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Preparation method of micro-mesoporous ZSM-5 zeolite molecular sieve

A zeolite molecular sieve, medium-micro double-porous technology, applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of complex preparation process and long synthesis period, and achieve simple process, Low cost and the effect of improving mass transfer efficiency

Inactive Publication Date: 2017-09-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to the above-mentioned crystal self-assembly and soft template methods, hard template methods, desilication, dealumination, etc. can lead to the synthesis of medium and micro double-porous molecular sieves. There is a certain degree of difficulty

Method used

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  • Preparation method of micro-mesoporous ZSM-5 zeolite molecular sieve
  • Preparation method of micro-mesoporous ZSM-5 zeolite molecular sieve
  • Preparation method of micro-mesoporous ZSM-5 zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Mix 1g of single-head quaternary ammonium salt surfactant and 18ml of deionized water to obtain liquid A, add 0.081g of sodium metaaluminate (44.7 wt% Na 2 O, 52 wt% Al 2 O 3 , J&K), 0.37g sodium hydroxide and 14ml deionized water are mixed uniformly to obtain B solution, 8.654g ethyl orthosilicate (98 wt%, J&K) and 0.404g tetrapropylammonium hydroxide (40wt% aqueous solution, ρ = 1.012g / ml) Mix well to obtain liquid C;

[0040] (2) Add liquid A to liquid B to obtain liquid D under stirring conditions of 55°C and 300 rpm, and continue stirring for 1 hour;

[0041] (3) Continue to add liquid C dropwise to liquid D under stirring conditions of 55°C and 300 rpm to obtain a gel, and continue stirring for 7 hours;

[0042] (4) Put the product of step (3) in an autoclave, hydrothermally crystallize at 140°C for 110 hours, filter and wash with deionized water after the crystallization reaction is completed, and dry at 120°C for 10 hours;

[0043] (5) Place the product of step (4) ...

Embodiment 2

[0045] (1) Mix 1g single-head quaternary ammonium salt surfactant and 18ml deionized water to obtain liquid A, add 0.078g sodium metaaluminate (44.7 wt% Na 2 O, 52 wt% Al 2 O 3 , J&K), 0.36g sodium hydroxide and 13ml deionized water mixed uniformly to obtain B solution. Combine 8.333g ethyl orthosilicate (98 wt%, J&K) and 0.404g tetrapropylammonium hydroxide (40 wt% aqueous solution, ρ = 1.012g / ml) Mix well to get C solution;

[0046] (2) Add liquid A to liquid B to obtain liquid D under stirring conditions of 60°C and 300 rpm, and continue stirring for 2 hours;

[0047] (3) Continue to add liquid C dropwise to liquid D under stirring conditions of 60°C and 300 rpm to obtain a gel, and continue stirring for 8 hours;

[0048] (4) Put the product of step (3) in an autoclave, hydrothermally crystallize at 150°C for 120h, filter and wash with deionized water after the crystallization reaction is completed, and dry at 120°C for 10h;

[0049] (5) Place the product of step (4) in a muffle fu...

Embodiment 3

[0051] (1) Mix 1g of single-head quaternary ammonium salt surfactant and 18ml of deionized water to obtain liquid A, add 0.076g of sodium metaaluminate (44.7 wt% Na 2 O, 52 wt% Al 2 O 3 , J&K), 0.33g sodium hydroxide and 10ml deionized water are mixed uniformly to obtain liquid B. Combine 8.119g ethyl orthosilicate (98 wt%, J&K) and 0.404g tetrapropylammonium hydroxide (40 wt% aqueous solution, ρ = 1.012g / ml) Mix well to get C solution;

[0052] (2) Add liquid A to liquid B to obtain liquid D under stirring conditions of 65°C and 300 rpm, and continue stirring for 3 hours;

[0053] (3) Continue to add liquid C dropwise to liquid D under stirring conditions of 65°C and 300 rpm to obtain a gel, and continue stirring for 9 hours;

[0054] (4) Put the product of step (3) in an autoclave, hydrothermally crystallize it at 150°C for 130h, filter and wash with deionized water after the crystallization reaction, and dry it at 120°C for 10h;

[0055] (5) Place the product of step (4) in a muffl...

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Abstract

The invention discloses a preparation method of a micro-mesoporous ZSM-5 zeolite molecular sieve. According to the method, sodium metaaluminate serves as an aluminum source, ethyl orthosilicate serves as a silicon source, single-end quaternary ammonium surfactants and tetrapropyl ammonium hydroxide serve as template agents, and the mesoporous zeolite molecular sieve with a ZSM-5 microporous structure is subjected to hydro-thermal synthesis in an alkaline environment. The single-end quaternary ammonium surfactants can form ZSM-5 micropores in an oriented manner, hydrophobic tail chains of the single-end quaternary ammonium surfactants can limit micro-crystal growth, mesopore formation is promoted, mesoporous uniformity is improved by introducing second template agents, specific surface area is increased, and the finally obtained ZSM-5 zeolite molecular sieve has the advantages of good hydrothermal stability, high acid catalysis activity and the like of a conventional zeolite molecular sieve, is quite beneficial to reaction with macromolecules and effectively solves the problem of mass transfer limitation of a single-pore zeolite molecular sieve. The application value of the zeolite molecular sieve in the field of catalysis, adsorption separation and the like is greatly improved.

Description

Technical field [0001] The invention belongs to the field of inorganic materials, and specifically relates to a preparation method of a medium-micro and double-pored ZSM-5 zeolite molecular sieve. Background technique [0002] Zeolite molecular sieves are widely used in the fields of catalysis, adsorption, separation and petrochemical industries due to their uniform pore structure, large specific surface area, good hydrothermal stability and acid catalytic activity. However, the traditional zeolite molecular sieve has a small pore size and is easy to deposit carbon. Most of the acidic sites are embedded in the microporous channels, which has an unsatisfactory catalytic effect on macromolecules, and the diffusion of reactive molecules is also restricted. The introduction of the mesoporous structure in the microporous molecular sieve greatly shortens the diffusion path and reduces the diffusion resistance, while retaining the excellent performance of the microporous molecular sieve...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/04C01P2006/16C01P2006/17
Inventor 奚红霞颜欣刘宝玉王敏
Owner SOUTH CHINA UNIV OF TECH
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