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Chiral covalent organic framework bonded silicon ball chromatographic stationary phase and preparation and application thereof

A technology of covalent organic framework and chromatographic stationary phase, applied in solid adsorbent liquid separation, material separation, instruments, etc., can solve the problems of rare reports, slow progress, uneven particle size of materials, etc., and achieve improvement Effects of mechanical strength, uniform particle size, and uniform pore size distribution

Pending Publication Date: 2021-05-11
苏州瑞恒嘉航医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the work on liquid chromatography has progressed slowly. It was not until 2018 that Cui Yong et al. used three-dimensional CCOF as a stationary phase for the separation of chiral liquid chromatography for the first time (J.Am.Chem.Soc., 2018, 140, 892), but COF As a liquid chromatography stationary phase, there has always been a problem of non-uniform particle size of the material
However, using silica spheres as the substrate, the preparation of chiral covalent organic framework-bonded silica sphere chromatographic stationary phase can solve the above problems very well, but reports in this area are rare (Chinese patent CN201710586820.7)

Method used

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  • Chiral covalent organic framework bonded silicon ball chromatographic stationary phase and preparation and application thereof
  • Chiral covalent organic framework bonded silicon ball chromatographic stationary phase and preparation and application thereof
  • Chiral covalent organic framework bonded silicon ball chromatographic stationary phase and preparation and application thereof

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Effect test

preparation Embodiment 2

[0048] Disperse 5g of silica gel particles (with a pore size of 20nm) in 40mL, 0.2mol / L dilute alkali solution, ultrasonically treat for 40min, wash with water until the solution is neutral, wash with anhydrous methanol for 5 times, and then wash with toluene once. Subsequently, the activated silica gel particles were dispersed in 40 mL of a mixed solution of toluene and 3-aminopropyltriethoxysilane (APTES) at a ratio of 10:1 (volume ratio), ultrasonically mixed and then heated to reflux for 20 h. Methanol cleaning and drying to obtain amino macroporous silicon spheres SiO 2 @NH 2 . On the surface of amino silica gel, add 0.5g of macroporous amino silica gel with a pore diameter of 20nm into 30mL of 1,4-dioxane to make it uniformly dispersed, and then add 2g of R,R-TTA (chiral 1,4- Glycol-derived tetraaldehyde monomer) and 100 mg p-phenylenediamine, ultrasonically until the monomer is completely dissolved; add 1 mL of acetic acid as a reaction catalyst, seal the reaction sys...

preparation Embodiment 3

[0050] Disperse 5 g of silica gel particles (with a pore size of 20 nm) in 50 mL of a 0.2 mol / L dilute alkali solution, sonicate for 40 min, wash with water until the solution is neutral, wash with anhydrous methanol for 5 times, and wash with toluene once. Subsequently, the activated silica gel particles were dispersed in 50 mL of a mixed solution of toluene and 3-aminopropyltriethoxysilane (APTES) at a ratio of 10:1 (volume ratio), ultrasonically mixed and heated to reflux for 20 h. Methanol cleaning and drying to obtain amino macroporous silicon spheres SiO 2 @NH 2 . On the surface of amino silica gel, add 0.5g of macroporous amino silica gel with a pore diameter of 20nm into 50mL of 1,4-dioxane to make it uniformly dispersed, then add 1g of R,R-TTA (chiral 1,4- Glycol-derived tetraaldehyde monomer) and 50mg p-phenylenediamine, sonicate until the monomer is completely dissolved; add 1mL acetic acid as a reaction catalyst, seal the reaction system, and fill it with nitroge...

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Abstract

The invention relates to preparation and application of a chiral covalent organic framework bonded macroporous silicon ball chromatographic stationary phase. A chiral covalent organic framework is formed by in-situ polymerization of a chiral monomer on the surface of a macroporous silicon ball and in a pore channel, and the material retains the chiral characteristic of a functional monomer, that is, a chiral compound can be effectively separated. The chiral covalent organic framework disclosed by the invention grows in situ on a bonding site, so that the chiral covalent organic framework can completely coat the silicon ball without end-capping; the novel stationary phase takes silicon balls as a matrix, so that the mechanical strength of the material is greatly improved, and the problem that the application of a chiral covalent organic framework material in the field of chromatographic stationary phases is limited due to insufficient rigidity and non-uniform particle sizes is solved; meanwhile, the advantages of high thermal stability, large specific surface area and uniform pore size distribution of the covalent organic framework are reserved; in addition, the used silicon balls are macroporous silicon balls, the loading capacity of the chiral stationary phase is effectively improved due to the proper aperture, and the stationary phase is expected to be applied to separation of chiral macromolecules.

Description

Technical field: [0001] The invention relates to the technical field of chromatographic separation stationary phase, in particular to the preparation and application of a chiral covalent organic framework-bonded silica sphere chromatographic stationary phase. Background technique: [0002] Since chiral drug enantiomers composed of pharmacologically active chiral compounds may have significant differences in pharmacological activity, metabolic process, and toxicity in vivo, it is necessary to develop single enantiomer products or convert racemic drugs into chiral drugs The research has become a hot spot in the field of pharmaceutical research. The enantiomer resolution technology of chiral drugs has also attracted widespread attention. Among the chiral resolution methods, chromatography has become a powerful chiral resolution tool due to its advantages of rapidity, high efficiency, and ease of preparation. Among them, the chiral stationary phase method is the most widely use...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/29B01J20/30B01D15/38G01N30/02
CPCG01N30/482G01N2030/484B01J20/226B01J20/29B01D15/3833
Inventor 张磊
Owner 苏州瑞恒嘉航医疗科技有限公司