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Method for preparing 2,6-di-tert-butyl-4-methylcyclohexanol by catalytic hydrogenation

A technology of methylcyclohexanol and di-tert-butyl, applied in the field of green technology, can solve the problems of difficult industrial application, harsh reaction conditions, cumbersome operation, etc., and achieve the effects of suppressing by-products, short reaction time and low reaction temperature Effect

Active Publication Date: 2022-07-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the problems of harsh reaction conditions, cumbersome operation, environmental pollution, and difficulty in industrial application in the prior art, thereby providing a method for preparing 2,6-di-tert-butyl-4-methylcyclocyanide by catalytic hydrogenation Hexanol method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Mix 100g of di-tert-butyl-4-methylphenol with 5g of 5% Ru / Al 2 O 3 The supported metal catalyst was added to the autoclave at the same time, and the nitrogen leak was tested first to ensure no gas leakage, and then replaced with nitrogen and hydrogen for 3 times respectively, and then filled with hydrogen to pressurize to 4MPa, and the temperature was raised to 140 ° C to start the reaction, and maintain After reacting for 1 hour, the temperature was lowered, and the samples were taken for detection and analysis. The conversion rate of BHT was 100%, and the selectivity of 2,6-di-tert-butyl-4-methylcyclohexanone was 99.7%; 10g of water was continued to be added to the reaction kettle, and a nitrogen test was carried out. To ensure no air leakage, replace it with nitrogen and hydrogen for 3 times respectively, then fill with hydrogen and pressurize to 4MPa, heat up to 200 ℃ to start the reaction, maintain the reaction for 1h, then cool down, take samples for detection and...

Embodiment 2

[0028] The content of 100g di-tert-butyl-4-methylphenol and 5g is 5%Rh / Al 2 O 3 The supported metal catalyst was added to the autoclave at the same time, and the nitrogen leak was first tested to ensure no gas leakage, and then replaced with nitrogen and hydrogen three times respectively, and then filled with hydrogen to pressurize to 3 MPa, and the temperature was raised to 130 ° C to start the reaction and maintain After 1 h of reaction, the temperature was lowered, and sampling was carried out for detection and analysis. The conversion rate of BHT was 100%, and the selectivity of 2,6-di-tert-butyl-4-methylcyclohexanone was 99.6%; 15g of ethanol was continued to be added to the reaction kettle, and a nitrogen test was carried out. To ensure no air leakage, replace it with nitrogen and hydrogen for 3 times respectively, then fill with hydrogen and pressurize to 5MPa, raise the temperature to 180 °C to start the reaction, maintain the reaction for 1h, then cool down, take samp...

Embodiment 3

[0030] Mix 100g of di-tert-butyl-4-methylphenol with 5g of 5% Ni / SO 2 The supported metal catalyst was added to the autoclave at the same time, and nitrogen was first tested for leaks to ensure no gas leakage, and then replaced with nitrogen and hydrogen for 3 times, respectively, and then filled with hydrogen and pressurized to 5MPa, and the temperature was raised to 150 °C to start the reaction and maintain After reacting for 2 hours, the temperature was lowered, and sampling was carried out for detection and analysis. The conversion rate of BHT was 100%, and the selectivity of 2,6-di-tert-butyl-4-methylcyclohexanone was 99.3%; 10 g of acetic acid was continued to be added to the reaction kettle, and a nitrogen test was carried out. To ensure no air leakage, replace it with nitrogen and hydrogen for 3 times respectively, then fill with hydrogen and pressurize to 5MPa, heat up to 190 °C to start the reaction, maintain the reaction for 2h, then cool down, take samples for detec...

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Abstract

The invention discloses a method for preparing 2,6-di-tert-butyl-4-methylcyclohexanol by catalytic hydrogenation. Di-tert-butyl-4-methylphenol (BHT) and a supported catalyst are added to a high-pressure reaction In the kettle, the transformation efficiency of BHT after the reaction finishes is 100%, and the 2,6-di-tert-butyl-4-methylcyclohexanone selectivity is greater than 99.2%; Cyclohexanone and auxiliary agent were added into the autoclave, the conversion rate of 2,6-di-tert-butyl-4-methylcyclohexanone after the reaction was 100%, The selectivity of cyclohexanol was greater than 98.1%. The invention solves the problems existing in the prior art, such as harsh reaction conditions, cumbersome operation, environmental pollution, difficulty in industrial application and the like.

Description

technical field [0001] The invention belongs to green technology and relates to a method for synthesizing 2,6-di-tert-butyl-4-methylcyclohexanol. Background technique [0002] 2,6-Di-tert-butyl-4-methylcyclohexanol (English: 2,6-Bis-tert-butyl-4-methylcyclohexanol) is mainly used in the field of photography; it can be used as a dispersant for color photography; also It can be used as a solvent in the field of dyes; at the same time, it can also be used as a pharmaceutical intermediate and a pesticide intermediate. At present, 2,6-di-tert-butyl-4-methylcyclohexanol is mainly prepared by kettle-type hydrogenation method. Di-tert-butyl-4-methyl phenol is used as raw material. To prepare 2,6-di-tert-butyl-4-methylcyclohexanol from hydrogen, the catalysts used in the preparation process are mainly noble metal supported catalysts, and the supported metals mainly include Ru, Rh, Pt, Ni, Pd, etc. Under this process condition, although 2,6-di-tert-butyl-4-methylcyclohexanone and 2,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/00C07C49/403C07C29/145C07C35/08
Inventor 何育苗袁俊秀黄冬
Owner CHINA PETROLEUM & CHEM CORP