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A post-synthesis modified mof-pc material and its preparation method and application

A MOF-PC, MOF technology, applied in the field of fluorescent probes, can solve the problems of long detection time, low sensitivity, and lack of active sites for MOF fluorescence sensing.

Active Publication Date: 2021-11-02
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a post-synthesis modified MOF-PC material and its preparation method and application in order to solve the problems of lack of active sites, long detection time and low sensitivity in the existing MOF fluorescence sensing

Method used

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  • A post-synthesis modified mof-pc material and its preparation method and application
  • A post-synthesis modified mof-pc material and its preparation method and application
  • A post-synthesis modified mof-pc material and its preparation method and application

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preparation example Construction

[0034] The present invention firstly provides a kind of preparation method of post-synthesis modified MOF-PC material, the method comprises:

[0035] Step 1: Synthesis of MOF materials

[0036] Add zirconium chloride to the N,N-dimethylformamide solvent, add hydrochloric acid (or acetic acid) dropwise, and ultrasonically dissolve the solid zirconium chloride. The ultrasonic time is preferably 10-15 minutes, and then add 2- N, N-dimethylformamide solution of aminoterephthalic acid, mix and stir evenly, the stirring time is preferably 20-25min; react at a constant temperature of 80°C to 120°C, and the reaction time is preferably 20-20min 24h; After the reaction is completed, centrifuge, wash, and vacuum-dry to obtain light yellow MOF solid powder; the mol ratio of the zirconium chloride and 2-aminoterephthalic acid is preferably (0.9~1.1):(1.3~1.6) , more preferably 1.08:1.5.

[0037] Step 2: Post-synthesis modification of MOF materials

[0038] Add the MOF solid powder prepa...

Embodiment 1

[0047] (1) Synthesis of MOF materials: ZrCl 4 (1.08mmol) was dissolved in 10mL N,N-dimethylformamide, 2mL hydrochloric acid was added, ultrasonicated for 10min, and 20mL N,N-dimethylformamide containing 2-aminoterephthalic acid (1.5mmol) was added solution, mixed at room temperature and stirred for 20 minutes, then moved the mixed solution into a reaction kettle, and placed the reaction kettle in an oven at 80°C for a constant temperature reaction for 24 hours. After the reaction was completed, the sample was centrifuged, washed, and vacuum-dried to obtain a light yellow solid powder.

[0048] (2) Post-synthesis modification of MOF materials: Weigh 100 mg of MOF materials and dissolve them in 8 mL of acetonitrile solvent, stir at room temperature for 20 min, then add 2-PC (0.6 mmol) and 10 μL of acetic acid, and react at a constant temperature of 45 °C for 48 h. After cooling, filtering, washing and vacuum drying, the modified MOF-PC material was synthesized.

[0049] Fluores...

Embodiment 2

[0051] (1) Synthesis of MOF materials: ZrCl 4 (1.08mmol) was dissolved in 10mL N,N-dimethylformamide, 2mL hydrochloric acid was added, ultrasonicated for 10min, and 20mL N,N-dimethylformamide containing 2-aminoterephthalic acid (1.5mmol) was added solution, mixed at room temperature and stirred for 20 minutes, then moved the mixed solution into a reaction kettle, and placed the reaction kettle in an oven at 80°C for a constant temperature reaction for 24 hours. After the reaction was completed, the sample was centrifuged, washed, and vacuum-dried to obtain a light yellow solid powder.

[0052] (2) Post-synthesis modification of MOF materials: Weigh 100 mg of MOF materials and dissolve them in 8 mL of ethanol solvent, stir at room temperature for 20 min, then add 2-PC (0.6 mmol) and 10 μL of acetic acid, and react at a constant temperature of 45 °C for 48 h. After cooling, filtering, washing and vacuum drying, the modified MOF-PC material was synthesized.

[0053] Fluorescence...

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Abstract

The invention provides a post-synthesis modified MOF-PC material and its preparation method and application, belonging to the technical field of fluorescent probes. The method comprises: adding zirconium chloride to N,N-dimethylformamide solvent, adding hydrochloric acid (or acetic acid) dropwise to dissolve the zirconium chloride solid ultrasonically, and then adding 2-aminoterephthalic acid-containing N , N-dimethylformamide solution, mixed and stirred evenly to react to obtain a light yellow MOF solid powder; the prepared MOF solid powder was added to the solvent, mixed and stirred evenly, and then pyridine-2-carboxaldehyde (2-PC ) reagents react with acetic acid to obtain a modified MOF-PC material. The MOF-PC material of the present invention has good fluorescence stability and high fluorescence emission efficiency, can realize the detection of TBHQ through the change of fluorescence "off-on", and detect Cr through the phenomenon of fluorescence "off" 2 o 7 2– .

Description

technical field [0001] The invention belongs to the technical field of fluorescent probes, and in particular relates to a post-synthesis modified MOF-PC material and a preparation method and application thereof. Background technique [0002] Tert-butylhydroquinone (TBHQ) is a common synthetic phenolic antioxidant, which has excellent chemical stability, antioxidant properties, high availability and low cost, and is widely used in the food industry, especially Used in cooking oil. However, due to the toxicological and mutagenic effects of phenolic antioxidants, excessive use of TBHQ will cause harm to human health and even cause cancer. In order to protect human health, many countries have clearly stipulated the maximum usage of TBHQ in food, among which my country stipulates that the maximum usage of TBHQ in food is 200mg / kg. Therefore, the determination of antioxidant content in food is very necessary. [0003] At present, a variety of analytical methods have been used f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/1029C09K2211/183G01N21/6428G01N2021/6432
Inventor 贾琼于清雅曹琪杨巾栏陈思涵郑海娇穆晋
Owner JILIN UNIV
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