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A kind of method for catalytic oxidation of cyclic ketone by nano-β molecular sieve

A technology for the catalytic oxidation of cyclic ketones and beta molecular sieves by molecular sieves, applied in molecular sieve catalysts, chemical instruments and methods, oxidation preparation of carboxylic acids, etc. The problem is to achieve the effect of good catalytic oxidation activity and catalytic activity stability, high catalytic oxidation activity and activity stability, and overcoming the complex production process.

Active Publication Date: 2014-10-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the industrialized production of ε-caprolactone mainly adopts the Baeyer-Villiger oxidation process of cyclohexanone and peroxycarboxylic acid, but peroxyacid oxidants also have relatively large disadvantages: (1) after the reaction, a large amount of Organic carboxylic acid (salt) waste has a greater impact on the environment, and it is more difficult to recycle or process; (2) the separation and purification of reaction products are more difficult, the selectivity is low, the atom economy is poor, and it does not meet the basic principles of green chemistry; ( 3) Organic peroxyacids need to use high-concentration hydrogen peroxide in the production process, which is unstable in nature, high in production costs, and dangerous in transportation, storage and operation, thus limiting its application in industrial production
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 for catalytic oxidation of cyclic ketone by nano-β molecular sieve
  • A kind of method for catalytic oxidation of cyclic ketone by nano-β molecular sieve
  • A kind of method for catalytic oxidation of cyclic ketone by nano-β molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Take by weighing 2.3 grams of acid-eluted aluminum nano-beta-molecular sieves (the mass fraction of aluminum oxide is 1.2wt%) catalyst and be loaded in a 100ml three-necked flask, then add a magnetic stirrer, 19.63 grams of cyclohexanone, 3.6 grams of water and 23ml The concentration is 30% hydrogen peroxide, and the molar ratio of cyclohexanone 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 70°C. After 2 hours of reaction, the conversion rate of cyclohexanone was 20.65%, the selectivity of generating ε-caprolactone was 46.45%, the selectivity of 6-hydroxycaproic acid was 21.98%, and the Acid selectivity was 14.19%.

Embodiment 2

[0046] Take by weighing 2.44 grams of acid-eluted aluminum nano-beta-molecular sieves (the mass fraction of aluminum oxide is 2.3wt%) catalyst and be loaded in a 100ml three-necked flask, then add magnetic stirrer, 19.63 grams of cyclohexanone, 24 grams of acetone and 23ml The concentration is 30% hydrogen peroxide, and the molar ratio of cyclohexanone 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 3 hours of reaction, the conversion rate of cyclohexanone was 27.82%, the selectivity of ε-caprolactone was 94.65%, the selectivity of 6-hydroxycaproic acid was 1.98%, and the Acid selectivity was 0.72%.

Embodiment 3

[0048]Weigh 2.65 grams of acid-eluted aluminum nano-beta-molecular sieve catalyst (the mass fraction of aluminum oxide is 3.7wt%) and put it in a 100ml three-necked flask, then add a magnetic stirrer, 19.63 grams of cyclohexanone, and 18 grams of dioxane ring and 46ml concentration of 30% hydrogen peroxide, the molar ratio of cyclohexanone to hydrogen peroxide is 1:2. 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 72°C. After 4 hours of reaction, the conversion rate of cyclohexanone was 58.57%, the selectivity of generating ε-caprolactone was 98.18%, the selectivity of 6-hydroxycaproic acid was 0.68%, and the Acid selectivity was 0.12%.

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Abstract

The invention discloses a method for catalytic oxidation of cyclic ketone by a nanometer Beta molecule sieve, wherein reacting cyclic ketone, solvent and hydrogen peroxide based on a mole proportion of cyclic ketone: solvent: hydrogen peroxide=1:(0-50): (0.2-20) at 5-200 degrees centigrade and a 0.1-3.0 MPa reaction pressure in the presence of a catalyst, and recycling the product, wherein the mass ratio of the catalyst to the cyclic ketone is 1:(5-300), and the catalyst is an acid washing dealumination nanometer Beta molecule sieve.

Description

technical field [0001] The invention relates to a method for catalytically oxidizing cyclic ketones, in particular to a method for oxidizing cyclic ketones with hydrogen peroxide in the presence of a catalyst. Background technique [0002] ε-caprolactone has the advantages of low viscosity, easy processing, and low VOC content. It is used as oligomer and denaturant in the process, which can improve the toughness, low temperature characteristics and reactivity and other functionalities; in terms of coatings, it is used as an improvement in solvents and latex coatings for automotive primers, surface coatings and various building materials. It can improve the toughness of the coating film, improve the low-temperature characteristics, reactivity, and increase the crosslinking density; in terms of adhesives, it can be used to improve the bonding properties of hot-melt adhesives and solvent-based adhesives; in resin modification On the one hand, it can be used to improve softness...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/00C07D313/04C07D309/30C07C51/31C07C59/01C07C51/285C07C55/14C07C55/12B01J29/70
CPCY02P20/582Y02P20/584
Inventor 林民夏长久朱斌龙立华邹飞艳舒兴田汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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