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A kind of ordered macropore-mesoporous hierarchical porous pure silica molecular sieve silicalite-1 single crystal with opal structure and its synthesis method

A technology of pure silicon molecular sieve and synthesis method, which is applied in the field of molecular sieve synthesis, can solve the problems of poor structural stability of multi-level pores, achieve good circulation and diffusion performance and structural stability, super large pore volume, and improve circulation and diffusion.

Active Publication Date: 2019-03-26
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the stability of the hierarchical channel structure of hierarchical molecular sieves 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 macropore-mesoporous hierarchical porous pure silica molecular sieve silicalite-1 single crystal with opal structure and its synthesis method
  • A kind of ordered macropore-mesoporous hierarchical porous pure silica molecular sieve silicalite-1 single crystal with opal structure and its synthesis method
  • A kind of ordered macropore-mesoporous hierarchical porous pure silica molecular sieve silicalite-1 single crystal with opal structure and its synthesis method

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Effect test

Embodiment 1

[0032] A kind of ordered macroporous-mesoporous multi-level porous pure silicon molecular sieve Silicalite-1 single crystal with opal structure, its synthesis method comprises the following steps:

[0033]0.832g tetrapropylammonium hydroxide aqueous solution (20wt%), 0.6g deionized water and 7.36g absolute ethanol were mixed drop by drop with 0.832g tetrapropyl ammonium hydroxide solution, and fully stirred to obtain a molecular sieve precursor solution. Wherein the mol ratio of silicon source, organic template agent, water (comprising deionized water and water in tetrapropyl ammonium hydroxide aqueous solution) and dehydrated alcohol is 1:0.15:20:40; Then add 0.8g hard template (with macroporous-mesoporous hierarchical porous carbon material, the macropore diameter is 400nm, and the mesopore diameter is 20nm), to obtain the mixed solution I, and the mixed solution I is placed in an 80°C water bath and evaporated to dryness to obtain dry glue; weigh 0.3g Dry glue was placed in...

Embodiment 2

[0036] A kind of ordered macroporous-mesoporous multi-level porous pure silicon molecular sieve Silicalite-1 single crystal with opal structure, its synthesis method comprises the following steps:

[0037] Add 0.555g tetrapropylammonium hydroxide solution (20wt%) dropwise to 0.555g tetrapropylammonium hydroxide aqueous solution (20wt%) and 2.45g absolute ethanol to mix, fully stir to obtain molecular sieve precursor solution, wherein silicon source, organic template , the molar ratio of water (water contained in tetrapropyl ammonium hydroxide aqueous solution) and dehydrated alcohol is 1:0.22:10:20; Then add 0.53g hard template (ordered macroporous-mesoporous hierarchical porous carbon material , the macropore diameter is 500nm, and the mesopore diameter is 10nm) to obtain the mixed solution I, put the mixed solution I in a water bath at 80°C and evaporate to dryness to obtain dry glue; weigh 0.1g dry glue and place it in a reaction kettle (volume is 100mL) , add 0.2g of deion...

Embodiment 3

[0040] A kind of ordered macroporous-mesoporous multi-level porous pure silicon molecular sieve Silicalite-1 single crystal with opal structure, its synthesis method comprises the following steps:

[0041] 1.109g tetrapropylammonium hydroxide aqueous solution (20wt%), 0.84g deionized water and 12.3g absolute ethanol were mixed dropwise with 1.109g tetrapropyl ammonium hydroxide solution dropwise, fully stirred uniformly to obtain molecular sieve precursor solution, wherein The molar ratio of silicon source, organic template, water (comprising deionized water and water in tetrapropylammonium hydroxide aqueous solution) and absolute ethanol is 1:0.25:20:50; Then add 1g hard template (ordered large Pore-Mesoporous Hierarchical Carbon Material, the macropore diameter is 300nm, and the mesopore diameter is 30nm) to obtain the mixed solution I, and the mixed solution I is placed in an 80°C water bath and evaporated to dryness to obtain dry glue; weigh 0.4g dry glue and place In a re...

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Abstract

The invention discloses an ordered macroporous-mesoporous multilevel-pore pure silicon molecular sieve Silicalite-1 monocrystal having an opal structure and a synthetic method of the monocrystal. The ordered macroporous-mesporous multilevel-pore pure silicon molecular sieve Silicalite-1 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 Silicalite-1 molecular sieve monocrystal successfully for the first time. The synthesized ordered macroporous-mesoporous multilevel-pore pure silicon molecular sieve Silicalite-1 monocrystal has the advantages of a multilevel-pore canal structure and a monocrystal structure, and has extra-large pore volume, relatively high specific surface area, excellent adsorption separation 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 pure silicon molecular sieve Silicalite-1 single crystal with an opal structure and a synthesis method thereof. Background technique [0002] Silicalite-1, as an all-silica zeolite, has relatively high thermal and chemical stability, and its special ten-membered ring pore structure and strong hydrophobic and lipophilic properties make it suitable for isomerization separation, pervaporation, It is widely used in organic matter removal system. However, the size of its micropores limits the transmission and diffusion of macromolecules in molecular sieves, thereby inhibiting its application in macromolecules. Therefore, constructing multi-stage pores in molecular sieves to improve the flow and diffusion properties of zeolite molecular sieves has become a major target for macromolecular applications. Urgent reques...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08C01B39/04
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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