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Reaction method for catalyzing cyclic ketone by total silicone molecular sieve

A molecular sieve technology for catalyzing cyclic ketones and all-silicon molecular sieves, which is applied in organic chemical methods, chemical instruments and methods, and the preparation of organic compounds. and other problems, to achieve catalytic oxidation activity and catalytic activity stability, overcome the complex production process, catalytic oxidation activity and high activity stability

Active Publication Date: 2014-08-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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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  • Reaction method for catalyzing cyclic ketone by total silicone molecular sieve
  • Reaction method for catalyzing cyclic ketone by total silicone molecular sieve
  • Reaction method for catalyzing cyclic ketone by total silicone molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh 2.3 grams of all-silicon molecular sieve S-1 (the product of Hunan Jianchang Company, the same below) as a catalyst and put it in a 100ml three-necked flask, then add a magnetic stirrer, 19.63 grams of cyclopentanone, 3.6 grams of water and 23ml of water to a concentration of 30 % hydrogen peroxide, at this moment the mol ratio of cyclopentanone and 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 7 hours of reaction, the conversion rate of cyclopentanone was 20.65%, the selectivity of generating δ-valerolactone was 36.45%, the selectivity of 5-hydroxypentanoic acid was 33.98%, and the selectivity of glutaric acid The selectivity is 18.46%.

Embodiment 2

[0044] Take by weighing 2.44 gram all-silicon molecular sieve S-1 catalysts and be packed in the 100ml three-necked flask, then add magnetic stirrer, 19.63 gram cyclopentanone, 34 gram acetone and 23ml concentration and be 30% hydrogen peroxide at this moment, cyclopentanone and The molar ratio of 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 5 hours of reaction, the conversion rate of cyclopentanone was 17.82%, the selectivity of generating δ-valerolactone was 96.65%, the selectivity of 5-hydroxypentanoic acid was 2.98%, and the selectivity of glutaric acid The selectivity is 0.62%.

Embodiment 3

[0046] Take by weighing 2.65 grams of all-silicon molecular sieve S-1 catalysts and put them in a 100ml three-necked flask, then add a magnetic stirrer, 19.63 grams of cyclopentanone, 28 grams of dioxane and 46ml of 30% hydrogen peroxide. The molar ratio of pentanone 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 73°C. After 4 hours of reaction, the conversion rate of cyclopentanone was 68.57%, the selectivity of generating δ-valerolactone was 97.98%, the selectivity of 5-hydroxypentanoic acid was 0.98%, and the selectivity of glutaric acid The selectivity is 0.46%.

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Abstract

The invention discloses a reaction method for catalyzing cyclic ketone by a total silicone molecular 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 10-200 degrees centigrade and a 0.1-3.0 MPa reaction pressure in the presence of a catalyst, wherein the mass ratio of the catalyst to the cyclic ketone is 1:(5-300), and the catalyst is a total silicone molecular 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): C07B41/12C07B41/08C07D313/04C07D309/30C07C51/31C07C51/285C07C59/01C07C55/14C07C55/12
CPCY02P20/582
Inventor 夏长久林民朱斌龙立华舒兴田邹飞艳汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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