Covalent organic framework fluorescent test paper for detecting palladium ions in water and preparation method thereof

A covalent organic framework, palladium ion technology, used in fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., to achieve wide application prospects, low detection limits, and fast analysis.

CN112341582AActive Publication Date: 2021-02-09HAINAN UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2021-02-09

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Abstract

The invention provides covalent organic framework fluorescent test paper for detecting palladium ions in water and a preparation method of the covalent organic framework fluorescent test paper, and belongs to the field of environmental detection. The XB-COF disclosed by the invention is prepared from monomer s-tribenzaldehyde and 2, 5-di(allyloxy)terephthaloyl hydrazine through a Schiff base reaction by using a solvothermal method; the XB-COF provided by the invention improves the crystallinity, porosity and chemical stability of the material through acylhydrazone bond connection. When the XB-COF is dispersed in water, strong fluorescence is shown, and after allyl in the XB-COF can interact with Pd2+ to form a COF-Pd ligand, the strong fluorescence of the XB-COF is quenched. The sensitivefluorescence change and regular allyl active sites enable the XB-COF to be used for constructing a high-performance fluorescence sensor with high sensitivity, high selectivity and high stability for detecting Pd 2+. The fluorescent test paper is a material growing on the filter paper in situ based on XB-COF. The fluorescent test paper can be used for detecting trace Pd2+ in water, and can be usedfor rapidly detecting the existence of Pd2+ in industrial wastewater, organic synthesis reaction, pharmaceutical industry and other wastewater.
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Description

[0001] The invention belongs to the technical field of the application of organic porous materials to environmental detection, and in particular relates to a method for preparing an organic covalent framework material connected by acylhydrazone bonds containing allyl groups. Background technique

[0002] Palladium belongs to the platinum group metal elements, it usually contains three valence states: Pd 0 , Pd 2+ and Pd 4+ . For a long time, palladium metal has been considered as a very important transition metal, which is widely used in jewelry industry, electronics and electrical industry, medical industry, fuel cell industry and industrial catalysis industry. Palladium plays a key role in the automotive industry as a precious metal catalyst, where it is one of the most important catalysts in catalytic converters for automotive exhaust emissions. During the driving process of the car, palladium ions will be discharged into the air together with the exhaust gas of the car,...

Examples

Embodiment 1

[0044] A method for preparing a covalent organic framework fluorescent test paper for detecting palladium ions in water, comprising the following steps:

[0045] (1) Soak the blank filter paper in the dioxane solution and mesitylene mixed with 0.025mmol organic small molecule tritylaldehyde, 2,5-bis(allyloxy)terephthalic hydrazide In the ampoule bottle of solution 3mL; The dioxane solution of described 2,5-bis(allyloxyl) terephthalic hydrazide is 2,5-bis(allyloxyl) terephthalamide of 9mg Prepared by dissolving hydrazide in 0.8mL of dioxane;

[0046] (2) Add 0.1mL acetic acid to the bottle, and ultrasonically disperse the solvent for 10 minutes; the concentration of the acetic acid solution is 3M;

[0047] (3) After the refrigeration cycle pumps air three times, seal the ampoule bottle and react at 120°C for 3 days;

[0048] (4) After the filter paper is taken out, wash it with acetone for 3 times, place it in a clean and ventilated place, and let it dry naturally to obtain t...

Embodiment 2

[0050] A method for preparing a covalent organic framework fluorescent test paper for detecting palladium ions in water, comprising the following steps:

[0051] (1) Soak blank filter paper in dioxane solution and mesitylene mixed with 0.03mmol organic small molecule tritylaldehyde, 2,5-bis(allyloxy)terephthalic hydrazide In the ampoule bottle of solution 3.5mL; The dioxane solution of described 2,5-bis(allyloxyl) terephthalhydrazide is 10mg of 2,5-bis(allyloxyl) terephthalamide Prepared by dissolving formylhydrazide in 1mL of dioxane;

[0052] (2) Add 0.15mL acetic acid to the bottle, and ultrasonically disperse the solvent for 10 minutes; the concentration of the acetic acid solution is 4.5M;

[0053] (3) After the refrigeration cycle pumps air three times, seal the ampoule bottle and react at 120°C for 3 days;

[0054] (4) After the filter paper is taken out, wash it with acetone for 3 times, place it in a clean and ventilated place, and let it dry naturally to obtain the...

Embodiment 3

[0056] A method for preparing a covalent organic framework fluorescent test paper for detecting palladium ions in water, comprising the following steps:

[0057] (1) Soak blank filter paper in dioxane solution and mesitylene mixed with 0.038mmol organic small molecule tritylaldehyde, 2,5-bis(allyloxy)terephthalic hydrazide In the ampoule bottle of solution 4.5mL; The dioxane solution of described 2,5-bis(allyloxyl) terephthalhydrazide is 11.5mg of 2,5-bis(allyloxyl)p-phenylene Prepared by dissolving dimethylhydrazide in 1.5mL of dioxane;

[0058] (2) Add 0.2mL acetic acid to the bottle, and ultrasonically disperse the solvent for 10 minutes; the concentration of the acetic acid solution is 6M;

[0059] (3) After the refrigeration cycle pumps air three times, seal the ampoule bottle and react at 120°C for 3 days;

[0060] (4) After the filter paper is taken out, wash it with acetone for 3 times, place it in a clean and ventilated place, and let it dry naturally to obtain the ...