Preparation method of high-purity p-methyl benzyl alcohol

A p-methylbenzyl alcohol, high-purity technology, applied in the field of preparation of high-purity p-methylbenzyl alcohol, can solve the problems of endangering the health of operators, difficult recycling, and polluting the production environment, so as to reduce energy consumption and cost, avoid Post-processing burden and the effect of reducing environmental emissions

Inactive Publication Date: 2019-05-10
WUHAN GEYUAN FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional preparation of p-methylbenzyl alcohol includes the hydrolysis of p-methylbenzyl chloride to obtain the product. This method usually needs to react for a long time under the action of a catalyst, and it is easy to produce by-products
Many researchers have improved this method at present, as New J.Chem., 2011,35,292-298 discloses a kind of method that prepares p-methyl benzyl alcohol with ionic liquid and ferric sulfate as catalyst, can effectively control generation of by-products, but the reaction obviously has the following deficiencies: (1) a co-catalyst system is used, the reaction cost is high, and it is not easy to recycle; (2) poisoned organic solvent toluene is used, which pollutes the production environment and endangers the health of operators; ( 3) This reaction is a small laboratory test. If it is extended to industrial production, there will be many unpredictable factors
[0003] In addition, the purity of the product obtained by the hydrolysis reaction cannot meet the solvent standards for high-grade pigments and coatings, let alone be used as an excellent solvent for high-grade printer oils. Therefore, the hydrolyzed products need to be further processed to a purity of more than 99.9% in order to meet certain high-grade chemical requirements. product demand

Method used

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  • Preparation method of high-purity p-methyl benzyl alcohol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A preparation method for high-purity p-methylbenzyl alcohol, comprising the following steps:

[0030] 1) Add 4000kg of pure water and 400kg of sodium carbonate to the reaction kettle, stir and heat to 50°C, then add 800kg of p-methylbenzyl chloride to the mixture, and check the initial pH value to be 8.7. Continue to heat up to 115°C, and increase the pressure of the batching tank to 0.15MPa. Take a sample after reacting for 5 hours, the pH test shows that the pH value is 7.8, the GC test shows that the content of p-methylbenzyl alcohol is 98.8%, the content of p-methylbenzyl chloride is 0.01%, and the content of di-p-methylbenzyl ether is 0.87%, stop the reaction .

[0031] Separate the liquid, collect the organic phase, and obtain 691.6 kg of crude p-methylbenzyl alcohol.

[0032] 2) Repeatedly evacuate and fill the rectification system with nitrogen until the oxygen content is lower than 0.5%, and press the crude p-methylbenzyl alcohol into the rectification kettle...

Embodiment 2

[0035] A preparation method for high-purity p-methylbenzyl alcohol, comprising the following steps:

[0036] 1) Add 4000kg of pure water and 400kg of sodium carbonate to the reaction kettle, stir and heat to 55°C, then add 800kg of p-methylbenzyl chloride to the mixture, and check the initial pH value to be 8.9. Continue to heat up to 115°C, and increase the pressure of the batching tank to 0.16MPa. After reacting for 5 hours, the sample was taken, and the pH test showed that the pH value was 7.9. The GC test showed that the content of p-methylbenzyl alcohol was 98.6%, the content of p-methylbenzyl chloride was 0.02%, and the content of di-p-methylbenzyl ether was 0.94%. Stop the reaction .

[0037] Separate the liquid, collect the organic phase, and obtain 695.6 kg of crude p-methylbenzyl alcohol.

[0038] 2) Repeatedly evacuate and fill the rectification system with nitrogen until the oxygen content is lower than 0.5%, and press the crude p-methylbenzyl alcohol into the re...

Embodiment 3

[0041] A preparation method for high-purity p-methylbenzyl alcohol, comprising the following steps:

[0042]1) Add 4000kg of pure water and 400kg of sodium carbonate to the reaction kettle, stir and heat to 60°C, then add 800kg of p-methylbenzyl chloride to the mixture, and check the initial pH value to be 8.8. Continue to heat up to 114°C, and increase the pressure of the batching tank to 0.15MPa. After reacting for 5 hours, take a sample, the pH detection shows that the pH value is 7.6, the GC detection shows that the content of p-methylbenzyl alcohol is 98.8%, the content of p-methylbenzyl chloride is 0.02%, and the content of di-p-methylbenzyl ether is 0.95%, stop the reaction .

[0043] Separate the liquid, collect the organic phase, and obtain 699.2kg of crude p-methylbenzyl alcohol.

[0044] 2) Repeatedly evacuate and fill the rectification system with nitrogen until the oxygen content is lower than 0.5%, and press the crude p-methylbenzyl alcohol into the rectificati...

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Abstract

The invention relates to a preparation method of high-purity p-methyl benzyl alcohol. The method comprises the following steps: carrying out the hydrolysis reaction for p-methyl benzyl chloride in a carbonate or bicarbonate saline solution under a pressure of 0.15 MPa to 0.2 MPa, wherein the pH value of the hydrolysis reaction is 7 to 9, the temperature of the hydrolysis reaction is 110 DEG C to 120 DEG C, and rectifying a crude product obtained in the hydrolysis reaction in a rectifying kettle to obtain high-purity p-methyl benzyl alcohol. The preparation method provided by the invention canbe directly applied to the industrial production, and has the advantages of high raw material conversion rate, high product purity, pollution-free reaction and environmental protection.

Description

technical field [0001] The invention belongs to the field of industrial production of p-methylbenzyl alcohol, and in particular relates to a preparation method of high-purity p-methylbenzyl alcohol. Background technique [0002] As an important mechano-synthetic intermediate, p-methylbenzyl alcohol can be widely used in chemical industry, dyestuff, pesticide and other fields. The traditional preparation of p-methylbenzyl alcohol includes hydrolyzing p-methylbenzyl chloride to obtain the product. This method usually needs to react for a long time under the action of a catalyst, and is prone to produce by-products. Many researchers have improved this method at present, as New J.Chem., 2011,35,292-298 discloses a kind of method that prepares p-methyl benzyl alcohol with ionic liquid and ferric sulfate as catalyst, can effectively control generation of by-products, but the reaction obviously has the following deficiencies: (1) a co-catalyst system is used, the reaction cost is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C29/80C07C33/20
Inventor 林齐伦
Owner WUHAN GEYUAN FINE CHEM CO LTD
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