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Method for preparing chemical intermediates by using mixed o/m/p-cresol

A technology for mixing cresols and intermediates, which is applied in the field of producing high-purity antioxidant intermediates, can solve uninvolved and other problems, and achieve the effects of reducing raw material consumption and production cost, high reaction conversion rate, and improving atomic utilization.

Inactive Publication Date: 2010-10-13
吴鸿宾
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

None of the above inventions involves the simultaneous preparation of three chemical intermediates using m-p-mixed cresols

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Put 1080kg of ortho-cresol mixture (the mass content of ortho-cresol is 32.5%, the mass content of m-cresol is 41.9%, and the mass content of p-cresol is 25.3%), and 20kg of cation exchange resin is put into the reaction kettle, start stirring, and heat up to 125°C, then continuously drop 924kg of methyl tert-butyl ether into the reactor within 3 hours, and 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; Reaction finishes, and filter removes catalyst, and mixed solution is through rectification under reduced pressure, and obtaining purity is 99.53% 6-tert-butyl o-cresol 485.3kg, and purity is 628.0kg of 99.57% 6-tert-butyl m-cresol, and purity is 99.56% 373.5kg of 2-tert-butyl-p-cresol.

Embodiment 2

[0015] Put 1080kg of ortho-cresol mixture (the mass content of ortho-cresol is 32.5%, the mass content of m-cresol is 41.9%, and the mass content of p-cresol is 25.3%), and 20kg of cation exchange resin is put into the reaction kettle, start stirring, and heat up to 70°C, then continuously drop 580kg of isobutene into the reactor within 3 hours, and 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; Catalyst, mixed solution rectification under reduced pressure, obtains the 6-tert-butyl o-cresol 487.5kg that purity is 99.54%, the 6-tert-butyl m-cresol 628.2kg that purity is 99.55%, the 2-tert-butyl cresol that purity is 99.55% p-cresol 372.9kg.

Embodiment 3

[0017] Put 1080kg of ortho-p-cresol mixture (the mass content of ortho-cresol is 32.5%, the mass content of m-cresol is 41.9%, and the mass content of p-cresol is 25.3%), and 20kg of loaded mesoporous molecular sieve catalyst is put into the reaction kettle, and the stirring is started , the temperature was raised to 125°C, and then 924kg of methyl tert-butyl ether was continuously added dropwise to the reaction kettle within 3 hours to maintain the reaction temperature at 125±2°C; after the dropwise addition, the reaction temperature was raised to 135°C and the reaction was maintained for 1 Hour; reaction finishes, removes catalyzer, and mixed liquor rectification under reduced pressure obtains that purity is 99.65% 6-tert-butyl o-cresol 477.1kg, and purity is 99.57% 6-tert-butyl m-cresol 616.3kg, and purity is 99.54% 362.2kg of 2-tert-butyl-p-cresol.

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Abstract

The invention provides a new method for preparing chemical intermediates by using mixed o / m / p-cresol. The method comprises the following steps of: taking mixed solution of o-cresol, m-cresol and p-cresol a raw material, performing alkylation on the mixed solution in the presence of an alkylating agent and a catalyst to obtain mixed solution of 6-tertbutyl-o-cresol, 6-tertbutyl-m-cresol and 2-tertbutyl-o-cresol, and rectifying the mixed solution to obtain high-purity chemical intermediate products of the 6-tertbutyl-o-cresol, the 6-tertbutyl-m-cresol and the 2-tertbutyl-o-cresol. The method has high reaction conversion rate, and can improve the utilization rate of atoms and reduce the raw material consumption and the production cost.

Description

technical field [0001] The invention relates to a method for preparing chemical intermediates by using m-p-mixed cresols, specifically using a mixture of o-cresols, m-cresols and p-cresols to produce high-purity antioxidant intermediates 6-tert-butyl o-cresol, 6-tert-butyl-m-cresol and 2-tert-butyl-p-cresol methods. Background technique [0002] 6-tert-butyl-o-cresol, 6-tert-butyl-m-cresol and 2-tert-butyl-p-cresol are important chemical intermediates. 6-tert-butyl-o-cresol is the main raw material for the preparation of asymmetric hindered phenolic antioxidants Irganox245, SumilizerGA / Mark AO-80, 736, etc.; 6-tert-butyl-m-cresol is mainly used in the production of 300, CA, BBM and other varieties 2-tert-butyl-p-cresol is an intermediate for synthesizing antioxidants 2246, 2246S, 264 and UV absorber UV326. The traditional production method of high-purity 6-tert-butyl-o-cresol, 6-tert-butyl-m-cresol and 2-tert-butyl-p-cresol is to use high-purity ortho-cresol, m-cresol and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/14C07C37/16
Inventor 吴鸿宾吴兆瑞韩成树
Owner 吴鸿宾
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