Synthetic method of isophorone diisocyanate

A technology of isophorone diisocyanate and isophorone diamine is applied in the field of synthesis of isophorone diisocyanate, which can solve the problems of danger in use, transportation and storage, high volatility and difficulty in metering, and achieve product Post-processing is simple and easy, high purity, and safe to use

Inactive Publication Date: 2013-06-12
CHAMBROAD CHEM IND RES INST CO LTD +1
View PDF6 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Traditional isocyanate synthesis methods include phosgene method, Curtius rearrangement method, halogen β elimination method, one-step carbonyl method, carbamate thermal decomposition method, etc., among which phosgene method is the most commonly used, but phosgene is a highly toxic gas , low boiling point, high volatility, there are great dangers in the process of use, transportation and storage, and a variety of strict safety measures need to be adopted. A little carelessness will cause catastrophic accidents. In addition, it is difficult to use measurement

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
  • Synthetic method of isophorone diisocyanate
  • Synthetic method of isophorone diisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] Example 1

[0023] (1) Dissolve 17 g of isophorone diamine in 195.5 g of chloroform, and dissolve 29.7 g of solid phosgene in 342 g of chloroform;

[0024] (2) Add the isophorone diamine solution dropwise to the solid phosgene solution at -20°C, and react for 7 hours. During this process, nitrogen is continuously introduced for gas replacement;

[0025] (3) The above reaction solution was heated to reflux, reacted for 5 hours, after the reaction was completed, cooled, filtered with suction, and the filtrate was distilled under reduced pressure to obtain 20.7 g of product. The product yield was 93.2% and the purity was 97.5%.

Example Embodiment

[0026] Example 2

[0027] (1) Dissolve 34 g of isophorone diamine and 0.64 g of N,N-dimethylformamide in 193 g of chloroform, and dissolve 29.7 g of solid phosgene in 168.3 g of chloroform;

[0028] (2) Add the isophorone diamine solution dropwise to the solid phosgene solution at 5°C, and react for 2 hours. During this process, nitrogen is continuously introduced for gas replacement;

[0029] (3) The above reaction liquid was heated to reflux, reacted for 2 hours, after the reaction was completed, cooled, filtered with suction, and the filtrate was distilled under reduced pressure to obtain the product 19.0, the product yield was 85.5%, and the purity was 94.3%.

Example Embodiment

[0030] Example 3

[0031] (1) Dissolve 25.5 g of isophorone diamine and 2.76 g of paraformaldehyde in 203.5 g of dichloroethane, and dissolve 29.7 g of solid phosgene in 240.3 g of dichloroethane;

[0032] (2) Add the isophorone diamine solution dropwise to the solid phosgene solution at -10°C, and react for 4.5 hours. During this process, nitrogen is continuously introduced for gas replacement;

[0033] (3) The above reaction solution was heated to reflux, reacted for 8 hours, after the reaction was completed, cooled, filtered with suction, and the filtrate was distilled under reduced pressure to obtain 20.2 g of product. The product yield was 90.8% and the purity was 93.1%.

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 relates to the technical field of organic synthesis, and particularly relates to a synthetic method of isophorone diisocyanate. According to the method, isophorone diamine and triphosgene are taken as materials to react; and phosgene or diphosgene in the past is replaced by triphosgene to react with the isophorone diamine, so as to prepare the isophorone diisocyanate. Therefore, the synthetic method is simple and reasonable in manufacturing process, safe and reliable to operate, high in reaction yield, low in production cost and easier to achieve industrial production; the operation environment is improved; and the environmental pollution is also reduced.

Description

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

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
Owner CHAMBROAD CHEM IND RES INST CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products