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A method for immobilizing covalent organic framework materials and its application

A covalent organic framework and coating technology, applied in the field of chromatographic columns, achieves the effects of less sample consumption, simple process and low cost

Active Publication Date: 2017-01-18
武汉长林医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boronic acid group in 1,4-benzenediboronic acid reacts with the phthalic dihydroxyl group in 2,3,6,7,10,11-hexahydroxytriphenyl to form O-B-O in the COF-5 framework. The modification of the framework material to the surface of the matrix is ​​an important reason for limiting its application in extraction, chromatographic separation, etc.

Method used

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  • A method for immobilizing covalent organic framework materials and its application
  • A method for immobilizing covalent organic framework materials and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A 31 cm long quartz capillary (50 μm i.d.×375 μm o.d.) was rinsed with methanol for 2 h and dried with nitrogen; at room temperature, the pre-oxidized dopamine aqueous solution (concentration 2 mg / mL, pH 8.5) was continuously passed into the quartz capillary for 10 h, Then rinse with pure water and dry with nitrogen to obtain a capillary with a uniform and stable polydopamine coating on the inner wall; Trimethylbenzene / 1,4-dioxane (v / v, 1:1) mixed reaction solution (concentrations of 1,4-benzenediboronic acid and 2,3,6,7,10,11-hexahydroxytriphenyl 0.75mM, 0.5mM respectively) into the quartz capillary with polydopamine coating on the inner wall for 5min, then seal both ends of the quartz capillary, place it in an ultrasonic instrument for ultrasonic treatment for 1h, heat the reaction in an oil bath at 100°C for 20h, and rinse with methanol for 8h , blown dry with nitrogen to obtain a quartz capillary with a COF-5 coating on the inner wall.

Embodiment 2

[0031] Rinse a 60cm-long polyetheretherketone capillary (PEEK tube) (50μm i.d.×360μm o.d.) with methanol for 2h, and dry it with nitrogen; Continue to pass through the PEEK tube for 8 hours, rinse with pure water, and blow dry with nitrogen to obtain a PEEK tube with a uniform and stable polydopamine coating on the inner wall; mix 1,4-benzenediboronic acid and 2,3,6,7,10,11 -Mesitylene / 1,4-dioxane (v / v, 1:1) mixed reaction solution of hexahydroxytriphenyl (1,4-benzenediboronic acid and 2,3,6,7,10,11 -The concentration of hexahydroxytriphenyl is 0.75mM, 0.75mM respectively) into the PEEK tube with polydopamine coating on the inner wall for 3min, then seal the two ends of the PEEK tube, place it in an ultrasonic instrument for ultrasonic treatment for 1.5h, and 110°C oil The reaction was heated in the bath for 30 hours, rinsed with methanol for 8 hours, and dried with nitrogen to obtain a PEEK tube with a COF-5 coating on the inner wall.

Embodiment 3

[0033] Rinse a 15cm-long polytetrafluoroethylene capillary (PTFE tube) (200μm i.d.×300μm o.d.) with methanol for 2h, and dry it with nitrogen; Continue to pass through the polytetrafluoroethylene capillary for 12 hours, rinse with pure water, and blow dry with nitrogen to obtain a polytetrafluoroethylene capillary with a uniform and stable polydopamine coating on the inner wall; mix 1,4-benzenediboronic acid and 2,3, 6,7,10,11-hexahydroxytriphenyl mesitylene / 1,4-dioxane (v / v, 1:1) mixed reaction solution (1,4-benzenediboronic acid and 2,3, The concentration of 6,7,10,11-hexahydroxytriphenyl is 0.75mM, 0.25mM respectively) into the polytetrafluoroethylene capillary with polydopamine coating on the inner wall for 1min, and then the two ends of the polytetrafluoroethylene capillary are sealed , placed in a sonicator for ultrasonic treatment for 2 hours, heated in an oil bath at 120°C for 10 hours, rinsed with methanol for 8 hours, and dried with nitrogen to obtain a polytetrafluo...

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Abstract

The invention provides a polydopamine-assisted method for fixing a covalent organic framework material, and an application thereof. First, a dopamine water solution is prepared; the pH value is regulated to weakly alkaline, and an oxidation treatment is carried out; a carrier with a clean surface is added under room temperature, and the surface of the carrier is modified with a polydopamine coating; the modified carrier is placed in a mixed solution of binary boric acid and 2,3,6,7,10,11-hexahydroxyl triphenyl; one boric acid group is subjected to a reaction with o-phenyldihydroxyl site provided by the polydopamine coating, and another boric acid group participates in COFs framework formation, such that COFs crystal is formed on site and fixed on the surface of the carrier. The preparation process provided by the invention is simple. With the wide adaptability of polydopamine modification, synthesis and fixing of COFs on the surfaces of various substrates can be realized. The method is applied in preparing open tubular electrochromatography columns. Prepared open tubular column based on COF-5 has good separation effect upon electrically neutral benzene-series substances in an electrochromatography mode.

Description

technical field [0001] The invention belongs to the technical field of chromatographic columns, and relates to a method and application of polydopamine-assisted fixation of covalent organic framework materials. Background technique [0002] Covalent organic frameworks are a class of crystalline microporous polymers in which organic ligands are linked by covalent bonds. Covalent organic frameworks have been widely used in gas storage due to their large specific surface area, excellent pore properties, low framework density, high thermal and chemical stability, controllable physical and chemical properties, and easy functionalization. , catalysis, optoelectronic materials and other fields. The covalent organic framework material COF-5 is a two-dimensional crystal material formed by the condensation reaction of 1,4-benzenediboronic acid and 2,3,6,7,10,11-hexahydroxytriphenyl. The boronic acid group in 1,4-benzenediboronic acid reacts with the phthalic dihydroxyl group in 2,3,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22
Inventor 陈子林包涛
Owner 武汉长林医药科技有限公司
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