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Spherical covalent organic framework material as well as preparation method and application thereof

A covalent organic framework and spherical technology, applied in the field of chromatographic materials, can solve the problems of pure spherical COFs materials that have not been reported, and achieve good application prospects, expand the pH application range, and controllable size

Active Publication Date: 2019-02-12
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pure spherical COFs materials have not been reported in the field of liquid chromatography stationary phases.

Method used

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  • Spherical covalent organic framework material as well as preparation method and application thereof
  • Spherical covalent organic framework material as well as preparation method and application thereof
  • Spherical covalent organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Disperse 32.4 mg (0.24 mmol) terephthalaldehyde (, 56.2 mg (0.16 mmol) 1,3,5-tris(4-aminophenylbenzene) homogeneously in 25 mL (0.43 mol) of absolute ethanol at room temperature Ultrasonic to make it uniformly dispersed, then quickly add 2 mL of 6mol / L acetic acid, and then ultrasonic for 3 minutes, then let stand at room temperature for 24 hours to obtain a spherical covalent organic framework material. The resulting material was added to a Soxhlet extractor and extracted with tetrahydrofuran After reflux washing for 24 hours, centrifugation and washing with ethanol for several times, they were dried in a vacuum oven at 120 °C for 24 hours.

[0027] figure 1 It is a scanning electron micrograph of the spherical covalent organic framework material obtained in Example 1. It can be clearly seen from the figure that the particle size of the spherical covalent organic framework material is uniform, and the size is about 1 μm.

[0028] figure 2 It is a transmission elect...

Embodiment 2

[0033] The spherical covalent organic framework material prepared in Example 1 was used as a chromatographic stationary phase, and filled into an empty stainless steel short column with an inner diameter of 2.1 mm and a length of 50 mm by a dry filling method (stainless steel short columns need to be filled in sequence before filling). Ultrasonic cleaning several times with acetone and ethanol). When loading the column, one end of the empty column is tightened and connected to a vacuum source, and the other end is equipped with a funnel, and the dry spherical covalent organic framework material is slowly added to it, and the column wall is gently tapped from all directions to make the material fall into the column. After the filling is completed, the mobile phase (acetonitrile:water=90:10, v:v) with a flow rate of 0.5 mL / min is used to wash and balance for a long time on the high-performance liquid chromatograph to obtain a tightly packed and uniform chromatographic column. Fi...

Embodiment 3

[0036] In liquid chromatography (HPLC) mode, water was used as mobile phase A, acetonitrile was used as mobile phase B, and the chromatographic conditions were 55% B; the pump flow rate was 0.5 mL / min, and the detection wavelength was 214 nm; the determination of thiourea (10 ppm ) and toluene (50 ppm), ethylbenzene (50 ppm), propylbenzene (50 ppm) single sample and mixed sample on the chromatographic column prepared in embodiment 2 separation situation, its chromatographic separation diagram is as follows Figure 7 shown.

[0037] Depend on Figure 7 It can be seen that the chromatographic column prepared by adopting the spherical covalent organic framework material of the present invention can effectively separate thiourea from toluene, ethylbenzene and propylbenzene.

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Abstract

The invention provides a spherical covalent organic framework material as well as a preparation method and application thereof. The preparation method comprises the following steps: dissolving two covalent organic framework construction elements containing an amino group and an aldehyde group into an organic solvent respectively; after carrying out ultrasonic dispersion, rapidly adding a catalyst;carrying out Schiff base reaction at certain temperature to synthesize the spherical covalent organic framework material. The preparation method has a simple preparation process and the reaction is moderate; the prepared spherical covalent organic framework material has the advantages of controllable size, uniform pore diameter, large specific surface area, good crystal form structure, good chemical stability, good mechanical stability and the like; the spherical covalent organic framework material is used as a chromatography stationary phase and a sample loading amount can be greatly increased; the spherical covalent organic framework material contains a lot of benzene ring structures and has relatively strong hydrophobic performance, so that rapid separation of hydrophobic organic compounds is easy to realize; the spherical covalent organic framework material has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of chromatographic materials, and in particular relates to a spherical covalent organic framework material, a preparation method thereof and its application as a stationary phase in chromatographic separation. Background technique [0002] As a separation technology and method, high performance liquid chromatography has been widely used in the fields of environmental science, food science and biological science, and the continuous development of these fields has also put forward higher requirements for the sensitivity and analysis speed of liquid chromatography. requirements. As the core component of the chromatographic column, the chromatographic stationary phase has a great influence on the separation effect of liquid chromatography, so researching and preparing an efficient chromatographic stationary phase is the key to improving the chromatographic separation efficiency. The spherical stationary phases ...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/281B01J20/22B01J20/30
CPCB01J20/22B01J20/281B01J2220/4812B01J2220/52B01J2220/54C08G83/008
Inventor 林子俺郑琼
Owner FUZHOU UNIV
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