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Method for preparing liquid chromatography monolithic column based on metal-organic frameworks

A metal-organic framework and liquid chromatography technology, which is applied in the field of polymer material preparation and chromatography application, can solve the problems of inappropriate reversed-phase system, poor reproducibility, time-consuming and labor-intensive, etc. Good stability and permeability

Active Publication Date: 2012-08-15
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a new class of separation and purification materials, MOFs not only expand the types of separation media, but also solve some important problems in separation science and related technologies. However, the research on using MOFs materials as chromatographic stationary phases is still in its infancy. The liquid chromatography stationary phase adopts the traditional filling mode, which requires more MOFs materials. Before filling, the materials need to be ground and sieved. Applicable to problems such as reversed phase systems

Method used

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  • Method for preparing liquid chromatography monolithic column based on metal-organic frameworks
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  • Method for preparing liquid chromatography monolithic column based on metal-organic frameworks

Examples

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Effect test

Embodiment 1

[0027] A method for preparing a liquid chromatography monolithic column based on a metal organic framework material includes the following steps:

[0028] 1) Preparation of stainless steel column tube:

[0029] The stainless steel column tube and column cap are soaked in ethanol, ultrasonically cleaned for 30 minutes, and then air-dried at room temperature; take two pieces of about 2cm silica gel tube, heat to soften them, and put them into the two ends of the column tube while they are softened. Fix the silicone tube and the column tube with the membrane, mark the filling direction, and seal the bottom of the column tube with tape to prepare for the filling of the whole column mixture;

[0030] 2) Preparation of MOFs suspension:

[0031] Add 2mmol of chromium nitrate nonahydrate, 2mmol of terephthalic acid, 2mmol of 40% hydrofluoric acid aqueous solution, 9.6mL of water to the reaction kettle, stir it evenly, seal it, and heat it in a blast drying oven at 220℃. After hours, the reac...

Embodiment 2

[0039] A method for preparing a liquid chromatography monolithic column based on a metal organic framework material includes the following steps:

[0040] 1) Same as Example 1;

[0041] 2) Preparation of MOFs suspension:

[0042] Add 1mmol of aluminum chloride hexahydrate, 1.67mmol of 2-aminoterephthalic acid, 15mL of N,N-dimethylformamide to the reaction kettle in sequence, stir well and seal, and heat in a 130℃ blast drying oven for 3 day. After the reaction kettle was cooled, it was centrifuged to obtain a light yellow solid, which was washed three times with N,N-dimethylformamide and once with ethanol. The obtained solid was vacuum dried at 150°C for 12 hours. Disperse 50 mg of the solid powder in 5 mL of N,N-dimethylformamide, and ultrasonically obtain a uniform MOFs suspension;

[0043] 3) Same as Example 1;

[0044] 4) Same as Example 1;

[0045] 5) Same as Example 1.

Embodiment 3

[0047] A method for preparing a liquid chromatography monolithic column based on a metal organic framework material includes the following steps:

[0048] 1) Same as Example 1;

[0049] 2) Preparation of MOFs suspension:

[0050] Add 5mmol of iron powder, 3.35mmol of trimesic acid, 10mmol of 40% hydrofluoric acid aqueous solution, 3mmol of 65% concentrated nitric acid, 25mL of water to the reaction kettle in turn, stir well, seal, and place at 150℃ for air drying Heat in the box for 12 hours. After the reaction kettle is cooled, it is washed with water and centrifuged to obtain a light orange solid. The solid was soaked in hot water at 80°C for 5 hours, and then soaked in hot ethanol at 60°C for 3 hours until the filtrate was colorless to obtain a purified MOF material. The obtained solid was vacuum dried at 150°C for 12 hours, and 50 mg of the solid powder was taken Disperse in 5mL N,N-dimethylformamide and ultrasonically obtain a uniform MOFs suspension;

[0051] 3) Same as Exampl...

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Abstract

A method for preparing a liquid chromatography monolithic column based on metal-organic frameworks. The porous MOFs (metal-organic frameworks) and organic polymer monolithic materials are used as separation media, and the stainless steel liquid chromatography monolithic column is prepared by means of in-situ polymerization. Firstly, the MOFs are prepared by means of self-assembly reaction of different metal centers and organic ligands, activated at a certain temperature and ultrasonically dispersed in solvents to obtain suspending liquid of the MOFs. Secondly, the suspending liquid is added into precursor solution, and the doped monolithic column is prepared by means of thermal-initiation polymerization. Thirdly, pore-foaming agents in the MOFs monolithic column are flushed at a high flow rate by a liquid high-pressure pump, and then the liquid chromatography monolithic column can be prepared. The method has the advantages that the superiority of double separation of the MOFs and the monolithic column is integrated, the shortcomings of large backpressure, high consumption of the separation media, complicated filling and the like of a traditional packed column are overcome, the types of the MOFs serving as separation media are expanded, and large-scale popularization and application are facilitated.

Description

Technical field [0001] The invention relates to the technical field of polymer material preparation and chromatographic application, in particular to a method for preparing a liquid chromatography monolithic column based on a metal organic framework material. Background technique [0002] Monolithic column, also known as continuous bed, no plunger column, is a new type of separation medium that emerged rapidly in the 1990s. It is different from the packing mode of traditional chromatographic columns, but under certain conditions , Through the reaction in the column to form a porous continuous whole, at the same time it has the advantages of fast separation of non-porous packing and membrane, high capacity and low back pressure of high performance liquid chromatography porous packing. [0003] Metal-Organic Frameworks (MOFs) materials, also known as coordination polymers (Coordination Polymers) materials, are porous materials formed by self-assembly of metal ions and organic ligands...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/20B01D15/22
Inventor 严秀平付艳艳王荷芳
Owner NANKAI UNIV
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