Unlock instant, AI-driven research and patent intelligence for your innovation.

Supported copper (II) trifluoromethanesulfonate catalyst, preparation method and application thereof, and cyclohexanone ethylene ketal preparation method

A technology of copper trifluoromethanesulfonate and catalyst, applied in chemical instruments and methods, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc., can solve problems such as equipment corrosion and complex process, To achieve the effect of preventing equipment corrosion, reducing side reactions, and the process is simple and easy to implement

Active Publication Date: 2014-02-19
CHINA PETROLEUM & CHEM CORP +1
View PDF3 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Supported copper (II) trifluoromethanesulfonate catalyst, preparation method and application thereof, and cyclohexanone ethylene ketal preparation method
  • Supported copper (II) trifluoromethanesulfonate catalyst, preparation method and application thereof, and cyclohexanone ethylene ketal preparation method
  • Supported copper (II) trifluoromethanesulfonate catalyst, preparation method and application thereof, and cyclohexanone ethylene ketal preparation method

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0031] The present invention also provides a method for preparing the catalyst, wherein the method comprises: ball milling the donut-shaped mesoporous silica carrier with copper trifluoromethanesulfonate, so that the copper trifluoromethanesulfonate is supported on the On the donut-shaped mesoporous silica carrier, based on the total weight of the donut-shaped mesoporous silica carrier and copper trifluoromethanesulfonate, the amount of copper trifluoromethanesulfonate is 10-90 wt. %, the amount of the donut-shaped mesoporous silica carrier is 10-90% by weight, more preferably, based on the total weight of the donut-shaped mesoporous silica carrier and copper trifluoromethanesulfonate, the The amount of copper trifluoromethanesulfonate is 30-60% by weight, and the amount of donut-shaped mesoporous silica carrier is 40-70% by weight.

[0032] According to the present invention, the particle diameter of the donut-shaped mesoporous silica carrier is 3-20 microns, preferably 3-10 ...

Embodiment approach

[0034] According to one embodiment of the present invention, the preparation method of the supported copper trifluoromethanesulfonate catalyst comprises: adding the doughnut-shaped mesoporous silica and copper trifluoromethanesulfonate into a ball mill tank of a ball mill, The inner wall of the ball mill tank is lined with polytetrafluoroethylene, the diameter of the balls 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 donut-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

[0035] According to a specific embodiment of the present invention, the preparation method of the supported copper trifluoromethanesulfonate catalyst comprises the following steps:

[0036] In the first step, the triblock copolymer polyethylene oxide-polyoxypropylene-polyethylene oxide (EO 20 PO 70 EO 20 , abbreviated as P123) and N, N-dimethylformamide (DMF), added to hydrochloric acid, according to the molar feed ratio,

[0037] Tri-block copolymer polyethylene oxide-polyoxypropylene-polyoxyethylene: N, N-dimethylformamide (DMF): water: hydrogen chloride = 1: 300-700: 10000-20000: 100-500 (actual ratio for 1:596:11411:326),

[0038] Mix until the solids are fully dissolved;

[0039] In the second step, add tetraethyl orthosilicate to the solution obtained in the previous step, and stir for 10 hours to 40 hours at a temperature of 25°C-60°C and a mechanical stirring rate of 100-400r / min; according to the molar feed ratio,

[0040] Tri-block copolymer polyoxyethylene-poly...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
diameteraaaaaaaaaa
specific surface areaaaaaaaaaaa
particle diameteraaaaaaaaaa
Login to View More

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 donut-shaped meso-porous silica; and the particle diameter, the specific surface area, the most probable aperture, the pore wall thickness and the internal diameter / external diameter ratio of the support are 3-20mum, 600-1000m<2> / g, 7-10nm, 3-4nm and 0.3-0.9 respectively. In the catalyst, the copper (II) trifluoromethanesulfonate is supported on the specific donut-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 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07D317/72
Inventor 亢宇张明森黄文氢杨菁张伟
Owner CHINA PETROLEUM & CHEM CORP