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

A kind of preparation method of 2-chloropropenyl isothiocyanate

A technology of chloropropenyl isothiocyanate and dichloropropene, which is applied in the field of preparation of 2-chloropropenyl isothiocyanate, can solve the problems of unsuitable for green and clean industrial production, complex experimental operation, and secondary environmental pollution and other problems, to achieve the effect of less three wastes, simple process and high safety factor

Active Publication Date: 2021-03-16
湖南海利常德农药化工有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, although it has advantages such as shorter reaction time and higher yield, its experimental operation is comparatively complicated; Simultaneously this method is greater than the molar charging capacity of 2,3-dichloropropene due to the molar charging capacity of sodium thiocyanate, There are a lot of thiocyanate ions in the wastewater, so this method is also not suitable for green and clean industrial production
[0005] In summary, there are following problems in the existing method for preparing 2-chloropropenyl isothiocyanate: complex process, difficult operation, high production cost, slow reaction speed, large amount of three wastes, easy to cause secondary pollution to the environment, etc.

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

[0027] A kind of preparation method of 2-chloropropenyl isothiocyanate, with 2,3-dichloropropene and ammonium thiocyanate as reaction raw material, with water as reaction solvent, under the effect of phase transfer catalyst in microreactor Prepare 2-chloropropenyl isothiocyanate, comprising the following steps:

[0028] (1) Dissolve 77.2g (1moL) ammonium thiocyanate in 85g water to obtain an aqueous solution of ammonium thiocyanate; stir and dissolve 2.3g of a phase transfer catalyst (tetrabutylammonium chloride) in an aqueous solution of ammonium thiocyanate , to obtain a mixed solution.

[0029] (2) The selected microreactor (commercially available) includes 10 reaction modules, and each reaction module is combined in series, numbered sequentially from the entrance to the exit as the first reaction module, the second reaction module, the third reaction module, and the fourth reaction module. module, fifth reaction module, sixth reaction module, seventh reaction module, eigh...

Embodiment 2

[0032] A kind of preparation method of 2-chloropropenyl isothiocyanate, with 2,3-dichloropropene and ammonium thiocyanate as reaction raw material, with water as reaction solvent, under the effect of phase transfer catalyst in microreactor Prepare 2-chloropropenyl isothiocyanate, comprising the following steps:

[0033] (1) Dissolve 77.2g (1moL) of ammonium thiocyanate in 85g of water to obtain an aqueous solution of ammonium thiocyanate; stir and dissolve 2.3g of a phase transfer catalyst (tetrabutylammonium bromide) in an aqueous solution of ammonium thiocyanate , to obtain a mixed solution.

[0034] (2) The selected microreactor includes 10 reaction modules, and each reaction module is combined in series, numbered sequentially from the entrance to the exit as the first reaction module, the second reaction module, the third reaction module...the tenth reaction module. Control the temperature of each reaction module in the microreactor to be 80 DEG C, the mixed solution obta...

Embodiment 3

[0037] A kind of preparation method of 2-chloropropenyl isothiocyanate, with 2,3-dichloropropene and ammonium thiocyanate as reaction raw material, with water as reaction solvent, under the effect of phase transfer catalyst in microreactor Prepare 2-chloropropenyl isothiocyanate, comprising the following steps:

[0038] (1) 77.2g (1moL) ammonium thiocyanate was dissolved in 85g water to obtain an aqueous solution of ammonium thiocyanate; 2.3g of phase transfer catalyst (benzyltriethylammonium bromide) was stirred and dissolved in ammonium thiocyanate aqueous solution to obtain a mixed solution.

[0039] (2) The selected microreactor includes 10 reaction modules, and each reaction module is combined in series, numbered sequentially from the entrance to the exit as the first reaction module, the second reaction module, the third reaction module...the tenth reaction module. Control the temperature of each reaction module in the microreactor to be 80 DEG C, the mixed solution obt...

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

No PUM Login to View More

Abstract

The invention discloses apreparation method of 2-chloro-3-isothiocyanato-prop-1-ene. According to the preparation method, the 2-chloro-3-isothiocyanato-prop-1-ene is prepared with 2,3-dichloropropeneand ammonium thiocyanate as reaction raw materials and water as a reaction solvent under the action of a phase transfer catalyst in a microreactor. Compared with a kettle type reactor adopted in the prior art, the microreactor adopted by the method has the advantages of full contact in a two phase reaction, good mass and heat transfer effect, high process controllability, high safety coefficient and the like, the 2-chloro-3-isothiocyanato-prop-1-ene can be prepared efficiently in an environmentally friendly manner at low cost, and high product yield and product content are realized. The preparation method has the advantages of ready availability of raw materials, simple process, easiness and convenience in operation, low cost, high reaction speed, less three wastes (waste gas, waste waterand industrial residue), high product yield, high product content, environmental friendliness and the like, is suitable for industrial production, and has a very good application prospect.

Description

technical field [0001] The invention relates to a preparation method of 2-chloropropenyl isothiocyanate. [0002] technical background [0003] 2-Chloropropenyl isothiocyanate is the precursor of 2-chloro-5-chloromethylthiazole, which is a second-generation nicotinic insecticide thiazole pesticide Clothiazole The key intermediate of oxazine and clothianidin. Therefore, it is of great significance to obtain high-quality 2-chloropropenyl isothiocyanate by an efficient and environmentally friendly preparation method for the research on the new process of 2-chloro-5-chloromethylthiazole. [0004] At present, there are many preparation methods of 2-chloroallyl isothiocyanate reported both at home and abroad, such as the Chinese patent literature whose publication number is CN102363605A discloses a kind of preparation method of 2-chloroallyl isothiocyanate, Using water as a solvent, react 2,3-dichloropropene with sodium thiocyanate, and react for 20 hours under the action of a ph...

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 Patents(China)
IPC IPC(8): C07C331/22
CPCC07C331/22
Inventor 程超刘卫东杜升华兰世林陈郭芹刘源
Owner 湖南海利常德农药化工有限公司
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