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Preparation method and application of an iron porphyrin chloride/methylene blue@metal organic framework composite electrode

A metal-organic framework, methylene blue technology, applied in the field of electrochemical sensing, can solve the problems of inability to meet high-precision trace detection, not yet seen, low sensitivity, etc., to increase specific surface area and catalytic ability, avoid self-degradation, detection range wide effect

Active Publication Date: 2018-08-07
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at 1.00×10 -3 In the presence of mol / LAA, the detection limit is only 1.00×10 -8 mol / L, low sensitivity, unable to meet the requirements of high-precision trace detection
[0006] So far, there have been no patent reports based on the application of iron porphyrin chloride in the metal organic framework of Zn and the adsorption of methylene blue as a composite material in the field of electrochemical sensing

Method used

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  • Preparation method and application of an iron porphyrin chloride/methylene blue@metal organic framework composite electrode
  • Preparation method and application of an iron porphyrin chloride/methylene blue@metal organic framework composite electrode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 2-(2'-pyridyl)imidazole (0.5g) and iron porphyrin (30mg) were dissolved in 7.5mL of ethanol and 7.5mL of N,N-dimethylformamide solvent, 0.5g of zinc chloride was added 10mL solution, sealed in a 50mL reaction kettle, put it into a high-pressure steam sterilizer and heat it at 50°C for 12 hours, let it cool to room temperature, collect the crystalline material by centrifugation, wash with ethanol, and dry under vacuum at 50°C After 14 hours, the FeTCPP@Zn-MOF composite material was obtained;

[0057] The FeTCPP@Zn-MOF composite material was dissolved in deionized water, and 2 mL of 0.1 mg / mL methylene blue solution was added, and slightly shaken for 50 min. The FeTCPP@Zn-MOF composite material adsorbed methylene blue electrostatically to form a MB / FeTCPP@Zn-MOF composite , collected by centrifugation;

[0058] 0.5 mg / mL of MB / FeTCPP@Zn-MOF was drop-coated on the electrode surface, and dried naturally at room temperature for 12 hours to prepare the MB / FeTCPP@Zn-MOF modif...

Embodiment 2

[0060] 2-(2'-pyridyl)imidazole (0.8g) and iron porphyrin (50mg) were dissolved in 7.5mL of ethanol and 7.5mL of N,N-dimethylformamide solvent, 0.8g of zinc chloride was added 10mL solution, sealed in a 50mL reaction kettle, put it into a high-pressure steam sterilizer and heat it at 50°C for 12 hours, let it cool to room temperature, collect the crystalline material by centrifugation, wash with ethanol, and dry under vacuum at 60°C After 13 hours, the FeTCPP@Zn-MOF composite material was obtained;

[0061] The FeTCPP@Zn-MOF composite material was dissolved in deionized water, and 2 mL of 0.15 mg / mL methylene blue solution was added, and slightly shaken for 55 minutes. The FeTCPP@Zn-MOF composite material adsorbed methylene blue electrostatically to form a MB / FeTCPP@Zn-MOF composite , collected by centrifugation;

[0062] 0.5 mg / mL of MB / FeTCPP@Zn-MOF was drop-coated on the electrode surface, and dried naturally at room temperature for 12 hours to prepare the MB / FeTCPP@Zn-MOF ...

Embodiment 3

[0064] 2-(2'-pyridyl)imidazole (1.2g) and iron porphyrin (70mg) were dissolved in 7.5mL of ethanol and 7.5mL of N,N-dimethylformamide solvent, and 1.2g of zinc chloride was added 10mL solution, sealed in a 50mL reaction kettle, put it into a high-pressure steam sterilizer and heat it at 60°C for 12 hours, let it cool to room temperature, collect the crystalline material by centrifugation, wash with ethanol, and dry under vacuum at 60°C After 12 hours, the FeTCPP@Zn-MOF composite material was obtained;

[0065] The FeTCPP@Zn-MOF composite material was dissolved in deionized water, and 2 mL of 0.2 mg / mL methylene blue solution was added, and slightly shaken for 60 minutes. The FeTCPP@Zn-MOF composite material adsorbed methylene blue electrostatically to form a MB / FeTCPP@Zn-MOF composite , collected by centrifugation;

[0066] 0.5 mg / mL of MB / FeTCPP@Zn-MOF was drop-coated on the electrode surface, and dried naturally at room temperature for 12 hours to prepare the MB / FeTCPP@Zn-M...

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Abstract

The invention provides a preparation method and application of an electrode of a composite material of an iron porphyrin chloride / methylene blue @metal-organic framework. Iron porphyrin chloride (FeTCPP) is encapsulated to a Zn metal-organic framework (MOF) by a one-pot method, a composite material of the metal-organic framework has negative charges in a solution, and cationic dye methylene blue (MB) with oxidation-reduction activity can be absorbed. The composite material is modified to the surface of a glass carbon electrode, and dopamine can be catalyzed and oxidized so that an electrical signal can be produced, sensitive detection for the dopamine is realized by an electrochemical method, the lowest detection limit can reach 0.48fM, and the detection range is wide. The composite material of the metal-organic framework disclosed by the invention is synthesized for the first time, and besides, the composite material of the metal-organic framework is also applied to the field of electrochemical sensing for the first time, the method is simple, the cost is low, and high electrochemical sensing sensitivity indicates that the composite material of the metal-organic framework functionalized by porphyrin and methylene blue has good application prospects in the field of electrochemical and biological sensing.

Description

technical field [0001] The invention belongs to the technical field of electrochemical sensing, in particular to a preparation method and application of an iron porphyrin chloride / methylene blue@metal organic framework composite electrode. Background technique [0002] Metal-organic frameworks (MOFs) materials not only have very high porosity and surface area, but also have strong controllability and easy functionalization. Functional MOFs materials are one of the effective methods for the heterogeneity of homogeneous catalysts developed in recent years. The homogeneous catalyst metalloporphyrin has good catalytic activity. There are two main ways to construct functional MOFs materials by porphyrin: one is to prepare MOFs materials with porphyrin as an organic building block, and the other is to encapsulate metalloporphyrin into MOFs. internal. Porphyrin MOFs materials have attracted widespread attention due to the combination of the microstructure controllability of MOFs ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22G01N27/31G01N27/48
CPCB01J31/183B01J31/226G01N27/31G01N27/48
Inventor 王宗花李军夏建飞龚世达张菲菲
Owner QINGDAO UNIV
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