Synthetic method of high-purity high-yield cyanate ester resin

A technology of cyanate ester resin and synthesis method, which is applied in the field of synthesis of high-purity and high-yield cyanate ester resin, can solve the problems of high impurity content in the product, complicated separation and purification process, and low synthesis yield, and achieve simple and easy operation Easy to use, simple purification process, and the effect of reducing side reactions

Inactive Publication Date: 2005-09-14
梁国正 +5
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the above method is that the temperature of the synthesis reaction is lower (less than 0°C), the time is long, and the reaction is difficult to control, the separation and purification process is complicated, the cost is high, the synthesis yield is low (about 70%), and the impurity content of the product is high (purity about 90%)

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

specific Embodiment 1

[0030] Specific implementation example 1: Synthesis of bisphenol A-type cyanate resin

[0031] Add 265g (2.5mol) BrCN and 300ml acetone to a 3000ml three-necked reaction flask, use an ice-salt bath to reduce the temperature of the solution in the reaction flask to below 0°C, dissolve 228g (1.0mol) of bisphenol A in 300ml of acetone solvent, put into the dripping bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 212g (2.1mol) acetone solution of triethylamine and bisphenol A at the same time, control the reaction temperature to be below 10°C, and continue to be between 0 and 10°C after the dropwise addition is completed. The reaction was continued for 3h, and the reaction was terminated. The salt formed by the reaction was filtered with a filter funnel, and the filtrate was poured into a 2000-ml distillation flask to distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, 1000 ml of a mixed solvent ...

specific Embodiment 2

[0032] Specific implementation example 2: synthesis amplification process of bisphenol A cyanate resin

[0033] 500g (4.7mol) BrCN and 600ml acetone were added to a 5000ml three-necked reaction flask, the temperature of the solution in the reaction flask was lowered to below 0°C with an ice-salt bath, and 460g (about 2.0mol) of bisphenol A was dissolved in 600ml of acetone solvent, Put into dropper bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 420g (about 4mol) of triethylamine and acetone solution of bisphenol A at the same time, control the reaction temperature to be below 10°C, and continue to be between 0 and 10°C after the dropwise addition is completed. The reaction was completed for 4 h. The salt formed by the reaction was filtered with a filter funnel, and the filtrate was poured into a 2000-ml distillation flask to distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, 2000 ml of a mi...

specific Embodiment 3

[0034] Specific Example Three: Synthesis of Bisphenol S-Type Cyanate Resin

[0035] 265g (2.5mol) BrCN and 300ml acetone were added to a 3000ml three-necked reaction flask, the temperature of the solution in the reaction flask was lowered to below 0°C with an ice-salt bath, 250g (1.0mol) bisphenol S was dissolved in 350ml acetone solvent, and the into the dripping bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 212g (2.1mol) acetone solution of triethylamine and bisphenol S at the same time. After 5 hours of reaction, the reaction was terminated. The salt formed by the reaction was filtered with a filter funnel, and the filtrate was poured into a 2000-ml distillation flask to distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, 1000 ml of a mixed solvent of isopropanol / chloroform is added. The bisphenol S-type cyanate resin is completely dissolved by heating, and then the temperature is lower...

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

A process for synthesizing high-purity cyanate ester resin with high output rate features that the cyanogen halide, triethylamine and phenol compound are used as raw materials, the ketone, alcohol, substituted benzene, or haloform is used as solvent, and the solution is triethylamine and phenol compound in acetone is dripped in the solution of cyanogen halide in acetone at temp lower than 10 deg.C. Its advantages are easy control, high output rate greater than 96.5% and high purity (more than 99%).

Description

1. Technical field: [0001] The invention belongs to the field of polymer synthesis, in particular to a method for synthesizing high-purity and high-yield cyanate resins. 2. Technical background: [0002] Cyanate ester resin is widely used in high-tech fields such as aviation, aerospace, and electronic technology due to its excellent dielectric properties, heat / humid heat resistance, good mechanical properties and processing performance. This is of great significance for developing my country's material research level and filling the gap in the research field of high-performance composite resin matrix in my country. [0003] At present, there are many methods for synthesizing cyanate esters. According to the organic synthesis mechanism, cyanate esters can be directly prepared from cyanic acid, but this synthesis method and yield cannot be controlled. The reason is that cyanic acid mainly exists in its isomerized form - isocyanic acid, and only isocyanates can be obtained. 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 Patents(China)
IPC IPC(8): C08G73/00
Inventor 梁国正王志强张民习轩立新李文峰杨洁颖
Owner 梁国正
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

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap