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A kind of ball-milled graphene-mofs composite material, its preparation and application

A composite material and graphene technology, applied in the fields of nanomaterial technology and electrochemical sensors, can solve the problems of toxic chemical reagents, the danger of complex preparation processes, etc., and achieve the effects of cost reduction, good electrochemical reactivity, and short reaction cycle.

Active Publication Date: 2020-05-19
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the above defects or improvement needs of the prior art, the present invention provides a ball-milled graphene-metal organic framework composite material, its preparation method and its application in the field of electrochemical sensing. Graphene-based MOFs composite materials are prepared at room temperature, thus solving technical problems such as the use of a large amount of toxic chemical reagents in the preparation process of the existing graphene-based MOFs composites, the complicated preparation process and the danger in the operation process

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  • A kind of ball-milled graphene-mofs composite material, its preparation and application
  • A kind of ball-milled graphene-mofs composite material, its preparation and application
  • A kind of ball-milled graphene-mofs composite material, its preparation and application

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preparation example Construction

[0036] The invention provides a method for preparing a ball milled graphene-MOFs composite material, comprising the steps of:

[0037] (1) The graphite powder is peeled off by wet ball milling, and the shear force is dominant in the ball milling peeling process to obtain a mixed system containing graphene nanosheets;

[0038] (2) the mixed system containing graphene nanosheets obtained in step (1) adopts gradient centrifugation to remove unexfoliated graphite in the mixed system, and obtains graphene nanosheets solid;

[0039](3) the metal salt dispersed in the organic solvent is mixed with the graphene nano-sheets obtained in step (2), and stirred so that the metal ions in the metal salt are adsorbed on the graphene nano-sheets to obtain the graphene nano-sheets loaded with metal ions piece;

[0040] (4) Mix the graphene nanosheets loaded with metal ions obtained in step (3) with organic ligands, and promote the in-situ synthesis of MOFs on the surface of graphene nanosheets...

Embodiment 1

[0071] A kind of preparation method of ball-milled graphene / Cu-BTC composite material is carried out according to the following steps:

[0072] Disperse 300 mg of 1200 mesh graphite powder and 300 mg of cetyltrimethylammonium bromide powder in 30 ml of aqueous solution containing 15% ethanol, and control the ball milling speed at 300 rpm to ensure that the shear force accounts for Dominance, after 12 hours of ball milling reaction, the graphene nanosheets mixed solution was obtained by exfoliation by ball milling.

[0073] The mixed solution was centrifuged at 2000 rpm for 20 minutes to remove the unexfoliated graphite powder precipitate. Then the obtained solution was centrifuged at 9000 rpm for 20 minutes to obtain a solid, which was repeatedly washed with ethanol and ultrapure water to remove residual cetyltrimethylammonium bromide, and finally air-dried at 60°C.

[0074] 0.7 g of Cu(NO 3 ) 2 ·3H 2 O was uniformly dispersed in 50 ml of DMF solution, then 50 mg of ball-m...

Embodiment 2

[0098] A kind of preparation method of ball-milled graphene / Co-BTC composite material is carried out according to the following steps:

[0099] Disperse 300 mg of 1200 mesh graphite powder and 300 mg of cetyltrimethylammonium bromide powder in 30 ml of aqueous solution containing 15% ethanol, and control the ball milling speed at 300 rpm to ensure that the shear force accounts for Dominance, after 12 hours of ball milling reaction, the graphene nanosheets mixed solution was obtained by exfoliation by ball milling.

[0100] The mixed solution was centrifuged at 2000 rpm for 20 minutes to remove the unexfoliated graphite powder precipitate. Then the obtained solution was centrifuged at 9000 rpm for 20 minutes to obtain a solid, which was repeatedly washed with ethanol and ultrapure water to remove residual cetyltrimethylammonium bromide, and finally air-dried at 60°C.

[0101] 0.85 g Co(NO 3 ) 2 ·6H 2 O was uniformly dispersed in 50 ml of DMF solution, then 50 mg of ball-mil...

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Abstract

The invention, which belongs to the field of the nano material technology and electrochemical sensor, more particularly relates to a ball milled graphene-metal organic framework (MOFs) composite material, a preparation method thereof and application in an electrochemical sensor. The graphene is a large graphene nanosheet prepared by ball milling and stripping. The metal organic framework is uniformly dispersed on the surface of the graphene nanosheet. The preparation method includes: step one, carrying out wet ball milling and stripping to prepare a graphene nanosheet; step two, sufficiently adsorbing metal ions on the surface of the graphene nanosheet; and step three, growing a metal organic framework at an original site on the surface of the graphene by combining an organic ligand. Therefore, a ball-milled graphene-metal organic framework composite having high stability and electrical conductivity and having a large specific surface area and high porosity is obtained. The prepared ball-milled graphene-metal organic framework composite has the excellent electrochemical performance and can be used for preparing the highly sensitive electrochemical sensing platform.

Description

technical field [0001] The invention belongs to the field of nanomaterial technology and electrochemical sensors, and more specifically relates to a ball-milled graphene-metal organic framework (MOFs) composite material, its preparation method and its application in the field of electrochemical sensing. Background technique [0002] In recent years, metal-organic frameworks (MOFs) have been widely used in the field of electrochemical sensing due to their large porosity and specific surface area, adjustable pore size and variable functional groups. . However, due to the inherent instability and poor electrical conductivity of MOFs, their practical application and future development are limited. In order to solve this problem, it has become a hot research direction to construct composite materials of MOFs and other materials to improve the stability, adsorption performance and electrical conductivity of MOFs. So far, a variety of materials have been reported to be used in co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/26G01N27/48C01B32/19C01B32/194
Inventor 吴康兵李晓宇李草灵
Owner HUAZHONG UNIV OF SCI & TECH
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