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Trimethoxybenzoic acid preparation method

A technology of trimethoxybenzoic acid and crude products, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve problems such as increased cost and low efficiency

Inactive Publication Date: 2015-11-04
ZUNYI XINXIANG BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a kind of preparation method of trimethoxybenzoic acid, to solve the cost increase that multistage reaction prepares in the prior art, the problem of low efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The invention provides a preparation method of trimethoxybenzoic acid, comprising the following steps:

[0021] A. 100 parts of gallnut powder, 55 parts of water, 90 parts of dimethyl sulfate, 135 parts of lye were added to the reaction kettle, then heated by steam, controlled reaction temperature 85 ℃, stirred with glass rod in the reaction process, controlled The pH value is 10, and the concentration of the lye solution is 30%;

[0022] B. after step A was reacted for 4 hours, the temperature was raised to 95 ° C, and the addition of 14 parts by mass of sulfuric acid was acidified, and the temperature was controlled at 75 ° C during acidification, and the pH value was 2;

[0023] C. the acidification reaction solution obtained from the step B reaction is crystallized by cooling to obtain the trimethoxybenzoic acid crude product;

[0024] D. 100 parts of trimethoxybenzoic acid crude products obtained in step C, 910 parts of water, 30 parts of activated carbon and 1 pa...

Embodiment 2

[0028] The invention provides a preparation method of trimethoxybenzoic acid, comprising the following steps:

[0029] A. 100 parts of gall powder, 48 parts of water, 80 parts of dimethyl sulfate, and 130 parts of lye were added to the reactor, then heated by steam, and the reaction temperature was controlled at 75°C, and a glass rod was used to stir during the reaction to control PH value is 9.4, and the concentration of lye is 30%;

[0030] B. after step A was reacted for 4 hours, the temperature was raised to 90 ° C, and 11 parts by mass of sulfuric acid were added for acidification, and the temperature was controlled at 75 ° C during acidification, and the pH value was 2;

[0031] C. the acidification reaction solution obtained from the step B reaction is crystallized by cooling to obtain the trimethoxybenzoic acid crude product;

[0032] D. 100 parts of the obtained trimethoxybenzoic acid crude product of step C, 900 parts of water, 25 parts of activated carbon and 1 par...

Embodiment 3

[0036] The invention provides a preparation method of trimethoxybenzoic acid, comprising the following steps:

[0037] A. 100 parts of gallnut powder, 58 parts of water, 100 parts of dimethyl sulfate, and 140 parts of lye were added to the reactor, then heated by steam, and the reaction temperature was controlled to 90° C. During the reaction, a glass rod was used to stir, control PH value is 10.3, and the concentration of lye is 30%;

[0038] B. after step A was reacted for 4 hours, the temperature was raised to 100 ° C, and 19 parts by mass of sulfuric acid were added for acidification, and the temperature was controlled at 75 ° C during acidification, and the pH value was 2;

[0039] C. the acidification reaction solution obtained from the step B reaction is crystallized by cooling to obtain the trimethoxybenzoic acid crude product;

[0040] D. 110 parts of the obtained trimethoxybenzoic acid crude product of step C, 970 parts of water, 40 parts of activated carbon and 3 p...

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PUM

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Abstract

The present invention discloses a trimethoxybenzoic acid preparation method, which comprises: A, adding 100 parts of Galla chinensis powder, 48-58 parts of water, 80-100 parts of Dimethylsulfate, and 130-140 parts of an alkali liquid to a reaction kettle, carrying out steam heating, controlling the temperature of 75-90 DEG C, stirring, and controlling the PH value of 9.4-10.3; B, after carrying out the reaction for 4-5 h, heating to the temperature of 90-100 DEG C, and adding 11-19 parts of sulfuric acid to carry out acidification; C, carrying out cooling crystallization to obtain a trimethoxybenzoic acid crude product; D, adding 85-110 parts of the trimethoxybenzoic acid crude product obtained in the step C, 900-970 parts of water, 25-40 parts of active carbon and 1-3 parts of EDTA to the reaction kettle to carry out a reaction for 2 h, and controlling the temperature of 100-105 DEG C and the pressure of 0.7-0.9 MPa; and E, adding the mixed liquid obtained in the step D to a centrifuge to carry out solid-liquid separation, and carrying out cooling crystallization on the obtained liquid to obtain the trimethoxybenzoic acid solid. According to the present invention, the purity of the trimethoxybenzoic acid prepared through the method is high, the cost and the production period are less, and the whole production efficiency is improved.

Description

technical field [0001] The invention belongs to the field of benzoic acid esters, and particularly relates to a preparation method of trimethoxybenzoic acid. Background technique [0002] Trimethoxybenzoic acid is also called trimethyl ether gallic acid, usually abbreviated as TMBA, white crystalline powder with molecular formula C 10 H 12 0 5 , the molecular weight of 212.2, is mainly an important fine chemical product produced with gallic tannin as raw material, and gallic tannic acid mainly exists in gallic. It is used as an additive in high-grade food, cigarettes and beverages, especially in the fields of organic synthesis and medicine, dyes, food and light industry. In terms of organic synthesis, it is mainly used to prepare organic compounds such as trimethoxybenzoyl chloride, syringic acid, trimethoxybenzoate, etc. In the pharmaceutical industry, it is mainly used to prepare anti-inflammatory drugs for the treatment of nervousness, phobia and neurotic syndrome. An...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/09C07C65/21
CPCC07C51/09C07C65/21
Inventor 宋时权
Owner ZUNYI XINXIANG BIOTECH CO LTD
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