Preparation method for Beta zeolite molecular sieve with hierarchical porous structure

A beta zeolite and multi-stage pore technology, which is applied in the field of preparation of Beta zeolite molecular sieves, can solve the problems that the acidity and hydrothermal stability of mesoporous materials cannot be fundamentally improved, so as to improve hydrothermal stability and strong acidity, simplify Synthesis steps, the effect of improving the order degree of the pore wall

Inactive Publication Date: 2012-12-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these existing technologies have achieved a gradient distribution of the pore structure of the hierarchical porous molecular sieve and a reasonable combination of acidity, the pore walls of the prepared hierarchical porous materials are still amorphous in nature, and cannot fundamentally improve the properties of the mesoporous materials. Acid and hydrothermal stability
The currently widely used soft template method to prepare molecular sieves can only synthesize mesoporous molecular sieves with a single amorphous pore wall structure or pure crystallized microporous zeolites.

Method used

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  • Preparation method for Beta zeolite molecular sieve with hierarchical porous structure
  • Preparation method for Beta zeolite molecular sieve with hierarchical porous structure
  • Preparation method for Beta zeolite molecular sieve with hierarchical porous structure

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Mix 0.2428g sodium hydroxide, 0.0745g sodium metaaluminate (44.7wt% Na 2 O, 52wt% Al 2 o 3 ), 1.1842g of hexaammonium-based quaternary ammonium salt surfactant and 21mL of water were stirred to obtain a clear solution;

[0035] (2) Add dropwise a mixed solution of 3.6 mL tetraethyl orthosilicate (98%, J￡K) and 3.8 mL ethanol to the clear solution obtained in step (1) under magnetic stirring at 50 °C to obtain a silica-alumina gel;

[0036] (3) Keep the silica-alumina gel obtained in step (2) at 50°C and continue to stir for 6 hours, then stand and age at 30°C for 16 hours;

[0037] (4) Put the product of step (3) into a sealed stainless steel reaction kettle, and crystallize at 145°C for 120 hours. After the crystallization, the solid is suction filtered, washed and dried, and then calcined in air at 550°C After 5 hours, the organic template was removed to obtain a Beta zeolite molecular sieve with a hierarchical pore structure.

Embodiment 2

[0039] (1) Mix 0.3623g sodium hydroxide, 0.1112g sodium metaaluminate (44.7wt% Na 2 O, 52wt% Al 2 o 3 ), 1.7675g of hexaammonium-based quaternary ammonium salt surfactant and 32mL of water were stirred to obtain a clear solution;

[0040] (2) Add dropwise a mixed solution of 5.4 mL of ethyl orthosilicate (98%, J￡K) and 5.6 mL of ethanol to the clear solution obtained in step (1) under magnetic stirring at 60°C to obtain a silica-alumina gel;

[0041] (3) Keep the silica-alumina gel obtained in step (2) at 60°C and continue to stir for 10 hours, then stand and age at 35°C for 18 hours;

[0042] (4) Put the product of step (3) into a sealed stainless steel reaction kettle, and crystallize at 140°C for 110 hours. After the crystallization, the solid is suction filtered, washed and dried, and then calcined in air at 500°C After 8 hours, the organic template was removed to obtain a Beta zeolite molecular sieve with a hierarchical pore structure.

Embodiment 3

[0044] (1) Mix 0.4536g sodium hydroxide, 0.1395g sodium metaaluminate (44.7wt% Na 2 O, 52wt% Al 2 o 3 ), 2.2094g of hexaammonium-based quaternary ammonium salt surfactant and 39.4mL of water were stirred to obtain a clear solution;

[0045] (2) Under magnetic stirring at 55°C, add dropwise a mixed solution of 6.8 mL of ethyl orthosilicate (98%, J￡K) and 7 mL of ethanol to the clear solution obtained in step (1) to obtain a silica-alumina gel;

[0046] (3) Keep the silica-alumina gel obtained in step (2) at 55°C and continue to stir for 12 hours, then stand and age at 40°C for 20 hours;

[0047] (4) Put the product of step (3) into a sealed stainless steel reaction kettle, and crystallize at 150°C for 130 hours. After the crystallization, the solid is suction filtered, washed and dried, and then calcined in air at 550°C After 6h, the organic template was removed to obtain a Beta zeolite molecular sieve with a hierarchical pore structure.

[0048] The Beta zeolite molecular ...

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Abstract

The invention discloses a preparation method for a Beta zeolite molecular sieve with a hierarchical porous structure. Ethyl orthosilicate is used as a silicon source, sodium metaaluminate is used as an aluminum source, hexaammonio cationic quaternary ammonium surfactant is used as a template, and then the hierarchical porous zeolite molecular sieve containing meso pores and Beta zeolite micropores is prepared by using a hydro-thermal synthesis process under an alkaline condition. According to the invention, the hexaammonio cationic quaternary ammonium surfactant is used as a Beta zeolite structure guiding agent and generates micropores, aggregation of hydrophobic long-chain alkyl groups on the surfactant forms the meso pores, so the prepared Beta zeolite molecular sieve has both meso pores and the crystalline micropores. The structure with both the meso pores and the micropores enables defects of a single pore structure to be avoided and mass transfer efficiency to be improved, and the Beta zeolite molecular sieve has a wide application prospect in aspects of macro-molecular catalysis, adsorption, separation, etc.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and relates to a zeolite molecular sieve and a preparation method thereof, in particular to a preparation method of a Beta zeolite molecular sieve with a multi-level pore structure including micropores and mesopores. Background technique [0002] Beta zeolite is a three-dimensional twelve-membered ring channel structure, along a direction and b Orientation has a twelve-membered ring straight hole, along the c A microporous molecular sieve with a slightly distorted twelve-membered ring channel structure. Due to its unique pore structure, high acidity and good hydrothermal stability, Beta zeolite has excellent industrial application prospects and has been successfully used in petrochemical fields such as isomerization, catalytic cracking and alkylation of aromatics. However, due to the relatively narrow pore structure of the microporous zeolite molecular sieve, the reaction product ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 刘宝玉奚红霞吴永标
Owner SOUTH CHINA UNIV OF TECH
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