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Process for synthesizing 2,3,6-trimethylphenol by phenol

A technology of trimethylphenol and dimethylphenol, applied in the field of medicine and chemical industry, can solve the problems of poor selectivity, shortened catalyst life, increased production cost, etc. Effect

Active Publication Date: 2013-03-20
益曼特健康产业(荆州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

That is, the raw material of this process can be directly prepared by phenol methylation, and then 2,3,6-trimethylphenol can be obtained by meta-methylating 2,6-dimethylphenol. It needs to react under high temperature and high pressure catalysis, so that the life of the catalyst is greatly reduced, and the selectivity is also poor, which greatly increases the production cost

Method used

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  • Process for synthesizing 2,3,6-trimethylphenol by phenol

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 500gFe(NO 3 ) 3 9H 2 O, 30gMn(NO 3 ) 2 4H 2 O, 5gCr(NO 3 ) 3 9H 2 O, 3gNa 2 SiO 3 9H 2 O and 1gCaCl 2 2H 2 0, be dissolved in 10l water and make aqueous solution, in aqueous solution, add 28% ammoniacal liquor precipitating agent to the pH value of aqueous solution to be 7.5, make it coprecipitate after leaving standstill aging 12 hours; Dry at 150°C for 6 hours, crush into 50-mesh granules, put in 300ml 1% K 2 CO 3 Immerse in the aqueous solution at room temperature for 30 hours; dry the impregnated particles again at 150°C for 5 hours, and roast at 500°C for 5 hours. After the oxides become particles like coal powder, add 1g of graphite as a lubricant and a setting agent , after the final tableting, the cylindrical iron oxide-based catalyst is pressed into a 3×3mm cylinder to obtain an iron oxide-based catalyst composed of iron oxide, manganese oxide, silicon dioxide, chromium oxide, calcium oxide, potassium oxide and graphite. Catalyst, the mol...

Embodiment 2

[0039] Weigh 550gFe(NO 3 ) 3 9H 2 O, 35gMn(NO 3 ) 2 4H 2 O, 5gCr(NO 3 ) 3 9H 2 O, 6gNa 2 SiO 3 9H 2 O and 1.5 g CaCl 2 2H 2 0, be dissolved in 10l water and make aqueous solution, in aqueous solution, add 28% ammoniacal liquor precipitating agent to the pH value of aqueous solution to be 7.5, make it co-precipitate after static aging 14 hours; After the throw out that obtains is filtered and washed with water, in Dry at 180°C for 4 hours, crush into 70-mesh particles, put in 300ml 1%K 2 CO 3 Immerse in aqueous solution at room temperature for 30 hours; dry the impregnated particles again at 180°C for 3 hours, and then roast at 550°C for 3 hours. agent and setting agent, after the final tableting, the cylindrical iron oxide-based catalyst is pressed into a 3×3mm cylinder to obtain a catalyst composed of iron oxide, manganese oxide, silicon dioxide, chromium oxide, calcium oxide, potassium oxide and graphite. The iron oxide-based catalyst, the molar ratio of eac...

Embodiment 3

[0049] Weigh 500gFe(NO 3 ) 3 9H 2 O, 30gMn(NO 3 ) 2 4H 2 O, 5gCr(NO 3 ) 3 9H 2 O, 4.5gNa 2 SiO 3 9H 2 O and 1.5 g CaCl 2 2H 2 0, be dissolved in 10l water and make aqueous solution, in aqueous solution, add 28% ammoniacal liquor precipitating agent to the pH value of aqueous solution to be 7.5, make it coprecipitate after leaving standstill aging 12 hours; Dry at 160°C for 5 hours, crush into 90-mesh particles, put in 300ml 1% K 2 CO 3 Immerse in aqueous solution at room temperature for 30 hours; dry the impregnated particles again at 160°C for 4.5 hours, and roast at 450°C for 7 hours. After the oxides become particles like coal powder, add 1.5g of graphite as lubricant and shape After the final tableting, the cylindrical iron oxide-based catalyst is pressed into a 3×3mm cylinder to obtain an iron oxide composed of iron oxide, manganese oxide, silicon dioxide, chromium oxide, calcium oxide, potassium oxide and graphite. is a catalyst, the molar ratio of each ...

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Abstract

The invention relates to a process for synthesizing 2,3,6-trimethylphenol by phenol, and belongs to the technical field of medicine chemical industry. The process comprises the following steps of: firstly, carrying out a gas-phase reaction by mixing the phenol with methyl alcohol through a catalyst to obtain 2,6-dimethylphenol; and preparing a 2,3,6-trimethylphenol finished product by carrying out a sulfonation reaction, an esterification reaction, a friedel-crafts acylation reaction and a desulfonation reaction. According to the process for synthesizing the 2,3,6-trimethylphenol by the phenol, the problems that the existing m-cresol raw material is lack so as to seriously restrict the yield of the 2,3,6-trimethylphenol, and the service life of a catalyst is largely reduced and the production cost is increased because a catalytic reaction needs to be carried out at high temperature under high pressure during meta-methylation are solved. According to the process for synthesizing the 2,3,6-trimethylphenol by the phenol, the transformation rate and the selectivity of a reaction are improved; and meanwhile, the preparation cost of products is largely reduced, and the economical benefits and the social benefits are excellent.

Description

technical field [0001] The invention relates to a process for synthesizing 2,3,6-trimethylphenol from phenol, which belongs to the technical field of medicine and chemical industry. Background technique [0002] Tricresol is 2,3,6-trimethylphenol, which is mainly used in the pharmaceutical industry to synthesize vitamin E ring 2,3,5-trimethyl-p-phenylhydroquinone, and is also used in the production of heat-resistant polyphenylene ether engineering plastics Raw materials for monomers and plastic alloys, and also indispensable intermediates in the production of certain pesticides and disinfectants. [0003] At present, there are many technological routes for synthesizing tricresol at home and abroad, but there are two main ones suitable for industrialized large-scale production. One is to use m-cresol as raw material, methanol as methylating agent, and use gas-solid phase reaction in one step under the action of catalyst Synthesis of 2,3,6-trimethylphenol. The problem with t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/00B01J23/889
CPCY02P20/52
Inventor 乔建成陈强蔡东伟
Owner 益曼特健康产业(荆州)有限公司
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