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Method for preparing tetramethyl bisphenol F type cyanate resin prepolymer

A technology of cyanate ester resin and tetramethylbisphenol, which is applied in the field of preparation of cyanate ester resin prepolymer to achieve the effect of maintaining excellent electrical properties and chemical properties

Active Publication Date: 2013-01-02
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it may produce other by-product isomers

Method used

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  • Method for preparing tetramethyl bisphenol F type cyanate resin prepolymer
  • Method for preparing tetramethyl bisphenol F type cyanate resin prepolymer

Examples

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Effect test

example 1

[0015] In a 1000ml four-neck flask, add 500g of solid tetramethylbisphenol F-type cyanate resin, feed nitrogen, slowly heat up the material to 120°C with an oil bath to melt, and add an appropriate amount of 0.05g of nonylphenol ; Then, continue to heat up to .170°C, and keep warm for 10 hours at 170±1°C under the protection of nitrogen. Then test its refractive index with a refractometer, and when it is 1.5750 / 84°C (1.5600 / 110°C), cool the reactant to about 75°C with cold oil. Then add 250 grams of butanone to form a liquid with a concentration of 65%, and cool to 20° C. to obtain a tetramethyl bisphenol F type cyanate resin prepolymer solution. Non-volatile matter ≥ 65.36%, viscosity: 500mPa·s / 25°C, yield: 99.85%.

example 2

[0017] In a 1000 ml four-neck flask, add 600 g of solid tetramethylbisphenol F-type cyanate resin, pass through nitrogen, and slowly heat up the material to 110 ° C with an oil bath to melt. When the material is completely melted, add benzene Ethylene 0.06 g; continue to heat up to 160 ° C, under the protection of nitrogen at 160 ± 1 ° C, heat preservation for 12 hours. Test its refractive index with a refractometer, and when it is 1.5700 / 84°C (1.5550 / 110°C), cool the reactant to about 75°C with cold oil. Slowly add 320 grams of butanone to form a liquid with a concentration of 65%, and cool to 30° C. to obtain a tetramethyl bisphenol F type cyanate resin prepolymer solution. Non-volatile matter ≥ 65.22%, viscosity: 250mPa·s / 25°C, yield: 99.9%.

example 3

[0019] In a 1000 ml four-necked flask, add 700 grams of solid tetramethylbisphenol F-type cyanate resin, feed nitrogen, use an oil bath to slowly heat up the material to 125 ° C for melting, add 0.07 grams of dimethylimidazole, Then continue to heat up to 150°C, and keep warm at 150±1°C for 15 hours under the protection of nitrogen. Then test its refractive index with a refractometer, and when it is 1.5650 / 84°C (1.5450 / 110°C), cool the reactant to about 75°C with cold oil. Slowly add 370 grams of butanone to form a liquid with a concentration of 65%, and cool to room temperature to obtain a tetramethyl bisphenol F type cyanate resin prepolymer solution. Non-volatile matter ≥ 65.42%, viscosity: 80mPa·s / 25°C, yield: 99.95%.

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Abstract

The invention relates to a method for preparing a tetramethyl bisphenol F type cyanate resin prepolymer and relates to a method for preparing a cyanate resin prepolymer. Different from the prior art, in the method, other byproduct isomers are not generated. The method comprises the following steps of: heating solid tetramethyl bisphenol F type cyanate resin serving as a major material for dissolving in a nitrogen atmosphere; adding a polymerization accelerant serving as an auxiliary material into the liquid etramethyl bisphenol F type cyanate resin, and stirring uniformly; continuing to raisethe temperature, and maintaining the temperature in an environment at 150 to 170 DEG C under the protection of nitrogen; when the refractive index is between 1.5750 and 1.5650 / 84 DEG C / 84 DEG C, cooling to obtain a liquid reactant; allowing the liquid reactant to break away from the nitrogen atmosphere; and adding butanone into the liquid reactant, stirring uniformly and cooling to obtain the tetramethyl bisphenol F type cyanate resin prepolymer, wherein the yield is 99.85 percent. By the method, the original chemical property and excellent electrical performance of the product are maintained, and the product is stable under the condition that curing time is shortened within one hour.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method of cyanate resin prepolymer. Background technique [0002] Tetramethyl bisphenol F type cyanate resin is mainly used in aerospace, aviation and electronics fields. Especially for the manufacture of advanced structural materials such as high-density multilayer printed circuit boards, anti-radiation guided missile fins, leading edges and spray heads, radomes, and stealth materials. It is a crystalline solid. The product has a very low viscosity of only about 20cPs / 25°C in the molten state. The resin molding process (fiber winding, molding, injection molding, resin transfer RTM) requires the viscosity of the resin matrix to be 80-500cPs / 25°C, the process of increasing the viscosity of this resin matrix is ​​relatively complicated, which brings a lot of inconvenience to users. [0003] On April 8, 2009, the State Intellectual Property Office published the inve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
Inventor 范春晖娄宝兴金中宝王钱康柳义波
Owner YANGZHOU TECHIA MATERIAL CO LTD
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