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Production process of acetamiprid

A production process and acetamiprid technology are applied in the production process field of acetamiprid, which can solve the problems of high odor of methylamine, high by-products, large amount of waste water, etc., and achieves less three wastes, less by-products, and high total yield Effect

Inactive Publication Date: 2017-12-22
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The currently reported process route is mainly to use 2-chloro-5-chloromethylpyridine and monomethylamine as raw materials to react to obtain N-(6-chloro-3-pyridylmethyl)methylamine, and then react with N-cyanoethyl Ethyl imidate is reacted to obtain acetamiprid. In the actual production process, methylamine has a strong odor, high by-products, and a large amount of waste water. Therefore, it is necessary to provide a new technical solution to solve the above problems

Method used

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  • Production process of acetamiprid
  • Production process of acetamiprid

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Embodiment 1

[0019] The production technology of acetamiprid comprises the following steps:

[0020] (1) Amination: Add 3500L dichloroethane to the amination reaction kettle, cool down to below 0°C, pass 310kg of monomethylamine gas into the solvent, raise the temperature to 45°C after completion, and drop 750kg into the reaction kettle 2-Chloro-5-chloromethylpyridine, after 8 hours of dropwise addition, keep warm at this temperature for 4 hours after the dropwise addition, after the reaction is completed, release the pressure and discharge the amine, and the discharged methylamine is passed into the absorption tank, passed through dichloroethane After absorption, it is used in the next batch. After the amine is discharged, the temperature is lowered to below 25°C and filtered, and the monomethylamine hydrochloride is filtered out. The filtrate is transferred to the next step after removing dichloroethane.

[0021] (2) Condensation: Put the materials in the previous step into the reactor, ...

Embodiment 2

[0023] The production technology of acetamiprid comprises the following steps:

[0024] (1) Amination: Add 3500L tetrahydrofuran into the amination reaction kettle, cool down to below 0°C, pass 310kg of monomethylamine gas into the solvent, raise the temperature to 45°C after completion, and drop 750kg of 2-chloro -5-Chloromethylpyridine, the 8-hour dropwise addition is completed. After the dropwise addition, the temperature is kept at this temperature for 4 hours. Batches, after amine removal, lower the temperature to below 25°C and filter, filter out monomethylamine hydrochloride, remove tetrahydrofuran from the filtrate and transfer to the next step of reaction.

[0025] (2) Condensation: Put the materials in the previous step into the reactor, raise the temperature to 75°C, add 520kg of cyanoethyl ester dropwise, and add dropwise for 5 hours. , to get acetamiprid, and then dry to obtain 990kg of finished product, with a content of 98.5% and a yield of 95%.

Embodiment 3

[0027] The production technology of acetamiprid comprises the following steps:

[0028] (1) Amination: Add 3500L toluene to the amination reaction kettle, cool down to below 0°C, pass 310kg of monomethylamine gas into the solvent, raise the temperature to 45°C after completion, and drop 750kg of 2-chloro -5-Chloromethylpyridine, the 8-hour dropwise addition is completed, the dropwise addition is completed, and the temperature is kept at this temperature for 4 hours. After the reaction is completed, the pressure is released and the amine is discharged. Batch, after amine removal, lower the temperature to below 25°C and filter, filter out monomethylamine hydrochloride, and transfer the filtrate to the next step after removing toluene.

[0029] (2) Condensation: Put the materials in the previous step into the reactor, raise the temperature to 75°C, add 520kg of cyanoethyl ester dropwise, and add dropwise for 5 hours. , to get acetamiprid, and then dry to obtain 980kg of finished...

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Abstract

The invention discloses a production process of acetamiprid. The production process comprises the following steps: (1) amination: adding a solvent into an amination reaction kettle, reducing the temperature, introducing a certain quantity of monomethylamine gas into the solvent, controlling under certain temperature conditions, adding 2-chloro-5-chloromethylpyridine into the reaction kettle, reacting, increasing the temperature for amine discharge, then reducing the temperature, filtering, filtering out methylamine hydrochloride, removing the solvent from a filtrate and transferring to the next step; and (2) condensation: controlling a material obtained from the above step under certain temperature conditions, dropwise adding ethyl N-cyanoethanimideate, reacting, reducing the temperature, filtering, obtaining the acetamiprid, drying, distilling a filtrate and recovering ethanol. The production process disclosed by the invention is high in amination reaction yield, simple in post-treatment, incapable of producing wastewater, simple in condensation reaction, high in yield and free from wastewater production.

Description

Technical field [0001] The invention relates to a production process of acetamiprid and belongs to the technical field of pesticide production. Background technique [0002] The currently reported process route mainly uses 2-chloro-5-chloromethylpyridine and monomethylamine as raw materials to react to obtain N-(6-chloro-3-pyridylmethyl)methylamine, which is then reacted with N-cyanoethyl Acetamiprid is obtained from the reaction of ethyl imidate. In the actual production process, methylamine has a strong smell, high by-products, and a large amount of waste water. Therefore, a new technical solution needs to be provided to solve the above problems. Contents of the invention [0003] The problem to be solved by the present invention is to provide a production technology of acetamiprid with reasonable technology and high total yield. [0004] In order to solve the above problems, the production process of acetamiprid of the present invention includes the following steps: ...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 吕良忠贺书泽马长庆丁华平
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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