Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Industrial production method of 2,6-difluoroaniline

A technology of difluoroaniline and its production method, which is applied in the field of pesticide preparation, can solve the problems of product impurities reducing product purity, impurities reducing product purity, product heat damage, etc., achieving industrial continuous production, controllable reaction, and improved production effect of ability

Inactive Publication Date: 2021-03-09
南京硕达生物科技有限公司
View PDF0 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A lot of practical experience shows that there will be an exothermic and gas-producing stage during the heating process of the Hofmann amide degradation reaction. This process will cause a short-term intense exothermic process, which will cause the product to be destroyed by heat, and impurities will be generated to reduce the purity of the product.
At the same time, short-term intense heat release may also lead to material loss during the production process.
[0004] Aiming at the problem of severe exothermic reaction in the traditional Hofmann degradation reaction process, which leads to the thermal damage of the product and the formation of impurities to reduce product purity and easy flushing in the production process, the present invention proposes a CSTR mode for the production and preparation of 2,6-difluoroaniline Methods

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of industrialized production method of 2,6-difluoroaniline, operation steps are as follows in sequence:

[0026] S1: Configuration solution: add sodium hydroxide aqueous solution and 2,6-difluorobenzamide to reaction kettle 1 in sequence, the mass fraction of sodium hydroxide in sodium hydroxide aqueous solution is 20%, sodium hydroxide aqueous solution and 2,6 -The mass ratio of difluorobenzamide is 1:3, and it is prepared into solution 1 by stirring evenly for subsequent use; water and sodium hypochlorite are added successively in reaction kettle 2, and the mass ratio of sodium hypochlorite and water is 1:8, and it is prepared by mixing uniformly to form solution 2 for subsequent use ;

[0027] S2: Set up equipment: connect the reactor 1 described in step S1 with the reactor 3 through the diaphragm pump 1, connect the reactor 2 described in the step S1 with the reactor 3 through the diaphragm pump 2, and connect the reactor 3 with the reactor The kettle 4 is c...

Embodiment 2

[0033] A kind of industrialized production method of 2,6-difluoroaniline, operation steps are as follows in sequence:

[0034] S1: Configuration solution: add sodium hydroxide aqueous solution and 2,6-difluorobenzamide to reaction kettle 1 in sequence, the mass fraction of sodium hydroxide in sodium hydroxide aqueous solution is 23%, sodium hydroxide aqueous solution and 2,6 -The mass ratio of difluorobenzamide is 1:3, and it is prepared into solution 1 by stirring evenly for subsequent use; water and sodium hypochlorite are added successively in reaction kettle 2, and the mass ratio of sodium hypochlorite and water is 1:8, and it is prepared by mixing uniformly to form solution 2 for subsequent use ;

[0035] S2: Set up equipment: connect the reactor 1 described in step S1 with the reactor 3 through the diaphragm pump 1, connect the reactor 2 described in the step S1 with the reactor 3 through the diaphragm pump 2, and connect the reactor 3 with the reactor The kettle 4 is c...

Embodiment 3

[0041] A kind of industrialized production method of 2,6-difluoroaniline, operation steps are as follows in sequence:

[0042] S1: Configuration solution: add sodium hydroxide aqueous solution and 2,6-difluorobenzamide to reaction kettle 1 in sequence, the mass fraction of sodium hydroxide in sodium hydroxide aqueous solution is 25%, sodium hydroxide aqueous solution and 2,6 - The mass ratio of difluorobenzamide is 1:2, and it is prepared into solution 1 by stirring evenly for subsequent use; water and sodium hypochlorite are added successively in reaction kettle 2, and the mass ratio of sodium hypochlorite and water is 1:8, and it is prepared by mixing evenly to form solution 2 for subsequent use ;

[0043] S2: Set up equipment: connect the reactor 1 described in step S1 with the reactor 3 through the diaphragm pump 1, connect the reactor 2 described in the step S1 with the reactor 3 through the diaphragm pump 2, and connect the reactor 3 with the reactor The kettle 4 is con...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
Login to View More

Abstract

The invention discloses an industrial production method of 2,6-difluoroaniline, wherein the industrial production method comprises the following steps: S1, preparation of a solution: mixing a sodium hydroxide aqueous solution and 2,6-difluorobenzamide to obtain a solution 1, and taking a sodium hypochlorite aqueous solution as a solution 2; S2, equipment building: connecting reaction kettles 1 and2 with a reaction kettle 3 through diaphragm pumps 1 and 2 respectively, and connecting the reaction kettle 3 with a reaction kettle 4 through an overflow pipe; S3, degradation reaction: simultaneously pumping the solution 1 and the solution 2 into the reaction kettle 3 by using the diaphragm pumps 1 and 2, and enabling a reaction liquid to flow out of an overflow pipe to the reaction kettle 4; S4, primary distillation: evaporating the product 2,6-difluoroaniline to a receiving kettle along with water vapor in the overflow pipe; and S5, rectifying of a crude product: rectifying after a liquidin the receiving kettle is layered. The CSTR mode is adopted to control the addition amount and time of the reaction liquid, so that the reaction is more controllable, and the problems of product heating damage and easy material flushing in the production process caused by violent material heat release in traditional kettle type reaction are avoided.

Description

technical field [0001] The invention relates to the field of preparation methods of pesticides, in particular to an industrial production method of 2,6-difluoroaniline. Background technique [0002] 2,6-Difluoroaniline, CAS: 5509-65-9, colorless or pale yellow liquid, boiling point 144°C-148°C. It is mainly used as a key intermediate for the synthesis of new pesticides, insecticides and herbicides, and can also be used to prepare liquid crystal materials for fuel cells and electronics industries. 2,6-Difluoroaniline is a key intermediate for the synthesis of new benzoylurea pesticides, which can be made into various insecticides and herbicides such as hexaflumuron, fluflubenzuron, diflubenuron, and fenfluranuron . This series of pesticides has the effect of preventing larvae from moulting and growing into adults, so that their dosage is small, their toxicity is low, and they have no drug resistance. They are new types of pesticides with high efficiency and low toxicity. T...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/56C07C209/84C07C209/86C07C211/52
CPCC07C209/56C07C209/84C07C209/86C07C211/52
Inventor 席亚男张俊
Owner 南京硕达生物科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products