Preparation method of hierarchical porous structure silica-alumina zeolite material

A technology of silica-alumina zeolite and multi-level pores, which is applied in the field of preparation of multi-level porous structure silica-aluminum oxide materials, and can solve the problems of difficulty in preparation and the like

Active Publication Date: 2016-02-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although researchers from various countries have developed many synthetic methods of hierarchical porous silica-alumina zeolites, the preparation of hierarchical porous silica-alumina zeolite monolithic materials is still one of the difficulties in the field of synthesis

Method used

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  • Preparation method of hierarchical porous structure silica-alumina zeolite material
  • Preparation method of hierarchical porous structure silica-alumina zeolite material
  • Preparation method of hierarchical porous structure silica-alumina zeolite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 4 grams of 1 mol / liter nitric acid solution and 5 grams of water, add 1 gram of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 5800, referred to as P123), stir and dissolve at room temperature, and add polyethylene oxide to the mixed solution. Diol (molecular weight 10000) 0.7 grams and 1.26 grams of aluminum nitrate (Al(NO 3 ) 3 9H 2 0), after stirring evenly, transfer to the ice-water mixing bath and continue to stir for 5 minutes. 5.1 g of tetramethyl orthosilicate was added to the mixed solution, and vigorously stirred for 20 minutes. Pour the mixture into a mold to seal it, and place it in an oven at 60°C for 72 hours of aging. Remove from the mold, dry at 25°C, and finally bake at 600°C for 8 hours to obtain a silicon-aluminum oxide monolithic material with a silicon-aluminum molar ratio Si / Al=16; Tetrapropylammonium hydroxide solution was added to the bottom of the kettle, and after crystallization at 130° C. for 3 days, the sample w...

Embodiment 2

[0026]Weigh 12 grams of 0.3 mol / liter phosphoric acid solution, add 4.0 grams of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 1500), stir and dissolve at room temperature, add polyethylene glycol (molecular weight 10000) 0.6 After stirring evenly, the mixed solution was added to the isopropanol solution containing 8.9 grams of tetrapropyl orthosilicate and 0.14 grams of aluminum isopropoxide, and vigorously stirred for 20 minutes. Pour the mixture into a mold and seal it, and place it in an oven at 80°C for 72 hours of aging. After taking it out, demoulding, drying at room temperature, and finally roasting at 550°C for 5 hours to obtain a silicon-aluminum oxide monolithic material with a silicon-aluminum molar ratio Si / Al=75; then place the silicon-aluminum oxide monolithic material on the upper part of the reactor, and Tetrapropylammonium hydroxide solution was added at the bottom, and after crystallization at 130°C for 3 days, the sample was washed, dri...

Embodiment 3～15

[0028] According to the various steps and conditions of [Example 1], the silicon-aluminum oxide material is obtained, but the silicon source (tetramethyl orthosilicate TMOS, tetraethyl orthosilicate TEOS, tetrapropyl orthosilicate TPOS, orthosilicate) is changed. tetrabutyl silicate (TBOS), aluminum source (aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum isopropoxide, aluminum isobutoxide and pseudoboehmite Al 2 o 3 ), the type of phase separation inducer R1 (polyethylene glycol PEG, polyoxyethylene PEO) or structure directing agent R2 (polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 12000, F127), polyoxyethylene-polyoxyethylene Oxypropylene-polyoxyethylene (molecular weight 2900, L64), cetyl trimethyl ammonium bromide CTAB, citric acid CA, lactic acid LA, tartaric acid TA, malic acid MA), organic amine template (tetrapropyl hydroxide Ammonium (POH), tetrapropylammonium bromide (PBr), tetraethylammonium hydroxide (EOH), tetraethylammonium br...

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Abstract

The invention relates to a preparation method of an hierarchical pore structure sliicon-aluminum zeolite material, and mainly solves the problem of difficult obtaining of a composite pore molecular sieve having macropores and micropores simultaneously in the prior art. The method of the invention adopts a technical scheme consisting of: subjecting the mixture of a phase separation inducer R1, a structure directing agent R2, an acid, water, a silicon source and an aluminum source to a hydrolysis reaction so as to obtain a silicon-aluminum oxide material precursor I; conducting gelation and aging on the silicon-aluminum oxide material precursor I to obtain a silicon-aluminum oxide material precursor II; drying and roasting the silicon-aluminum oxide material precursor II so as to obtain a mesopore / macropore composite pore structure silicon-aluminum oxide III; putting the silicon-aluminum oxide material III at the upper part of a reaction kettle, adding an organic ammonium solution to the bottom of the reaction vessel, then carrying out crystallization, washing, drying and roasting, thus obtaining the hierarchical pore structure sliicon-aluminum zeolite material. The technical scheme of the invention well solves the problem, and can be used in industrial production of hierarchical pore structure sliicon-aluminum zeolite materials.

Description

technical field [0001] The invention relates to a preparation method of a silicon-aluminum oxide material with a hierarchical porous structure. Background technique [0002] Traditional silica-alumina zeolites have shown excellent catalytic performance in olefin epoxidation reactions due to their suitable acid center distribution and special pore structure, but due to the problems of pore structure, morphology and preparation methods, etc. The application of traditional silica-alumina zeolites is restricted. The first is the pore structure, because the traditional silica-alumina zeolite only has a microporous structure, which greatly limits the mass transfer and diffusion of macromolecules such as heavy oil components in the catalyst, thereby inhibiting the reactivity, selectivity and life of the catalyst. . Secondly, in terms of morphology, traditional zeolites are powders, which can only be used in industrial production after complex molding steps. However, the addition ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/00C01B39/04
Inventor 杨贺勤刘志成高焕新
Owner CHINA PETROLEUM & CHEM CORP
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