Ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal with opal structure and synthesis method thereof

A titanium-silicon molecular sieve, TS-1 technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem of poor stability of the multi-level pore structure, and achieve the goal of improving selective catalytic performance, large pore volume, and high catalytic activity Effect

Active Publication Date: 2017-01-04
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 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 import...

Method used

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  • Ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal with opal structure and synthesis method thereof
  • Ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal with opal structure and synthesis method thereof
  • Ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal with opal structure and synthesis method thereof

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Effect test

Embodiment 1

[0033] An ordered macroporous-mesoporous hierarchically porous titanium-silicon molecular sieve TS-1 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0034]1) Add 0.022g of titanium isopropoxide into a mixed solution formed by 0.3g of tetrapropylammonium hydroxide aqueous solution (organic templating agent, the concentration is 40wt%) and 0.9g of deionized water and stir well, then add 0.832g of orthosilicon Acetate ethyl ester, stir fully, obtain titanium silicon precursor solution, wherein the mol ratio of silicon source, titanium source, organic template agent and water (comprising the water in deionized water and tetrapropyl ammonium hydroxide aqueous solution) is 1: 0.02:0.15:15; then add 0.8g hard template (ordered macroporous-mesoporous hierarchical porous carbon material, macropore diameter is 400nm, mesopore diameter is 30nm) to obtain mixed solution I, mixed solution I is placed in 80 °C in a water bath to obtain d...

Embodiment 2

[0038] An ordered macroporous-mesoporous hierarchically porous titanium-silicon molecular sieve TS-1 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0039] 1) Add 0.0425g of tetrabutyl titanate into a mixed solution formed by 0.63g of tetrapropylammonium hydroxide aqueous solution (40wt%) and 1.42g of deionized water and stir well, then add 0.832g of ethyl orthosilicate, fully Stir evenly to obtain a titanium-silicon precursor solution, wherein the molar ratio of silicon source, titanium source, organic template agent and water (including deionized water and water in tetrapropylammonium hydroxide aqueous solution) is 1:0.031:0.3:25 ; Then add 0.8g hard template (ordered macroporous-mesoporous hierarchical carbon material, macropore diameter is 400nm, mesopore diameter is 20nm) to obtain mixed solution I, mixed solution I is placed in 80 ℃ water bath and evaporated to dryness Get dry glue.

[0040] 2) Weigh 0.8g of dry glue...

Embodiment 3

[0043] An ordered macroporous-mesoporous hierarchically porous titanium-silicon molecular sieve TS-1 single crystal with an opal structure, the synthesis method of which comprises the following steps:

[0044] 1) Add 0.0085g tetrabutyl titanate into a mixed solution formed by 0.5g tetrapropylammonium hydroxide aqueous solution (40wt%) and 0.42g deionized water and stir well, then add 0.416g ethyl orthosilicate, fully Stir evenly to obtain a titanium-silicon precursor solution, wherein the molar ratio of silicon source, titanium source, organic template agent and water (including water in deionized water and tetrapropylammonium hydroxide aqueous solution) is 1:0.0125:0.5:20 ), then add 0.4g ordered hard template (ordered macroporous-mesoporous hierarchical carbon material, macropore diameter is 400nm, mesopore diameter is 20nm) to obtain mixed solution I, mixed solution I is placed in 80 ℃ water bath evaporate to dryness to obtain dry glue;

[0045] 2) Weigh 0.3g of dry glue a...

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Abstract

The invention discloses an ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal with an opal structure and a synthesis method thereof. The ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal is formed by connected molecular sieve nanostructure units in a highly-ordered face-centered dense packing mode. By combining a hard template method and a dry glue method, macropore channels and mesopore channels are successfully introduced into a molecular sieve TS-1 single crystal at the same time for the first time. The synthesized ordered macropore-mesopore hierarchical pore titanium silicalite molecular sieve TS-1 single crystal has both the advantage of a hierarchical pore channel structure and the advantage of a single-crystal structure, has a super-large pore volume, a high specific area, high catalytic activity, high catalytic oxidation performance and high structural stability, and has broad application prospects.

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 titanium-silicon molecular sieve TS-1 single crystal with an opal structure and a synthesis method thereof. Background technique [0002] Titanium silicate molecular sieve TS-1 belongs to the ZSM-5 series molecular sieve and has a typical MFI topology. The introduction of titanium endows titanium-silicon molecular sieves with unique catalytic oxidation properties, enabling them to efficiently catalyze the selective oxidation of organic matter with hydrogen peroxide as the oxidant under mild conditions, and the by-product is water, which is non-polluting to the environment. Therefore, it has been widely concerned by researchers at home and abroad. However, its narrow micropores hinder the diffusion of larger molecules, which seriously hinders its industrial application. [0003] Introducing a multi-level pore...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 陈丽华孙明慧陈晨欧阳逸挺邓兆李昱苏宝连
Owner WUHAN UNIV OF TECH
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