Method for preparing and purifying cyanate

A technology of cyanate ester and cyanogen halide, applied in the direction of organic chemistry, can solve the problems of large equipment, heavy workload, energy consumption, etc., and achieve the effect of high purity

Inactive Publication Date: 2005-09-07
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 disadvantage of using this method is that the solvent recovery req

Method used

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Examples

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Embodiment 1

[0023] A 3000ml three-neck flask was equipped with a stirrer, a thermometer and a dropping funnel, 1150g of toluene was added, cooled to 3°C, and 250g of cyanogen chloride was added. After stirring for 30 minutes, a solution of 380 g of bisphenol A and 371 g of triethylamine in 500 g of toluene was added dropwise at a temperature lower than 3°C. After the dropwise addition, stirring was continued for 30 minutes. The reaction solution was washed with acid, alkali and water to remove salt, then reduced pressure at 50°C, concentrated until the material became cloudy, cooled to 3°C while stirring for 2 hours, and filtered. The filter cake was rinsed twice with 130 g of isopropanol, vacuum-dried at 50° C., and then analyzed by liquid chromatography to obtain a purity of 99.3%.

Embodiment 2

[0025] The 1000ml three-necked flask is equipped with a stirrer, a thermometer and a dropping funnel. Add 100 g of methyl ethyl ketone and cool to 3°C, then add 57.6 g of cyanogen chloride. A solution of 100 g of 3,3',5,5'-tetramethylbisphenol F and 86.6 g of triethylamine in 500 g of butanone was added dropwise at a temperature lower than 3° C. for 30 minutes under stirring. After the dropwise addition was complete, stirring was continued for 30 minutes. After removing triethylamine hydrochloride by filtration, the filtrate was concentrated under reduced pressure at 50°C until the material became cloudy, then cooled to 3°C while stirring for 2 hours, and filtered. The filter cake was rinsed twice with 50 g of isopropanol. After vacuum drying at 50°C, the purity of the product was analyzed by liquid chromatography, and the obtained purity was 98.2%.

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Abstract

The invention discloses a method for preparing and purifying cyanate, which comprises dissolving the dihydroxy compound into dissolvent, reacting with cyanogen halide at the presence of acid absorption agent, obtaining corresponding cyanate product, removing by-product through filtering or washing, subjecting the cyanate solution to decompression concentration, stirring and cooling, separating white crystal, then carrying out filtration, scouring and drying.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a method for preparing cyanate, and further, the invention relates to a method for preparing and purifying cyanate. Background technique [0002] U.S. Patent No. 5,932,762 discloses a preparation method of cyanate ester (Cyanate Ester). The purity of the bisphenol A cyanate ester produced by this method is 97.5%-99.5%, which cannot meet the high requirements of the market. [0003] U.S. Patent No. 6,225,492 and US No. 6,603,035 disclose a method for preparing high-purity cyanate esters. The method describes that the finished cyanate ester products add another organic solvent with low solubility to cyanate esters in the solvent, and the high-purity cyanate A method for ester crystallization, the purity of bisphenol A cyanate prepared by this method reaches 99%. However, the disadvantage of using this method is that the solvent recovery requires a lot of work, requires a lot of equi...

Claims

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Application Information

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IPC IPC(8): C07C261/00
Inventor 韩竞赛葛芳荪娄宝兴严连发徐家敏
Owner 上海慧峰化工科技有限公司
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