Preparation method of orthocresol

A technology of o-cresol and o-chlorotoluene, applied in the field of preparation of o-cresol, can solve the problems of low selectivity of o-cresol, low conversion rate of chlorotoluene, low yield and the like, and achieve high selectivity and high conversion high-efficiency, high-activity effect

Active Publication Date: 2015-07-01
济南尚博医药股份有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

But adopt chlorotoluene hydrolysis method to prepare cresol, usually productive rate is lower, in the prior art, usually improve its productive rate by adding catalyst, usually used catalyzer is copper or copper compound, but the transformation rate of chlorotoluene Low, the selectivity of o-cresol is also low, the total yield of cresol is about 80%, and the selectivity of o-cresol is about 50%

Method used

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preparation example Construction

[0020] The invention provides a kind of preparation method of o-cresol, comprising:

[0021] Mix and react o-chlorotoluene, basic compound, water and catalyst to obtain o-cresol;

[0022] The catalyst is selected from the mixture of copper and / or copper-containing compounds and M chloride, hydroxide, oxide, acetate or sulfate; the M is selected from Fe, Mn, Zn, Ni or Ti.

[0023] In the present invention, copper, copper-containing compounds and other metal salts are used as composite catalysts, and o-cresol is prepared by hydrolyzing chlorotoluene. At a lower reaction temperature, the reaction can be made to have higher activity, and the raw materials have higher The conversion rate has higher selectivity to o-cresol, and the o-cresol prepared has higher purity.

[0024] In the preparation method of o-cresol provided by the invention, firstly, o-chlorotoluene, basic compound, water and catalyst are mixed and reacted.

[0025] The basic compound is preferably sodium carbonate...

Embodiment 1

[0035] Add 100g of o-chlorotoluene, 95g of potassium hydroxide, 184.4g of water, 1g of copper and 1g of ferric chloride into the autoclave and mix them. After tightening the screws, start stirring and start heating. The reaction system is kept at 220°C for 3 hours, and then cooled down. When the temperature of the system reaches room temperature, discharge the material to obtain the o-cresol crude product; then use hydrochloric acid to adjust the pH value of the o-cresol crude product to 4.0, then extract three times with 300mL toluene, combine the organic phases, and concentrate under reduced pressure to obtain o-cresol finished product.

[0036] Detect the composition of the o-cresol finished product with gas chromatography, the result shows, it contains o-cresol 93.73wt%, o-chlorotoluene 1.2wt%, phenol 0.78wt%, m-cresol 0.2wt%, o-cresol selectivity is 95.2%.

Embodiment 2

[0038] Add 20g of o-chlorotoluene, 19g of potassium carbonate, 171g of water, 0.4g of cuprous chloride and 0.6g of nickel hydroxide into the autoclave and mix them. After tightening the screws, turn on the stirring and start heating, and react the reaction system at a constant temperature of 280°C for 20min. , then lower the temperature; when the temperature of the system reaches room temperature, unload to obtain the crude product of o-cresol; then use sulfuric acid to adjust the pH value of the crude product of o-cresol to 3.0, then extract three times with 120mL of chloroform, combine the organic phases, Concentrate under reduced pressure to obtain o-cresol finished product.

[0039] Detect the composition of the o-cresol finished product with gas chromatography, the result shows, it contains o-chlorotoluene 64.2wt%, phenol 1.78wt%, o-cresol 27.5wt%, m-cresol 1.2wt%, o-cresol selectivity 76.8 %.

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Abstract

The invention provides a preparation method of orthocresol, which comprises the steps of mixing ortho-chlorotoluene, an alkaline compound, water and a catalyst for reaction to obtain orthocresol, wherein the catalyst is selected from cuprum and / or a mixture of a cuprum-bearing compound with chloride, hydroxide, oxide, acetate or sulfate of M; and the M is selected from Fe, Mn, Zn, Ni or Ti. According to the method, orthocresol is prepared by taking cuprum, the cuprum-bearing compound and other metal salt as the composite catalyst and adopting a chloro-toluene hydrolysis method; the reaction can have higher activity at lower reaction temperature; raw materials are higher in conversion rate; the method has higher selectivity for orthocresol; and prepared orthocresol has higher purity.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of o-cresol. Background technique [0002] Cresol is a widely used chemical intermediate, which has three isomers of o-cresol, m-cresol and p-cresol, and each isomer plays an important role in different fields. [0003] Among them, o-cresol is an important fine chemical intermediate for the synthesis of pesticides, medicines, resins, dyes, antioxidants, polymerization inhibitors and spices, etc. It can be mainly used to prepare p-chloro-o-cresol, o-hydroxybenzaldehyde, and o-cresol novolac Resin and epoxy o-cresol phenolic resin, o-methyl salicylic acid, etc. At present, the domestic production process of o-cresol is relatively backward, and the domestic consumption of o-cresol mainly depends on imports. Therefore, the optimization of the preparation process of o-cresol is an urgent problem to be solved, and has broad application prospects. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/02B01J27/128B01J27/138B01J31/28B01J27/055
Inventor 孟庆文胡廷峰张恩选焦芬王芳芳
Owner 济南尚博医药股份有限公司
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