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Liquid phase oxidation method for preparing trimesic acid/trimellitic acid

A technology for trimesic acid and trimellitic acid, which is used in the preparation of carbonyl compounds by oxidation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of insufficient contact between oxidant molecules and raw material molecules, insufficient utilization of oxidants, and difficult A large number of problems such as obtaining, to achieve the effect of suitable for large-scale production, improve oxidation capacity, improve miscibility

Active Publication Date: 2019-08-20
HUANGSHAN HUAHUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its purity is high, but the yield needs to be improved, and the raw material used is 3,5-dimethylbenzoic acid, the relative yield is low, and it is not easy to obtain in large quantities
In addition, although the above-mentioned method adopts the air oxidation method at a low temperature, the utilization rate of the oxidant is insufficient by using an open bubbling device, and the yield of the final product is low. There is a clear phase interface, and the contact between oxidant molecules and raw material molecules is insufficient, resulting in low oxidation efficiency

Method used

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  • Liquid phase oxidation method for preparing trimesic acid/trimellitic acid
  • Liquid phase oxidation method for preparing trimesic acid/trimellitic acid
  • Liquid phase oxidation method for preparing trimesic acid/trimellitic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for preparing trimellitic acid / trimellitic acid by a liquid-phase oxidation method comprises the following steps:

[0043] (1) 12mol% mesitylene, 12mol% cerium ammonium nitrate, 10mol% hydrogen peroxide solution and 1mol% phase transfer catalyst are added in the stainless steel autoclave;

[0044] (2) Close the autoclave, start stirring, heat up to 80°C, and fully react for 3 hours;

[0045] (3) Then add 1mol% composite catalyst, 20mol% acetic acid and 10mol% concentrated nitric acid to the above-mentioned mixed material, after fully mixing, heat up to 100°C, add 34mol% oxygen, keep the pressure in the kettle to be 3.0Mpa, heat preservation reaction 6h;

[0046] (4) Cool down to 5 DEG C by cooling to 5 DEG C to carry out cooling crystallization in reactor, open pressure relief valve slowly to remove pressure, suction filtration obtains trimesic acid crude product;

[0047] (5) Add hot water at 100°C to recrystallize the crude product, the mass ratio of hot wa...

Embodiment 2

[0052] In Example 2: the phase transfer catalyst is cyclodextrin; the mass ratio of nickel nitrate and titanium nitrate in the composite catalyst is 1:2; the rest of the raw materials without special instructions are the same as in Example 1, and the following examples are all the same; The pressure is 5.0Mpa,

Embodiment 3

[0053] In Example 3: the mass ratio of nickel nitrate to titanium nitrate is 1:3; the pressure in the kettle is kept at 4.0Mpa;

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Abstract

The invention belongs to the technical field of chemical raw material production, and specifically relates to a liquid phase oxidation method for preparing trimesic acid / trimellitic acid. The method is characterized by comprising following raw materials: mesitylene / pseudocumene, cerium ammonium nitrate, hydrogen peroxide, acetic acid, concentrated nitric acid, and oxygen. The method comprises following steps: carrying out primary oxidation reactions among mesitylene / pseudocumene, cerium ammonium nitrate, hydrogen peroxide, and a phase transfer agent; then adding acetic acid, concentrated nitric acid, a catalyst, and a gas oxidizing agent to carry out secondary oxidation reactions; and carrying out crystallization and suction filtration to obtain a crude product of trimesic acid / trimelliticacid. A two-step liquid oxidation system is adopted, the product yield is largely increased, and the production of trimesic acid / trimellitic acid is greatly promoted.

Description

technical field [0001] The invention belongs to the technical field of chemical raw material production, and in particular relates to a method for preparing trimellitic acid / trimellitic acid by a liquid phase oxidation method. Background technique [0002] At present, trimellitic acid and trimellitic acid are mainly oxidized by potassium permanganate, or glacial acetic acid solvent system, cobalt acetate is used as a catalyst, and air is used as an oxidant. Although the potassium permanganate oxidation method is feasible in a small laboratory test, it has various shortcomings such as low yield and many side reactions, and is rarely used in industry. [0003] CN106431887A discloses a preparation method of trimesic acid, which is characterized in that 3,5-dimethylbenzoic acid is oxidized under the action of a catalytic system to generate trimesic acid by a liquid phase oxidation method. More specifically, the method of embodiment 1 disclosed in this document is as follows: ...

Claims

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Application Information

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IPC IPC(8): C07C51/285C07C51/255C07C63/307
CPCC07C51/285C07C51/255C07C45/28C07C63/307C07C47/52
Inventor 项纯林光伟杨志萍何领汤增荣
Owner HUANGSHAN HUAHUI TECH
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