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Method for production of high-purity m-cresol

A technology for the production of m-cresol and m-cresol, applied in chemical instruments and methods, ion exchange regeneration, preparation of organic compounds, etc., can solve problems such as low quality m-cresol products and complicated process flow, and achieve good economic benefits, Simple production process and low production cost

Active Publication Date: 2018-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The application provides a method for the production of m-cresol, to solve the problems of complex technological process and low quality of m-cresol products in the previous technology of producing m-cresol

Method used

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  • Method for production of high-purity m-cresol
  • Method for production of high-purity m-cresol
  • Method for production of high-purity m-cresol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The preparation of embodiment 1 molecular sieve adsorbent sample

[0062] Mix the molecular sieve and the binder in a certain proportion, add an appropriate amount of 5% dilute nitric acid as an auxiliary agent, extrude into a strip, dry at 120°C, and bake at 550°C for 10 hours to obtain a shaped sample. Cut the above molded sample into 1-2 mm to obtain a columnar matrix. Add 1,500 grams of the parent body into 5,000 mL of potassium hydroxide solution, treat at a certain temperature for a period of time and a certain number of times, and then wash with deionized water until neutral. Dry at 120°C and bake at 500°C for 10 hours to prepare potassium hydroxide modified samples. Add 1500 grams of potassium hydroxide modified sample into 5000 mL of metal nitrate aqueous solution containing a certain concentration for ion exchange modification, treat it at a certain temperature for a period of time and a certain number of times, and wash it with deionized water until neutral....

Embodiment 2

[0068] The preparation of embodiment 2 isomerization catalyst samples

[0069] Mix the molecular sieve and the binder in a certain proportion, add an appropriate amount of 5% dilute nitric acid as an auxiliary agent, extrude into a strip, dry at 120°C, and bake at 550°C for 10 hours to obtain a shaped sample. The above-mentioned molded sample is cut into 1-3 mm to prepare a columnar matrix. A certain amount of columnar matrix is ​​placed in a certain amount of metal solution for ion exchange modification, then dried at 120°C and calcined at 600°C for 3 hours to obtain an isomerization catalyst.

[0070] The serial number of the obtained product, the added amount of molecular sieve and binder, the concentration of the solution used for ion exchange, the content of molecular sieve and the content of metal oxide in the isomerization catalyst are shown in Table 2.

[0071] Table 2

[0072]

Embodiment 3～12

[0073] The production of embodiment 3~12 m-cresols

[0074] Using the molecular sieve adsorbent sample in embodiment 1 and the isomerization catalyst sample in embodiment 2, according to the attached figure 1 The flow diagram is shown for the production of m-cresol. Among them, the isomerization reaction is carried out on a fixed bed reaction device; the weight space velocity is 0.5 to 5 hours -1 , The reaction temperature is 320-450°C, and the diluent gas is water vapor.

[0075] In Examples 3 to 12, the conditions of the adsorption unit, the conditions of the isomerization reaction unit, and the reaction results in each example are shown in Table 3. In Examples 3-12, the purity of the obtained m-cresol products is greater than 99.5%.

[0076] table 3

[0077]

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Abstract

The invention provides a method for production of high-purity m-cresol. The method comprises the following steps: (1) injecting a material I containing m-cresol and p-cresol into an adsorption unit for adsorptive separation to obtain an m-cresol product, wherein an adsorption unit comprises one or more adsorbent bed layer, and the at least one adsorbent bed layer comprises a molecular sieve adsorbent; (2) injecting a material II containing a desorbent into the adsorption unit to desorb the adsorbent bed layer in the adsorption unit so as to obtain a desorption material III, injecting the desorption material III into a separation unit, and performing separation to obtain a desorbent material IV and a mixed cresol material V; (3) returning the desorbent material IV obtained through separation in the step (2) into the adsorption unit for recycling; and (4) injecting the mixed cresol material V obtained through separation in the step (2) into an isomerization reaction unit for a reaction to obtain an isomerization product material VI, and returning the isomerization product material VI into the desorption unit.

Description

technical field [0001] The application relates to a method for producing high-purity m-cresol, which belongs to the field of chemistry and chemical engineering. Background technique [0002] m-cresol is mainly used as a pesticide intermediate to produce insecticides fenitrothion, fenthion, medicarb, permethrin, and also an intermediate of color film, resin, plasticizer and spice. [0003] At present, the main process route for synthesizing m-cresol at home and abroad is to use cumene to be converted into methyl cumene hydroperoxide under the initiation of hydrogen peroxide free radicals, and then oxidize with oxygen in the air to produce It is rich in m- and p-cresol, and acetone is produced by-product, but the complexity of the reaction is much higher than that of phenol. The product obtained by this method has almost no ortho-position products, and the ratio of inter-position and para-position is about 7:3. And this method distillation purification cost is high. [0004...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/00C07C37/82C07C39/07B01J29/76B01J29/80B01J20/16B01J20/30B01D15/08
CPCB01D15/08B01J20/041B01J20/16B01J29/76B01J29/7676B01J29/80B01J2220/4812B01J2229/18C07C37/00C07C37/82C07C39/07
Inventor 王坤院刘中民徐云鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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