Method for preparing trimesic acid

A technology of trimesic acid and dimethyl benzoic acid is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of environmental pollution production process danger, low conversion rate and high cost , to achieve the effects of environmental protection and product purification, less tar content, and improved utilization

Active Publication Date: 2017-02-22
黄石市利福达医药化工有限公司
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  • Claims
  • Application Information

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Problems solved by technology

Among them, a large amount of waste water and waste residue are produced in the reaction process of the potassium permanganate oxidation method, and the post-treatment is difficult, and the conversion rate is low, and the purification is more complicated; the raw material cost of the nitric acid method is high, the selectivity to the target product is poor, and the product is difficult to refine. The environment is seriously polluted and the production process is dangerous; the oxygen oxidation method uses glacial acetic acid as a solvent. Due to the strong activity of mesitylene, a large amount of tar is produced during the reaction process, which is costly and difficult to separate and purify.

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[0029] In the preparation method of trimesic acid provided by the invention, 3,5-dimethylbenzoic acid is oxidized to generate trimesic acid by a liquid phase oxidation method under the action of a catalytic system.

[0030] In the prior art, mesitylene is usually used to prepare trimesic acid. Compared with mesitylene, the 3,5-dimethylbenzoic acid provided by the present invention produces less tar in the process flow and has a higher yield , not only reduces pollution, but also facilitates product purification.

[0031] The liquid-phase oxidation method has the characteristics of fast reaction speed, short process and suitable for large-scale production.

[0032] Preferably, when carrying out the liquid-phase oxidation method, glacial acetic acid is used as a solvent.

[0033] Glacial acetic acid has a very high solubility to oxygen, which is beneficial to the rapid progress of the reaction.

[0034] Preferably, when performing the liquid-phase oxidation method, the oxidant...

Embodiment 1

[0065] Put 100g 3,5-dimethylbenzoic acid, 680g glacial acetic acid, 8g cobalt acetate, 3g bromine Potassium chloride, 3g of zirconium acetate, and 1g of triethanolamine were heated up to 75°C, and oxygen was turned on at 1L / min until reflux, and the oxygen reaction was maintained under reflux for 6 hours. The raw material was less than 0.5% as the reaction end point, and the crude product and Mother liquor, the crude product is to be refined, and the mother liquor is absorbed by activated carbon and used mechanically.

[0066] Add 10g of activated carbon to the mother liquor in the upper batch, raise the temperature to 80°C to 90°C and keep it for adsorption for 1 hour, then cool to 60°C for filtration, weigh it and use it for the next batch. Add 100g of 3,5-dimethylbenzoic acid into a 1000ml reaction bottle; measure the water content of the mother liquor, if not enough, add acetic anhydride to make up to 680g of acetic acid, add 0.8g of cobalt acetate, 0.3g of potassium bromi...

Embodiment 2

[0069] Put 140g of 3,5-dimethylbenzoic acid, 760g of glacial acetic acid, 3g of cobalt acetate, and 5g of acetic acid into a 1000mL reaction flask equipped with a mechanical stirring device, an oxygen-passing glass tube, a constant-pressure dropping funnel, a thermometer, and a reflux condenser. Manganese, 5g sodium bromide, 5g cerium acetate, and 3g triethanolamine, heat up to 85°C, turn on oxygen 1L / min, until reflux, keep reflux and react with oxygen for 7 hours, take a sample to detect that the raw material is less than 0.5% as the reaction end point, cool The crude product and the mother liquor are obtained by filtration, the crude product is to be refined, and the mother liquor is absorbed by activated carbon and used mechanically.

[0070] Add 10g of activated carbon to the mother liquor in the upper batch, raise the temperature to 80°C to 90°C and keep it for adsorption for 1 hour, then cool to 60°C for filtration, weigh it and use it for the next batch. Add 140g of 3,...

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Abstract

The invention relate to the field of compound production and preparation, in particular to a method for preparing trimesic acid. The method includes oxidizing 3, 5-dimethylbenzoic acid under the effects of catalytic systems by the aid of liquid-phase oxidation processes to generate the trimesic acid. Compared with the traditional method for preparing trimesic acid from mesitylene which is used as an initial raw material, the method has the advantages that tar substances generated by the 3, 5-dimethylbenzoic acid in reaction procedures are low in content, and accordingly the method is high in yield and favorable for environmental protection and product purification; mother liquor is recycled, accordingly, the utilization rates of various raw materials can be increased, and the productivity can be improved.

Description

technical field [0001] The invention relates to the field of production and preparation of compounds, in particular to a method for preparing trimesic acid. Background technique [0002] Trimellitic acid is 1,3,5-benzenetricarboxylic acid, English name: 1,3,5-Benzenetricarboxylic acid. Trimellitic acid is a needle-like or prismatic crystal, which is an important chemical raw material, used as a pharmaceutical intermediate, and is also widely used in plastics, artificial fibers, water-soluble alkyl resins, plasticizers, fungicides, anti-mildew Agents and crosslinking agents, etc., or intermediates for special polymers and resins. [0003] Trimellitic acid is an emerging important chemical raw material, and there are many researches on its preparation methods at home and abroad, but none of them are ideal. At present, three methods are usually used for the synthesis of trimesic acid: mesitylene potassium permanganate oxidation method, mesitylene nitric acid oxidation method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265C07C63/307
CPCC07C51/265C07C63/307
Inventor 成家钢
Owner 黄石市利福达医药化工有限公司
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