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Preparation method for hierarchical-pore ZSM-5 zeolite microspheres

A ZSM-5, multi-level pore technology, applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of difficult filtration separation reaction molecular diffusion limitation, difficult filtration separation and other problems, Achieving the effect of good zeolite structure retention, simple and economical method, and good interconnectivity

Active Publication Date: 2018-12-11
TAIYUAN UNIV OF TECH
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  • Abstract
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Problems solved by technology

[0004] The present invention provides a method for preparing multi-level porous ZSM-5 zeolite microspheres in order to solve the problems of difficult filtration separation and diffusion limitation of reaction molecules in micron ZSM-5 zeolite during the preparation and use of nano zeolite. The micron-sized microspheres are stacked by nano-sized zeolite rod-like grains, thus forming abundant intercrystalline mesopores
The material maintains the inherent skeleton crystal structure of ZSM-5, and at the same time, due to the nanonization of zeolite crystal grains and the existence of intercrystalline mesopores, it can effectively improve the diffusion limitation of reactive molecules such as hydrocarbons in micron-sized ZSM-5 zeolite , improve the utilization rate of zeolite active sites; at the same time, it solves the problem of difficult filtration and separation of nano zeolite in the process of preparation and use, and provides a new material and its preparation method for the field of zeolite catalysis

Method used

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  • Preparation method for hierarchical-pore ZSM-5 zeolite microspheres
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  • Preparation method for hierarchical-pore ZSM-5 zeolite microspheres

Examples

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Embodiment 1

[0016] Embodiment 1: A kind of preparation method of hierarchical porous ZSM-5 zeolite microsphere, with long-chain alkyltrimethylammonium bromide surfactant as a single template, synthesized in NaOH-water-ethanol crystallization system ZSM-5 zeolite microspheres with hierarchical pore structure.

[0017] Specific steps are as follows:

[0018](1) Preparation of gel: according to SiO 2 :Al 2 o 3 : Na 2 O: surfactant CTAB: deionized water: C 2 h 5 The molar ratio of OH is 1:0.0067:0.17:0.04:54.7:2.8. Add 0.35g of surfactant CTAB and 4mL of absolute ethanol to deionized water to obtain a mixture. The mixture is placed in a water bath at 30°C and stirred. After the surfactant is fully dissolved until the solution is clear, add 0.32g of sodium hydroxide and continue to stir. After the solution is clear, add 0.04g of sodium metaaluminate. After stirring, add 1.48g of fumed silica (Aerosil@200), and continue to Stir in a water bath at ℃ for 2 hours to obtain a well-stirred ge...

Embodiment 2

[0022] Example 2: A preparation method of hierarchically porous ZSM-5 zeolite microspheres, using CTAB surfactant as a single template, synthesizing ZSM-5 zeolite with hierarchically porous structure in NaOH-water-ethanol crystallization system Microspheres. Concrete steps are as follows: according to the feeding molar ratio is SiO 2 :Al 2 o 3 : Na 2 O:CTAB:H 2 O: C 2 h 5 OH is 1:0.0067:0.17:0.02:54.7:2.8, and other conditions are the same as in Example 1, only the addition of CTAB is changed to 0.2g to obtain hierarchically porous ZSM-5 zeolite microspheres. Named ZSM-5-2. Its structural properties are shown in Table 1.

Embodiment 3

[0023] Example 3: A preparation method of hierarchically porous ZSM-5 zeolite microspheres, using CTAB surfactant as a single template, and synthesizing ZSM-5 zeolite with hierarchically porous structure in NaOH-water-ethanol crystallization system Microspheres. Concrete steps are as follows: according to the feeding molar ratio is SiO 2 :Al 2 o 3 : Na 2 O:CTAB:H 2 O: C 2 h 5 OH is 1:0.0067:0.17:0.01:54.7:2.8, and other conditions are the same as in Example 1, except that the amount of CTAB added is changed to 0.1 g, that is, hierarchically porous ZSM-5 zeolite microspheres are obtained. Named ZSM-5-3. Its structural properties are shown in Table 1.

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Abstract

The invention belongs to the technical field of preparation of inorganic non-metal materials and catalysts, and provides a preparation method for hierarchical-pore ZSM-5 zeolite microspheres, aiming to solve the problems that nano-zeolite is not easy to filter and separate in the preparation and application process and diffusion of reaction molecules in micron-size ZSM-5 zeolite is limited. According to the preparation method, a long-chain alkyl trimethyl ammonium bromide surfactant is taken as a single templating agent, and the hierarchical-pore ZSM-5 zeolite microspheres are compounded in aNaOH-water-ethanol crystallization system. The preparation method has the advantages that the intrinsic framework microporous crystal structure is maintained, and the utilization rate of the active site of the zeolite is increased due to nanocrystallization of zeolite grains and presence of intercrystalline mesopores; the preparation method is simple, economical and green; the diffusion limitationof the reaction molecules such as hydrocarbons in the micron-sized ZSM-5 zeolite is relieved, and the utilization rate of the active site of the zeolite is increased; the problem that the nano-zeolite is not easy to filter and separate during preparation and application is solved, and a new preparation method is provided for the field of zeolite catalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic non-metallic materials and catalysts, and in particular relates to a preparation method of hierarchically porous ZSM-5 zeolite microspheres. A preparation method for synthesizing a spherical ZSM-5 zeolite molecular sieve with a multi-level pore structure by using a long-chain alkyltrimethylammonium bromide surfactant as a single template and stacking nanometer zeolite rod-like grains. Background technique [0002] ZSM-5 zeolite molecular sieve is a high silica zeolite molecular sieve with MFI topology, with three-dimensional intersecting channels and ten-membered ring pore structure. ZSM-5 zeolite's unique pore structure and wide adjustable silicon-aluminum ratio endow it with good shape-selective catalytic properties and universal applicability to a variety of catalytic reactions, and it performs well in various catalytic conversion reactions of hydrocarbons catalytic properties...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/04
Inventor 马静红胡素芳李瑞丰
Owner TAIYUAN UNIV OF TECH
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