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Method for continuously producing imidacloprid intermediate cycloheptene-2-aldehyde-5-alkene

A production method and intermediate technology, applied in the field of pesticide production, to achieve the effects of short reaction time, high selectivity and high yield

Inactive Publication Date: 2011-05-04
荆州沙隆达控股有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Purpose of the present invention is exactly at the defective of existing imidacloprid intermediate cyclohept-2-aldehyde-5-ene intermittent production method, provides a kind of imidacloprid intermediate cyclohepta-2-aldehyde-5-ene continuous production method, with Make up for the shortcomings of existing technology

Method used

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  • Method for continuously producing imidacloprid intermediate cycloheptene-2-aldehyde-5-alkene
  • Method for continuously producing imidacloprid intermediate cycloheptene-2-aldehyde-5-alkene

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Effect test

Embodiment 1

[0010] The cyclopentadiene and acrolein are transported to the tubular mixed reaction condenser 3 through the volume ratio of 1.1:1 through the metering pumps 1 and 2 for reaction, and then to the tubular reactor 4 and the retention tank 5 in the form of overflow 1. Receiving kettle 6 for continuous reaction, and finally going to distillation kettle 7 for separation. After separation, the product is stored in storage tank 8, and the reaction temperature is 30°C. After 2 hours of feeding, the temperature was kept for 1 hour, and the content of the materials in the kettle was measured: 0.1% cyclopentadiene, 0.05% acrolein, 95% cycloheptanal, and the yield was 97.19%.

[0011] The process equipment of the continuous production method of the imidacloprid intermediate cyclohept-2-alde-5-ene comprises a tubular mixed reaction condenser, and the bottom outlet of the tubular mixed reaction condenser is connected to the feed port of the tubular reactor 1. The discharge port of the tubu...

Embodiment 2

[0013] The cyclopentadiene and acrolein are transported to the tubular mixed reaction condenser 3 through the volume ratio of 1.5:1 through the metering pumps 1 and 2 for reaction, and then to the tubular reactor 4 and the retention tank 5 sequentially in the form of overflow 1. Receiving tank 6 for continuous reaction, and finally going to distillation tank 7 for separation. After separation, the product is stored in storage tank 8, and the reaction temperature is 60°C. After 2 hours of feeding, the temperature was kept for 1 hour, and the content of the materials in the kettle was measured: 0.5% cyclopentadiene, 1.0% acrolein, 93% cycloheptanal, and the yield was 93.38%.

[0014] The process equipment of the continuous production method of the imidacloprid intermediate cyclohept-2-alde-5-ene comprises a tubular mixed reaction condenser, and the bottom outlet of the tubular mixed reaction condenser is connected to the feed port of the tubular reactor 1. The discharge port of ...

Embodiment 3

[0016] The cyclopentadiene and acrolein are transported to the tubular mixed reaction condenser 3 through the volume ratio of 1.3:1 through the metering pumps 1 and 2 for reaction, and then sequentially sent to the tubular reactor 4 and the residence tank 5 in the form of overflow 1. Receiving tank 6 for continuous reaction, and finally going to distillation tank 7 for separation. After separation, the product is stored in storage tank 8, and the reaction temperature is 40°C. After 2 hours of feeding, the heat preservation was carried out for 1 hour, and the content of the materials in the kettle was measured: 0.1% cyclopentadiene, 4.0% acrolein, 95.0% cycloheptaldehyde, and the yield was 86.68%.

[0017] The process equipment of the continuous production method of the imidacloprid intermediate cyclohept-2-alde-5-ene comprises a tubular mixed reaction condenser, and the bottom outlet of the tubular mixed reaction condenser is connected to the feed port of the tubular reactor 1...

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Abstract

The invention relates to a method for producing pesticides, in particular to a method for continuously producing imidacloprid intermediate cycloheptene-2-aldehyde-5-alkene. The method comprises the following steps of: conveying cyclopentadiene and acrolein according to the volume ratio of the cyclopentadiene to the acrolein of 1.1-1.5:1 to a tube type mixed reaction condenser by using a metering pump to react; performing continuous reactions in a tubular reactor, a tubular reactor, a residence kettle and an acceptance kettle sequentially in an overflow mode; and separating in a distilling kettle, wherein the reaction temperature is between 30 and 60 DEG C. The method overcomes the defects that power consumption of a batch reaction is large, materials are mixed non-uniformly, temperature is difficult to control and blanking accidents are easy to occur and has the advantages of short reaction time, high selectivity of a chemical synthetic reaction and high yield, wherein the yield is increased from 93 percent to 97 percent. On the basis of stabilizing the yield, the consumption of raw material acrolein is reduced from 900 kilograms per ton to 780 kilograms per ton.

Description

technical field [0001] The invention relates to a method for producing pesticides, in particular to a method for continuously producing cyclohept-2-aldehyde-5-ene, an intermediate of the pesticide insecticide imidacloprid. Background technique [0002] Imidacloprid, that is, 1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylamine is a systemic, contact, stomach poisoning and nitromethylene insecticide The agent is the action body of nicotinic acid acetylcholinesterase receptor, which interferes with the motor nervous system of pests and causes the chemical signal transmission to fail. There is no problem of cross-resistance, and it is used to control piercing-sucking mouthparts pests and their resistant strains. It can be widely used in various crops such as rice, wheat, cotton, vegetables, tea, flowers and fruit trees to control piercing and sucking pests such as rice planthopper, aphid, leafhopper, pear psyllid, thrips and whitefly. It is also a good root systemic inse...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/43C07C45/69
Inventor 鄢圣光薛光才熊金华李传林刘孝平张涛廖艳
Owner 荆州沙隆达控股有限公司
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