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Large-aperture SBA-15 mesoporous material-copper trifluoromethanesulfonate composite catalyst, preparation method and application

A technology of copper trifluoromethanesulfonate, SBA-15, applied in organic compound/hydride/coordination complex catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve problems such as limited loading capacity and affecting catalytic performance , to achieve the effect of not easy to corrode the instrument and high reactivity

Active Publication Date: 2010-10-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the commonly used mesoporous material SBA-15 has a pore diameter of 6-7 nm, a pore volume and a specific surface area of ​​1.0 cm 3 / g and 500m 2 / g or so, the load capacity is limited, which directly affects its catalytic performance

Method used

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  • Large-aperture SBA-15 mesoporous material-copper trifluoromethanesulfonate composite catalyst, preparation method and application
  • Large-aperture SBA-15 mesoporous material-copper trifluoromethanesulfonate composite catalyst, preparation method and application
  • Large-aperture SBA-15 mesoporous material-copper trifluoromethanesulfonate composite catalyst, preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Example 1: Preparation of a copper trifluoromethanesulfonate-loaded mesoporous material

[0021] The mesoporous material SBA-15 with a pore diameter of 10-11nm was vacuum-dried at 150°C for 6 hours. After cooling to room temperature, 1g was weighed, and 20ml methyl ethyl ketone and 1g copper trifluoromethanesulfonate were weighed and put into 100ml poly In a reaction kettle lined with tetrafluoroethylene, close the reaction kettle, stir at a temperature of 25°C for 8 hours, centrifuge, and filter the liquid to obtain the solid product SBA-Cu(OTf) 2 , after vacuum-drying it at 150° C. to remove impurities, it weighed 1.2 g.

[0022] figure 1 gives SBA-15(a), SBA-Cu(OTf) 2 (b) and SBA-Cu(OTf) 2 (c) XRD patterns after two catalytic reactions. From the above three spectra, it can be seen that the macroporous mesoporous material SBA-15 has an ordered mesoporous structure, and after loading copper trifluoromethanesulfonate, it still maintains an ordered mesoporous structu...

Embodiment 2

[0023] Example 2: Preparation of a copper trifluoromethanesulfonate-loaded mesoporous material

[0024] The mesoporous material SBA-15 with a pore diameter of 10-11nm was vacuum-dried at 150°C for 6 hours. After cooling to room temperature, 1g was weighed, and 20ml methyl ethyl ketone and 1g copper trifluoromethanesulfonate were weighed and put into 100ml poly In a reaction kettle lined with tetrafluoroethylene, close the reaction kettle, stir at a temperature of 35°C for 8 hours, centrifuge, and filter the liquid to obtain the solid product SBA-Cu(OTf) 2 , after vacuum-drying it at 150° C. to remove impurities, it weighed 1.2 g.

Embodiment 3

[0025] Example 3: Preparation and application of a copper triflate-loaded mesoporous material

[0026] The mesoporous material SBA-15 with a pore diameter of 10-11nm was vacuum-dried at 150°C for 6 hours. After cooling to room temperature, 1g was weighed, and 20ml methyl ethyl ketone and 1g copper trifluoromethanesulfonate were weighed and put into 100ml poly In a reaction kettle lined with tetrafluoroethylene, close the reaction kettle, stir for 8 hours at a temperature of 25 ° C, centrifuge and obtain the solid product SBA-Cu(OTf) 2 .

[0027] Add 1,2-propylene oxide 7.7g, methyl ethyl ketone 22g, SBA-Cu(OTf) successively in 100ml polytetrafluoroethylene lining reactor 2 1.2g, reacted in a 55°C oil bath for 24 hours under stirring conditions, centrifuged, and analyzed the components of the reaction product liquid by gas chromatography, the conversion rate of 1,2-propylene oxide was 100%, and the conversion rate of 2,4-dimethyl- 75% selectivity to 2-ethyl-1,3-dioxolane. , ...

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Abstract

The invention relates to a large-aperture mesoporous material loaded with copper trifluoromethanesulfonate, a preparation method thereof and a process for utilizing the material as a catalyst for catalyzing the condensation reaction of 1,2-epoxypropane and ketone. The SBA-15 mesoporous material loaded with the copper trifluoromethanesulfonate comprises a mesoporous material with an aperture of 10-11 nm and loaded copper trifluoromethanesulfonate. The mesoporous material is adopted as a catalyst for the condensation reaction of the 1,2-epoxypropane and the ketone to prepare food industry perfume 2,4-dimethyl-2-ethyl-1,3-dioxolane (named as butanone-1,2 propanediol ketal) and has higher reaction activity, easy separation of the catalyst and a product, difficult corrosion of instruments and recycling, and the reaction process for producing the food industry perfume 2,4-dimethyl-2-ethyl-1,3-dioxolane at present becomes an environmental-friendly reaction process.

Description

technical field [0001] The invention belongs to the technical field of catalyst synthesis, and in particular relates to a macroporous SBA-15 mesoporous material loaded with copper trifluoromethanesulfonate and a preparation method thereof, and the catalyst catalyzes the reaction of 1,2-propylene oxide and butanone to obtain a A reaction process of spice 2,4-dimethyl-2-ethyl-1,3-dioxolane (alias: butanone-1,2-propanediol ketal) in the food industry. Background technique [0002] Butanone-1,2-propanediol ketal has a fresh fruity aroma and can be used in a variety of daily chemical fragrance formulations. The traditional synthesis method is to synthesize butanone and 1,2-propanediol under the action of protonic acid, and the protonic acid used is generally sulfuric acid, phosphoric acid, hydrochloric acid, p-toluenesulfonic acid, oxalic acid, etc. Its advantages are that the catalyst is cheap and easy to obtain, and the product yield is high, but there are many side reactions ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J29/70B01J35/10C07D317/12A23L1/235A23L27/29
Inventor 谢伦嘉亢宇王伟赵思源田宇冯华升孙竹芳冯再兴
Owner CHINA PETROLEUM & CHEM CORP