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Bonded three-dimensional covalent organic framework chromatographic column and separation application thereof

A technology of covalent organic framework and chromatographic column, which is applied in the field of bonding three-dimensional covalent organic framework chromatographic column and its separation application, can solve the problem that the application of gas chromatography stationary phase has not yet been reported, and achieve high resolution and high column efficiency separation. Effect

Active Publication Date: 2022-03-18
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the application capabilities of 3D COFs in high performance liquid chromatography have been initially explored, the application of 3D COFs as stationary phases in gas chromatography has not been reported yet.

Method used

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  • Bonded three-dimensional covalent organic framework chromatographic column and separation application thereof
  • Bonded three-dimensional covalent organic framework chromatographic column and separation application thereof
  • Bonded three-dimensional covalent organic framework chromatographic column and separation application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of a three-dimensional covalent organic framework-based capillary gas chromatography column: a bonded JNU-5 capillary column was prepared by an in-situ growth method, which specifically included the following steps:

[0038] (1) Fused silica capillary (10m long × 0.53mm inner diameter) was treated with 1M sodium hydroxide (NaOH) for 2h, 0.1M hydrochloric acid (HCl) for 2h, water until the effluent pH=7.0, and then treated with methanol for 30min.

[0039] (2) Then fill the methanol solution (50%, v / v) of 3-aminopropyltrimethoxysilane (APTES) into the capillary, react overnight at 40°C, rinse with methanol, and use nitrogen flow at 120°C After drying for 2 hours, APTES-modified capillaries were prepared.

[0040] (3) An ethanol solution of tetrakis(4-formylphenyl)-methane (TFPM) (21.6 mg of TFPM dissolved in 3 mL of ethanol) was further filled and reacted at 60° C. for 2 hours. Finally, the capillary column was rinsed with methanol to wash away the residue, ...

Embodiment 2

[0048] Preparation of a three-dimensional covalent organic framework-based capillary gas chromatography column:

[0049] (1) Fused silica capillary (1m, 100m long × 0.53mm inner diameter) was treated with 1M sodium hydroxide (NaOH) for 2h, 0.1M hydrochloric acid (HCl) for 2h, water treatment until the pH of the effluent = 7.0, and then treated with methanol 30min.

[0050] (2) Then fill the methanol solution (50%, v / v) of 3-aminopropyltrimethoxysilane (APTES) into the capillary, react overnight at 40°C, rinse with methanol, and use nitrogen flow at 120°C After drying for 2 hours, APTES-modified capillaries were prepared.

[0051] (3) An ethanol solution of tetrakis(4-formylphenyl)-methane (TFPM) (21.6 mg of TFPM dissolved in 3 mL of ethanol) was further filled and reacted at 60° C. for 2 hours. Finally, the capillary column was flushed with methanol to wash away the residue, and dried at 120 °C with a nitrogen stream for 2 h to obtain TFPM-modified capillaries.

[0052] (4)...

Embodiment 3

[0056] Preparation of a three-dimensional covalent organic framework-based capillary gas chromatography column:

[0057] (1) Fused silica capillary (10m long × 0.075, 0.53mm inner diameter) was treated with 1M sodium hydroxide (NaOH) for 2h, 0.1M hydrochloric acid (HCl) for 2h, water treatment until the effluent pH = 7.0, and then treated with methanol 30min.

[0058] (2) Then fill the methanol solution (50%, v / v) of 3-aminopropyltrimethoxysilane (APTES) into the capillary, react overnight at 40°C, rinse with methanol, and use nitrogen flow at 120°C After drying for 2 hours, APTES-modified capillaries were prepared.

[0059] (3) An ethanol solution of tetrakis(4-formylphenyl)-methane (TFPM) (21.6 mg of TFPM dissolved in 3 mL of ethanol) was further filled and reacted at 60° C. for 2 hours. Finally, the capillary column was flushed with methanol to wash away the residue, and dried at 120 °C with a nitrogen stream for 2 h to obtain TFPM-modified capillaries.

[0060] (4) TFPM...

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Abstract

The invention discloses a bonded three-dimensional covalent organic framework chromatographic column and separation application thereof. An aromatic structure three-dimensional covalent organic framework JNU-5 with high thermal stability and rich amino groups is prepared as a gas chromatography stationary phase, a JNU-5 covalent bonded capillary column is further prepared through an in-situ growth method, and high-performance gas chromatography separation of xylene, dichlorobenzene, propylbenzene and other isomers is successfully achieved. Besides the isomeride, the prepared JNU-5 covalent bonding capillary column also has a good separation effect on common substances such as n-alkanes, benzene homologues, normal alcohols and the like, and the chromatographic column can be repeatedly used for multiple times. The invention not only provides a preparation method of the bonded three-dimensional covalent organic framework-based capillary gas chromatographic column, but also provides a new solution for efficient separation of isomeride.

Description

technical field [0001] The invention belongs to the technical field of chromatographic separation, in particular to a bonded three-dimensional covalent organic framework chromatographic column and its separation application. Background technique [0002] Isomers are often difficult to separate due to their similar chemical properties. For example, p-xylene is an indispensable raw material for polyethylene terephthalate, but o-xylene, m-xylene and ethylbenzene, which have similar particle size, boiling point and polarizability, always exist in p-xylene in the form of impurities. In toluene, the difficulty of its separation is increased. Therefore, it is of great significance to develop new chromatographic stationary phases for the separation of isomers by gas chromatography. Currently, although novel porous materials such as metal-organic frameworks MOFs, metal-organic nanosheets MONs, and porous organic cages have been reported as stationary phases for gas chromatographic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/281B01D15/08C07C7/12C07C15/02C07C15/06C07C15/067C07C15/073C07C15/085C07C9/14C07C9/15C07C9/16C07C29/76C07C31/10C07C31/12C07C31/125
CPCB01J20/226B01J20/281B01D15/08C07C7/12C07C29/76C07C15/02C07C15/06C07C15/067C07C15/073C07C15/085C07C9/14C07C9/15C07C9/16C07C31/10
Inventor 钱海龙杨静王子翰
Owner JIANGNAN UNIV
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