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A kind of preparation method of bisphenol A type cyanate resin monomer

A type of cyanate ester and resin monomer technology, which is applied in the field of organic polymer material synthesis, can solve the problems of large amount of waste gas and waste water, long reaction time, large amount of solvent used, etc., and achieves less by-products and process efficiency. Improved, low-cost effects

Active Publication Date: 2017-03-22
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese invention patent CN1629137A discloses a method for preparing cyanate esters, but the amount of solvent used is large and the reaction time is long. The extraction process of cyanate esters involves complicated processes such as vacuum distillation concentration and crystallization, and the generation of waste gas and waste water is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 22.8kg of bisphenol A in 25L of cyclohexane, lower the temperature to 0°C, and then pass 7.4g of liquid cyanogen chloride and 13.2kg of triethylamine through three different feeding tubes with an inner diameter of 1cm, respectively, at 25kg / min, 6.5kg / min, 11kg / min are sprayed into the reactor with intense turbulent flow, and the reaction temperature is controlled at -5°C-5°C. body.

Embodiment 2

[0027] Dissolve 22.8kg of bisphenol A in 30L of cyclopentane, lower the temperature to 0°C, and then pass 8kg of liquid cyanogen chloride and 15.2kg of triethylamine through three different feeding tubes with an inner diameter of 1.5cm, respectively with 28kg / min, 7.1kg / min, 11.8kg / min are sprayed into the intense turbulent flow reactor, and the reaction temperature is controlled from 0°C to 5°C. After the reaction is completed, it is washed with water, filtered, and dried to obtain bisphenol A cyanate resin. body.

Embodiment 3

[0029] Take 22.8kg of bisphenol A and dissolve it in 35L of methylcyclohexane, cool down to -2°C, then feed 9kg of liquid cyanogen chloride and 18kg of triethylamine through three different feeding tubes with an inner diameter of 3cm, respectively 30kg / min, 7.5kg / min, 12.3kg / min are sprayed into the reactor with intense turbulent flow, and the reaction temperature is controlled at 5°C-10°C. After the reaction, wash with water, filter, and dry to obtain bisphenol A cyanate resin monomer.

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Abstract

The present invention belongs to the field of organic polymer material synthesis, and particularly relates to a bisphenol A type cyanate resin monomer synthesis method, which specifically comprises: dissolving bisphenol A in an alkane organic solvent containing 5-8 c atoms; spraying the bisphenol A solution, cyanogen halide and triethylamine into a reaction container achieving turbulent flow through different feeding pipelines at a high speed, wherein a molar ratio of the bisphenol A to the cyanogen halide to the triethylamine is 1:1.1-1.5:1.2-1.9, the reaction temperature is -5 to 15 DEG C, and the reaction time is 3-15 min; and after completing the reaction, self-precipitating the bisphenol A cyanate without application of other methods to extract. According to the present invention, the bisphenol A type cyanate resin monomer preparation method is achieved.

Description

technical field [0001] The invention belongs to the field of synthesis of organic polymer materials, and relates to a preparation method of a bisphenol A type cyanate resin monomer. Background technique [0002] Cyanate resin is a new type of high-performance thermosetting resin, which has outstanding electrical properties, and has excellent dielectric properties and dielectric loss values ​​in a wide frequency range. The basic raw material of materials and aerospace structural materials, cyanate ester resin has been recognized as one of the most competitive resin qualities in the 21st century. [0003] At present, the cyanate ester varieties on the market mainly include bisphenol A type, dicyclopentadiene type, bisphenol E type, phenolic type, bisphenol M type and other models. Among them, bisphenol A cyanate has the characteristics of excellent cost performance, mature synthesis process, and high heat resistance, and has been widely used. [0004] Chinese invention paten...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C261/00
Inventor 季静静朱芝峰王跃彪金中宝柳义波范春晖
Owner YANGZHOU TECHIA MATERIAL CO LTD
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