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Separation method of m-cresol and p-cresol mixture

A separation method and a technology for mixing cresols, which are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effects of high atomic utilization, low raw material consumption and production cost, and high reaction conversion rate.

Inactive Publication Date: 2010-10-20
吴鸿宾
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above invention cannot fundamentally solve the problem of effective utilization of m-p-cresol in coal chemical by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 1080kg m-p-cresol mixture (m-cresol mass content is 62.90%, p-cresol mass content is 37.06%), 20kg cation exchange resin is put into the reaction kettle, start stirring, heat up to 125 ℃; Then 924kg methyl tertiary Butyl ether was continuously added dropwise into the reaction kettle within 3 hours, and the reaction temperature was maintained at 125±2°C. After the dropwise addition, the temperature of the kettle was raised to 135°C and maintained for 1 hour; Pressure rectification, obtain the 6-tert-butyl m-cresol 943.8kg that purity is 99.73%, the 2-tert-butyl-p-cresol 558.5kg that purity is 99.57%;

[0018] Put 943.8kg of 6-tert-butyl m-cresol and 20kg of cation exchange resin into the reaction kettle, start stirring, raise the temperature to 100°C, and keep it warm for three hours; the isobutene produced by decomposition is recovered by freezing and compressing to obtain 273.2kg of isobutene; Pressure rectification, obtaining purity is 99.58% m-cresol 557.8kg;

...

Embodiment 2

[0021] 1080kg m-p-cresol mixture (m-cresol mass content is 62.90%, p-cresol mass content is 37.06%), 20kg cation exchange resin is put into reactor, start stirring, be warming up to 70 ℃; Add it dropwise into the reaction kettle continuously within 1 hour, maintain the reaction temperature at 70±2°C, after the dropwise addition, raise the reaction temperature to 80°C, and maintain the reaction for 1 hour; after the reaction is completed, filter the catalyst, and rectify the mixture under reduced pressure to obtain 950.5kg of 6-tert-butyl m-cresol with a purity of 99.65%, and 557.2 kg of 2-tert-butyl-p-cresol with a purity of 99.51%;

[0022] Put 950.5kg of 6-tert-butyl m-cresol and 20kg of cation exchange resin into the reaction kettle, start stirring, raise the temperature to 100°C, and keep it warm for three hours; the isobutene produced by decomposition is recovered by freezing and compressing to obtain 276.1kg of isobutene; Pressure rectification, obtaining purity is 99.63...

Embodiment 3

[0025] Put 1080kg of m-p-cresol mixture (the mass content of m-cresol is 62.90%, and the mass content of p-cresol is 37.06%), and 20kg of loaded mesoporous molecular sieve catalysts are put into the reactor, and the stirring is started, and the temperature is raised to 125°C; Continuously drop tert-butyl ether into the reaction kettle within 3 hours, maintain the reaction temperature at 125±2°C, after the dropwise addition, raise the reaction temperature to 135°C, and maintain the reaction for 1 hour; The liquid was rectified under reduced pressure to obtain 949.3kg of 6-tert-butyl m-cresol with a purity of 99.70%, and 560.3 kg of 2-tert-butyl-p-cresol with a purity of 99.69%;

[0026] Put 949.3kg of 6-tert-butyl m-cresol and 20kg of loaded mesoporous molecular sieve catalyst into the reaction kettle, start stirring, raise the temperature to 100°C, and keep it warm for three hours; the isobutene produced by decomposition is recovered by freezing and compressing to obtain 274.3k...

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Abstract

The invention discloses a novel method for separating an m-cresol and p-cresol mixture to obtain high-purity m-cresol and p-cresol. The method comprises the following steps: carrying out alkylation reaction on the m-cresol and the p-cresol as raw materials under the existence of an alkylating agent and a catalyst to obtain the mixed solution of 2-tertiary butyl-p-cresol and 6-tertiary butyl-m-cresol; rectifying the mixed solution to obtain the products of high-purity 2-tertiary butyl-p-cresol and 6-tertiary butyl-m-cresol; respectively carrying out dealkylation reaction and rectification on the obtained high-purity 2-tertiary butyl-p-cresol and 6-tertiary butyl-m-cresol under the existence of the catalyst to respectively obtain the products of the high-purity m-cresol and p-cresol; and recovering isobutene generated by dealkylation. The invention has high reaction conversion rate, high atom use ratio, low raw material consumption and production cost and reliable safety performance.

Description

technical field [0001] The invention relates to a method for separating m-p-mixed cresols, in particular to a method for separating m-cresol and p-cresol mixtures to obtain high-purity m-cresol and p-cresol. Background technique [0002] m-cresol and p-cresol are important organic synthesis intermediates. The traditional production method of high-purity m-cresol is the diazotization hydrolysis method, and the traditional production method of p-cresol is the sulfonation alkali solution method. Both methods have low atom utilization and are highly polluting process routes, which do not conform to modern green chemistry. idea. Coal chemical by-product mixed cresol, because the boiling point of m-cresol is 203°C, the boiling point of p-cresol is 202.8°C, and the other physical and chemical properties of the two are also very close, so m-p-cresol in the by-product of coal chemical industry cannot be effectively separated, affecting effective use of both. [0003] U.S. Patent N...

Claims

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Application Information

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IPC IPC(8): C07C39/07C07C37/68C07C37/86
Inventor 吴鸿宾吴兆瑞韩成树
Owner 吴鸿宾
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