A kind of ordered macroporous-mesoporous hierarchical porous silicon-aluminum molecular sieve zsm-5 single crystal with opal structure and its synthesis method

A silica-alumina molecular sieve, ZSM-5 technology, applied in molecular sieves and alkali exchange compounds, crystalline aluminosilicate zeolites, chemical instruments and methods, etc., can solve problems such as poor stability, achieve high structural stability, improve circulation The effect of diffusivity and high specific surface area

Active Publication Date: 2019-04-26
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the stability of the hierarchical channel structure of the above-mentioned hierarchical molecular sieve stacked by nano-molecular sieves is far inferior to that of molecular sieve single crystals with hierarchical channels, so the construction of hierarchical molecular sieve single crystals has important research significance
At the same time, so far, the existing research on hierarchically porous zeolite molecular sieves is limited to the construction of a single pore structure, and there is no report on a hierarchically porous molecular sieve single crystal with both macropores and mesoporous pores.

Method used

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  • A kind of ordered macroporous-mesoporous hierarchical porous silicon-aluminum molecular sieve zsm-5 single crystal with opal structure and its synthesis method
  • A kind of ordered macroporous-mesoporous hierarchical porous silicon-aluminum molecular sieve zsm-5 single crystal with opal structure and its synthesis method
  • A kind of ordered macroporous-mesoporous hierarchical porous silicon-aluminum molecular sieve zsm-5 single crystal with opal structure and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] An ordered macroporous-mesoporous multi-level porous silica-alumina molecular sieve ZSM-5 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0034] Add 0.832g tetraethyl orthosilicate (TEOS) and 0.016g aluminum isopropoxide to 1.46g aqueous solution of tetrapropylammonium hydroxide (20wt.%), 0.28g deionized water and 0.74g absolute ethanol (Sinopharm) In the mixed solution formed, after fully stirring and aging for 12 hours, add 0.8g hard template (ordered macroporous-mesoporous hierarchical porous carbon material, macropore diameter is 400nm, mesopore diameter is 20nm) to obtain mixed solution I, wherein The molar ratio of silicon source, aluminum source, organic template agent, deionized water, and absolute ethanol is 1:0.02:0.36:20:4, and the mixed solution I is evaporated to dryness in a water bath at 80°C to obtain dry glue; weigh 0.5 Put 1 g of dry glue in the reaction kettle, add 1 g of deionized water to the bot...

Embodiment 2

[0037] An ordered macroporous-mesoporous multi-level porous silica-alumina molecular sieve ZSM-5 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0038] Add 1.25g tetraethyl orthosilicate (TEOS) and 0.025g sodium metaaluminate to a mixture of 2.18g aqueous solution (20wt%) of tetrapropylammonium hydroxide, 0.42g deionized water and 1.10g absolute ethanol In the solution, after fully stirring and aging for 12 hours, add 1.2g of hard template (ordered macroporous-mesoporous hierarchical carbon material, macropore diameter is 500nm, mesopore diameter is 30nm) to obtain mixed solution I, wherein silicon source, The molar ratio of aluminum source, organic template agent, deionized water, and absolute ethanol is 1:0.05:0.36:20:4, and the mixed solution I is evaporated to dryness in a water bath at 80°C to obtain dried glue; weigh 1g of dried glue and place In the reaction kettle, add 2g of deionized water to the bottom of the kett...

Embodiment 3

[0042] An ordered macroporous-mesoporous multi-level porous silica-alumina molecular sieve ZSM-5 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0043] Add 1.25g tetraethyl orthosilicate (TEOS) and 0.025g sodium metaaluminate to a mixed solution formed by adding 2.26g tetrapropylammonium hydroxide aqueous solution (20wt%), 0.9g deionized water and 1.66g absolute ethanol 1.2g hard template (ordered macroporous-mesoporous hierarchical carbon material, macropore diameter is 500nm, mesopore diameter is 30nm) is added after fully stirring uniformly and aging 12h to obtain mixed solution I, wherein silicon source, aluminum The molar ratio of source, organic template agent, deionized water, and absolute ethanol is 1:0.05:0.37:25:6, and the mixed solution I is placed in an 80°C water bath and evaporated to dryness to obtain dry glue; weigh 1g of dry glue and place In the reaction kettle, add 2g of deionized water to the bottom of t...

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Abstract

The invention discloses an ordered macroporous-mesoporous multilevel-pore silicon-aluminum molecular sieve ZSM-5 monocrystal having an opal structure and a synthetic method of the monocrystal. The ordered macroporous-mesoporous multilevel-pore silicon-aluminum molecular sieve ZSM-5 monocrystal is formed by molecular sieve nano structural units connected with one another in a highly-ordered surface-center close-packed manner. By combining a hard template method and a dry-gel conversion method, macroporous and mesoporous pore canals are simultaneously introduced into the ZSM-5 molecular sieve monocrystal successfully for the first time. The synthesized ordered macroporous-mesoporous multilevel-pore pure silicon molecular sieve ZSM-5 monocrystal has the advantages of a multilevel-pore canal structure and a monocrystal structure, and has better circulation dispersion performance and structural stability and wide application prospect.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to an ordered macroporous-mesoporous multi-level porous silica-alumina molecular sieve ZSM-5 single crystal with an opal structure and a synthesis method thereof. Background technique [0002] ZSM-5 molecular sieve is a high-silicon molecular sieve with MFI structure. It has a unique pore structure, good thermal stability and hydrothermal stability, moderate acidity, high specific surface area and highly ordered micropore channels. It is used in modern petroleum processing industries such as catalytic cracking, aromatization, and alkylation. However, the pore size of ZSM-5 molecular sieve is small, it is difficult for macromolecules to enter the pores, and the diffusion resistance is large, and the macromolecules formed in the pores cannot diffuse out quickly, thus limiting its application in macromolecular catalytic reactions. [0003] By introducing a multi-leve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B39/02C01B39/00
Inventor 陈丽华孙明慧陈晨邓兆李昱苏宝连
Owner WUHAN UNIV OF TECH
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