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 complicated separation and purification process, high impurity content of the product, and low synthesis yield, and achieve simple purification process , easy to operate, reduce the effect of side reactions

Inactive Publication Date: 2004-01-14
梁国正 +5
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  • Summary
  • Abstract
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  • 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

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0025] Specific implementation example one: the synthesis of bisphenol A type cyanate resin

[0026] Add 265g (2.5mol) of BrCN and 300ml of acetone into a 3000ml three-necked reaction flask, use an ice-salt water bath to lower 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, and put into the dropper bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 212g (2.1mol) of triethylamine and bisphenol A in acetone solution at the same time, control the reaction temperature below 10°C, and continue to keep it between 0 and 10°C after the dropwise addition is completed After 3 hours of reaction, the reaction was terminated. Filter the salt formed by the reaction with a filter funnel, pour the filtrate into a 2000ml distillation bottle and distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, add 1000ml isopropanol / chlorofo...

specific Embodiment 2

[0027] Concrete implementation example two: the synthetic amplification technique of bisphenol A type cyanic acid resin

[0028] Add 500g (4.7mol) BrCN and 600ml acetone in a 5000ml three-necked reaction flask, use an ice-salt water bath to lower the temperature of the solution in the reaction flask below 0°C, and dissolve 460g (about 2.0mol) of bisphenol A in 600ml of acetone solvent, Put in the dropper bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 420g (about 4mol) of triethylamine and bisphenol A in acetone solution at the same time, control the reaction temperature below 10°C, and continue to keep it between 0 and 10°C after the dropwise addition Reaction 4h, end reaction. Filter the salt formed by the reaction with a filter funnel, pour the filtrate into a 2000ml distillation bottle and distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, add 2000ml of isopropanol / chloroform mixed solve...

specific Embodiment 3

[0029] Specific implementation example three: the synthesis of bisphenol S type cyanic acid resin

[0030] Add 265g (2.5mol) BrCN and 300ml acetone into a 3000ml three-necked reaction flask, use an ice-salt water bath to lower the temperature of the solution in the reaction flask below 0°C, dissolve 250g (1.0mol) bisphenol S in 350ml acetone solvent, and put into the dropper bottle. Under the condition of vigorous stirring (about 130N / min), slowly add 212g (2.1mol) of triethylamine and bisphenol S in acetone solution at the same time, control the reaction temperature below 10°C, and continue to keep it between 0 and 10°C after the dropwise addition After 5 hours of reaction, the reaction was terminated. Filter the salt formed by the reaction with a filter funnel, pour the filtrate into a 2000ml distillation bottle and distill the acetone solvent under reduced pressure below 40°C. When the solvent content is less than 20%, add 1000ml isopropanol / chloroform mixed solvent. Hea...

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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 synthesis method of high-purity and high-yield cyanate resin. 2. Technical background: [0002] Because cyanate resin has excellent dielectric properties, heat / humid heat resistance, good mechanical properties and processing performance, it is widely used in high-tech fields such as aviation, aerospace, and electronic technology. This is of great significance to the development of my country's material research level and to fill 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 mechanism of organic synthesis, 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 are obtained. T...

Claims

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Application Information

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Patent Type & Authority Applications(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
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