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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 cyclohexanone ethylene glycol ketal and copper trifluoromethanesulfonate is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. Complex, equipment corrosion and other problems, to achieve the effect of reducing side reactions, preventing equipment corrosion, and the process is simple and easy to implement

Active Publication Date: 2016-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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 complicated process, and provide a novel catalyst for the synthesis of ketals and the preparation of cyclohexanone ethylene glycol ketal method

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

[0029]The present invention also provides a method for preparing the catalyst, wherein the method comprises: milling the rod-shaped mesoporous silica carrier together with copper trifluoromethanesulfonate in a sealed ball mill jar to make the copper trifluoromethanesulfonate Loaded on the rod-shaped mesoporous silica carrier, based on the total weight of the rod-shaped mesoporous silica carrier and copper trifluoromethanesulfonate, the amount of copper trifluoromethanesulfonate is 10-90 % by weight, the amount of the rod-shaped mesoporous silica carrier is 10-90% by weight, more preferably, based on the total weight of the rod-shaped mesoporous silica carrier and copper trifluoromethanesulfonate, the The amount of copper trifluoromethanesulfonate is 30-60% by weight, and the amount of the rod-shaped mesoporous silica carrier is 40-70% by weight.

[0030] According to the present invention, the rod-shaped mesoporous silica carrier has a rod length of 0.5-2 microns, preferably 0...

Embodiment approach

[0032] According to one embodiment of the present invention, the preparation method of the supported copper trifluoromethanesulfonate catalyst comprises: adding rod-shaped 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 rod-shaped 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] Step 2, add tetraethyl orthosilicate to the solution obtained in the previous step, stir slowly for 1-10 ...

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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 rod-shaped meso-porous silica; and the rod length, the specific surface area, the most probable aperture, the pore wall thickness and the average aspect ratio of the support are 0.5-2mum, 600-800m<2> / g, 6-9nm, 1-3nm and 1-3 respectively In the catalyst, the copper (II) trifluoromethanesulfonate is supported on the specific rod-shaped 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 ketal synthesis reactions, and cyclohexanone ethylene glycol ketal method of preparation. Background technique [0002] In 1992, Mobile Company synthesized mesoporous materials (BeckJS, VartuliJC, RothWJ, etal.J.Am.Chem.Soc., 1992, 114(27):10834-10843), the mesoporous materials have a high specific surface, regular The excellent pore structure and narrow pore size distribution have made mesoporous materials attract great attention in the fields of catalysis, separation, and medicine; 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, etalScience279 (1998) 548-550), the material has a highly ordered cubic single crystal mesoporous material pore size (6-30nm), large pore ...

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孙姝琦
Owner CHINA PETROLEUM & CHEM CORP