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Metal-organic framework complex chromatographic material, and preparation method and applications thereof

A metal-organic framework and chromatographic material technology, applied in the field of metal-organic framework complex chromatographic materials and their preparation

Inactive Publication Date: 2018-08-07
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the purposeful design of metal-organic framework complex chromatographic material structure to improve its specificity in the process of enrichment and separation.

Method used

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  • Metal-organic framework complex chromatographic material, and preparation method and applications thereof
  • Metal-organic framework complex chromatographic material, and preparation method and applications thereof
  • Metal-organic framework complex chromatographic material, and preparation method and applications thereof

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preparation example Construction

[0021] The invention provides a method for preparing a metal-organic framework complex chromatographic material, comprising: in the presence of an initiator, sulfamide SFA, three (2,3-epoxypropyl) isocyanate TEPIC, MOF-5-NH 2 Copolymerization in the first organic solvent to prepare a novel metal-organic framework complex chromatographic material MOF-5-NH 2 @P(TEPIC-co-SFA); where MOF-5-NH 2 For aminated MOF-5.

[0022] In the present invention, the amount of each raw material can be selected within a wide range. In order to make the prepared chromatographic material have more excellent enrichment and separation effects on compounds containing disulfide bonds, preferably, SFA, TEPIC, MOF-5 -NH 2 The weight ratio of SFA and initiator is 1:1-10:0.5-10; more preferably, the weight ratio of SFA and initiator is 1:0.01-0.5; further preferably, the weight ratio of SFA and first organic solvent is 1:200- 600.

[0023] In the present invention, the conditions of the copolymerizatio...

preparation example 1

[0039] 0.8925g of zinc nitrate hexahydrate, 0.2717g of 2-aminoterephthalic acid and 50mL of DMF (dimethylformamide) were placed in a 50mL beaker, magnetically stirred and ultrasonically degassed to obtain a uniformly mixed solution, and the solution was Transfer to a 150mL three-necked flask, and react in an oil bath at 140°C under high-speed stirring for 2h; after the reaction, wash with DMF and ethanol three times in succession, and dry in an oven at 75°C for 12h to obtain MOF-5-NH 2 .

Embodiment 1

[0041] 1) Dissolve 0.49g of aminated MOF-5 in 25mL of DMSO, then add 0.49g of cross-linking agent TEPIC, 0.10g of sulfamide, and 0.025g of sodium hydroxide in sequence, vortex and oscillate to fully dissolve, and ultrasonically degas at 10.0 min to obtain a homogeneously mixed polymerization solution, and continue to react in an oven at 75°C for 12 hours to obtain block material M1.

[0042] 2) The bulk material M1 is washed continuously with methanol for 3 times, and the solvent DMSO and unreacted substances are washed away to obtain the bulk material M2.

[0043] 3) Put the bulk material M2 in a vacuum drying oven and dry it at 50°C for 12 hours to obtain a metal-organic framework complex chromatographic material, that is, the copolymer MOF-5-NH 2 @P(TEPIC-co-SFA).

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Abstract

The invention discloses a metal-organic framework complex chromatographic material, and a preparation method and applications thereof. The preparation method comprises following steps: in the presenceof an initiator, sulfamide SFA, tri(2,3-glycidyl) isocyanate TEPIC, and MOF-5-NH2 are subjected to copolymerization reaction in a first organic solvent so as to obtain the novel metal-organic framework complex chromatographic material MOF-5-NH2@P(TEPIC-co-SFA), wherein MOF-5-NH2 is aminated MOF-5. The metal-organic framework complex chromatographic material is high in heat stability, is convenient to store, and is excellent in dispersion performance, and possesses excellent enrichment and separation capacity on compounds containing disulfide bonds, so that the metal-organic framework complexchromatographic material can be used for separation and enrichment of compounds containing disulfide bonds; the preparation method is simple; and the raw materials are easily available.

Description

technical field [0001] The invention relates to sulfur-loving materials, in particular to a metal-organic framework complex chromatographic material and its preparation method and application. Background technique [0002] Metal organic framework complexes (Metal Organic Frameworks (MOFs), also known as coordination polymers) are transition metal ions or metal clusters and organic ligands obtained by molecular self-assembly methods with a certain size and shape with a cavity. Bit polymers are a new class of porous materials. In the 1990s, the research group of Professor Yaghi in the United States pioneered the application of multi-dentate carboxyl organic ligands and metal ion bridges to synthesize MOFs. Among them, the most classic representative structure is MOF-5, and the specific surface area of ​​MOF-5 is as high as 2500-3000m 2 / g, high thermal stability (see "Science" 2003, No. 300, pages 16-19), compared with traditional porous materials (such as zeolite molecular s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/285B01J20/30B01D15/38
CPCB01D15/3804B01J20/226B01J20/285
Inventor 刘云春闻琪娟
Owner ANHUI NORMAL UNIV