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Process for preparing phenol addition compound cyanate of dicyclopentadiene

A technology of dicyclopentadiene and cyanate ester is applied in the preparation of cyanate ester and the preparation of phenol adduct cyanate ester. It is difficult to obtain cyanogen chloride, etc.

Inactive Publication Date: 2005-01-26
上海慧峰化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the problem of using this method is that it is difficult to obtain pure cyanogen chloride, and the impurity of cyanogen chloride will directly affect the quality of cyanate ester
But, the required cyanogen chloride of the method described in this patent is difficult to directly buy from the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation of embodiment 1 cyanogen chloride

[0015] Quantitatively pass 14% sodium cyanide aqueous solution and gaseous chlorine into the gas-liquid separator through the static reactor, and condense the cyanogen chloride gas to obtain colorless pure cyanogen chloride.

Embodiment 2

[0016] The preparation of the phenol adduct cyanate of embodiment 2 cyclopentadiene

[0017] Preparation method 1:

[0018] Add 1285 ml of dichloromethane into a 2000 ml flask equipped with stirring, cooling and dripping devices, add 120 g of phenol adduct of dicyclopentadiene under stirring, cool to -10 ° C after complete dissolution, and add After the addition of 50.4 g of cyanogen chloride was completed, 84.1 g of triethylamine was added dropwise, and the temperature was kept below -10°C, followed by stirring for 15 minutes. Wash with sodium bicarbonate aqueous solution and hydrochloric acid aqueous solution, separate, evaporate in vacuo at 40-50°C, remove water and solvent, and obtain the finished product of cyanate ester of phenol adduct of dicyclopentadiene.

[0019] Preparation method 2:

[0020] Prepare a 10-liter enamel reactor, add 3,600 ml of butanone into it, add 2,000 grams of phenol adduct of dicyclopentadiene under stirring, cool to -10°C after the dissolution...

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Abstract

The invention discloses a process for preparing phenol addition compound cyanate of dicyclopentadiene which comprises first preparing cyanogen chloride, then further obtaining cyanate. The cyanate of dicyclopentadiene obtained has high quality, after being poured in to trimer resin, the dielectric constant is < 3, the dielectric loss is less than 0.0022.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation method of cyanate ester. Further, the present invention relates to a preparation method of dicyclopentadiene phenol adduct cyanate ester. Background technique [0002] Cyanate ester resin is used in high-tech fields such as aviation and aerospace high-speed printed circuit boards due to its good mechanical properties, high glass transition temperature and excellent electrical properties. [0003] A kind of preparation method of the phenol adduct cyanate of dicyclopentadiene is disclosed in U.S. Patent No. 4,748,270, and its method is at first the methylene chloride solution of chlorine and the aqueous solution of sodium cyanide are reacted at low temperature, and the water layer is separated Obtain the dichloromethane solution of cyanogen chloride, then add the above solution into the dichloromethane solution of the phenol adduct of dicyclopentadiene, then add triethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C261/02
Inventor 韩竞赛葛芳荪严连发娄宝兴
Owner 上海慧峰化工科技有限公司
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