A kind of method that catalytic oxidation reaction prepares dibasic carboxylic acid

A technology of catalytic oxidation and dibasic carboxylic acid, which is applied in the direction of oxidative preparation of carboxylic acid, chemical industry, organic chemistry, etc. It can solve the problems of heteropolyacid catalyst unstable properties, short service life, small specific surface, etc., and achieve the purpose of inhibiting the product Effects of side reactions, easy addition and removal, and prevention of thermal decomposition

Active Publication Date: 2015-08-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, heteropolyacid catalysts have shortcomings such as unstable properties, small specific surface area, easy deactivation, difficult recovery and short service life, so they have not been widely promoted at present.

Method used

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  • A kind of method that catalytic oxidation reaction prepares dibasic carboxylic acid
  • A kind of method that catalytic oxidation reaction prepares dibasic carboxylic acid
  • A kind of method that catalytic oxidation reaction prepares dibasic carboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] This example illustrates the direct oxidation of cyclohexanone to adipic acid.

[0038] The reaction tower is a sieve plate tower, the catalyst used is HTS, and the catalyst particle diameter distribution is 1-200 μm; the reaction raw materials are 30% hydrogen peroxide and more than 99.9% cyclohexanone; the solvent is acetone. Prepare the acetone slurry with a catalyst concentration of 5% in the catalyst storage tank, and fully stir and disperse it for later use. Use acetone to test the device under the set conditions. After the device is stable, mix the catalyst slurry, hydrogen peroxide, and cyclohexanone Add to the reaction section in the tower. The absolute pressure is 0.23MPa, the temperature of the reaction section is 110°C, the molar ratio of cyclohexanone to acetone in the reaction section is 1:5, and the mass space velocity of cyclohexanone is 1.5h -1 , The reflux ratio of the top material is 6:1. The feed molar ratio of cyclohexanone and hydrogen peroxide i...

Embodiment 2

[0040] This example illustrates the direct oxidation of cyclohexanone to adipic acid.

[0041] The reaction tower is a sieve plate tower, and the catalyst used is HTS spray-molded with silica sol as a binder. The content of HTS is 50%, and the particle diameter distribution of the catalyst is 40-600 μm; Hexanone; solvent is acetone. Prepare the acetone slurry with a catalyst concentration of 15% in the catalyst storage tank, and fully stir and disperse it for standby. Use acetone to test run the device under the set conditions. After the device is stable, mix the catalyst slurry, hydrogen peroxide, and cyclohexanone Add to the reaction section in the tower. The absolute pressure is 0.20MPa, the temperature of the reaction section is 108°C, the molar ratio of cyclohexanone to acetone in the reaction section is 1:7, and the mass space velocity of cyclohexanone is 1.5h -1 , The reflux ratio of the top material is 8:1. The feed molar ratio of cyclohexanone and hydrogen peroxide...

Embodiment 3

[0043] This example illustrates the direct oxidation of cyclopentane to glutaric acid.

[0044] The reaction tower is a sieve plate tower, the catalyst used is HTS, and the catalyst particle diameter distribution is 1-200 μm; the reaction raw materials are 30% hydrogen peroxide and more than 99.9% cyclopentanone; the solvent is acetone. Prepare the acetone slurry with a catalyst concentration of 5% in the catalyst storage tank, and fully stir and disperse it for later use. Use acetone to test the device under the set conditions. After the device is stable, mix the catalyst slurry, hydrogen peroxide, and cyclopentanone. Add to the reaction section in the tower. The absolute pressure is 0.19MPa, the temperature of the reaction section is 108°C, the molar ratio of cyclopentane to acetone in the reaction section is 1:5, and the mass space velocity of cyclopentane is 1.5h -1 , The reflux ratio of the top material is 6:1. The feed molar ratio of cyclopentane to hydrogen peroxide i...

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Abstract

The invention relates to a method for preparing dicarboxylic acid through catalytic oxidization reaction. The method is characterized by comprising the following steps of adding a catalyst and liquid reaction materials including a solvent, aqueous hydrogen peroxide solution and cyclane or derivatives of cyclane into a reaction section of a catalytic distillation tower; enabling the liquid reaction materail to generate catalytic oxidization reaction while the mixture of the catalyst and the liquid reaction materail flows in the tower; separating the solvent from the vaporized catalytic-oxidized materal so as to be recycled, separating the catalyst and unvaporized catalytic-oxidized liquid materal so as to be recycled, separating the material at the tower top or tower kettle to obtain unreacted cyclane or derivatives of cyclane to be recycled, and separating the product dicarboxylic acid from the material in the tower kettle, wherein the catalyst is a titanium silicalite molecular sieve or a modified titanium silicalite molecular sieve. The method is high in reaction heat utilization rate, the selectivity of oxidized product dicarboxylic acid can be improved, and the thermal decomposition of hydrogen peroxide can be effectively prevented.

Description

technical field [0001] The invention relates to a suspension catalytic process for preparing corresponding dicarboxylic acids by oxidation of cycloalkane and its derivatives. More specifically, the present invention relates to the oxidation reaction of naphthenes and their derivatives and hydrogen peroxide under the catalysis of fine-grained titanium-silicon molecular sieves, and the method for producing corresponding oxides with high selectivity through simultaneous distillation and separation. Background technique [0002] Adipic acid is white crystal at room temperature, melting point 153°C, boiling point 332.7°C (101kPa decomposition), relative density 1.360 (25 / 4°C), flash point (open cup) 209.85°C, ignition point (open cup) 231.85°C, melt viscosity 4.54mPa·s (160°C), flash point 196°C. Slightly soluble in water (15°C, 1.44g / 100ml), adipic acid is an industrially important dicarboxylic acid, and its output ranks second among all dicarboxylic acids. It is mainly used t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/31C07C55/14C07C55/12
CPCY02P20/10Y02P20/584
Inventor 林民夏长久朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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