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Method for separating m,p-cresol mixture by adopting selective oxidation catalyst

A technology of p-cresol and mixtures, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of large equipment investment constraints, cumbersome steps, and difficulty in large-scale production, and achieve low production costs and responsiveness. Ease of operation and high value-added utilization

Inactive Publication Date: 2019-05-21
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, cumbersome steps and large investment in equipment restrict the scale of production, making it difficult to achieve large-scale production

Method used

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  • Method for separating m,p-cresol mixture by adopting selective oxidation catalyst
  • Method for separating m,p-cresol mixture by adopting selective oxidation catalyst
  • Method for separating m,p-cresol mixture by adopting selective oxidation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Oxidation of m-p-cresol mixture: with m-p-cresol mixture (1.08g, m-cresol: p-cresol=1:1, molar ratio), catalyst (4.5wt%) and solvent (acetonitrile: 80ml and water : 4ml) into the autoclave, close the autoclave and start stirring, fill with oxygen to 1.0MPa, heat up to 40°C and keep for 8 hours. Cool to room temperature after the reaction is over, vent the gas and open the reactor to collect the mother liquor after the reaction;

[0023] Determination of conversion and yield by HPLC or silica gel column chromatography: HPLC uses EclipePlus C18 column (250mm × 4.6mm, 5.0um) on Waters 1525 and 2707 autosampler with 2489UV-Vis detector High-performance liquid chromatography is performed on a certified standard sample to determine the characteristics of the product. Silica gel column Use 200-300 mesh silica gel (petroleum ether / ethyl acetate) for column chromatography analysis.

[0024] The NMR data of m-cresol oxidation products are as follows:

[0025] 1 H NMR (600M...

Embodiment 2 to 4

[0031] Separation of p-cresol was carried out in the same manner as in Example 1, and specific parameters were listed according to numbers 2 to 4 in Table 1 below.

[0032]

[0033] It can be seen that pure p-cresol can be obtained after rectification treatment, with a purity of more than 99%, which can meet the purity requirements of production.

Embodiment 5 to 14

[0034] Examples 5 to 14: Comparison of catalytic oxidation results of m-p-cresol mixture by cuprous chloride catalyst.

[0035] Carry out the oxidation of m-p-cresol mixture in the same manner as step 1) in Example 1, and the reaction parameters are listed in Table 2 below.

[0036] Table 2

[0037]

[0038]

[0039] According to the data of Examples 5 to 14, it can be seen that the conversion of m-cresol can be efficiently realized by using CuCl.

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Abstract

The invention provides a method for separating an m,p-cresol mixture by adopting a selective oxidation catalyst. According to the method, the m,p-cresol mixture can be oxidized by using the selectiveoxidation catalyst, m-cresol in the mixture is completely oxidized into a benzoquinone compound, and p-cresol does not react. After the oxidation reaction is carried out, the boiling point differencebetween the benzoquinone compound (186-187 DEG C) and the p-cresol is significant, therefore, the complete separation of the p-cresol can be achieved through rectification. According to the separationmethod, during the oxidation reaction, oxygen or air is used as an oxidizing agent, the reaction conditions are very mild, the reaction operation is simple, the production cost is low, and the industrial production is easy. In addition, the generated benzoquinone compound through the reaction is an important dye and a raw material of an antioxidant, the high added value utilization can be achieved, and the economic benefit is good.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for separating m-p-cresol mixture by using a selective oxidation catalyst. Background technique [0002] P-cresol is an important fine chemical raw material and auxiliary agent. It has important uses in synthetic plastics, dyes, antioxidants, etc. It is also used as a raw material for disinfectants and preservatives in medicine. Therefore, the preparation of pure p-cresol monomer has attracted much attention. However, in industrial production, p-cresol is generally sold as a mixture with m-cresol, and the required pure p-cresol monomer needs further separation and purification to obtain. In the process of separating mixed cresols, since the difference between m-cresol and p-cresol is only 0.4°C in boiling point and 24.6°C in melting point, it is difficult to separate them by ordinary distillation or rectification techniques, so it is necessary to find a suit...

Claims

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Application Information

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IPC IPC(8): C07C37/68C07C37/86C07C37/74C07C39/07
Inventor 安增建徐国强
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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