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

Method for preparing cyclohexyl isocyanate from solid phosgene

A technology of solid phosgene and isocyanic acid, which is applied in the preparation of isocyanic acid derivatives, chemical instruments and methods, preparation of organic compounds, etc. problem, to achieve high competitive advantage, no significant toxicity, chemical stability effect

Inactive Publication Date: 2020-09-15
XINYI AGRI CHEM PLANT JIANGSU PROV
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosgene is a colorless gas at normal temperature with a smell of rotten grass. It is a yellow-green liquid at low temperature. It is chemically unstable and will be hydrolyzed rapidly when it meets water to generate hydrogen chloride, which will increase the safety production cost in the production process of cyclohexyl isocyanate.

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing cyclohexyl isocyanate from solid phosgene
  • Method for preparing cyclohexyl isocyanate from solid phosgene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The invention provides a kind of method that solid phosgene prepares cyclohexyl isocyanate, comprises the steps:

[0045] S1. Put 151g of solid phosgene into a four-necked flask, add toluene into the solid phosgene, and dissolve the solid phosgene in the toluene solvent; wherein, the mass ratio of solid phosgene to toluene is 1.15:1; it is used to dissolve solid The system temperature of phosgene is 30°C;

[0046] S2. Slowly add the toluene solution containing 151g of solid phosgene to a 2000ml four-neck flask equipped with cyclohexylamine hydrochloride at a rate of 3ml / min, heat to 100°C, and conduct the reaction between solid phosgene and cyclohexylamine hydrochloride. Phosgenation reaction until the solution in the four-necked flask is clarified to obtain the crude product of cyclohexyl isocyanate; wherein, the rate of addition of the toluene solution of solid phosgene is controlled so that the slight negative pressure of the phosgenation reaction system is -80mm wat...

Embodiment 2

[0057] S1. Put 151g of solid phosgene into a four-necked flask, add toluene into the solid phosgene, and dissolve the solid phosgene in the toluene solvent; wherein, the mass ratio of solid phosgene to toluene is 1.15:1; it is used to dissolve solid The system temperature of phosgene is 30°C;

[0058] S2, in the 2000ml four-neck flask that cyclohexylamine hydrochloride is housed, add 4g triethylamine catalyst, the toluene solution that will contain 151g solid phosgene is slowly added with the speed of 3ml / min and cyclohexylamine hydrochloride is housed , heated to 100°C, the solid phosgene and cyclohexylamine hydrochloride undergo phosgenation until the solution in the four-necked flask is clear, and the crude product of cyclohexyl isocyanate is obtained; among them, the toluene solution of the solid phosgene is controlled The addition rate makes the slight negative pressure of the phosgenation reaction system -80mm water column;

[0059] S3. Separating and purifying the cycl...

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 provides a method for preparing cyclohexyl isocyanate from solid phosgene. The method comprises the following steps: S1, dissolving the solid phosgene in a solvent; S2, slowly adding thesolid phosgene solution into cyclohexylamine hydrochloride, heating, and carrying out a phosgenation reaction to obtain a crude product of cyclohexyl isocyanate; and S3, separating and purifying to obtain the cyclohexyl isocyanate. According to the method provided by the invention, the cyclohexyl isocyanate is prepared through the reaction of the solid phosgene and the cyclohexylamine hydrochloride, so that the yield of the cyclohexyl isocyanate is guaranteed, the chemical property of the solid phosgene is relatively stable, no obvious toxicity exists, and the method has the advantages of improving the safety and reducing the safety production cost.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing cyclohexyl isocyanate from solid phosgene Background technique [0002] Cyclohexyl isocyanate is an organic raw material, used as an intermediate in the synthesis of medicines or pesticides, used in the production of herbicides such as hexazinone in pesticides, and used in the production of western medicines and hexythiazox in medicine. [0003] The existing cyclohexyl isocyanate is synthesized by phosgene and cyclohexylamine hydrochloride. The raw material phosgene is highly toxic, non-combustible, has high chemical reactivity, and is highly corrosive when exposed to water. Phosgene is produced from the synthesis of carbon monoxide and chlorine. Phosgene is a colorless gas at normal temperature with a smell of rotten grass. It is a yellow-green liquid at low temperature. It is chemically unstable and will be hydrolyzed rapidly when it ...

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
IPC IPC(8): C07C263/10C07C265/10
CPCC07C263/10C07C2601/14C07C265/10
Inventor 纪传武魏星姚仲用孙新许思茹
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com