Synthesis of novel covalent organic framework material and application thereof in metal ion recognition and dye adsorption

A covalent organic framework and a new technology, applied in the field of material chemistry, can solve the problems of toxic dyes, water system and human health hazards, and achieve the effects of high selectivity and sensitivity, simple synthesis method and high efficiency

Active Publication Date: 2019-11-22
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The treatment of dye-contaminated wastewater has become one of the most serious environmental problems b

Method used

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  • Synthesis of novel covalent organic framework material and application thereof in metal ion recognition and dye adsorption
  • Synthesis of novel covalent organic framework material and application thereof in metal ion recognition and dye adsorption
  • Synthesis of novel covalent organic framework material and application thereof in metal ion recognition and dye adsorption

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 0.0857g of 2,4,6-tri-(4-bromo-phenyl)-[1,3,5]-triazide and 0.1069g of pyrene-2,7-bis(4,4,5 ,5-Tetramethyl-[1,3,2]dioxaborolane), added to 10mL of N,N dimethylformamide, and ultrasonicated for 10 minutes, so that the monomer was evenly dispersed in N, In N-dimethylformamide, after degassing through three cycles, add 2.5mL saturated potassium carbonate aqueous solution and 0.0179g tetrakistriphenylphosphine palladium into the Shrek tube, vacuumize and fill with nitrogen, degas through three cycles, and use argon Purge, seal the tube, place in an oil bath at 110°C and stir for 24 hours, collect the precipitate by suction filtration, wash thoroughly with water, N,N-dimethylformamide, methanol, ethanol and dichloromethane, and wash with Tetrahydrofuran and methanol were used as solvents to pass Soxhlet extracts through reflux washing for 24 h and dry in vacuo to prepare covalent organic framework (COF) materials.

[0031] The structure morphology of the COF material t...

Embodiment 2

[0051] Weigh 0.0857g of 2,4,6-tri-(4-bromo-phenyl)-[1,3,5]-triazide and 0.1069g of pyrene-2,7-bis(4,4,5 ,5-Tetramethyl-[1,3,2]dioxaborolane), added to 20mL of 1,4-dioxane, and ultrasonicated for 10 minutes to disperse the monomer evenly in 1, In 4-dioxane, after degassing through three cycles, add 5mL saturated cesium carbonate aqueous solution and 0.0179g tetrakistriphenylphosphine palladium into the Shrek tube, vacuumize and fill with nitrogen, degas through three cycles, blow with argon Sweep, seal the tube, stir in an oil bath at 90°C for 21 hours, collect the precipitate by suction filtration, wash thoroughly with water, N,N-dimethylformamide, methanol, ethanol and dichloromethane, wash with tetrahydrofuran The covalent organic framework (COF) material was prepared by refluxing the Soxhlet extract with methanol as a solvent for 24 h and drying in vacuo.

Embodiment 3

[0053] Weigh 0.0857g of 2,4,6-tri-(4-bromo-phenyl)-[1,3,5]-triazide and 0.1069g of pyrene-2,7-bis(4,4,5 ,5-Tetramethyl-[1,3,2]dioxaborolane), added to 30mL of toluene, and ultrasonicated for 10 minutes, so that the monomer was evenly dispersed in toluene, after three cycles of degassing , add 7.5mL saturated aqueous sodium carbonate solution and 0.0179g tetrakistriphenylphosphine palladium into the Shrek tube, vacuumize and fill with nitrogen, degas through three cycles, blow with argon, seal the tube, and place it in an oil bath at a temperature of 120°C Stir in the pot for 18 hours, collect the precipitate by suction filtration, wash thoroughly with water, N,N-dimethylformamide, methanol, ethanol and dichloromethane, and use tetrahydrofuran and methanol as solvents to wash back through the Soxhlet extract for 24 hours , and dried in vacuum to prepare covalent organic framework (COF) materials.

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Abstract

The invention discloses preparation of a covalent organic framework material and an application thereof in metal ion recognition and dye adsorption. The preparation method comprises the following steps: adding 2,4,6-tri-(4-bromo-phenyl)-[1,3,5]-triazinide and pyrene-2,7-bis(4,4,5,5-tetramethyl-[1,3,2]dioxaboropentane) into an organic solvent, carrying out ultrasonic treatment, and carrying out cyclic degassing; and adding a palladium catalyst and an alkaline solution, adding the raw materials into a Schleck tube, vacuumizing the tube and introducing nitrogen, performing circular degassing forthree times, purging the tube with argon, sealing the tube, performing stirring reaction, carrying out suction filtration, washing the product, and carrying out vacuum drying to obtain the covalent organic framework material. The synthesis method is simple to operate and high in yield; the synthesized covalent organic framework material is high in sensitivity and good in selectivity and has good application performance. Metal ions can be quickly and sensitively recognized, a good adsorption effect on the neutral red dye is achieved, and a large amount of the neutral red dye can be adsorbed inan aqueous solution within a short time.

Description

technical field [0001] The invention belongs to the technical field of material chemistry and relates to the synthesis of a novel covalent organic framework material; the invention also relates to the application of the covalent organic framework material synthesized by the synthesis method in metal ion recognition and dye adsorption. Background technique [0002] Covalent organic frameworks (COFs) are a new class of porous materials connected by covalent bonds and possess crystallinity, and are one of the hotspots in the research of functional materials. Intrinsic structure and tunable organic linkers endow COF materials with low density, large surface area, adjustable pore size, highly ordered pore structure, diverse synthesis methods and easy functional modification, so in catalysis, gas separation, dye adsorption, drug It is widely used in transportation, gas storage and other fields. In various applications, it has attracted increasing attention in different fields due...

Claims

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Application Information

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IPC IPC(8): C08G61/12C08G61/10B01J20/26B01J20/30C02F1/28C02F101/30
CPCC08G61/122C08G61/10B01J20/262C02F1/285C02F2101/308B01J2220/4812C08G2261/411C08G2261/124C08G2261/314C08G2261/3221C08G2261/522
Inventor 宋鹏飞于丽张宗莲陈亚伦曹雪梅王佩
Owner NORTHWEST NORMAL UNIVERSITY
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