After the reaction stops, the reaction materials are filtered and centrifuged, and then the centrifugal liquid is subjected to vacuum distillation, and the low boiling point liquid is transferred to the inside of the reactor for circulation. reaction, the high boiling point liquid is methyl isothiocyanate;

[0055] The enamel reaction kettle in the step 1 is connected to the external circulati...

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Abstract

The invention relates to a new synthesis method for improving the quality of thiophanate methyl. The synthesis method specifically comprises the following steps that ethyl acetate is added into a reaction kettle as a solvent, then sodium thiocyanate is added, the reaction temperature is controlled to be about 59 DEG C, stirring is started, and methyl chloroformate is dropwise added at a medium orhigh speed; methyl chloroformate and sodium thiocyanate react in the reaction kettle and subjected to reduced pressure distillation after being centrifuged, and methyl isothiocyanate is obtained; theobtained methyl isothiocyanate is put into an enamel reaction kettle, stirring is started, o-phenylenediamine is added in the ratio of 2:1 for addition reaction, the reaction temperature is controlledto be 40-70 DEG C, and centrifugation is carried out after the reaction stops; the temperature of solid is increased to 110-160 DEG C, and thiophanate methyl is obtained after liquid-solid separation. The purity of the thiophanate methyl synthesized through the method reaches 98% or above, the reaction conversion rate reaches 95% or above, the safety is good, the temperature is easy to control, generation of pollutants is reduced, and generation of by-products is reduced.

Description

technical field [0001] The invention relates to the technical field of thiophanate-methyl synthesis, in particular to a new synthesis method for improving the quality of thiophanate-methyl. Background technique [0002] The chemical name of thiophanate-methyl is 1,2-bis(3-methoxycarbonyl-2-thioureido)benzene, and the trade name is thiophanate-methyl. It is a broad-spectrum fungicide with apical conduction It has the functions of preventing and treating various diseases, and inhibiting spider mites and pathogenic nematodes. Thiophanate-methyl is prepared through the synthetic reaction of thiocyanic acid and o-phenylenediamine. Thiophanate-methyl preparations include thiophanate-methyl 70% wettable powder, thiophanate-methyl 50% suspension, thiophanate-methyl 36% suspension, and 3% paste. The pure product is a colorless crystal, the original powder with a content of about 93% is a light yellow crystal, the specific gravity is 1.5 (20°C), the melting point is 172°C (decomposi...

Claims

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Application Information

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IPC IPC(8): C07C335/28
CPCC07C335/28
Inventor 过学军徐小兵袁树林刘长庆李红卫吴建平黄显超李波
Owner ANHUI GUANGXIN AGROCHEM
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