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Method for preparing bisphenol A cyanate

A cyanate ester and bisphenol technology, which is applied in the field of organic polymer material synthesis, can solve problems such as environmental pollution, excessive product impurity content, complex post-processing, etc., and achieve the goal of ensuring high purity, reducing impurity content, and improving product purity. Effect

Inactive Publication Date: 2005-06-22
ZHEJIANG KINGLYUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In order to overcome the shortcomings of excessive product impurity content, complex post-treatment, and environmental pollution in the existing synthesis process, the purpose of the present invention is to provide a method for preparing bisphenol A cyanate that can improve the purity and realize clean production

Method used

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  • Method for preparing bisphenol A cyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A 1000ml four-necked flask equipped with a stirrer, a dropping funnel and a thermometer was first put into 200ml of acetone, cooled to -5°C, and then 61.5g (1.0mol) of cyanogen chloride was added.

[0038] 114g (0.5mol) of bisphenol A was dissolved in 250ml of acetone, 101g (1.0mol) of triethylamine was added to dissolve in 250ml of acetone, and 101g (1.0mol) of triethylamine was added and stirred uniformly.

[0039] The reaction temperature is controlled from -5°C to 0°C, and the above-mentioned mixed liquid is added dropwise to the acetone solution of cyanogen chloride for 2 hours. After the dropwise addition is completed, the reaction is completed after the temperature is kept for 30 minutes.

[0040] Under rapid stirring, the reaction solution was poured into ice water to make the reactant appear as white crystals, filtered, washed, and dried to obtain bisphenol A cyanate. The yield was 93%.

[0041] Appearance: white crystalline powder; content: 99.9% (HPLC method); mo...

Embodiment 2

[0043] As described in Example 1, add 500ml of isopropanol and add 68g (1.1mol) of cyanogen chloride after cooling. 114g (0.5mol) of bisphenol A, 105g (1.04mol) of triethylamine and 500ml of isopropanol, mix and dissolve, control for about 2 hours, add dropwise to cyanogen chloride solution, reaction temperature 3~6℃, and filter the reaction liquid , Wash, dry, and get the product. The yield was 89%.

[0044] Appearance: white crystalline powder; content: 99.8% (HPLC method); moisture: 0.05% melting moment: 77.5-80.2

Embodiment 3

[0046] As in the device described in implementation 1, first add 100 g of toluene, cool to below 10° C. and add 80 g (1.3 mol) of cyanogen chloride.

[0047] Bisphenol A 148.2g (0.65mol) triethylamine 131.3g (1.3mol) and toluene 250g are mixed uniformly. The mixed solution was added dropwise to the toluene solution of cyanogen chloride at a temperature below -5°C, and the dropping temperature was controlled at -5°C and the dropping time was 2 hours. After the addition is complete, keep the temperature at -5°C for 30 minutes, and the reaction is complete.

[0048] Add 200g of water to the reaction solution, separate with a separatory funnel after mixing, and continue to use 2×200g of water for the oil layer. After mixing and separating two times, the reactants are vacuum distilled to evaporate the toluene, and then add 15% isopropyl cooled to 5℃ The alcohol aqueous solution is rapidly stirred to crystallize the material, and filtered to obtain the target bisphenol A cyanate. The yi...

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Abstract

The invention provides a method for preparing bisphenol A cyanate which comprises the steps of, dissolving the cyanogen chloride with a purity of 95-100% into organic solvent, dissolving bisphenol an and triethylamine into the same organic solvent, dropping the solution of bisphenol an and triethylamine into the cyanogen chloride solution, wherein the mol ratio of bisphenol A, cyanogen chloride and catalyst is 1 : 2-5 : 2-6, then extracting bisphenol A cyanate through conventional methods. The invention can realize improved purity and clean production.

Description

Technical field [0001] The invention belongs to the field of organic polymer material synthesis, and specifically relates to a preparation method of bisphenol A cyanate. Background technique [0002] With the development of modern high-tech, resin-based composite materials are required to have better comprehensive properties. Traditional resin matrixes such as unsaturated polyhydric resins, phenolic resins and epoxy resin acrylic resins, modified bismaleimide resins The heat resistance, toughness and dielectric properties are poor, and the high molding temperature can no longer meet certain high-tech fields, and the new high performance with high heat and humidity resistance, good compatibility, excellent dielectric properties, and excellent manufacturability The thermosetting resin, cyanate resin (CE for short) overcomes these shortcomings. The typical varieties of CE are cyanate esters. Bisphenol A cyanate esters are synthesized by the reaction of polyphenols (usually dihydric ...

Claims

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Application Information

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IPC IPC(8): C07C261/00
Inventor 卢小逸盛金火杨光新
Owner ZHEJIANG KINGLYUAN PHARMA
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