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A core-shell hydrophilic chromatographic stationary phase with a metal-organic framework as the shell, its preparation method and application

A metal-organic framework and hydrophilic chromatography technology, applied in the field of core-shell hydrophilic chromatography stationary phase and its preparation, can solve the problems of narrow application range and low column efficiency, and achieve easy popularization and application, uniform distribution, and mild reaction conditions Effect

Active Publication Date: 2017-08-25
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above studies have shown the separation potential of liquid chromatography stationary phases based on MOFs, which can realize the separation and analysis of non-polar or weakly polar compounds, but the column efficiency is often low, and the application range is relatively narrow. Currently, it is only used in standard Separation and analysis of test samples, while core-shell chromatographic stationary phases based on MOFs that can achieve separation and analysis of polar compounds are rarely reported

Method used

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  • A core-shell hydrophilic chromatographic stationary phase with a metal-organic framework as the shell, its preparation method and application
  • A core-shell hydrophilic chromatographic stationary phase with a metal-organic framework as the shell, its preparation method and application
  • A core-shell hydrophilic chromatographic stationary phase with a metal-organic framework as the shell, its preparation method and application

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Experimental program
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Embodiment 1

[0027] Silica gel pretreatment: Add glutaric anhydride and silicon spheres bonded with amino groups to N,N-dimethylformamide, the mass ratio of the two is 2:1, react at 30°C for 24h, after the reaction, centrifuge The solvent was removed, and the obtained silicon spheres were washed three times with absolute ethanol to remove unreacted glutaric anhydride to obtain carboxyl-functionalized silicon spheres.

[0028] Synthesis of 1,3-bis(4-carboxybutyl)imidazole bromide: under nitrogen protection, use methyl 4-bromobutyrate and N-trimethylsilimidazole as raw materials, and control the molar ratio of the two 2:1, reacted at 60°C for 24h, after the reaction was completed, washed 3 times with anhydrous ether to remove unreacted methyl 4-bromobutyrate to obtain ester-modified imidazole; add 37% concentrated hydrochloric acid to control the two The molar ratio is 1:2.5, reflux reaction at 100°C for 2 hours, after the reaction is completed, the solvent is removed by rotary evaporation, ...

Embodiment 2

[0034] Silica gel pretreatment: Add glutaric anhydride and silicon spheres bonded with amino groups to N,N-dimethylformamide, the mass ratio of the two is 3:1, react at 30°C for 24h, after the reaction, centrifuge The solvent was removed, and the obtained silicon spheres were washed three times with absolute ethanol to remove unreacted glutaric anhydride to obtain carboxyl-functionalized silicon spheres.

[0035] Synthesis of 1,3-bis(4-carboxybutyl)imidazole bromide: under nitrogen protection, use methyl 4-bromobutyrate and N-trimethylsilimidazole as raw materials, and control the molar ratio of the two 3:1, reacted at 60°C for 24h, after the reaction was completed, washed 3 times with anhydrous ether to remove unreacted methyl 4-bromobutyrate to obtain ester-modified imidazole; add 37% concentrated hydrochloric acid to control the two The molar ratio is 1:2.5, reflux reaction at 100°C for 2 hours, after the reaction is completed, the solvent is removed by rotary evaporation, ...

Embodiment 3

[0038] Silica gel pretreatment: Add glutaric anhydride and silicon spheres bonded with amino groups to N,N-dimethylformamide, the mass ratio of the two is 2:1, react at 30°C for 24h, after the reaction, centrifuge The solvent was removed, and the obtained silicon spheres were washed three times with absolute ethanol to remove unreacted glutaric anhydride to obtain carboxyl-functionalized silicon spheres.

[0039] Synthesis of chlorinated 1,3-bis(4-carboxybutyl)imidazole: under nitrogen protection, use methyl 4-chlorobutyrate and N-trimethylsilimidazole as raw materials, and control the molar ratio of the two 1:1, reacted at 60°C for 24h, after the reaction was completed, washed 3 times with anhydrous ether to remove unreacted methyl 4-chlorobutyrate to obtain ester-modified imidazole; add 37% concentrated hydrochloric acid to control two The molar ratio is 1:2.5, reflux reaction at 100°C for 2 hours, after the reaction is completed, the solvent is removed by rotary evaporation...

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Abstract

The invention provides a core-shell hydrophilic chromatographic stationary phase with a metal-organic framework material as the shell and its preparation method and application. The stationary phase uses the metal-organic framework prepared by imidazole ionic liquid as an organic ligand to modify spherical silica gel Particles, which have a wide range of applications, can realize the separation and analysis of most polar compounds by hydrophilic interaction chromatography. At the same time, the core-shell type hydrophilic interaction chromatography stationary phase provided by the present invention has simple preparation process, mild reaction conditions, good preparation reproducibility, and is easy to popularize and use.

Description

technical field [0001] The invention relates to a novel chromatographic stationary phase and a preparation method thereof, in particular to a core-shell hydrophilic chromatographic stationary phase with a metal organic framework material as the shell, a preparation method and application thereof. Background technique [0002] In recent years, the research on the synthesis and application of core-shell materials has become a hot spot in the field of materials. Broadly speaking, core-shell structure materials are nanoscale structures formed by one material uniformly coated on the surface of another material through physical and chemical interactions. Ordered core-shell structure, which exhibits different properties than single-component core or shell. Core-shell structure materials are classified according to the shell, mainly including metal / non-metal, non-metal / metal compounds, molecular sieves, and metal-organic frameworks. Among them, the research on core-shell materials w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30G01N30/02
Inventor 乔晓强杨艳军代倩
Owner HEBEI UNIVERSITY
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