Two-dimensional metal organic framework nanosheet-based capillary gas chromatography column and preparation method and application thereof

A technology of metal-organic framework and gas chromatography column, which is applied in the field of chromatographic separation, can solve problems such as the limitation of the range of separable target compounds, and achieve the effects of significant production and practical significance, improved separation, and large specific surface area

Pending Publication Date: 2019-03-15
NANJING NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the heterogeneous characteristics of three-dimensional MOFs, such as dispersion and solubility, also face technical difficulties in the actual preparation of capillary columns, and at the same time, they have limitations in the range of target compounds that can be separated.
At present, there are no reports on the application of two-dimensional MOFs materials as stationary phases in gas chromatography.

Method used

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  • Two-dimensional metal organic framework nanosheet-based capillary gas chromatography column and preparation method and application thereof
  • Two-dimensional metal organic framework nanosheet-based capillary gas chromatography column and preparation method and application thereof
  • Two-dimensional metal organic framework nanosheet-based capillary gas chromatography column and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 10.12mg of zirconium tetrachloride, 12.50mg of 1,3,5-tris(4-carboxyphenyl)benzene, 5mL of N,N-dimethylformamide solvent and sonicate for 10 minutes in a 22mL glass upright vial, and then Add 1.11 g of formic acid and 60 μL of water, seal the bottle and cover it, and heat the glass vial in an oven at 120° C. for 48 hours. After cooling down to room temperature, centrifuge at 12,000 rpm to obtain white nanosheets, soak in N, N-dimethylformamide and ethanol solutions in turn and then wash to remove unreacted reagents in the pores of the nanosheets. Finally, the product was vacuum-dried and activated at 80°C for 12 hours, and the prepared nanosheets were labeled as multilayer Zr-BTB-FA.

[0042] Take 10 mg of multilayer Zr-BTB-FA nanosheet powder and disperse it in 3 mL of ethanol solution, ultrasonicate for 30 minutes to obtain a uniform suspension, take 1 mL of the above suspension in a syringe, slowly pour it into the pretreated capillary column, and then Driven by ...

Embodiment 2

[0052] Add 10mg zirconium tetrachloride, 10mg 1,3,5-tris(4-carboxyphenyl)benzene, 3mL N,N-dimethylformamide solvent and sonicate for 10 minutes, then add 600mg Benzoic acid and 250 μL of water, seal the bottle and cover it, and place the glass vial in an oven at 120°C for 48 hours. After cooling down to room temperature, centrifuge at 12,000 rpm to obtain white nanosheets, soak in N, N-dimethylformamide and ethanol solutions in turn and then wash to remove unreacted reagents in the pores of the nanosheets. Finally, the product was vacuum-dried and activated at 80°C for 12 hours, and the prepared nanosheets were labeled as multilayer Zr-BTB-BA.

[0053] The process of the capillary acid-base pretreatment and amino functional pretreatment is the same as above.

[0054] Take 10 mg of multilayer Zr-BTB-BA nanosheet powder and disperse it in 3 mL of ethanol solution, and ultrasonicate for 30 minutes to obtain a uniform suspension, take 1 mL of the above suspension in a syringe, sl...

Embodiment 3

[0057] Add 10.12mg of zirconium tetrachloride, 12.50mg of 1,3,5-tris(4-carboxyphenyl)benzene, 5mL of N,N-dimethylformamide solvent and sonicate for 10 minutes in a 22mL glass upright vial, and then Add 1.11 g of formic acid and 60 μL of water, seal the bottle and cover it, and heat the glass vial in an oven at 120° C. for 48 hours. After cooling down to room temperature, centrifuge at 12,000 rpm to obtain white nanosheets, soak in N,N-dimethylformamide solution for several times and then wash, take 30mL of N,N-dimethylformamide solution containing about 100mg of nanosheets Add 1000 mg p-aminobenzoic acid ligand to a single-necked round-bottom glass flask for post-synthesis modification, and heat the mixture at 120°C for 72 hours under oil bath conditions to fully bond the post-modification ligand p-aminobenzoic acid on the zirconium metal clusters . The solution was cooled to room temperature, centrifuged at 12,000 rpm to obtain white nanosheet solids, soaked in N, N-dimethyl...

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Abstract

The invention discloses a two-dimensional metal organic framework nanosheet-based capillary gas chromatography column and a preparation method and the application thereof. In an organic solvent, by taking zirconium tetrachloride as a metal source, taking 1,3,5-tri(4-carboxyphenyl)benzene as an organic ligand and taking at least one of formic acid, benzoic acid and p-aminobenzoic acid as an acid regulator, the metal and the organic ligand are self-assembled to form a nanosheet which is activated in vacuum, and then the inner wall of a capillary column is coated with the nanosheet to prepare thecapillary gas chromatography column, so that a substituted benzene isomer mixture can be efficiently separated to show unique para-isomer selectivity, which greatly improves the separation degree bycompared with a commercial column meta/para-substituted benzene structural isomer; baseline separation can be achieved for mixed straight-chain alkane and mixed benzene series; in addition, the nanosheet of a multilayer stack structure is an important reason for efficient separation of the isomers. The capillary gas chromatography column disclosed by the invention has excellent properties of wideapplication range, high selectivity, high thermal stability and the like.

Description

technical field [0001] The invention relates to the technical field of chromatographic separation applications, in particular to a capillary gas chromatography column based on two-dimensional metal-organic framework nanosheets and a preparation method and application thereof. Background technique [0002] Metal-organic frameworks (Meatal-Organic Frameworks, MOFs) are inorganic-organic hybrid porous materials formed by the self-assembly of metal ions or metal clusters and organic ligands through coordination bonds. Compared with traditional porous materials, due to the introduction of organic Ligands can control the pore size and pore chemical environment by regulating the type and size of the ligands; its unique properties have a wide range of applications in molecular catalysis, gas separation, fluorescence sensing, energy storage, etc. In recent years, two-dimensional MOFs nanosheets, also known as inorganic metal-organic layers (MOL) or metal-organic surfaces (MOS), are s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/282B01J20/32G01N30/60B01D15/22
CPCB01D15/22B01J20/282B01J20/32B01J2220/84G01N30/60
Inventor 古志远陶泽榕
Owner NANJING NORMAL UNIVERSITY
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