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Production process for synthesizing carbendazim by hydrogen chloride method

A production process and technology for carbendazim, which is applied in the field of production technology for synthesizing carbendazim by hydrogen chloride method, can solve the problems of hydrochloric acid easily containing impurities, reducing product quality, and a large amount of waste water, achieving uniform heating, improving heating effect, and reducing waste water. volume effect

Pending Publication Date: 2022-02-08
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The following disadvantages exist in the existing carbendazim production: using hydrochloric acid to adjust the pH value produces a large amount of waste water, and the hydrochloric acid is easy to contain impurities, which reduces the quality of the product

Method used

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  • Production process for synthesizing carbendazim by hydrogen chloride method
  • Production process for synthesizing carbendazim by hydrogen chloride method
  • Production process for synthesizing carbendazim by hydrogen chloride method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A production process for synthesizing carbendazim by hydrogen chloride method, specifically comprising the following steps:

[0039] Step S1, pouring methyl cyanamide and o-phenylenediamine into the reaction kettle 1 in turn, starting the stirring motor 3, and the stirring motor 3 drives the stirring frame 2 to rotate, and the methyl cyanamide and o-phenylenediamine added successively The diamine is stirred to form a mixed solution;

[0040] Step S2, introducing the hydrogen chloride gas inside the hydrogen chloride storage tank 4 into the reaction kettle 1 with the gas guide tube 8, and the reaction kettle 1 has a pH=4.4, and the aeration is stopped;

[0041] Step S3, start the coil heater 5 to heat the mixed solution in the reaction kettle 1 to 100° C. at a heating rate of 4° C. / min. When the pH in the kettle is 4.6, feed hydrogen chloride gas until the pH = 4. Stop ventilation at 4 o'clock, stir until the pH remains unchanged, and the reaction ends;

[0042] Step S...

Embodiment 2

[0045] A production process for synthesizing carbendazim by hydrogen chloride method, specifically comprising the following steps:

[0046] Step S1, pouring methyl cyanamide and o-phenylenediamine into the reaction kettle 1 in turn, starting the stirring motor 3, and the stirring motor 3 drives the stirring frame 2 to rotate, and the methyl cyanamide and o-phenylenediamine added successively The diamine is stirred to form a mixed solution;

[0047] Step S2, introducing the hydrogen chloride gas inside the hydrogen chloride storage tank 4 into the reaction kettle 1 with the gas guide tube 8, and the reaction kettle 1 has a pH=4.5, and the aeration is stopped;

[0048] Step S3, start the coil heater 5 to heat the mixed solution in the reaction kettle 1 to 100° C. at a heating rate of 6° C. / min. When the pH in the kettle is 4.6, feed hydrogen chloride gas until the pH = 4. Stop ventilation at 4 o'clock, stir until the pH remains unchanged, and the reaction ends;

[0049] Step S...

Embodiment 3

[0052] Step S1, pouring methyl cyanamide and o-phenylenediamine into the reaction kettle 1 in turn, starting the stirring motor 3, and the stirring motor 3 drives the stirring frame 2 to rotate, and the methyl cyanamide and o-phenylenediamine added successively The diamine is stirred to form a mixed solution;

[0053]Step S2, introducing the hydrogen chloride gas inside the hydrogen chloride storage tank 4 into the reaction kettle 1 with the gas guide tube 8, and the reaction kettle 1 has a pH=4.6, and the ventilation is stopped;

[0054] Step S3, start the coil heater 5 to heat the mixed liquid in the reaction kettle 1 to 100° C. at a heating rate of 8° C. / min. When the pH in the kettle is 4.6, feed hydrogen chloride gas until the pH = 4. Stop ventilation at 4 o'clock, stir until the pH remains unchanged, and the reaction ends;

[0055] Step S4, washing the reaction kettle 1 after the reaction in step S3 with discharging water to obtain a water-washed product;

[0056] Step...

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Abstract

The invention relates to a production process for synthesizing carbendazim by a hydrogen chloride method, and belongs to the technical field of farm chemical synthesis. The production process specifically comprises the following steps: S1, sequentially adding methyl cyanocarbamate and o-phenylenediamine into a reaction kettle, and starting a stirring motor to stir the methyl cyanocarbamate and the o-phenylenediamine which are sequentially added to form a mixed solution; S2, introducing hydrogen chloride gas in a hydrogen chloride storage tank into the reaction kettle by using a gas guide pipe, and stopping gas introduction; S3, starting a coil heater to heat the mixed solution in the reaction kettle, raising the temperature to 100 DEG C at a temperature raising rate of 4-8 DEG C / min, introducing hydrogen chloride gas when the pH value in the kettle is 4.6 until the pH value is 4.4, stirring until the pH value is not changed, and ending the reaction. The hydrogen chloride is directly used for adjusting the pH value, so that the wastewater generation amount can be effectively reduced, no impurity is carried in the hydrogen chloride, and the product quality is obviously improved.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and in particular relates to a production process for synthesizing carbendazim by a hydrogen chloride method. Background technique [0002] Carbendazim, also known as cotton wilt, etc., its industrial product is light brown powder. The product was first proposed by H-Hampel and his colleagues in the early 1970s for its bactericidal activity, which is a broad-spectrum fungicide. It is mainly used for various diseases caused by fungi in wheat, vegetables, fruits and other crops, and with its high efficiency and low toxicity, it has been widely used in industrial fields and paint anti-mold, livestock and poultry parasite insecticides (intermediates) . [0003] Carbendazim is a broad-spectrum systemic fungicide, which can be absorbed by seeds, roots and leaves of plants, and can be transported in plant tissues, with protective and therapeutic effects. The 800-1000-fold dilution with 50...

Claims

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Application Information

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IPC IPC(8): C07D235/32
CPCC07D235/32
Inventor 罗利忠吴双齐黄多头刘建清杨荷勤吴兆平鲍习文
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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