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Preparation method of 2,4,6-trimethylbenzoic acid

A technology of trimethylbenzoic acid and mesitylene, applied in the direction of carboxylate preparation, organic compound preparation, chemical instruments and methods, etc., can solve the problem of low purity of trimethylbenzoic acid and achieve the effect of continuous reaction

Active Publication Date: 2019-02-12
贵州新天鑫化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the above reaction process, a large amount of anhydrous aluminum chloride needs to be used, and the prepared 2,4,6-trimethylbenzoic acid has a low purity of about 92-96%, which cannot meet people's needs

Method used

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  • Preparation method of 2,4,6-trimethylbenzoic acid
  • Preparation method of 2,4,6-trimethylbenzoic acid
  • Preparation method of 2,4,6-trimethylbenzoic acid

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preparation example Construction

[0019] The invention provides a kind of preparation method of 2,4,6-trimethylbenzoic acid, comprising the following steps:

[0020] Reaction of mesitylene and carbon dioxide under the action of a catalyst to obtain 2,4,6-trimethylbenzoic acid; the catalyst is hydrogen chloride or concentrated hydrochloric acid.

[0021] In the present invention, unless otherwise specified, all raw materials are commercially available goods.

[0022] In the invention, mesitylene and carbon dioxide are reacted under the action of a catalyst to obtain 2,4,6-trimethylbenzoic acid.

[0023] In the present invention, the carbon dioxide is preferably liquid carbon dioxide. In the present invention, the catalyst is hydrogen chloride or concentrated hydrochloric acid; when the catalyst is concentrated hydrochloric acid, the mass concentration of the concentrated hydrochloric acid is preferably 37%-40%, more preferably 38%-39%. The mass of the catalyst is 0.1%-20% of the mass of mesitylene, more prefe...

Embodiment 1

[0037] Add various reaction raw materials into the material tank, control the flow of mesitylene to 50mL / min, the temperature in the microreactor to 70°C, the pressure to 3.0MPa, the molar ratio of mesitylene to carbon dioxide is 1:0.5, and the catalyst is a mass concentration of 38%. Concentrated hydrochloric acid, use the length of the coil to control the reaction time to 25s, separate layers after the reaction, the lower layer concentrated hydrochloric acid is recovered, the upper layer is cooled and centrifugally filtered, the solid is collected to obtain 2,4,6-trimethylbenzoic acid, and the filtered filtrate is transported Return to the material tank to continue the reaction, and the product has a purity of 99.1%.

[0038] Carry out nuclear magnetic analysis and mass spectrometry to the 2,4,6-trimethylbenzoic acid that embodiment 1 prepares, analysis result is as follows figure 1 with figure 2 shown, where figure 1 It is the NMR spectrum of 2,4,6-trimethylbenzoic acid,...

Embodiment 2

[0040] Add various reaction raw materials into the material tank, control the flow rate of mesitylene to 100mL / min, the temperature in the microreactor to 40°C, the pressure to 3.5MPa, the molar ratio of mesitylene to carbon dioxide is 1:0.3, and the catalyst is hydrogen chloride gas. The length of the tube is controlled and the reaction time is 25s. After the reaction is completed, the solid is collected by cooling and centrifugal filtration to obtain 2,4,6-trimethylbenzoic acid. The filtered filtrate is sent back to the material tank to continue the reaction. The product purity is 99.0%.

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Abstract

The invention provides a preparation method of 2,4,6-trimethylbenzoic acid. The preparation method comprises the following steps that mesitylene and carbon dioxide react under the effect of a catalyst; the 2,4,6-trimethylbenzoic acid is obtained, wherein the catalyst is hydrogen chloride or concentrated hydrochloric acid. The preparation method provided by the invention has the advantages that thehydrogen chloride or concentrated hydrochloric acid is used for replacing anhydrous aluminium chloride in the prior art; the problem that a large amount of anhydrous aluminium chloride is needed in the reaction process is avoided; the purity of the 2,4,6-trimethylbenzoic acid prepared by the method provided by the invention is high and can reach 98.1 to 99.1 percent. In addition, the preparationmethod provided by the invention can realize continuous reaction and is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of 2,4,6-trimethylbenzoic acid. Background technique [0002] 2,4,6 Trimethylbenzoic acid is an important intermediate in organic synthesis, widely used in the production of dyes, pesticides, pharmaceuticals and photoinitiators. In recent years, with the continuous increase of its application fields, the market potential of 2,4,6 trimethylbenzoic acid has also increased, and the industrial preparation has attracted more and more attention. [0003] At present, the method for synthesizing 2,4,6-trimethylbenzoic acid is mainly the direct carboxylation of mesitylene with carbon dioxide, that is, using anhydrous aluminum chloride as a catalyst to catalyze the synthesis of 2,4,6-trimethylbenzene and carbon dioxide. Methylbenzoic acid method. However, in the above reaction process, a large amount of anhydrous aluminum chloride needs to be used, and the...

Claims

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Application Information

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IPC IPC(8): C07C51/15C07C51/42C07C51/47C07C51/48C07C63/04B01J27/08
CPCC07C51/15C07C51/42C07C51/47C07C51/48B01J27/08C07C63/04
Inventor 王洪培胡雷冯高飞甘立炜沈鑫王忠卫
Owner 贵州新天鑫化工有限公司
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