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A kind of synthetic method of multi-stage ordered mesoporous silica-alumina molecular sieve

A technology of mesoporous silica-alumina and synthesis method, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high price and unfavorable industrial application, achieve good catalytic activity, reduce production cost, improve hydrothermal stability and mechanical properties. The effect of stability

Inactive Publication Date: 2019-09-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the problem of high price in the process of synthesizing multi-level ordered mesoporous molecular sieves in the prior art, which is not conducive to industrial application, and to provide a method for synthesizing multi-level ordered mesoporous silica-alumina molecular sieves with low cost

Method used

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  • A kind of synthetic method of multi-stage ordered mesoporous silica-alumina molecular sieve
  • A kind of synthetic method of multi-stage ordered mesoporous silica-alumina molecular sieve
  • A kind of synthetic method of multi-stage ordered mesoporous silica-alumina molecular sieve

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Comparison scheme
Effect test

Embodiment 1

[0018] A method for synthesizing a multi-level ordered mesoporous silica-alumina molecular sieve, comprising the following steps: adding a template agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - Put in water, heat up to 70°C, dissolve, add tetraethyl orthosilicate, sodium hydroxide and aluminum sulfate, cool down to room temperature, stir for 1 hour, obtain the aged gel liquid, transfer to stainless steel hydrothermal synthesis reactor Sealed in the medium, crystallized at 130°C for 11 days, centrifuged, washed with water, dried, and calcined at 550°C for 6 hours to obtain a multi-level ordered mesoporous silica-alumina molecular sieve;

[0019] The templating agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - , tetraethyl orthosilicate, sodium hydroxide and the mol ratio of aluminum sulfate are 6:2:1:1, and described templating agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - The mass ratio to water is 1:1100; see ...

Embodiment 2

[0022] A method for synthesizing a multi-level ordered mesoporous silica-alumina molecular sieve, comprising the following steps: adding a template agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - Put it into water, heat up to 65°C, dissolve, add sodium silicate, potassium hydroxide and sodium aluminate, cool down to room temperature, stir for 1.5 hours to obtain the aged gel liquid, transfer it to a stainless steel hydrothermal synthesis reaction kettle and seal it , crystallized at 100°C for 14 days, centrifuged, washed the solid with water, dried, and calcined at 550°C for 6 hours to obtain a multi-level ordered mesoporous silica-alumina molecular sieve;

[0023] The templating agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - , sodium silicate, potassium hydroxide and sodium aluminate in a mol ratio of 6:50:20:0.1, the [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2]Br - The mass ratio with water is 1:1000.

[0024] It is u...

Embodiment 3

[0026] A method for synthesizing a multi-level ordered mesoporous silica-alumina molecular sieve, comprising the following steps: the template agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - Put it into water, heat up to 75°C, dissolve, add water glass, ammonium hydroxide and tert-butylaluminum, cool down to room temperature, stir for 0.5 hours to obtain the aged gel liquid, transfer it to a stainless steel hydrothermal synthesis reaction kettle and seal it , crystallized at 160°C for 8 days, centrifuged, washed the solid with water, dried, and calcined at 550°C for 6 hours to obtain a multi-level ordered mesoporous silica-alumina molecular sieve;

[0027] The templating agent [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - , water glass, ammonium hydroxide and tert-butyl aluminum are in a mol ratio of 6:70:30:10, and the template [C 18 h 37 -N + (CH 3 ) 2 -C 6 h 12 -N(CH 3 ) 2 ]Br - The mass ratio with water is 1:1200.

[0028] I...

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Abstract

The invention discloses a synthesis method of a multi-stage ordered mesoporous silicon aluminum molecular sieve. The method comprises the following steps: putting a template agent into water, heating,dissolving, adding a silicon source, alkali and an aluminum source, cooling to room temperature, stirring to obtain aged gel liquid, transferring to a stainless steel hydrothermal synthesis reactionkettle, sealing, crystallizing, centrifuging, washing, drying and calcining to obtain the multi-stage ordered mesoporous silicon aluminum molecular sieve. The method is low in cost, simple in technological process and suitable for industrialized production. The prepared molecular sieve has high mesoporous orderness, completely combines high hydrothermal stability and mechanical stability of a microporous molecular sieve, can combine the acidity advantage of a microporous zeolite molecular sieve, has high catalytic activity, and is suitable for the fields of petrochemical industry, preparationof fine chemical products and the like. The molecular sieve combines the advantages of a microporous MFI molecular sieve and a mesoporous MCM-41 molecular sieve, and can be widely applied in the fields of adsorption separation, membrane separation and the like due to the special pore channel structure.

Description

technical field [0001] The invention belongs to the field of porous materials and catalysis, in particular to a method for synthesizing a multi-level ordered mesoporous silicon-aluminum molecular sieve. Background technique [0002] Molecular sieves are a class of aluminosilicates or aluminophosphates with a crystal structure, with TO 4 It is an ordered porous material whose basic structural units form a certain topological network structure through oxygen bridge bonds. It is widely used in many fields such as adsorption, catalysis, ion exchange and separation. Mesoporous molecular sieves are widely used in the field of catalysis due to their large pore size distribution, which is conducive to the adsorption and diffusion of macromolecules during the reaction process, and their large specific surface area makes them widely used in the field of catalysis, but ordered mesoporous molecular sieves The pore walls of molecular sieves are amorphous, resulting in poor hydrothermal ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 郭翔海张景双于川
Owner TIANJIN UNIV