Preparation method of covalent organic framework composite microspheres with core-shell structures

A technology of covalent organic framework and composite microspheres, which is applied in the field of covalent bond connection preparation, can solve problems such as methods that have not been reported yet, achieve good mechanical stability, reduce height, and the effect of cheap and easy-to-obtain raw materials

Inactive Publication Date: 2017-09-19
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the preparation of covalent organic framework composite microspheres with core-shell structure has not been reported

Method used

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  • Preparation method of covalent organic framework composite microspheres with core-shell structures
  • Preparation method of covalent organic framework composite microspheres with core-shell structures
  • Preparation method of covalent organic framework composite microspheres with core-shell structures

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation of the covalent organic framework composite microsphere of core-shell structure, it comprises the steps:

[0032] 80 mg of silica microspheres, 48 ​​mg of trimesaldehyde, and 82.9 mg of benzidine were uniformly dispersed in 60 mL of dimethyl sulfoxide solvent, ultrasonically mixed for 25 min, and 2 mL of acetic acid was added, and then ultrasonically maintained for 30 min to obtain the obtained Covalent organic framework composite silicon spheres with core-shell structure. Wash with tetrahydrofuran and ethanol several times by centrifugation, and dry the obtained material at 150 °C.

[0033] figure 1 Middle A is the transmission electron microscope image of the silica microspheres in Example 1. It can be clearly seen from the figure that the average particle size of the silica bare spheres with smooth surface morphology is about 2 μm. figure 1 Middle B is the transmission electron microscope image of the covalent organic framework composite microsphere...

Embodiment 2

[0038] The covalent organic framework composite microspheres with the core-shell structure prepared in Example 1 were 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. Sonicated several times with acetone, secondary water and methanol in sequence. When loading the column, one end of the column is connected to a vacuum source, and the other end is equipped with a funnel, and the dry core-shell structure covalent organic framework composite microspheres are slowly fed into it, and the column wall is gently tapped to make the microspheres fall into the column. middle. Ethanol can be added dropwise when filling the microspheres to make them more compact. After the filling is completed, the mobile phase (water:acetonitrile=10:90, v:v) with a flow rate of 0.1 mL / min is used to wash and balance for a long time on the high-performance liquid chromatograph to...

Embodiment 3

[0040] In liquid chromatography (HPLC) mode, acetonitrile:water solution (5:95, v / v) was used as mobile phase A, water:acetonitrile solution (5:95, v / v) was used as mobile phase B, and the chromatographic condition was 55 %B; pump flow rate 0.2 mL / min, detection wavelength 214 nm; mixture of thiourea (20ppm), benzene (100 ppm), toluene (100 ppm), ethylbenzene (100 ppm), naphthalene (100 ppm) Realize efficient and selective separation on the chromatographic column that embodiment 2 makes, its chromatographic separation figure is as follows Figure 6 As shown, the peaks in the chromatogram are 1: thiourea, 2: benzene, 3: toluene, 4: ethylbenzene, 5: naphthalene.

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Abstract

The invention relates to a preparation method of covalent organic framework composite microspheres with core-shell structures. The method comprises the following steps: dissolving silicon dioxide microspheres, a first construction element and a second construction element in an organic solvent; and after adding a catalyst, rapidly synthesizing into the composite microspheres with core-shell structures at a certain temperature. In a preparation process, reaction conditions are gentle, the method is simple, and the yield is high; the prepared covalent organic framework composite microspheres have the advantages of good core-shell morphology, high specific surface area, ordered pore structures, good mechanical stability, thermal stability, chemical stability and the like, if the microspheres are used as a chromatographic stationary phase, the chromatographic mass transfer resistance can be reduced effectively, the theoretical plate height is improved, and finally, column efficiency and degree of separation are improved; and if the microspheres are used as solid-phase extracting filler, the enrichment effect can be improved remarkably. The covalent organic framework composite microspheres with core-shell structures have good application prospects in the aspect of separation and enrichment of small organic molecules.

Description

technical field [0001] The invention relates to the field of covalent bond connection preparation methods, in particular to a preparation method of covalent organic framework composite microspheres with a core-shell structure. Background technique [0002] With the continuous emergence and development of new research fields such as life sciences, environmental sciences, food sciences, and medical sciences, the separation and analysis of complex systems with high resolution, high selectivity, high precision, high sensitivity, and high throughput has been proposed. higher requirement. As a powerful means of separation and analysis, chromatography technology has always promoted the development of the above-mentioned related disciplines. As the core of chromatographic technology, chromatographic stationary phase has always been the foreword and hot spot in the field of chromatographic research. Traditional chemical bonded phase chromatography mostly uses silica gel as a carrie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B01J20/22B01J20/30B01D53/02B01D15/26B01D15/34
CPCB01D15/265B01D15/34B01D53/02B01J13/02B01J20/10B01J20/22B01J2220/46
Inventor 林子俺高超鸿郑琼雷智显陈磊贺燕庭
Owner FUZHOU UNIV
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