New process for preparing food-grade 2,6-di-tert-butyl-p-methylphenol

A technology of p-cresol and di-tert-butyl, which is applied in the new process field of preparing food-grade 2,6-di-tert-butyl-p-cresol, which can solve the problems of long reaction time, low conversion efficiency and large amount of waste water , to achieve the effect of convenient purification and shortened reaction time

Inactive Publication Date: 2019-09-10
江苏迈达新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthesis of traditional 2,6-di-tert-butyl-p-cresol is usually based on p-cresol or recycled monobutylphenol and isobutene as raw materials, with concentrated sulfuric acid or p-toluenesulfonic acid liquid as a catalyst, in an alkylation tank Synthesize 2,6-di-tert-butyl p-cresol, heat the reaction product in a neutralization tank, neutralize excess acid catalyst with saturated sodium carbonate solution, but most conversion efficiencies are rel...

Method used

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  • New process for preparing food-grade 2,6-di-tert-butyl-p-methylphenol
  • New process for preparing food-grade 2,6-di-tert-butyl-p-methylphenol
  • New process for preparing food-grade 2,6-di-tert-butyl-p-methylphenol

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Experimental program
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Effect test

Embodiment 1

[0016] Use 10g of solid acid catalyst cerium sulfate, 200g of p-cresol, the mass ratio of catalyst to p-cresol is 5%, the reaction temperature is 90-110°C, after the temperature in the flask reaches the set value, start to pass isobutylene, the reaction time is 6h, and the catalyst is separated and removed According to gas chromatography analysis, the content of 2,6-di-tert-butyl-p-cresol in the alkylation liquid is 87.21%, and after recrystallization and drying, the purity reaches 99.22%.

[0017] Described alkylation reaction equation is:

[0018]

Embodiment 2

[0020] 16g of cerium sulfate as a solid acid catalyst, 200g of p-cresol, 8% mass ratio of catalyst to p-cresol, and a reaction temperature of 90-110°C were used. After the temperature in the flask reached the set value, isobutylene was started to flow for a reaction time of 6h. The catalyst was separated and removed, and analyzed by gas chromatography, the content of 2,6-di-tert-butyl-p-methylphenol in the alkylation liquid was 85.8%, and after recrystallization and drying, the purity reached 99.3%.

[0021] Described alkylation reaction equation is:

[0022]

Embodiment 3

[0024] Use 20g of cerium sulfate as a solid acid catalyst, 200g of p-cresol, 10% mass ratio of catalyst to p-cresol, and a reaction temperature of 90-110°C. After the temperature in the flask reaches the set value, start to pass isobutylene for a reaction time of 8 hours. The catalyst was separated and removed, and analyzed by gas chromatography, the content of 2,6-di-tert-butyl-p-methylphenol in the alkylation liquid was 86.6%, and after recrystallization and drying, the purity reached 99.7%.

[0025] Described alkylation reaction equation is:

[0026]

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Abstract

The invention belongs to the technical field of organic synthesis technologies, and particularly relates to a new process for preparing food-grade 2,6-di-tert-butyl-p-methylphenol. The process comprises the steps: using p-cresol and isobutylene as reaction raw materials, selecting a solid acid catalyst, and performing an alkylation reaction under the heating condition so as to obtain the product,wherein the solid acid catalyst is cerium sulfate, ammonium ferric sulfate or phosphotungstic acid. According to the preparation process, the reaction yield of 2,6-di-tert-butyl-p-methylphenol which is prepared from cresol and isobutylene can be improved by using the solid acid catalyst, the reaction time is shortened, purification in the later stage is convenient, and the product can reach the food-grade requirement.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a new technology for preparing food-grade 2,6-di-tert-butyl-p-cresol. Background technique [0002] The synthesis of traditional 2,6-di-tert-butyl-p-cresol is usually based on p-cresol or recycled monobutylphenol and isobutene as raw materials, with concentrated sulfuric acid or p-toluenesulfonic acid liquid as a catalyst, in an alkylation tank Synthesize 2,6-di-tert-butyl p-cresol, heat the reaction product in a neutralization tank, neutralize excess acid catalyst with saturated sodium carbonate solution, but most conversion efficiencies are relatively low, generally at 70-78 %, the reaction time is relatively long, and there are many by-products, and the liquid acid used in the process needs a large amount of saturated alkali solution to neutralize, which will produce a large amount of waste water, and the production cost is relatively high; in ...

Claims

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Application Information

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IPC IPC(8): C07C37/14C07C39/06
CPCC07C37/14C07C39/06Y02P20/584
Inventor 陈福新陈琦朱志宏王建全
Owner 江苏迈达新材料股份有限公司
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