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A metal-organic framework polymer-coated silica gel material, its preparation method and application
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A metal organic framework and polymer technology, applied in the field of chromatographic separation, can solve the problems of poor packing repeatability, high column pressure, limited separation efficiency, etc., and achieve the effects of high mechanical strength, large specific surface area, and cheap and easy-to-obtain raw materials
Active Publication Date: 2021-09-21
JIANGSU ALPHA PHARM CO LTD
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[0005] The purpose of the present invention is to provide a method for preparing a metal-organic framework polymer-coated silica gel material on the basis of the prior art. Using silica gel microspheres as a substrate, 3-aminopropyltriethoxy The base silane is bonded to the surface of silica gel microspheres, and then the chiral metal-organic framework polymer is coated on the silica gel surface by self-assembly, thereby forming a metal-organic framework polymer-coated silica gel material, which is used as a chiral chromatography The stationary phase solves the problems of poor filling repeatability, high column pressure after filling, and limited separation efficiency when pure chiral MOFs are used as liquid chromatography stationary phases
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Embodiment 1
[0046] According to the following steps, MOFs-coated silica gel composite chiral chromatography stationary phase was synthesized and used for the resolution of chiral enantiomers in liquid chromatography. The specific steps are:
[0047] (1) Take 10g of silica gel microspheres (10μm, ), put it into a clean reaction vessel, add NaOH solution (pH=13), ultrasonicate for 30 minutes at 20-30°C, filter with suction, separate the above-mentioned silica gel microspheres, and then mix with dilute hydrochloric acid to adjust the pH value 5-6; the silica gel microspheres were separated again, washed with water until the pH value was 6.5-7.5, and dried;
[0048] (2) Place the above-mentioned treated silica gel microspheres in a clean reaction vessel with a reflux device, add 100 mL of toluene, then add 12 g of 3-aminopropyltriethoxysilane, and heat to 110 ° C for 24 hours;
[0049] (3) After the product obtained in step (2) is cleaned and suction-filtered, fully cleaned with methanol, d...
Embodiment 2
[0054] According to the following steps, MOFs-coated silica gel composite chiral chromatography stationary phase was synthesized and used for the resolution of chiral enantiomers in liquid chromatography. The specific steps are:
[0055] (1) Get 10g of silica gel microspheres (12μm, ), put it into a clean reaction vessel, add potassium hydroxide solution (pH=13), ultrasonicate for 30 minutes under the condition of 20-30°C, and filter with suction to separate the above-mentioned silica gel microspheres, and then mix them with acetic acid to adjust the pH The value is 5-6; the silica gel microspheres are separated again, then washed with water until the pH value is 6.5-7.5, and dried;
[0056] (2) Place the above-mentioned treated silica gel microspheres in a clean reaction vessel with a reflux device, add 120 mL of ethylbenzene, then add 20 g of 3-aminopropyltriethoxysilane, and heat to 137 ° C for 24 hours;
[0057] (3) After the product obtained in step (2) is cleaned and s...
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Abstract
The invention relates to a metal-organic framework polymer-coated silica gel material, a preparation method and application thereof. The invention uses silica gel microspheres as the substrate, bonds 3-aminopropyltriethoxysilane to the surface of the silica gel microspheres by chemical bonding, and then coats the chiral metal-organic framework polymer by self-assembly On the surface of silica gel, a metal-organic framework polymer-coated silica gel material is formed. Using this material as a chiral chromatography stationary phase combines the advantages of high selectivity and large specific surface area of MOFs with high mechanical strength and uniform particle size of silica gel microspheres. It can obtain good chromatographic column filling repeatability and excellent chromatographic separation ability, and can be applied in the field of chromatographic separation.
Description
technical field [0001] The invention belongs to the technical field of chromatographic separation, and in particular relates to a metal-organic framework polymer-coated silica gel material, a preparation method thereof and an application as a chiral chromatographic stationary phase. Background technique [0002] Metal-organic frameworks (MOFs) have attracted much attention because of their uniform and controllable pore size, large specific surface area, selective adsorption capacity, and good heat resistance. In the field of chromatographic separation, a variety of MOFs materials have been used in gas chromatography, liquid chromatography, capillary liquid chromatography, capillary electrochromatography and other chromatographic separation modes, and have shown outstanding separation ability in the separation of small molecular compounds . [0003] In order to meet people's separation requirements for chiral compounds, more and more chiral chromatography stationary phases h...
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