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Double-layer walled microporous self-assembled material with fluorescent recognition effect and preparation method thereof

A fluorescent recognition and self-assembly technology, applied in the direction of luminescent materials, chemical instruments and methods, zinc organic compounds, etc., can solve problems such as poor operability, weakened fluorescence of adsorbents, and many external factors

Inactive Publication Date: 2012-12-26
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Jing's research group at Rutgers University recently synthesized a self-assembled material with three-dimensional interpenetrating micropores using 4,4-oxobis(benzoic acid) and 4,4-bipyridine as ligands. It can adsorb nitrobenzene compounds, and at the same time, due to the adsorption of nitrobenzene, the fluorescence of the adsorbent itself is weakened
However, the evaluation standard of fluorescence weakening is poor in operability. On the one hand, it is affected by many external factors, and on the other hand, the ability to identify fluorescence weakening is low.
Therefore, the application prospects of this self-assembled material are limited

Method used

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  • Double-layer walled microporous self-assembled material with fluorescent recognition effect and preparation method thereof
  • Double-layer walled microporous self-assembled material with fluorescent recognition effect and preparation method thereof
  • Double-layer walled microporous self-assembled material with fluorescent recognition effect and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 0.208 g of zinc nitrate, 0.097 g of 4,4'-biphenyl dicarboxylic acid and 0.034 g of 4-(3,5-dimethyl-1H-pyrazole-4-)pyridine to 10 ml of N,N'-bis In the ethyl formamide solvent, after stirring at room temperature for 30 minutes, a white emulsion was obtained, which was moved to a stainless steel reactor lined with polytetrafluoroethylene, and reacted at 140 ° C for about 72 hours, and then naturally cooled to room temperature ( The preferred cooling rate is about 5°C / h), filter to obtain light yellow crystals, wash the crystals three times with N,N'-diethylformamide and acetone, and dry them in an oven at 60°C for 30 minutes to obtain the micropores self-assembling materials.

Embodiment 2

[0026]Add 0.198 g of zinc acetate, 0.097 g of 4,4'-diphenyldicarboxylic acid, and 0.034 g of 4-(3,5-diethyl-1H-pyrazole-4-)pyridine into 10 mL of N,N'- In dimethylacetamide solvent, stir at room temperature for 10 minutes, add 1 to 5 drops of nitric acid and continue stirring for 20 minutes. Move it to a stainless steel reactor lined with polytetrafluoroethylene, react at 60°C for about 8 hours, then cool naturally to room temperature, filter to obtain light yellow crystals, and use N,N'-dimethylacetamide, acetone The crystals were washed three times respectively, and vacuum-dried for 30 minutes to obtain the microporous self-assembled material.

Embodiment 3

[0028] Add 0.104 g of zinc nitrate, 0.048 g of 4,4'-biphenyldicarboxylic acid, and 0.018 g of 4-(3,5-dimethyl-1H-pyrazole-4-)pyridine to 1 mL of N,N'- Dimethylformamide and 9 mL of N,N'-diethylformamide solvent, stirred at room temperature for 500 minutes. Move it to a stainless steel reactor lined with polytetrafluoroethylene, react at 180°C for about 120 hours, then cool to room temperature at a rate of about 5°C / h, filter to obtain light yellow crystals, and use N,N'- The crystals were washed three times with dimethylformamide and acetone respectively, and dried in an oven at 80° C. for 30 minutes to obtain the microporous self-assembled material.

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Abstract

The invention in particular relates to a double-layer walled microporous self-assembled material with a fluorescent recognition effect and a preparation method thereof, which belong to the technical field of advanced porous materials. According to the invention, by using rigid dicarboxylic acid or rigid azacyclo organic ligands as a supporting wall of a microporous material and using a metal ion with a multi-ligand-field geometry configuration as a central metal, the microporous self-assembled material with a double-layer organic wall is prepared through a solvent hot self-assembled growth method. A porous channel of the prepared microporous self-assembled material with the double-layer organic wall has a size of 5-20 angstroms and is a three-dimensional interconnected porous channel. The microporous self-assembled material provided by the invention has the advantage of characteristic fluorescence; and the fluorescence is weakened and obviously red-shifted when the microporous self-assembled material meets nitrobenzene explosive compounds, so that a recognition purpose is achieved. The double-layer walled microporous self-assembled material with the fluorescent recognition effect, provided by the invention, has the advantages of simple synthesis method and strong controllability and has broad application prospects in inspection and detection aspects of the nitrobenzene explosive compounds.

Description

technical field [0001] The invention belongs to the technical field of advanced porous materials, and in particular relates to a microporous self-assembly material with double-layer walls with fluorescence recognition function and a preparation method thereof. technical background [0002] In recent years, the synthesis and application of microporous self-assembled materials has become a hotspot in the research of advanced porous materials and the development of new materials. This kind of microporous self-assembled materials has wide application prospects in the adsorption, storage and identification of toxic, harmful, flammable and explosive molecules due to the adjustable force in the pores and the controllable size of the pores. [0003] So far, there have been some reports on the synthesis of microporous self-assembled materials with the ability to adsorb and store toxic, harmful, flammable and explosive molecules, but most of the microporous materials involved in the e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C09K11/06
Inventor 凌云郑庆舒周亚明陈珍霞刘小锋杨永泰翁林红
Owner FUDAN UNIV
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