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Production process of acetamiprid

A production process and acetamiprid technology, which is applied in the production process field of acetamiprid, can solve the problems of high consumption, high odor of monomethylamine, easy volatility and the like, and achieve the effects of less waste water, less three wastes, and less by-products

Inactive Publication Date: 2015-07-29
JIANGSU CHANGQING AGROCHEM NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process of acetamiprid, the reaction raw material monomethylamine has a strong smell and is volatile, so the consumption of monomethylamine is relatively high

Method used

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  • Production process of acetamiprid
  • Production process of acetamiprid

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Experimental program
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Effect test

Embodiment 1

[0018] The production technology of acetamiprid comprises the following steps:

[0019] a. Amination: At room temperature, add 5000L chloroform into the amination reaction kettle, turn on the cooling system, lower the temperature in the kettle to 3°C, and start inserting 200kg of monomethylamine gas into the chloroform solution under the liquid , and at this temperature, add 1000kg of 2-chloro-5-chloromethylpyridine dropwise to the reactor under normal pressure, and control the dropping rate to 4Kg / min, so that the reaction temperature does not exceed 20°C, keep the reaction for 4h, and take samples for analysis After passing the test, heat the reaction kettle to 45°C, drive out the excess methylamine dissolved in chloroform, pass the driven out methylamine into the absorption tank and absorb it with chloroform for the next batch of reactions, cool the material to room temperature, add water and stir 1h, standing for stratification, water layer wastewater to be treated, organi...

Embodiment 2

[0022] The production technology of acetamiprid comprises the following steps:

[0023] a. Amination: At room temperature, add 5000L chloroform into the amination reaction kettle, turn on the cooling system, lower the temperature in the kettle to 4°C, and start inserting 204kg of monomethylamine gas into the chloroform solution under the liquid , and at this temperature, add 1040 kg of 2-chloro-5-chloromethylpyridine dropwise to the reactor under normal pressure, and control the dropping rate at 5Kg / min, so that the reaction temperature does not exceed 20°C, keep the temperature for 5 hours, and take samples for analysis After passing the test, heat the reaction kettle to 46°C, drive out the excess methylamine dissolved in chloroform, pass the driven out methylamine into the absorption tank and absorb it with chloroform for the next batch of reactions, cool the material to room temperature, add water and stir 1h, standing for stratification, water layer wastewater to be treate...

Embodiment 3

[0026] The production technology of acetamiprid comprises the following steps:

[0027] a. Amination: At room temperature, add 5000L chloroform into the amination reaction kettle, turn on the cooling system, lower the temperature in the kettle to 4°C, and start inserting 208kg of monomethylamine gas into the chloroform solution under the liquid , and at this temperature, add 1080kg of 2-chloro-5-chloromethylpyridine dropwise to the reactor under normal pressure, control the dropping rate at 5Kg / min, keep the reaction temperature not exceeding 20°C, keep the reaction for 45h, and take samples for analysis After passing the test, heat the reaction kettle to 47°C, drive out the excess methylamine dissolved in chloroform, pass the driven out methylamine into the absorption tank and absorb it with chloroform for the next batch of reactions, cool the material to room temperature, add water and stir 1h, standing for stratification, water layer wastewater to be treated, organic layer,...

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Abstract

The invention discloses a production process of acetamiprid. The production process comprises steps as follows: a, amination: chloroform is added to an amination reaction kettle at the room temperature and methylamine gas is introduced into a chloroform solution and below the liquid level, 2-chloro-5-nitrapyrin is dropwise added to the reaction kettle under the normal pressure at the room temperature, the reaction temperature is not higher than 20 DEG C, the materials are cooled to the room temperature, added with water, stirred for 1-2 h and left to stand for layering, chloroform is recovered through distillation under the normal pressure, and the materials after desolvation are cooled to the room temperature, added with ethanol for dissolving and then transferred to a next step for reaction; b, condensation: an ethanol solution of amide and ethyl n-cyanoethanimideate are proportionally put into a condensation kettle to be stirred, chilled brine is introduced, the mixture is cooled to 0 DEG C for crystallization, white solids are precipitated and then are filtered and dried, and a filtrate is sent to an ethanol distillation kettle for distillation at the temperature of 78-80 DEG C under the normal pressure, so that ethanol is recovered. The temperature of the amination reaction is lower, few by-products and little waste water are produced, the condensation reaction is simple, the reaction time is short, energy is saved, besides, the condensation reaction is an anhydrous reaction, and no waste water is produced.

Description

technical field [0001] The invention relates to a production process of acetamiprid. Background technique [0002] The currently reported process route is mainly based on 2-chloro-5-chloromethylpyridine as a raw material, and reacts with monomethylamine under the condition of ethanol as a solvent to obtain N-(6-chloro-3-pyridylmethyl)methylamine , followed by the reaction of acetamiprid with ethyl N-cyanoacetimate. In the production process of acetamiprid, the reaction raw material monomethylamine has a strong smell and is volatile, so the consumption of monomethylamine is relatively high. [0003] Therefore, it is necessary to provide a new technical solution to solve the above problems. Contents of the invention [0004] The technical problem to be solved by the present invention is to provide a production process of acetamiprid. [0005] In order to solve the problems of the technologies described above, the production process of Acetamiprid of the present invention ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 洪晓冬张振明赵晶刘凯
Owner JIANGSU CHANGQING AGROCHEM NANTONG
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