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Palladium-graphitic carbon nitride-carbon nanotube composite electrode, and preparation method and application thereof

A composite technology of graphite phase carbon nitride and carbon nanotubes, which is applied in the direction of material electrochemical variables, material analysis through electromagnetic means, and measuring devices, etc., to achieve less chemical raw materials and reagents, mild reaction conditions, and less environmental pollution. Effect

Inactive Publication Date: 2018-06-22
甘肃政法大学
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The technical problem solved by the present invention is to overcome the defects of the performance and preparation method of the existing electrochemical sensor for detecting estradiol, and obtain it through the solid grinding thermal polymerization method by π-π stacking and electrostatic interaction between melamine and carbon nanotubes A carbon nitride-carbon nanotube composite material with a graphite-like phase was obtained, and then palladium nanoparticles were used as a precursor to further functionalize it through self-assembly to obtain a composite material with good catalytic performance and stability, and finally prepared a catalytic performance And palladium-graphite phase carbon nitride-carbon nanotube composite electrode with stronger stability and higher sensitivity for rapid detection of estradiol content in samples

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  • Palladium-graphitic carbon nitride-carbon nanotube composite electrode, and preparation method and application thereof
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  • Palladium-graphitic carbon nitride-carbon nanotube composite electrode, and preparation method and application thereof

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Embodiment 1

[0045] A preparation method of a palladium-like graphite phase carbon nitride-carbon nanotube composite electrode, comprising the steps of:

[0046] (1) Preparation of graphite-like carbon nitride-carbon nanotube composites: take 0.12g carbon nanotubes and 2.5g melamine and place them in an agate mortar for grinding, wrap them in aluminum plastic, put them in a crucible, and heat up to 520 Keep at ℃ for 4h, then cool down to room temperature to obtain graphite-like phase carbon nitride-carbon nanotube composite material;

[0047] (2) Preparation of graphite-like phase carbon nitride-carbon nanotube composites modified by palladium nanoparticles: Weigh 10 mg of graphite-like phase carbon nitride-carbon nanotube composite material composite powder prepared in step (1), and use 20 mL Secondary deionized water dispersion, add 0.6mL, 20mM Na 2 PdCl 4 Solution and 60 μL, 6M HCl, followed by magnetic stirring for 4.5 h, then added 4 mL, 0.1 M ascorbic acid, and reacted at a constan...

Embodiment 2

[0057] A preparation method of a palladium-like graphite phase carbon nitride-carbon nanotube composite electrode, comprising the steps of:

[0058] (1) Preparation of graphite-like phase carbon nitride-carbon nanotube composites: Take 0.05g carbon nanotubes and 1g melamine and grind them in an agate mortar, wrap them in aluminum plastic, put them in a crucible, and heat up to 300°C Keep for 1h, then cool down to room temperature to obtain graphite-like phase carbon nitride-carbon nanotube composite material;

[0059] (2) Preparation of graphite-like phase carbon nitride-carbon nanotube composites modified by palladium nanoparticles: Weigh 5 mg of graphite-like phase carbon nitride-carbon nanotube composite material composite powder prepared in step (1), and use 10 mL Secondary deionized water dispersion, adding 0.5mL, 20mM Na 2 PdCl 4 solution and 20 μL, 6M HCl, then magnetically stirred for 1 h, then added 2 mL, 0.1 M ascorbic acid, and reacted at a constant temperature fo...

Embodiment 3

[0069] A preparation method of a palladium-like graphite phase carbon nitride-carbon nanotube composite electrode, comprising the steps of:

[0070](1) Preparation of graphite-like carbon nitride-carbon nanotube composites: Take 0.3g carbon nanotubes and 5g melamine and grind them in an agate mortar, wrap them in aluminum plastic, put them in a crucible, and heat up to 600°C Keep for 8h, then cool down to room temperature to obtain graphite-like phase carbon nitride-carbon nanotube composite material;

[0071] (2) Preparation of graphite-like phase carbon nitride-carbon nanotube composites modified by palladium nanoparticles: Weigh 30 mg of graphite-like phase carbon nitride-carbon nanotube composite material composite powder prepared in step (1), and use 30 mL Secondary deionized water dispersion, add 2mL, 20mM Na 2 PdCl 4 Solution and 100 μL, 6M HCl, followed by magnetic stirring for 6 h, and then 5 mL, 0.1 M ascorbic acid was added, at a temperature of 150 ° C, constant t...

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Abstract

The invention discloses a palladium-graphitic carbon nitride-carbon nanotube composite electrode, and a preparation method and application thereof. According to the preparation method, a graphitic carbon nitride-carbon nanotube composite is prepared by using a solid grinding thermopolymerization process in virtue of Pi-Pi accumulation and electrostatic action between melamine and carbon nanotubes;then palladium nanoparticles are used as a precursor for further functionalized modification of the graphitic carbon nitride-carbon nanotube composite through self-assembing so as to obtain a composite material with good catalysis performance and stability; so electrocatalytic activity is improved, problems in the dispersibility of graphitic carbon nitride are overcome, and the application scopeof the composite material is broadened. The preparation method is simple in process, convenient to operate, low in the amount of consumed chemical raw materials and reagents, mild in reaction conditions, small in the number of used equipment, low in production cost, capable of realizing large-scale production, low in environmental pollution and beneficial for environmental protection; and the prepared composite electrode has higher sensitivity and better catalytic performance and stability, and is especially suitable for direct and rapid detection of estradiol in water samples, food samples, feed samples, biochemical product samples and other samples.

Description

technical field [0001] The invention relates to the preparation of a non-metallic graphite phase carbon nitride electrode, in particular to a palladium-like graphite phase carbon nitride-carbon nanotube composite electrode and its preparation method and application. Background technique [0002] Environmental endocrine disruptor compounds (Endocrine disruptor compounds, EDCs), defined by the European Commission in 1996 as exogenous chemical substances, have estrogen-like effects and can interfere with the endocrine system of humans and animals, and have attracted widespread attention in the academic community. EDCs can disrupt hormone balance, have many adverse effects on human and animal health, and directly threaten human survival. In the "Stockholm Convention on Persistent Organic Pollutants" signed in 2002, the first batch of 12 environmental hormones identified as having persistent pollution were banned from use. 17β-estradiol is a common EDCs. Estradiol is the natura...

Claims

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Application Information

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IPC IPC(8): G01N27/30
CPCG01N27/308
Inventor 郑志祥王玫闫乾顺马璀
Owner 甘肃政法大学
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