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Loaded zinc trifluoromethanesulfonate catalyst, its preparation method, and preparation method of butanone-glycol ketal

A technology of zinc trifluoromethanesulfonate and catalysts, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problems of low product purity, equipment corrosion, and environmental problems. Pollution and other problems, to achieve good catalytic performance and less side reactions

Active Publication Date: 2013-11-06
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 disadvantages of many side reactions, low product purity, serious equipment corrosion, and a large amount of acidic waste water in the post-treatment, which cause environmental pollution, etc. Provide a new type of catalyst for the synthesis of butanone-ethylene glycol ketal

Method used

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  • Loaded zinc trifluoromethanesulfonate catalyst, its preparation method, and preparation method of butanone-glycol ketal
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  • Loaded zinc trifluoromethanesulfonate catalyst, its preparation method, and preparation method of butanone-glycol ketal

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preparation example Construction

[0018] The present invention also provides a method for preparing the catalyst, wherein the method comprises: impregnating the mesoporous silica carrier with a zinc trifluoromethanesulfonate solution, so that the zinc trifluoromethanesulfonate is supported on the mesoporous silica On the carrier, the loading of the zinc trifluoromethanesulfonate is such that in the obtained catalyst, based on the total weight of the catalyst, the content of the zinc trifluoromethanesulfonate is 10-60% by weight, and the mesoporous dioxide The content of the silicon carrier is 40-90% by weight. More preferably, based on the total weight of the catalyst, the content of the zinc trifluoromethanesulfonate is 10-15% by weight, and the content of the mesoporous silica carrier is 85-90% by weight.

[0019] The size of the hollow spherical mesoporous silica can be changed in a wide range, preferably, the diameter of the hollow spherical mesoporous silica carrier is 3-20 microns, and the specific surfa...

Embodiment 1

[0035] Add 1.0 gram of three-stage copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene (Aldrich, P123) and 1.69 gram of ethanol into the buffer solution of acetic acid and sodium acetate of pH=4.4 of 28ml, stir at 15 ℃ Until the polyoxyethylene-polyoxypropylene-polyoxyethylene is completely dissolved, then add 6g of trimethylpentane to the above solution, stir at 15°C for 8 hours, then add 2.13g of tetramethoxysilane to the above solution After stirring at 15°C for 20 hours, the solution was transferred to a polytetrafluoroethylene-lined reaction kettle, oven crystallized at 60°C for 24 hours, filtered, washed with distilled water, and dried to obtain hollow spherical mesoporous silica Original powder.

[0036] The hollow spherical mesoporous silica raw powder was calcined in a muffle furnace at 550° C. for 24 hours to obtain hollow spherical mesoporous silica (named MS-1).

[0037] Stir 1 gram of hollow spherical mesoporous silica and 1 gram of zinc trifluoromethanesu...

experiment Embodiment 1

[0046] This experimental example is used to illustrate the catalytic activity of the supported zinc trifluoromethanesulfonate catalyst according to the present invention.

[0047] The supported zinc trifluoromethanesulfonate catalyst (MS-Zn) was vacuum-dried at 150°C for 6 hours, and after cooling to room temperature, weighed 0.3 g, then weighed 21.6 g of butanone and 22.3 g of ethylene glycol, and sequentially Put into a 100ml three-necked flask, stir for 4 hours under heating conditions at 120°C, and after cooling to room temperature, centrifuge and analyze the components of the reaction product liquid by gas chromatography. The results are: the content of ethylene glycol is 13% by weight, and the product D The ketone-ethylene glycol ketal content was 41.7% by weight. It is determined through calculation that the catalytic efficiency of the catalyst is 87%, the catalytic selectivity is 99%, and the catalytic yield is 42%.

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Abstract

The invention provides a loaded zinc trifluoromethanesulfonate catalyst, which comprises a mesoporous silica hollow sphere carrier and zinc trifluoromethanesulfonate loaded on the mesoporous silica hollow sphere carrier. And for the totally weight of the catalyst, the zinc trifluoromethanesulfonate accounts for 10-60 wt%, while the mesoporous silica hollow sphere carrier accounts for 40-90 wt%. The invention also provides a preparation method of the catalyst. In addition, the invention also provides a preparation method of butanone-glycol ketal using the loaded zinc trifluoromethanesulfonate catalyst of the invention. The loaded zinc trifluoromethanesulfonate catalyst provided in the invention can be recovered and recycled, and has fewer side reaction as well as no corrosion to equipment.

Description

technical field [0001] The invention relates to a supported zinc trifluoromethanesulfonate catalyst and a preparation method thereof, and also relates to a preparation method of butanone-ethylene glycol ketal using the catalyst. Background technique [0002] Butanone-ethylene glycol ketal has a special fragrance and can be used in essences, as well as intermediates or solvents in organic synthesis (Perfume Chemistry. Beijing: Light Industry Press. 1984.250, N H Platus; Silicon tungstic acid doping Catalyzed synthesis of butanone-ethylene glycol ketal by polyaniline catalyst, Chemical Reagents, 2005, 27(2), 121-123, Yang Shuijin; Tong Wenlong; Sun Jutang). [0003] The traditional synthesis method of butanone-ethylene glycol ketal is synthesized under the catalysis of a homogeneous catalyst (inorganic acid), but this method has many side reactions, low product purity, serious equipment corrosion, and a large amount of acidic wastewater in post-treatment , causing environment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02
CPCY02P20/584
Inventor 亢宇谢伦嘉郭顺王彦强赵思源田宇姜健准冯华生
Owner CHINA PETROLEUM & CHEM CORP
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