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Preparation method and application of composite solid superacid catalyst

A solid superacid and catalyst technology, which is applied in the preparation of organic compounds, catalytic reactions, and carboxylate preparations, can solve the problems of cumbersome catalyst preparation steps, and achieve the effects of easy recovery, high catalytic efficiency, and obvious economic benefits

Active Publication Date: 2016-06-15
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the magnetic nanoparticles Co 0.5 Fe 2.5 o 4 The introduction of the catalyst leads to more cumbersome preparation steps

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The perfluorosulfonic acid resin with an exchange capacity of 1.05 was added to the alcohol-water solution, mechanically stirred at 250°C for 5.0 h under high pressure and in a reflux device, evaporated and concentrated to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.

[0037]Add 17.30 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.50 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 42.39 In the mixture of g perfluorosulfonic acid resin solution and 46.63g 0.05mol / L NaOH solution, the solution gels quickly; cover the gel with aluminum foil at 75°C and dry for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain ...

Embodiment 2

[0041] Add the perfluorosulfonic acid resin with an exchange capacity of 1.10 to the alcohol-water solution, and mechanically stir at 250°C for 8.0 hours under high pressure and reflux, evaporate and concentrate to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.

[0042] Add 17.30 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.50 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 48.05 In the mixed solution of perfluorosulfonic acid resin solution and 48.05g of 0.05mol / L NaOH solution, the solution gels quickly; dry the gel at 75°C covered with aluminum foil for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain complete...

Embodiment 3

[0046] Add the perfluorosulfonic acid resin with an exchange capacity of 0.98 to the alcohol-water solution, and mechanically stir at 250° C. for 6.0 h under high pressure and reflux, evaporate and concentrate to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.

[0047] Add 16.50 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.00 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 48.05 In the mixture of g perfluorosulfonic acid resin solution and 52.86g 0.05mol / L NaOH solution, the solution gels quickly; cover the gel with aluminum foil at 75°C and dry for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain completely dried...

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Abstract

The invention relates to a preparation method and an application of a composite solid superacid catalyst, and belongs to the technical field of solid superacid catalysts. The preparation method of the composite solid superacid catalyst comprises the following steps: preparing SiO2 supported perfluorosulfonic acid resin solid particles through adopting a sol-gel technology, and calcining the solid particles to obtain the perfluorosulfonic acid resin / SiO2 composite solid superacid catalyst. The preparation method of the composite solid superacid catalyst is simple and easy, and the catalyst prepared in the invention has the advantages of certain crystal form, crystal size, aperture structure and specific surface area, high mechanical strength, full exposure of acidic sites, stable catalysis activity, and high catalysis efficiency and reuse rate; and the invention also provides the simple and convenient application of the composite solid superacid catalyst.

Description

technical field [0001] The invention relates to a preparation method and application of a composite solid superacid catalyst, and belongs to the technical field of solid superacid catalysts. Background technique [0002] Ethyl acetate is usually prepared by the esterification of ethanol and acetic acid. It is a fine chemical product with a wide range of uses. It is a very important organic chemical raw material and an excellent industrial solvent. It is widely used in industrial production and organic synthesis. Applications. In addition, it can also be used as adhesives and spices, etc., and is one of the indispensable raw materials in production and life. [0003] The types of catalysts used in esterification have always been the focus of research, but the catalysts used in industry are usually concentrated sulfuric acid, p-toluenesulfonic acid, thionyl chloride, etc., which have the disadvantages of difficult separation and low esterification yield. It is replaced by ne...

Claims

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Application Information

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IPC IPC(8): B01J31/10B01J35/02C07C67/08C07C69/14
CPCC07C67/08B01J21/08B01J31/10B01J2231/49B01J35/50C07C69/14
Inventor 王汉利王晓燕王军
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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