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Synthesis method of multi-stage ordered mesoporous silicon aluminum 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: 2018-01-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Synthesis method of multi-stage ordered mesoporous silicon aluminum molecular sieve
  • Synthesis method of multi-stage ordered mesoporous silicon aluminum molecular sieve
  • Synthesis method of multi-stage ordered mesoporous silicon aluminum molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0018] A method for synthesizing multi-stage ordered mesoporous silica-alumina molecular sieve, including the following steps: the template [C 18 H 37 -N + (CH 3 ) 2 -C 6 H 12 -N(CH 3 ) 2 ]Br - Put it in water, heat up to 70℃, dissolve, add tetraethyl orthosilicate, sodium hydroxide and aluminum sulfate, cool to room temperature, stir for 1 hour to obtain the aged gel solution, and transfer to the stainless steel hydrothermal synthesis reactor Medium-sealed, crystallized at 130°C for 11 days, centrifuged, the solid was 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 - The molar ratio of tetraethyl orthosilicate, sodium hydroxide and aluminum sulfate is 6:2:1:1, and the 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 figure 1 , figure 2 , image 3 , Figu...

Embodiment 2

[0022] A method for synthesizing multi-stage ordered mesoporous silica-alumina molecular sieve, including the following steps: the template [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℃, dissolve, add sodium silicate, potassium hydroxide and sodium aluminate, cool to room temperature, stir for 1.5 hours to obtain the aged gel liquid, transfer it to the stainless steel hydrothermal synthesis reactor 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-stage 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 - The molar ratio of sodium silicate, potassium hydroxide and sodium aluminate is 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 used in the aldehyde-ketone condensation reaction of benzal...

Embodiment 3

[0026] A method for synthesizing multi-stage ordered mesoporous silica aluminum molecular sieve, including the following steps: the template [C 18 H 37 -N + (CH 3 ) 2 -C 6 H 12 -N(CH 3 ) 2 ]Br - Put it in water, heat up to 75°C, dissolve, add water glass, ammonium hydroxide and tert-butyl aluminum, cool to room temperature, stir for 0.5 hours to obtain the aged gel liquid, transfer it to the stainless steel hydrothermal synthesis reactor 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 template 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 molar ratio is 6:70:30:10, 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] It is used in the aldehyde-ketone condensation reaction of benzaldehy...

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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, and particularly relates to a method for synthesizing multi-stage ordered mesoporous silica alumina molecular sieve. Background technique [0002] Molecular sieve is a kind of aluminosilicate or phosphoaluminate with crystal structure. 4 It is an ordered porous material whose basic structural unit is linked by oxygen bridge bonds to form a certain topological network structure. It is widely used in many fields such as adsorption, catalysis, ion exchange and separation. Since the pores of mesoporous molecular sieves are between 2-50nm, its large pore size distribution is conducive to the adsorption and diffusion of macromolecules in the reaction process, and its large specific surface area makes it widely used in the field of catalysis, but ordered mesopores The pore wall of molecular sieve has an amorphous structure, which results in poor hydrothermal and mechanical stability. At the same...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 郭翔海张景双于川
Owner TIANJIN UNIV