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Synthetic method of 1,1-dichloro-2-nitroethylene and nitenpyram

A synthetic method and technology of nitroethylene, which is applied in the field of pesticides, can solve the problems of low process yield, achieve large specific surface area, increase product yield, and reduce the degree of salt pollution

Inactive Publication Date: 2019-09-03
江苏克胜集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The second object of the present invention is to provide a synthetic method of nitenpyram, which solves the problem of low yield in the existing process

Method used

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  • Synthetic method of 1,1-dichloro-2-nitroethylene and nitenpyram
  • Synthetic method of 1,1-dichloro-2-nitroethylene and nitenpyram
  • Synthetic method of 1,1-dichloro-2-nitroethylene and nitenpyram

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Synthesis of 1,1-dichloro-2-nitroethylene:

[0060] 1. Turn on the hydrochloric acid feed pump and nitric acid feed pump, and pour hydrochloric acid and nitric acid into the mixer quantitatively.

[0061] 2. Open the feed pump of 1,1-dichloroethylene, pump raw materials into the microchannel reactor, and control the flow rate ratio of 1,1-dichloroethylene, hydrochloric acid and nitric acid to be 1:1.4:1.3 (mass ratio, Hereinafter the same), at this moment, the mol ratio of 1,1-dichloroethylene, hydrochloric acid and nitric acid was 1:1.1:1.3, and the residence time of the raw material in the microchannel reactor was 2min.

[0062] 3. The reaction solution in the second step enters the layered kettle, and is allowed to stand for layering. The acid water in the upper layer is discharged to the pollution control center, and the material liquid in the lower layer is the intermediate 1,1,1-trichloro-2-nitroethane. The quality of the product was detected: the content of 1,1,...

Embodiment 2

[0066] The difference from Example 1 is mainly that the molar ratio of 1,1,1-trichloro-2-nitroethane to liquid caustic soda is different in the fourth step reaction, which is 1:2. The specific synthesis method is as follows:

[0067] 1. Turn on the hydrochloric acid feed pump and nitric acid feed pump, and pour hydrochloric acid and nitric acid into the mixer quantitatively.

[0068] 2. Turn on the feed pump of 1,1-dichloroethylene, pump raw materials into the microchannel reactor, and control the flow rate ratio of 1,1-dichloroethylene, hydrochloric acid and nitric acid to 1:1.4:1.3, at this time 1 , The molar ratio of 1-dichloroethylene, hydrochloric acid and nitric acid is 1:1.1:1.3.

[0069] 3. The reaction solution in the second step enters the layered kettle, and is allowed to stand for layering. The acid water in the upper layer is discharged to the pollution control center, and the material liquid in the lower layer is the intermediate 1,1,1-trichloro-2-nitroethane. T...

Embodiment 3

[0073] Its main difference with embodiment 1 is that the concentration of liquid caustic soda is different, is 20%, and concrete process is as follows:

[0074] 1. Turn on the hydrochloric acid feed pump and nitric acid feed pump, and pour hydrochloric acid and nitric acid into the mixer quantitatively.

[0075] 2. Turn on the feed pump of 1,1-dichloroethylene, pump raw materials into the microchannel reactor, and control the flow rate ratio of 1,1-dichloroethylene, hydrochloric acid and nitric acid to 1:1.4:1.3, at this time 1 , The molar ratio of 1-dichloroethylene, hydrochloric acid and nitric acid is 1:1.1:1.3.

[0076] 3. The reaction solution in the second step enters the layered kettle, and is allowed to stand for layering. The acid water in the upper layer is discharged to the pollution control center, and the material liquid in the lower layer is the intermediate 1,1,1-trichloro-2-nitroethane. The quality of the product was detected: the content of 1,1,1-trichloro-2-...

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Abstract

The invention provides synthesis methods of 1,1-dichloro-2-nitroethylene and nitenpyram. The synthesis method of the 1,1-dichloro-2-nitroethylene comprises the following steps of enabling 1,1,1-trichloro-nitroethane and caustic soda liquid to react in a micro-channel reactor, layering an obtained product, and taking subnatant feed liquid which is the 1,1-dichloro-2-nitroethylene. The synthesis method is carried out in the micro-channel reactor; the 1,1-dichloro-2-nitroethylene has a bigger specific surface area; the contact efficiency between the 1,1,1-trichloro-nitroethane and the caustic soda liquid can be improved; thus, the reaction rate of raw materials is improved; the product yield is improved. The micro-channel reactor is utilized; the yield of the 1,1-dichloro-2-nitroethylene is up to 90 percent or above; the purity is also increased to 90 percent or above. The improvement of the utilization rate, to the caustic soda liquid, of the synthesis method is also shown from a side; the levels of caused alkali population and salt pollution are decreased; the treatment difficulty of tail water is lowered.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a synthesis method of 1,1-dichloro-2-nitroethylene and nitenpyram. Background technique [0002] Nitenpyram is a new species of important neonicotinoid insecticides, which has the characteristics of high efficiency, broad spectrum, low toxicity, and resistance. It has been widely used in the world and is an important food crop. , economic crops and other excellent control pesticides. For some insect pests that are difficult to be controlled by existing domestic insecticides, especially aphids, leafhoppers, hemiptera pests, rice planthoppers, etc., it has shown excellent activity, and the control cost is low. Nitenpyram has been widely used in veterinary medicine due to its low toxicity and specific effects on target pests. At present, it has been widely used in the world (including China), and the prospect is very broad. [0003] The traditional synthetic route of nitenpyram is: [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C201/12C07C205/02C07D213/61
Inventor 秦立华吴成伟吴言富刘冰
Owner 江苏克胜集团股份有限公司
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