Method for preparing corresponding dicarboxylic acid by catalytic oxidation of hydroxy acid

A dicarboxylic acid, catalytic oxidation technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of short service life, easy deactivation, difficult recovery, etc., to overcome the production process Complexity, increased mass transfer and diffusion speed, good activity and stability

Active Publication Date: 2014-03-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for preparing corresponding dicarboxylic acid by catalytic oxidation of hydroxy acid
  • Method for preparing corresponding dicarboxylic acid by catalytic oxidation of hydroxy acid

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0026]This example illustrates the synthesis process of TS-1 molecular sieve and the synthesis process of tin-titanium-silicon molecular sieve according to the method of Zeolites, 1992, Vol.12, pages 943-950.

[0027] Mix 22.5 grams of tetraethyl orthosilicate with 7.0 grams of tetrapropylammonium hydroxide, add 59.8 grams of distilled water, mix well, and then hydrolyze at normal pressure and 60°C for 1.0 hour to obtain a hydrolysis solution of tetraethyl orthosilicate A solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of anhydrous isopropanol was slowly added under vigorous stirring, and the resulting mixture was stirred at 75° C. for 3 hours until it became a clear and transparent colloid. Put the colloid into a stainless steel sealed reaction kettle, and place it at a constant temperature of 170°C and autogenous pressure for 6 days to obtain a mixture of crystallized products; filter the mixture, wash it with water until the pH is 6-8, and dry it at 110°C Afte...

preparation example 2

[0029] Take the TS-1 molecular sieve obtained in Catalyst Preparation Example 1 according to the ratio of molecular sieve (g): sulfuric acid (mol): water (mol) = 100: 0.15: 15 and mix evenly, react at 90 ° C for 5.0 hours, and then follow the conventional method Filtration, washing and drying yielded acid-treated TS-1 molecular sieves.

[0030] The above-mentioned acid-treated TS-1 molecular sieves were mixed uniformly according to the ratio of molecular sieve (gram): triethanolamine (mol): tetrapropylammonium hydroxide (mol): water (mol) = 100: 0.20: 0.15: 180, and put into A stainless steel sealed reaction kettle was placed at a constant temperature of 190°C and autogenous pressure for 0.5 days. After cooling and pressure relief, it was filtered, washed, dried according to conventional methods, and roasted in an air atmosphere at 550°C for 3 hours to obtain a hollow structure molecular sieve.

[0031] According to X-ray diffraction analysis, it is a titanium-silicon molecula...

Embodiment 1

[0034] Weigh 2.3 grams of tin-containing hollow titanium-silicon molecular sieve Sn-HTS (in terms of oxides, the same below, SnO 2 The mass percentage is 2.1wt%, TiO 2 The mass percent is 4.3wt%) catalyzer is contained in the 100ml three-necked flask, then adds magnetic stirrer, 26.42 grams of 6-hydroxycaproic acid, 3.6 grams of water and 23ml concentration and is the hydrogen peroxide of 30% at this moment, 6-hydroxycaproic acid The molar ratio of acid to hydrogen peroxide is 1:1. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of the three-necked flask is condensed and refluxed with a condenser, and the magnetic stirrer and heating device are started to start the reaction. The reaction temperature was controlled at about 60°C. After 2 hours of reaction, the conversion rate of 6-hydroxycaproic acid was 23.27%, and the selectivity to adipic acid was 76.23%.

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Abstract

The invention discloses a method for preparing corresponding dicarboxylic acid by catalytic oxidation of hydroxy acid. The method is characterized in that: under the conditions that the molar ratio of hydroxy acid to solvent to hydrogen peroxide is 1:(0-80):(0.2-20), the temperature is 40-200 DEG C and the reaction pressure is 0.1-3.0MPa, the reaction is carried out in the presence of a catalyst, and products are recovered, wherein the mass ratio of the catalyst to cycloolefin is 1:(5-300), and the catalyst is a tin-titanium-silicon molecular sieve.

Description

technical field [0001] The invention relates to a green catalytic method for preparing corresponding dicarboxylic acids by oxidizing hydroxyacids, and more specifically relates to a method for preparing corresponding dicarboxylic acids by oxidizing hydroxyacids with hydrogen peroxide as an oxidant. Background technique [0002] Dicarboxylic acid is an important organic chemical raw material. Taking adipic acid as an example, it is a dicarboxylic acid with important industrial significance. It is mainly used to make adiponitrile, and then produce hexamethylenediamine Together to produce nylon 66 (polyamide) and engineering plastics. In addition, it is also used in the production of various ester products, as plasticizers and advanced lubricants, as raw materials for polyurethane elastomers, in the production of unsaturated polyesters, hexanediol and adipate, and in various foods And beverage acidulant, medicine, yeast purifying agent, insecticide, adhesive, raw material for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/285C07C55/14C07C55/12B01J29/89
Inventor 朱斌林民夏长久龙立华邹飞艳汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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