Continuous production method of high-efficiency and low-toxicity pesticide-acephate

A kind of acephate, production method technology, is applied in the continuous production field of high-efficiency and low-toxicity insecticide acephate, can solve the disadvantageous large-scale production of acephate, poor production stability and safety, occupying To solve problems such as large land area, to optimize the reaction effect, overcome the effects of large equipment volume and long residence time

Active Publication Date: 2015-01-07
安道麦股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the production of acephate is still at the traditional intermittent production level, with small production capacity, many equipments, large floor area, low device efficiency...

Method used

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  • Continuous production method of high-efficiency and low-toxicity pesticide-acephate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Acylation reaction process

[0031] Control the flow rate of 70% methamidophos to 2000Kg / h, acetic anhydride to 1240Kg / h, catalyst sulfuric acid to 60Kg / h, mix with the solvent dichloromethane, and continuously enter the first-stage acylation reactor, keep at 60°C, stay for 30min and then overflow to II Grade acylation reactor, keep at 70°C, stay for 120min and then enter the neutralization reaction process. Sampling analysis: the content of acephate in the acylation reaction liquid is 54.3%, and the content of methamidophos is <0.05%.

[0032] 2. Neutralization reaction process

[0033] Control the acylation reaction solution to 3300Kg / h, water to 500Kg / h, ammonia gas flow to 250Kg / h, control the neutralization reaction temperature to 35°C, pH=7.5, and enter the extraction process after staying for 30 minutes.

[0034] 3. Extraction process

[0035] Control the neutralization liquid at the bottom of the extraction tower to 4050Kg / h, the flow of chloroform at the ...

Embodiment 2

[0042] 1. Acylation reaction process

[0043] Control the flow rate of 70% methamidophos to 1800Kg / h, acetic anhydride to 1500Kg / h, catalyst phosphoric acid to 60Kg / h, mix with the solvent chloroform, continuously enter the first-stage acylation reactor, keep at 20°C, and overflow to the second-stage acylation reactor after staying for 60 minutes. The reactor was kept at 80°C, and after staying for 180 minutes, it entered the neutralization reaction process. Sampling analysis: the content of acephate in the acylation reaction liquid is 53.5%, and the content of methamidophos is <0.05%.

[0044] 2. Neutralization reaction process

[0045] Control the acylation reaction solution to 3000Kg / h, water to 500Kg / h, ammonia gas flow rate to 250Kg / h, control the neutralization reaction temperature to 10°C, pH=8, and enter the extraction process after staying for 60 minutes.

[0046] 3. Extraction process

[0047] Control the neutralization liquid at the bottom of the extraction tower...

Embodiment 3

[0054] 1. Acylation reaction process

[0055] Control the flow rate of 70% methamidophos to 2000Kg / h, acetic anhydride to 1300Kg / h, catalyst dimethyl sulfate to 60Kg / h, mix with solvent chloroform, and continuously enter the first-stage acylation reactor, keep at 80°C, and overflow to In the second-stage acylation reactor, keep at 80°C, stay for 60 minutes, and then enter the neutralization reaction process. Sampling analysis: the content of acephate in the acylation reaction liquid is 53.8%, and the content of methamidophos is <0.05%.

[0056] 2. Neutralization reaction process

[0057] Control the acylation reaction solution to 3500Kg / h, water to 500Kg / h, ammonia water flow rate to 250Kg / h, control the neutralization reaction temperature to 50°C, pH=7, and enter the extraction process after staying for 5 minutes.

[0058] 3. Extraction process

[0059] Control the neutralization liquid at the bottom of the extraction tower to 4150Kg / h, the flow of chloroform at the top of...

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Abstract

The invention provides a continuous production method of acephate. The continuous production method comprises the following steps: (1) acylation reaction: continuously adding methamidophos, acetic anhydride, a solvent and a catalyst into an acylation device in a certain proportion, and reacting for 65-240 minutes at 20-80 DEG C to obtain a reaction liquid; (2) neutralization reaction: introducing the reaction liquid obtained in the step (1) into a neutralization reactor, and continuously mixing with ammonia or ammonia water for 5-60 minutes at 10-50 DEG C to obtain a neutralization liquid; (3) extraction: introducing the neutralization liquid into an extraction tower to perform reverse extraction; (4) evaporation and concentration: performing evaporation and concentration on an extraction liquid in a double-effect evaporator; and (5) crystallization and drying: crystallizing a concentrated extraction liquid at 5-25 DEG C, then filtering crystallized solids by virtue of a filtering machine, and finally drying the solids in a dryer to obtain acephate. The continuous production method provided by the invention achieves the continuous operation and automatic control in a production process of acephate, and has very strong practicability.

Description

technical field [0001] The invention relates to the field of pesticide production methods, in particular to a continuous production method for the high-efficiency and low-toxicity insecticide acephate. Background technique [0002] Acephate (also known as total effect phosphorus), the chemical name is O,S-dimethyl-N-acetylthiophosphoramide, is an N-acetylated derivative of the organophosphorus insecticide methamidophos. Its structural formula is: [0003] [0004] Compared with methamidophos, due to the change of structure (increased acetyl group), the drug effect on lower organisms remains basically unchanged, while the toxicity to higher organisms is greatly reduced. The efficacy experiments show that acephate can effectively control aphids, thrips, moths, sawflies and lepidoptera pests. The characteristic high-efficiency, low-toxicity, low-residue, broad-spectrum organophosphorus insecticide is one of the most promising substitutes for the highly toxic methamidophos ...

Claims

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Application Information

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IPC IPC(8): C07F9/24
Inventor 刘安平殷宏薛光才刘孝平肖国华周骋王洪群杨雄吴军
Owner 安道麦股份有限公司
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