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A supported copper trifluoromethanesulfonate catalyst, its preparation method and application, and the preparation method of cyclohexanone ethylene glycol ketal

A technology of copper trifluoromethanesulfonate and catalyst, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., and can solve problems such as equipment corrosion and complex processes. Achieve the effects of preventing equipment corrosion, reducing side reactions, and improving product purity

Active Publication Date: 2015-08-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of the existing catalysts for catalyzing the synthesis of ketals, such as serious equipment corrosion and complex process, and provide a novel catalyst for synthesizing ketals and a preparation method for ketals

Method used

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  • A supported copper trifluoromethanesulfonate catalyst, its preparation method and application, and the preparation method of cyclohexanone ethylene glycol ketal
  • A supported copper trifluoromethanesulfonate catalyst, its preparation method and application, and the preparation method of cyclohexanone ethylene glycol ketal
  • A supported copper trifluoromethanesulfonate catalyst, its preparation method and application, and the preparation method of cyclohexanone ethylene glycol ketal

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preparation example Construction

[0030] The present invention also provides a method for preparing the catalyst, wherein the method comprises: ball milling the spherical mesoporous silica carrier and copper trifluoromethanesulfonate in a sealed ball mill jar to make the copper trifluoromethanesulfonate Loaded on the spherical mesoporous silica carrier, based on the total weight of the spherical mesoporous silica carrier and copper trifluoromethanesulfonate, the amount of copper trifluoromethanesulfonate is 10-90 % by weight, the content of the spherical mesoporous silica carrier is 10-90% by weight; more preferably, based on the total weight of the spherical mesoporous silica carrier and copper trifluoromethanesulfonate, the The consumption of copper triflate is 30-60% by weight, the consumption of the spherical mesoporous silica carrier is 40-70% by weight; the particle diameter of the spherical mesoporous silica carrier is 0.5-1.5 micron , preferably 0.6-1.0 micron, more preferably 0.7 micron; specific surf...

Embodiment approach

[0032] According to one embodiment of the present invention, the preparation method of the supported copper trifluoromethanesulfonate catalyst comprises: adding spherical mesoporous silica and copper trifluoromethanesulfonate into the ball milling jar of the ball mill, and the inner wall of the ball milling jar is It is lined with polytetrafluoroethylene, the diameter of the grinding ball is 2-3mm, and the rotation speed is 300-500r / min. Continuously grind for 0.1-100 hours at a temperature of 15-100° C. in a ball mill tank, and then take out the solid powder to obtain spherical mesoporous silicon dioxide loaded with copper trifluoromethanesulfonate. The number of grinding balls depends on the size of the grinding jar, for a grinding jar size of 50-150ml, 1 grinding ball can be used. The material of the grinding ball can be agate, polytetrafluoroethylene, preferably polytetrafluoroethylene.

specific Embodiment approach

[0033] According to a specific embodiment of the present invention, the preparation method of the supported copper trifluoromethanesulfonate catalyst comprises the following steps:

[0034] In the first step, the triblock copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene (EO 20 PO 70 EO 20 , abbreviated as P123) and glycerol, added to hydrochloric acid, according to molar feed ratio,

[0035] Tri-block copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene: glycerol: water: hydrogen chloride = 1: 10-800: 10000-30000: 100-9000, preferably 1: 50-700: 12000-25000 : 500-8500, particularly preferably 1: 63: 14320: 1846, wherein the molar number of polyoxyethylene-polyoxypropylene-polyoxyethylene is calculated according to the average molecular weight of polyoxyethylene-polyoxypropylene-polyoxyethylene,

[0036] Mix until the solids are fully dissolved;

[0037] In the second step, add tetraethyl orthosilicate to the solution obtained in the previous step, stir at a...

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Abstract

The invention discloses a supported copper (II) trifluoromethanesulfonate catalyst, a preparation method thereof, and a cyclohexanone ethylene ketal preparation method. The catalyst is composed of 10-90wt% of a support and 10-90wt% of copper (II) trifluoromethanesulfonate supported on the support, and the support is spherical meso-porous silica; and the particle diameter, the specific surface area, the most probable aperture and the pore wall thickness of the support are 0.5-1.5mum, 710-800m<2> / g, 5-10nm and 1-3nm respectively. In the catalyst, the copper (II) trifluoromethanesulfonate is supported on the specific spherical meso-porous silica support, so the ketalation catalysis activity of the catalyst is high, and is still high after repeated use, thereby the catalyst can be recovered and recycled.

Description

technical field [0001] The invention relates to a supported copper trifluoromethanesulfonate catalyst and a preparation method thereof, and also relates to the application of the supported copper trifluoromethanesulfonate catalyst in the synthesis of ketal, and the preparation of cyclohexanone ethylene glycol ketal Preparation. Background technique [0002] In 1992, Mobile Company synthesized mesoporous material (Beck J S, Vartuli J C, Roth W J, et al. J. Am. Chem. Soc., 1992, 114(27): 10834-10843), which has high The specific surface, regular pore structure and narrow pore size distribution have made mesoporous materials attract great attention in the fields of catalysis, separation, medicine and other fields; in 1998, Zhao Dongyuan and others synthesized a new type of material - mesoporous material SBA -15 (D.Y.Zhao, J.L.Feng, Q.S.Huo, et al Science 279 (1998) 548-550), the material has a highly ordered cubic single crystal mesoporous material pore size (6-30nm), large po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J35/10C07D317/72
Inventor 亢宇张明森黄文氢杨菁张伟王焕茹
Owner CHINA PETROLEUM & CHEM CORP