Preparation method of zeolite imidazole framework material hybridized silicon ball

A zeolite imidazole framework and silicon sphere technology, applied in chemical instruments and methods, inorganic chemistry, alkali metal compounds, etc., can solve the problems of low internal surface loading efficiency, broadening, chromatographic peak tailing, etc. Separation effect, the effect of improving the contact area of ​​chromatographic separation

Inactive Publication Date: 2018-08-03
LISHUI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method reported in the literature for the loading of ZIF-8 on the surface of silica spheres mainly uses carboxyl or mercapto as bridging groups, and the remaining carboxyl (Chemistry-A European Journal, 2013, 19(40):13484-13491.) or mercapto Can introduce interfering active sites, leading to tailing or broadening of chromatographic peaks
In addition, the ZIFs hybrid silicon materials reported in the literature have the problem of low loading efficiency on the inner surface.

Method used

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  • Preparation method of zeolite imidazole framework material hybridized silicon ball
  • Preparation method of zeolite imidazole framework material hybridized silicon ball
  • Preparation method of zeolite imidazole framework material hybridized silicon ball

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Activation of silicon spheres: add 15g of high-purity silica gel (diameter 5μm, pore size 30nm), add 22mL concentrated hydrochloric acid and 18mL water, magnetically stir and reflux for 6h. Dry in vacuum for 24 hours at °C for later use.

[0023] Preparation of imidazole functionalized silicon spheres: add 40mL of dry toluene to 2g of activated silicon spheres (preliminary drying with molecular sieve, deep drying with sodium reflux), pass nitrogen gas for 15min, reflux for 4h under nitrogen protection, add 2mL [2-(triethoxy and silane Base) ethyl] imidazole, continue to reflux for 12h. After the reaction, wash with dry toluene 3 times, wash with acetone once, wash with acetonitrile once, and dry in vacuum at 70°C for 24 hours for later use.

[0024] Preparation of ZIF-8 hybrid silicon spheres: add 200 mg of imidazole functionalized silicon spheres into 40 mL of methanol dissolved with 0.588 g of zinc nitrate, shake at 150 rpm for 30 min, then add 40 mL of methanol diss...

Embodiment 2

[0032] Activation of silicon spheres: add 15g of high-purity silica gel (diameter 5μm, pore size 30nm), add 22mL concentrated hydrochloric acid and 18mL water, magnetically stir and reflux for 6h. Dry in vacuum for 24 hours at °C for later use.

[0033] Preparation of imidazole functionalized silicon spheres: add 40mL of dry toluene to 2g of activated silicon spheres (preliminary drying with molecular sieve, deep drying with sodium reflux), pass nitrogen gas for 15min, reflux for 4h under nitrogen protection, add 2mL [2-(triethoxy and silane Base) ethyl] imidazole, continue to reflux for 12h. After the reaction, wash with dry toluene 3 times, wash with acetone once, wash with acetonitrile once, and dry in vacuum at 70°C for 24 hours for later use.

[0034] Preparation of ZIF-8 hybrid silicon spheres: Add 200 mg of imidazole-functionalized silicon spheres into 40 mL of methanol dissolved with 0.588 g of zinc nitrate, shake at 150 rpm for 30 min, then add 1.773 g of 4-hydroxyme...

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Abstract

The invention relates to a preparation method of a zeolite imidazole framework material hybridized silicon ball. The zeolite imidazole framework material (ZIFs) hybridized silicon ball takes a chromatography silicon ball with the pore diameter being 20-100nm and the granular size being 3-5 microns as a substrate, [2-(triethyl and silylation)ethyl]imidazole is grafted on the monomolecular layer ofthe surface of the substrate, and then through a mode of in-situ growth, a ZIFs material such as ZIF-8 or ZIF-97 is loaded on the inner surface and the outer surface of the silicon ball one-time. Thepreparation method of the zeolite imidazole framework material hybridized silicon ball has a mild loading condition and simple and rapid steps, the material prepared by adopting the preparation methodhas the very good inner surface loading efficiency, and has a very good application prospect in the fields of chromatography separation, adsorption, enrichment purifying and the like.

Description

technical field [0001] The invention relates to a preparation method of a zeolite imidazole framework material hybrid silicon ball, belonging to the field of preparation of novel composite materials and chromatographic stationary phase materials. Background technique [0002] Metal-organic frameworks (Metal organic frameworks, MOFs) are crystalline materials with a periodic network structure formed by the complexation of metal ions and organic ligands through self-assembly coordination, also known as mesoporous coordination polymers. MOFs have the characteristics of large specific surface area, high porosity, adjustable skeleton structure, and pore surface modification, and have great application potential in gas storage, separation, heterogeneous catalysis, molecular recognition, chromatographic separation, and sensing. Zeolitic imidazolate frameworks (ZIFs) are coordination polymers formed by the coordination and self-assembly of transition metal ions such as zinc or cobal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/283B01J20/30
CPCB01J20/103B01J20/226B01J20/28019B01J20/283
Inventor 孙晓丽王慕华黄达云杨罗星徐玲玲
Owner LISHUI UNIV
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