Method for fixed bed alkylation separation of m-cresol and p-cresol

A technology of fixed bed and p-cresol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as increased production costs, strong corrosion, difficult separation of products, etc., to reduce consumption and load , to suppress the effect of generating

Inactive Publication Date: 2015-04-08
ANQING FULLTIME CHEM INDAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above two alkylation methods use liquid acid (sulfuric acid, toluenesulfonic acid) catalysts, which are very corrosive to the equipment, and after the alkylation, alkali washing and water washing are required to remove residual acid , if the acid is not removed, the dehydrogenation reaction will occur in the product distillation process, which will bring many problems, increase the production cost, the catalyst cannot be recycled well, and the side reactions cannot be well controlled, making it difficult to separate the product
[0005] Aiming at the deficiencies of the traditional alkylation method for separating m-p-cresol, the present invention proposes a method for separating m-p-cresol by fixed-bed alkylation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 1 unit volume of silica gel-loaded 1-(3-sulfonic acid)-3-methylimidazolium bisulfate into a tubular fixed-bed reactor, raise the temperature of the reactor to 40°C, and feed 20% mass of butylphenol mixed m-p-methylphenol raw material, the space velocity is 0.1h -1 , while feeding isobutene, mixing m-p-methylphenol raw material: isobutene (n:n)=1:0.2, and carrying out alkylation reaction to obtain a reaction mixture. The resulting reaction mixture is subjected to conventional rectification to obtain mixed m-p-cresol, 4-methyl-2-tert-butylphenol, 3-methyl-4-tert-butylphenol and high-boiling methyldi-tert-butylphenol , The results of chromatographic analysis show that the mixed m-p-methylphenol is 65.7%, 4-methyl-2-tert-butylphenol 4.8%, 3-methyl-4-tert-butylphenol 10.4% and high boiling point methyl di Tert-butylphenol 19.1%.

Embodiment 2

[0018] Add 1 unit volume of silica gel-loaded 1-(3-sulfonic acid)-3-methylimidazolium bisulfate into the tubular fixed-bed reactor, increase the temperature of the reactor to 60°C, and feed 20% mass of butylphenol mixed m-p-methylphenol raw material, the space velocity is 0.3h -1 , while feeding isobutene, mixing m-p-methylphenol raw material: isobutene (n:n)=1:0.2, and carrying out alkylation reaction to obtain a reaction mixture. The resulting reaction mixture is subjected to conventional rectification to obtain mixed m-p-cresol, 4-methyl-2-tert-butylphenol, 3-methyl-4-tert-butylphenol and high-boiling methyldi-tert-butylphenol , The results of chromatographic analysis show that the mixed m-p-methylphenol is 56.9%, 4-methyl-2-tert-butylphenol 8.0%, 3-methyl-4-tert-butylphenol 16.6% and high boiling point methyl di tert-butylphenol 19.5%.

Embodiment 3

[0020] Add 1 unit volume of silica gel-loaded 1-(3-sulfonic acid)-3-methylimidazolium bisulfate into a tubular fixed-bed reactor, increase the temperature of the reactor to 80°C, and feed 20% mass of butylphenol mixed m-p-methylphenol raw material, the space velocity is 0.6h -1 , while feeding isobutene, mixing m-p-methylphenol raw material: isobutene (n:n)=1:0.2, and carrying out alkylation reaction to obtain a reaction mixture. The resulting reaction mixture is subjected to conventional rectification to obtain mixed m-p-cresol, 4-methyl-2-tert-butylphenol, 3-methyl-4-tert-butylphenol and high-boiling methyldi-tert-butylphenol , The results of chromatographic analysis show that the mixed m-p-methylphenol is 56.6%, 4-methyl-2-tert-butylphenol 8.1%, 3-methyl-4-tert-butylphenol 16.4% and high boiling point methyl di tert-butylphenol 18.9%.

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Abstract

Relating to the field of m-cresol and p-cresol separation and its technology, the invention discloses a new method of separating an m-cresol and p-cresol mixture to obtain high-purity m-cresol and p-cresol. The method takes a m-cresol and p-cresol mixed solution and isobutene gas as the raw materials, and employs a solid supported acidic ionic liquid as the catalyst to carry out alkylation reaction in a fixed bed, the obtained alkylation product is separated to obtain mono-t-butyl cresol, which is subjected to de-tert-butylation, thus obtaining the high purity m-cresol and p-cresol.

Description

technical field [0001] The invention relates to a method for separating m-cresol by fixed-bed alkylation, specifically for separating m-cresol and p-cresol mixture, and obtaining high-purity m-cresol and p-cresol, which belongs to chemical separation field of purification. technical background [0002] m-cresol and p-cresol are important fine chemical intermediates. The organic chemical industry and synthesis industry started from cresol are very developed. Its products cover many industries including resin, medicine, dye, fragrance, antioxidant and so on. [0003] With the development and utilization of downstream products, a large number of high-purity products with a mass content (the same below) greater than 99.0% are required in a large number of industries, resulting in a tight demand for high-purity cresols with a mass content ≥ 99.0%, especially ≥ 99.5%. . In order to obtain high-purity chemical products, high-purity p-cresol or m-cresol must be used as raw materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/86
CPCC07C37/86
Inventor 周沛方岩雄蔡晓兰王东方萍谭伟张维刚
Owner ANQING FULLTIME CHEM INDAL
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