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Sponge-supported porphyrin covalent organic framework integral material as well as preparation method and application thereof

A covalent organic framework, monolithic material technology, applied in separation methods, material excitation analysis, chemical instruments and methods, etc., can solve the problems of poor Cd2+ affinity, hindering the large-scale practical application of adsorption materials, slow adsorption kinetics, etc. Excellent physical and chemical stability, short adsorption equilibrium time, fast adsorption kinetics

Pending Publication Date: 2022-05-27
AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, poor thermal stability, weak acid-base adaptability, low adsorption capacity, slow adsorption kinetics, and 2+ The poor affinity of the adsorbent hinders the large-scale practical application of most adsorbent materials.

Method used

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  • Sponge-supported porphyrin covalent organic framework integral material as well as preparation method and application thereof
  • Sponge-supported porphyrin covalent organic framework integral material as well as preparation method and application thereof
  • Sponge-supported porphyrin covalent organic framework integral material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A method for synthesizing a sponge-supported porphyrin covalent organic framework material, comprising the steps of:

[0042] A polyurethane sponge (50 mg) was immersed in a 0.1 mol / L dopamine solution (Tris-HCl buffer, pH=8.5), and after magnetic stirring for 24 hours, the sponge was taken out and vacuum-dried.

[0043] Starting with meso-tetrakis(4-aminophenyl)porphyrin (Tph) (67.5 mg, 0.1 mmol) and 2,3-dihydroxyterephthalaldehyde (2,3-Dha) (33.2 mg, 0.2 mmol) The starting materials were mixed in a 20 mL reaction vessel with o-dichlorobenzene (6 mL) and n-butanol (6 mL) as solvent and glacial acetic acid solution (6 M, 1 mL) as catalyst. The mixture was sonicated for 5 minutes. The treated dry sponge was added, then the reaction vessel was sealed and heated at 120°C for 3 days. After cooling to room temperature, the precipitate of the crude product was obtained by filtration. The precipitate was washed with tetrahydrofuran in a Soxhlet extractor for 12 hours, washed...

Embodiment 2

[0045] A method for synthesizing a sponge-supported porphyrin covalent organic framework material, comprising the steps of:

[0046] A polyurethane sponge (50 mg) was immersed in a 0.1 mol / L dopamine solution (Tris-HCl buffer, pH=8.5), and after magnetic stirring for 24 hours, the sponge was taken out and vacuum-dried.

[0047] Starting with meso-tetrakis(4-aminophenyl)porphyrin (Tph) (67.5 mg, 0.1 mmol) and 2,5-dihydroxyterephthalaldehyde (2,5-Dha) (33.2 mg, 0.2 mmol) The starting materials were mixed in a 20 mL reaction vessel with o-dichlorobenzene (6 mL) and n-butanol (6 mL) as solvent and glacial acetic acid solution (6 M, 1 mL) as catalyst. The mixture was sonicated for 5 minutes. The treated dry sponge was added, then the reaction vessel was sealed and heated at 120°C for 3 days. After cooling to room temperature, the precipitate of the crude product was obtained by filtration. The precipitate was washed with tetrahydrofuran in a Soxhlet extractor for 12 hours, washed...

Embodiment 3

[0049] The synthetic method of 2,3-DhaTph comprises the following steps:

[0050] Tph (67.5 mg, 0.1 mmol), 2,3-Dha (33.2 mg, 0.2 mmol), o-dichlorobenzene (6 mL), n-butanol (6 mL) and aqueous glacial acetic acid (6 M, 1 mL) in a 20 mL Mix in reaction vessel. The mixture was sonicated for 5 minutes. Then, the reaction vessel was sealed and heated at 120°C for 3 days. After cooling to room temperature, a precipitate of crude product was obtained by filtration. The precipitate was washed in a Soxhlet extractor with tetrahydrofuran for 12 hours, dichloromethane for 12 hours, and then dried at 60°C for 5 hours.

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Abstract

The invention relates to a sponge-supported porphyrin covalent organic framework integral material as well as a preparation method and application thereof, and the method comprises the following steps: meso-tetra (4-aminophenyl) porphyrin and 2, 3-dihydroxy terephthalaldehyde or 2, 5-dihydroxy terephthalaldehyde are used as initial raw materials, in a reaction solvent, a glacial acetic acid solution is used as a catalyst, and the sponge-supported porphyrin covalent organic framework integral material is obtained through a one-step reaction. Performing ultrasonic treatment on the mixture, adding pretreated dry sponge, sealing the reaction container, performing heating reaction, cooling to room temperature after the reaction, filtering to obtain precipitate of a crude product, and washing and drying the precipitate to obtain the product. The sponge-supported porphyrin covalent organic framework material disclosed by the invention realizes dual functions of specific optical recognition and efficient adsorption of heavy metal ions (such as Cd < 2 + >).

Description

technical field [0001] The invention belongs to the technical field of heavy metal ion adsorption, and in particular relates to a method for synthesizing a sponge-supported porphyrin covalent organic framework integral material and its application in the environmental fields such as heavy metal ion adsorption and removal and fluorescence detection. Background technique [0002] Heavy metals are one of the pollutants in industrial and mining wastewater. Food pollution caused by heavy metals has also become a problem of widespread concern. Through various pathways, heavy metal ions easily accumulate in organisms and exhibit high biotoxicity. The removal of these contaminants from wastewater and food is an important environmental and livelihood issue, therefore, exploring effective removal methods is critical. Cadmium (Cd) is one of the harmful heavy metals, and the incubation period of cadmium ions in organisms can be as long as 10-30 years. 0.001-0.01mg·L -1 Cadmium ions ...

Claims

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Application Information

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IPC IPC(8): C08J9/40C08G12/26B01J20/22B01J20/30C02F1/28B01D15/00G01N21/64C02F101/20C08L75/04
CPCC08J9/405C08G12/26B01J20/226C02F1/285B01D15/00G01N21/64C02F2101/20C08J2375/04
Inventor 姜红新靳伟良朱莉娜孔德明刘潇威周其文赵玉杰
Owner AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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