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Beta-ketone enamine chiral COFs (covalent organic frameworks) as well as preparation method and application of bonded capillary gas chromatographic column prepared from same

A technology of covalent organic framework and capillary column, which is applied in the direction of separation methods, chemical instruments and methods, and other chemical processes, and achieves the effects of being conducive to popularization and application, high thermal stability, and saving synthetic raw materials

Active Publication Date: 2019-07-12
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are currently very few reports on the adoption of covalent organic framework materials as novel stationary phases for gas chromatography separations
In particular, β-ketoenamine chiral covalent organic framework materials have never been reported. Therefore, it is worthwhile to explore the preparation methods of new covalent organic framework materials and apply them to the separation of capillary gas chromatography.

Method used

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  • Beta-ketone enamine chiral COFs (covalent organic frameworks) as well as preparation method and application of bonded capillary gas chromatographic column prepared from same
  • Beta-ketone enamine chiral COFs (covalent organic frameworks) as well as preparation method and application of bonded capillary gas chromatographic column prepared from same
  • Beta-ketone enamine chiral COFs (covalent organic frameworks) as well as preparation method and application of bonded capillary gas chromatographic column prepared from same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Synthesis of β-ketoenamine chiral covalent organic framework materials

[0050] The chiral precursors (S)-2,5-bis(2-methylbutoxy)terephthalic acid dihydrazide (22.0 mg, 0.06 mmol), 2,4,6-trihydroxy-triphenylenetricarbaldehyde ( 8.4mg, 0.04mmol), 0.5mL of dioxane and 0.5mL of mesitylene were placed in a pressure-resistant reaction flask, mixed well and then added with 0.1mL of 3M acetic acid solution. The pressure-resistant reaction bottle was replaced with argon three times, and then quickly sealed with a sealing cap, and then placed in an oven preheated to 110° C. for 3 days. After the reaction, cool to room temperature, collect the solid by suction filtration, wash with 1,4-dioxane, tetrahydrofuran and acetone in sequence, and finally place and vacuum dry to obtain 25 mg of orange-yellow solid powder with a yield of 84%.

[0051] The performance measurement results of the hydroxyl functional group-containing β-ketoenamine chiral covalent organic framework ma...

Embodiment 2

[0060] Example 2: Preparation of bonded β-ketoenamine chiral covalent organic framework capillary column

[0061] (1) Pretreatment of capillary column: Quartz capillary column (10m×0.32mm) was washed with 1M sodium hydroxide solution for 2 hours, rinsed with deionized water for 30 minutes, then rinsed with 0.1M hydrochloric acid for 2 hours, and then used Rinse with deionized water until the eluate is neutral, then rinse with methanol for 30 minutes, and then fill the above-treated capillary with a methanol solution of 3-aminopropyltriethoxysilane (APTES) (50%, v / v) , both ends of the capillary were sealed with rubber stoppers and placed in a 40°C water bath overnight, then the residual solvent was flushed out with methanol, and finally, under the protection of nitrogen, the temperature was raised to 120°C and kept for 6 hours to dry the capillary column, thus obtaining the amino-modified Capillary, spare.

[0062] (2) Under ice-water bath conditions, 2,4,6-trihydroxy-pyrylen...

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Abstract

The invention discloses beta-ketone enamine chiral COFs (covalent organic frameworks) as well as a preparation method and an application of a bonded capillary gas chromatographic column prepared fromthe same. The beta-ketone enamine chiral COFs have advantages of high thermal stability, large specific surface area and uniform pore diameter distribution and can be applied to chiral recognition andseparation. The beta-ketone enamine chiral COFs and the bonded beta-ketone enamine chiral COFs capillary column prepared from the same can realize separation of mixed components of straight-chain paraffin and branched paraffin or mixed components of ethylbenzene and styrene and have good application prospects.

Description

technical field [0001] The invention relates to the field of covalent organic framework functional materials, in particular to a preparation method of a β-ketoenamine chiral covalent organic framework material and a bonded capillary gas chromatographic column and its application in capillary gas chromatographic separation . Background technique [0002] Covalent organic frameworks (COFs) are a new type of ordered porous crystalline materials, which are composed of small organic molecules containing light elements (C, H, N, O, B, etc.) linked by covalent bonds. . As one of the typical representatives of new porous materials, covalent organic framework materials have the advantages of light weight, low density, adjustable skeleton size, pore modification, highly ordered permanent porosity and large specific surface area, as well as thermal stability and chemical With good stability and other characteristics, it is widely used in gas storage, heterogeneous catalysis, proton c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/29B01D15/38B01J20/30
CPCB01J20/29B01J20/22B01D15/3833
Inventor 蔡松亮黄晓玲章伟光郑盛润范军
Owner SOUTH CHINA NORMAL UNIVERSITY
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