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Novel capillary gas chromatographic column based on MOFs and preparation method thereof

A gas chromatographic column and capillary technology, applied in the field of chromatographic applications, can solve the problems of limited separation efficiency, time-consuming and laborious, etc., achieve novel topology, overcome cumbersome preparation, and adjust the size

Inactive Publication Date: 2010-05-12
北京安星达环保技术发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, MOFs are mostly used as chromatographic stationary phases in the form of packed columns, which require more MOFs materials. When filling, grinding, sieving, and filling are required. In addition, plungers need to be made. limits

Method used

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  • Novel capillary gas chromatographic column based on MOFs and preparation method thereof
  • Novel capillary gas chromatographic column based on MOFs and preparation method thereof
  • Novel capillary gas chromatographic column based on MOFs and preparation method thereof

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preparation example Construction

[0035] In the present invention, in order to prepare the novel capillary gas chromatography column based on MOFs, the present invention also provides a preparation method of the novel capillary gas chromatography column based on MOFs. The method uses MOFs material as the stationary phase of gas chromatography, and adopts the method of dynamic coating to prepare capillary gas chromatography, which specifically includes the following steps:

[0036] The first step, synthesizing solid particles of MOFs materials, and preparing a suspension of the synthesized MOFs materials;

[0037] In the present invention, the self-assembly reaction of metal and organic ligands is firstly used to generate MOFs materials with super large specific surface area. Then, the solvent and residual reactants in the pores of the MOFs material are washed away by an organic solvent, and the MOFs material is activated at a predetermined temperature. Finally, the powder of the MOFs material is taken to form...

Embodiment 1

[0054] In the reactor, add 20 mL of water, 2 mmol of chromium nitrate, and 1 to 3 mmol of terephthalic acid, and seal it. Heat the reactor at 220 ° C for 12 hours. After filtering, green particles are obtained, and sequentially use toluene, N, N-di Soak in methylformamide and dichloromethane for 1 hour, then filter again, and dry the obtained solid in vacuum at 150°C for 24 hours. Take 20 mg of the solid powder and disperse it in 10 mL of acetone to obtain a uniform suspension; pour the above uniform suspension into In the pretreated capillary, ensure that the length of the liquid column is 3-5m. Under the pressure of 10-50kPa, make the liquid column in the capillary at a rate of 10cm min -1 Moving at a constant speed until all the liquid flows out of the capillary. In order to ensure that the liquid column at the end of the capillary can still move at this speed, it is necessary to connect a 5m-long empty capillary; after coating, continue to pass nitrogen for 2 hours to dry ...

Embodiment 2

[0057] In the reaction kettle, add 20mL N,N-dimethylformamide, 2mmol zinc nitrate, 1mmol terephthalic acid, and seal it. The autoclave was heated at 120°C for 24 hours. After filtration, colorless particles were obtained, which were soaked in N,N-dimethylformamide and dichloromethane for 1 hour in sequence, and then filtered again, and the obtained solid was vacuum-dried at 150° C. for 24 hours. Take 20 mg of the solid powder and disperse it in 10 mL of acetone to obtain a uniform suspension; pour the above uniform suspension into a pretreated capillary to ensure that the length of the liquid column is 3 to 5 m. Under the pressure condition of 10 ~ 50kPa, make the liquid column in the capillary at 10cm min -1 Moving at a constant speed until all the liquid flows out of the capillary. In order to ensure that the liquid column at the end of the capillary can still move at this speed, it is necessary to connect a 5m-long empty capillary; after coating, continue to pass nitrogen...

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Abstract

The invention discloses a novel capillary gas chromatographic column based on metal-organic frameworks (MOFs) and a preparation method thereof. The MOFs have huge specific surface areas (generally 2000-5000m2 / g), novel topological structures and good thermal stability. Compared with the traditional silicone-based materials, the MOFs have diverse structures and adjustable pore canal sizes. The capillary gas chromatographic column provided by the invention has the capability of rapidly and efficiently separating isomers. The invention also provides the preparation method of the capillary gas chromatographic column. The method adopts the dynamic coating mode to prepare the capillary gas chromatographic column based on MOFs, thus overcoming the defect of complex preparation of the current packed columns based on MOFs and greatly saving the demanded MOFs; therefore, the method is favorable to large-scale popularization and application.

Description

technical field [0001] The invention relates to the technical field of chromatographic applications, in particular to a novel capillary gas chromatography column based on metal-organic framework (Metal-Organic Frameworks, MOFs) materials and a preparation method thereof. Background technique [0002] MOFs are a class of porous materials based on the interaction between metals and organic ligands. The formation of such substances is usually a self-assembly process of metals and organic ligands. Metals provide empty orbitals as electron acceptors, and atoms such as nitrogen and oxygen in the ligands provide electron pairs as electron donors. Different from traditional molecular sieve materials (porous aluminosilicate, phosphate, arsenate, germanate and other inorganic porous framework materials), this type of material has a three-dimensional structure formed by the interaction between metal and organic ligands. After removing the solvent, the framework can still keep from col...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCB01J20/281B01J20/226B01J20/282B01J2220/86
Inventor 严秀平古志远王荷芳
Owner 北京安星达环保技术发展有限公司
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