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Preparation method of m-cresol

A cresol and methyl technology, applied in the preparation of organic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of difficult separation and purification of products, harsh reaction conditions, etc., and achieve novel synthetic routes, simple operation, The effect of good application prospects

Active Publication Date: 2021-01-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis method of m-cresol has severe reaction conditions (alkali fusion, high temperature hydrolysis, peroxide cracking), difficult product separation and purification (separation of m-cresol and p-cresol), etc.

Method used

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  • Preparation method of m-cresol
  • Preparation method of m-cresol
  • Preparation method of m-cresol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Synthesis of 5-Methyl-2-Cyclohexenone by Gas Phase Condensation of Crotonaldehyde and Acetone

[0040] The gas-phase condensation reaction is carried out in a tubular reactor. The length of the reaction tube is 60 cm, and the inner diameter is 2.3 cm. The middle part of the reaction tube is filled with a spherical zinc oxide catalyst (100 g, with a purity of 95%), and the top and bottom ends are filled with ceramic ring fillers. When conducting condensation experiments, first turn on the power of the fixed bed reactor, open the inlet and outlet valves of the reaction tube carrier gas, and turn on the nitrogen carrier gas at a flow rate of 100mL / min, and the carrier gas goes in and out of the reaction tube. Turn on the heating mantle of the reaction tube to raise the temperature of the reaction tube to 260°C; turn on the heat tracing of the preheating tank on the feed line to raise its temperature to 220°C. After the temperature of the preheating tank and the reaction tu...

Embodiment 2

[0043] Synthesis of 5-Methyl-2-Cyclohexenone by Vapor Phase Condensation of 3-Hydroxybutyraldehyde and Acetone

[0044] The gas-phase condensation reaction is carried out in a tubular reactor. The length of the reaction tube is 60 cm, and the inner diameter is 2.3 cm. The middle part of the reaction tube is filled with a spherical zinc oxide catalyst (100 g, with a purity of 95%), and the top and bottom ends are filled with ceramic ring fillers. When conducting condensation experiments, first turn on the power of the fixed-bed reactor, open the inlet and outlet valves of the reaction tube carrier gas, and turn on the nitrogen carrier gas at a flow rate of 35mL / min. The carrier gas goes in and out of the reaction tube. Turn on the heating mantle of the reaction tube to raise the temperature of the reaction tube to 270°C; turn on the heat tracing of the preheating tank on the feed line to raise its temperature to 220°C. After the temperature of the preheating tank and the reacti...

Embodiment 3

[0046] Synthesis of 5-Methyl-2-Cyclohexenone by Vapor Phase Condensation of 3-Methoxybutyraldehyde and Acetone

[0047] First configure the raw material solution, 3-methoxybutyraldehyde (143.0g, 1.4mol), acetone (813.1g, 14.0mol) and trimethyl phosphate (0.2g, 0.0014mol), the appearance is a colorless transparent solution . Start the power supply of the fixed bed device, feed nitrogen carrier gas at 120mL / min, and the carrier gas goes in and out of the reaction tube; turn on the preheating tank and the reaction tube to heat, and raise the temperature to 220°C and 280°C respectively. After the temperature of the preheating tank and the reaction tube is stable for 0.5h, start the feed pump to feed the raw material liquid, the feed rate is 1.0g / min, and the weight hourly space velocity is 0.6h -1 . The reaction tube has a length of 60 cm and an inner diameter of 2.3 cm. The middle part of the reaction tube is filled with a spherical barium oxide catalyst (100 g, with a purity o...

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Abstract

The invention provides a method for synthesizing m-cresol through condensation and dehydrogenation reactions, which specifically comprises the following steps: carrying out condensation reaction on C4aldehyde or ketone and acetone under the catalysis of an alkali to obtain a 5-methyl-2-cyclohexenone intermediate, and carrying out dehydrogenation aromatization on the intermediate under the actionof a dehydrogenation catalyst to obtain m-cresol. The synthetic route is novel and cheap, easily available C4 aldehyde or ketone and acetone are taken as starting materials, m-cresol is obtained through two-step reaction, the synthetic route is short, the yield is high, and the cost advantage is better. Secondly, solid alkali is used as a catalyst, phosphate ester is used as a reaction promoter, areaction substrate is subjected to a condensation reaction in a gas phase, and the cyclohexenone intermediate is obtained with high selectivity.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and specifically relates to a method for synthesizing m-cresol by using C4 aldehyde or ketone and acetone as raw materials, first performing condensation reaction, and then dehydroaromatizing. Background technique [0002] m-cresol, scientific name 3-methylphenol, is one of the simplest alkylphenols. m-cresol is a colorless or light yellow liquid with phenol smell, which is naturally present in organisms, with a boiling point of 202.2°C and a melting point of 12.2°C. m-cresol has a wide range of uses, and has corresponding applications in the fields of pesticides, medicines, synthetic materials, spices, and organic dyes. [0003] In view of the wide use and huge demand of m-cresol, there are many industrial production methods of m-cresol, including natural extraction and artificial chemical synthesis. As early as the 1940s and 1950s, people began to extract m-cresol from coal tar. Coal ta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/07
CPCC07C37/07C07C45/74C07C2601/16C07C39/07C07C49/603
Inventor 黄文学国建茂宋明焱张永振张涛
Owner WANHUA CHEM GRP CO LTD
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