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Covalent organic framework doped liquid chromatography monolithic column and preparation method thereof

A technology of covalent organic framework and doped liquid phase, applied in the field of chromatographic separation, can solve problems such as the need to improve the selectivity of the monolithic column, and achieve the effects of solving high column pressure, simple operation, and improving permeability and column efficiency.

Active Publication Date: 2020-10-16
JIANGNAN UNIV
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Monolithic column is a new type of chromatographic column technology that originated in the 1990s. It is a continuous bed stationary phase that performs in-situ polymerization in the chromatographic column by organic or inorganic methods. However, the selectivity of the monolithic column remains to be determined. improve

Method used

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  • Covalent organic framework doped liquid chromatography monolithic column and preparation method thereof
  • Covalent organic framework doped liquid chromatography monolithic column and preparation method thereof
  • Covalent organic framework doped liquid chromatography monolithic column and preparation method thereof

Examples

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Effect test

Embodiment 1

[0037] Example 1: Preparation of Chiral Covalent Organic Framework Doped Liquid Chromatography Monolithic Column

[0038] (1) Preparation of chiral covalent organic framework CTzDa: take 31mg (0.09mmol) 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (Tz) and 21.6mg (0.13 mmol) 1,4-dihydroxyterephthalaldehyde (Da), placed in 1mL dichlorobenzene and 1mL ethanol mixed solution, then add 0.2mL 6mol L -1 Acetic acid solution, after ultrasonication for 10min, left to react at room temperature for 3d, centrifuged and dried, mixed and dispersed the obtained powder with 1.3mmol D-camphoryl chloride in 40mL of anhydrous tetrahydrofuran, added 400μL of triethylamine, and reacted at room temperature for 12h. After the reaction, the product was washed with water and tetrahydrofuran respectively, replaced with dichloromethane for one day, and dried in a vacuum oven at 50°C for 12 hours to obtain the chiral covalent organic framework CTzDa;

[0039] (2) Disperse 15 mg of chiral covalent organic f...

Embodiment 2

[0046] A method for preparing a covalent organic framework doped liquid chromatography monolithic column, the steps and method are basically the same as in Example 1, the difference is that the covalent organic framework used is enol TpBD, and other conditions remain unchanged, and the obtained The covalent organic framework characterization results are similar to Example 1. The obtained covalent organic framework has good mechanical strength and low column pressure (not more than 1800 psi).

Embodiment 3

[0048] A method for preparing a covalent organic framework-doped liquid chromatography monolithic column, the steps and method are basically the same as in Example 1, the difference is that the solvent used is ethanol, and other conditions remain unchanged, and the prepared covalent organic framework is characterized The result is similar to Example 1. The obtained covalent organic framework has good mechanical strength and low column pressure (not more than 1800 psi).

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Abstract

The invention discloses a covalent organic framework doped liquid chromatography monolithic column and a preparation method thereof, and belongs to the technical field of chromatographic separation. The preparation method comprises the following steps: firstly, uniformly dispersing a covalent organic framework in a solvent, adding a methacrylic acid cross-linking agent, a pore-foaming agent and aninitiator, and carrying out in-situ polymerization reaction in an empty column to obtain the covalent organic framework doped liquid chromatography monolithic column for liquid chromatographic separation. The method disclosed by the invention is simple and suitable for all covalent organic frameworks, and the problems of high column pressure, poor reproducibility and the like when the covalent organic frameworks are directly used as a liquid chromatogram stationary phase are solved; meanwhile, the permeability, the column efficiency and the special separation capability of the original polymer monolithic column are also improved.

Description

technical field [0001] The invention relates to a covalent organic framework-doped liquid chromatography integral column and a preparation method thereof, belonging to the technical field of chromatography separation. Background technique [0002] Covalent organic frameworks (COFs) have been widely used in gas adsorption and storage, catalysis, separation, sensing, drug delivery, and optoelectronics due to their porosity, low density, large specific surface area, and high crystallinity. It is a kind of high-potential chromatographic stationary phase, but COFs have irregular morphology, wide particle size distribution and low mechanical strength. Direct use as chromatographic stationary phase will lead to problems such as high column pressure and low column efficiency. The preparation of covalent organic framework-doped liquid chromatography monolithic column can effectively solve the above problems, and the doped monolithic column is easy to operate and has a wide range of a...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/281B01J20/30B01D15/22
CPCB01D15/22B01J20/226B01J20/281
Inventor 钱海龙刘芳严秀平
Owner JIANGNAN UNIV
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