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A kind of spherical aluminum-containing mesoporous composite material and supported catalyst, its preparation method and application, and the method of cyclohexanone glycerol ketal

A composite material and aluminum mesoporous technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve equipment corrosion, low conversion rate of reaction raw materials, process Complicated and other issues, to achieve the effect of less side reactions, environmental protection, and high product purity

Active Publication Date: 2019-06-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of low reaction raw material conversion rate, serious equipment corrosion and complicated process in the ketal reaction process of the supported catalyst made of existing mesoporous molecular sieve materials, and provide a suitable A spherical aluminum-containing mesoporous composite material used as a carrier, a supported catalyst containing the spherical aluminum-containing mesoporous composite material, a preparation method of the supported catalyst, a supported catalyst prepared by the method, and the supported catalyst in shrinkage Application in ketone reaction, and the method for preparing cyclohexanone glycerol ketal using the supported catalyst

Method used

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  • A kind of spherical aluminum-containing mesoporous composite material and supported catalyst, its preparation method and application, and the method of cyclohexanone glycerol ketal
  • A kind of spherical aluminum-containing mesoporous composite material and supported catalyst, its preparation method and application, and the method of cyclohexanone glycerol ketal
  • A kind of spherical aluminum-containing mesoporous composite material and supported catalyst, its preparation method and application, and the method of cyclohexanone glycerol ketal

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preparation example Construction

[0033] The present invention also provides a method for preparing a spherical aluminum-containing mesoporous composite material, which comprises the following steps:

[0034] (1) providing a mesoporous molecular sieve material with a hexagonal pore structure or preparing a filter cake of the mesoporous molecular sieve material with a hexagonal pore structure, as component a;

[0035] (2) providing silica gel or a filter cake for preparing silica gel as component b;

[0036] (3) mixing the component a and the component b and performing ball milling in a high-alumina ceramic tank, slurries the solid powder obtained after the ball milling with water, and then spray-dries the obtained slurry;

[0037]Wherein, the component a makes the spherical aluminum-containing mesoporous composite material have an average particle size of 20-80 microns, a specific surface area of ​​100-200 square meters / g, a pore volume of 0.5-1.5 ml / g, and a pore size of A bimodal distribution, and the most ...

Embodiment 1

[0074] This example is used to illustrate the spherical aluminum-containing mesoporous composite material and the supported catalyst of the present invention and their preparation methods.

[0075] (1) Preparation of spherical aluminum-containing mesoporous composites

[0076] Cetyltrimethylammonium bromide and tetraethyl orthosilicate are added in the ammonia solution that the concentration is 25% by weight, wherein, the addition of tetraethyl orthosilicate is 1.0g, and the molar feeding ratio is orthosilicic acid. Ethyl ester: cetyl trimethyl ammonium bromide: ammonia water (25%): deionized water = actual ratio 1: 0.37: 2.8: 142, stirred at 80 ° C until dissolved, the solution was suction filtered and obtained Porous material filter cake, the filter cake is washed to pH 7 to obtain filter cake A1 of mesoporous molecular sieve material with hexagonal structure;

[0077] The water glass with a concentration of 15% by weight and the sulfuric acid solution with a concentration ...

experiment Embodiment 1

[0093] This experimental example is used to illustrate the catalytic activity of the supported phosphotungstic acid catalyst according to the present invention.

[0094] The supported phosphotungstic acid catalyst (MCMAL-HPA-1) in Example 1 was vacuum-dried at 150 ° C for 6 hours, cooled to room temperature, weighed 0.5 g, and then weighed 11.3 g of cyclohexanone and 9.2 g of propylene The triol was placed in a 100ml three-necked flask in turn, stirred at 100°C under reflux for 2 hours, cooled to room temperature, separated by suction filtration, and analyzed by gas chromatography-mass spectrometry to analyze the liquid phase composition of the reaction product and the conversion of cyclohexanone. The yield was 75%, and the yield of cyclohexanone glycerol ketal was 70%.

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Abstract

The invention relates to a spherical aluminum-containing mesoporous composite material, a preparation method of the spherical aluminum-containing mesoporous composite material, the spherical aluminum-containing mesoporous composite material prepared by the method, and a load-bearing type of the spherical aluminum-containing mesoporous composite material. Catalyst, the preparation method of the supported catalyst, the supported catalyst prepared by the method, the application of the supported catalyst in the ketal reaction, and the method of using the supported catalyst to carry out the ketal reaction, wherein the supported catalyst The catalyst contains the spherical aluminum-containing mesoporous composite material and phosphotungstic acid supported thereon. The supported catalyst made by using the spherical aluminum-containing mesoporous composite material of the present invention as a carrier has high catalytic activity in the process of preparing cyclohexanone glycerol ketal, and at the same time does not cause corrosion to the equipment, and the present invention The supported phosphotungstic acid catalyst provided can be recycled and used repeatedly, and the post-treatment process is simple.

Description

technical field [0001] The invention relates to a spherical aluminum-containing mesoporous composite material, a preparation method of the spherical aluminum-containing mesoporous composite material, the spherical aluminum-containing mesoporous composite material prepared by the method, and a load-type composite material containing the spherical aluminum-containing mesoporous composite material. A catalyst, a preparation method of the supported catalyst, a supported catalyst prepared by the method, the application of the supported catalyst in a ketal reaction, and a method for preparing a cyclohexanone glycerol ketal using the supported catalyst. Background technique [0002] In 1992, Mobile company synthesized regular mesoporous materials with highly ordered channels, with high specific surface area, regular channel structure and narrow pore size distribution, which made mesoporous materials widely used in catalysis, separation, medicine and other fields. In 1998, Zhao Dong...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26B01J35/10C07D317/72
CPCC07D317/72B01J21/04B01J29/00B01J31/16B01J31/26B01J35/19B01J35/638B01J35/69B01J35/635B01J35/615Y02P20/584
Inventor 亢宇张明森
Owner CHINA PETROLEUM & CHEM CORP
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