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Preparation method for mesoporous ZSM-5 zeolite molecular sieve

A technology of ZSM-5 and zeolite molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of not fundamentally improving the acidity and hydrothermal stability of mesoporous materials, etc. Problems, to achieve the effect of low cost, increase crystallinity, easy to obtain and cheap raw materials

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

However, the pore walls of these composite molecular sieves are still amorphous in nature, which does not fundamentally improve the acidity and hydrothermal stability of mesoporous materials.

Method used

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  • Preparation method for mesoporous ZSM-5 zeolite molecular sieve
  • Preparation method for mesoporous ZSM-5 zeolite molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Dissolve 1.189g (0.0012mol) of triammonium-based quaternary ammonium salt surfactant and 5.6mL of ethanol in 12mL of water to form liquid A, mix 0.111g (0.0012mol) of sodium metaaluminate and 0.36g (0.009mol) Sodium hydroxide was dissolved in 19.5mL of water to obtain liquid B;

[0032] (2) Under the condition of stirring, add liquid A to liquid B to form liquid C;

[0033] (3) Under magnetic stirring at 60°C, slowly add 5.077g (0.024mol) ethyl orthosilicate dropwise into liquid C to form a gel, continue stirring for 6 hours, and age at 50°C for 12 hours;

[0034] (4) Put the product of step (3) into a sealed crystallization reaction kettle, crystallize at 150°C for 120 hours, wash, filter, and dry, and then calcinate in air at 550°C for 6 hours to remove the template agent, and obtain intermediate Pore ​​ZSM-5 zeolite molecular sieve.

Embodiment 2

[0036] (1) Dissolve 0.797g (0.0008mol) of triammonium-based quaternary ammonium salt surfactant and 3.8mL of ethanol in 9mL of water to form liquid A, mix 0.075g (0.0008mol) of sodium metaaluminate and 0.24g (0.006mol) Sodium hydroxide was dissolved in 12mL of water to obtain liquid B;

[0037] (2) Under the condition of stirring, add liquid A to liquid B to form liquid C;

[0038] (3) Under magnetic stirring at 60°C, slowly add 3.418g (0.016mol) ethyl orthosilicate dropwise into liquid C to form a gel, continue stirring for 6 hours, and age at 60°C for 10 hours;

[0039] (4) Put the product of step (3) into a sealed crystallization reaction kettle, crystallize at 140°C for 96 hours, wash, filter, and dry, then calcinate in air at 550°C for 5 hours to remove the template agent, and obtain intermediate Pore ​​ZSM-5 zeolite molecular sieve.

Embodiment 3

[0041] (1) Dissolve 1.487g (0.0015mol) of triammonium-based quaternary ammonium salt surfactant and 7mL of ethanol in 18mL of water to form a liquid A, mix 0.139g (0.0015mol) of sodium metaaluminate and 0.44g (0.011mol) of hydrogen Sodium oxide was dissolved in 21.4mL of water to obtain liquid B;

[0042] (2) Under the condition of stirring, add liquid A to liquid B to form liquid C;

[0043] (3) Under magnetic stirring at 60°C, slowly add 6.346g (0.03mol) ethyl orthosilicate dropwise into liquid C to form a gel, continue to stir for 6 hours, and age at 50°C for 12 hours;

[0044] (4) Put the product of step (3) into a sealed crystallization reaction kettle, crystallize at 140°C for 120 hours, wash, filter, and dry, then calcinate in air at 550°C for 6 hours to remove the template agent, and obtain intermediate Pore ​​ZSM-5 zeolite molecular sieve.

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Abstract

The invention discloses a preparation method for a mesoporous ZSM-5 zeolite molecular sieve. The mesoporous zeolite molecular sieve with ZSM-5 microporous crystalline pore walls is prepared by using tetraethoxysilane as a silicon source, sodium metaaluminate as an aluminum source and a difunctional triammonio quaternary ammonium salt cationic surfactant as a template through a hydrothermal synthesis process under an alkaline condition. According to the invention, the quaternary ammonium surfactant is used as a ZSM-5 zeolite structure directing agent and generates micropores, and aggregation of long hydrophobic alkyl groups at two ends of the surfactant forms meso pores. The method provided by the invention effectively changes an amorphous pore wall structure of traditional mesoporous materials and allows the ZSM-5 zeolite molecular sieve to have crystalline pore walls, which enables acidity and hydrothermal stability of mesoporous materials to be greatly improved; the prepared mesoporous ZSM-5 zeolite molecular sieve has a unique mesoporous / microporous multiple pore structure, so defects of a single pore structure are avoided, mass transfer efficiency is improved, and the ZSM-5 zeolite molecular sieve has a wide application prospect in aspects like macro-molecular catalysis, adsorption, separation, etc.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and relates to a mesoporous zeolite material and a preparation method thereof, in particular to a mesoporous zeolite material with a ZSM-5 crystalline zeolite pore wall structure prepared by using a triammonium-based quaternary ammonium salt surfactant as a template Porous zeolite molecular sieve method. Background technique [0002] ZSM-5 is a microporous molecular sieve with MFI structure. Due to its unique pore structure, unique shape selectivity, strong acidity and good hydrothermal stability, it is widely used in petroleum processing, coal chemical industry and fine chemical industry. . However, due to the small pore size of microporous molecular sieves, on the one hand, it is difficult for macromolecules to enter the pores; Molecular sieves have certain limitations in catalytic reactions involving macromolecules. [0003] In order to solve the problem of difficult diffusion ...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 刘宝玉奚红霞李超
Owner SOUTH CHINA UNIV OF TECH
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