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Nitrogen-doped three-dimensional porous graphene-based electrode material as well as preparation method and application thereof

A three-dimensional porous, graphene-based technology, applied in the field of electrochemistry, can solve problems such as hindering the application of graphene-based electrochemical sensors, affecting sensor performance, easy agglomeration and overlapping, and achieving good application potential, short response time, and long-term stability. good effect

Active Publication Date: 2020-11-17
SPECIAL EQUIP SAFETY SUPERVISION INSPECTION INST OF JIANGSU PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, during the application process, it was found that graphene-based electrode materials are prone to agglomeration and overlap, and graphene does not have an energy gap, and its conductivity cannot be controlled as easily as traditional semiconductors, which greatly affects the performance of the sensor. ; In addition, the surface of graphene is smooth and inert, which is not conducive to its further compounding with other materials
The above-mentioned problems have seriously hindered the application of graphene-based electrochemical sensors in pesticide detection.

Method used

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  • Nitrogen-doped three-dimensional porous graphene-based electrode material as well as preparation method and application thereof
  • Nitrogen-doped three-dimensional porous graphene-based electrode material as well as preparation method and application thereof
  • Nitrogen-doped three-dimensional porous graphene-based electrode material as well as preparation method and application thereof

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Embodiment 1

[0034] A preparation method of a nitrogen-doped three-dimensional porous graphene-based electrode material, comprising the following steps:

[0035] 1) Take 50mL graphene oxide (2mg / mL) solution, according to the volume ratio of graphene oxide solution and hydrogen peroxide solution 15:1, add hydrogen peroxide solution (30wt.%), ultrasonic treatment for 15min, and then graphene oxide The mixed solution with hydrogen peroxide was transferred to a round-bottomed flask, and reacted at 95°C for 5 h; the resulting product was immersed in ultrapure water and dialyzed for 4 days to remove excess hydrogen peroxide impurities, and then quickly frozen in liquid nitrogen, and Continue freeze-drying in a freeze dryer for 10 hours to obtain a three-dimensional porous graphene oxide solid;

[0036] 2) Take 70 mg of the three-dimensional porous graphene oxide solid obtained above and dissolve it in 70 mL of ultrapure water, then add urea according to the mass ratio of urea solid to three-dim...

Embodiment 2

[0039] A preparation method of a nitrogen-doped three-dimensional porous graphene-based electrode material, comprising the following steps:

[0040]1) Take 50mL graphene oxide (2mg / mL) solution, according to the volume ratio of graphene oxide solution and hydrogen peroxide solution 12:1, add hydrogen peroxide solution (20wt.%), ultrasonic treatment for 20min, and then the graphene oxide The mixed solution with hydrogen peroxide was transferred to a round-bottomed flask, and reacted at 100°C for 3 h; the resulting product was immersed in ultrapure water and dialyzed for 5 days to remove excess hydrogen peroxide impurities, and then quickly frozen in liquid nitrogen, and Continue freeze-drying in a freeze dryer for 12 hours to obtain a three-dimensional porous graphene oxide solid;

[0041] 2) Take 70 mg of the three-dimensional porous graphene oxide solid obtained above and dissolve it in 50 mL of ultrapure water, then add urea according to the mass ratio of urea solid to three...

Embodiment 3

[0044] A preparation method of a nitrogen-doped three-dimensional porous graphene-based electrode material, comprising the following steps:

[0045] 1) Take 50mL graphene oxide (2mg / mL) solution, according to the volume ratio of graphene oxide solution and hydrogen peroxide solution 10:1, add hydrogen peroxide solution (40wt.%), ultrasonic treatment for 15min, and then graphene oxide The mixed solution with hydrogen peroxide was transferred to a round-bottomed flask, and reacted at 100°C for 3.5 hours; the resulting product was immersed in ultrapure water and dialyzed for 6 days to remove excess hydrogen peroxide impurities, and then quickly frozen in liquid nitrogen. And continue to freeze-dry for 12 hours in a freeze dryer to obtain a three-dimensional porous graphene oxide solid;

[0046] 2) Dissolve 70 mg of the three-dimensional porous graphene oxide solid obtained above in 35 mL of ultrapure water, add urea at a mass ratio of 50:1 between urea solid and three-dimensional...

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Abstract

The invention discloses a nitrogen-doped three-dimensional porous graphene-based electrode material and a preparation method and application thereof, and belongs to the technical field of electrochemistry. The preparation method comprises the following specific steps: (1) mixing a graphene oxide solution with a hydrogen peroxide solution, and conducting reacting to obtain three-dimensional porousgraphene oxide; 2) mixing the three-dimensional porous graphene oxide with urea, and performing hydrothermal reaction to obtain nitrogen-doped three-dimensional porous graphene; and 3) preparing nitrogen-doped three-dimensional porous graphene into a dispersion liquid, and dropwise adding the dispersion liquid to the center of a glassy carbon electrode substrate to obtain the nitrogen-doped three-dimensional porous graphene-based electrode material. The preparation method is simple in process and high in operability, and the nitrogen-doped three-dimensional porous graphene-based electrode material prepared by the preparation method is used in an electrochemical sensor, can be used for detecting the content of organophosphorus pesticide methyl parathion, and has the advantages of high sensitivity, short response time, high anti-interference capability, good repeatability, good long-term stability and high recovery rate.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry, and in particular relates to a nitrogen-doped three-dimensional porous graphene-based electrode material and a preparation method and application thereof. Background technique [0002] Organophosphorus pesticides (OPs) have been used in agricultural production all year round to improve agricultural productivity due to their strong toxicity and good efficacy. Methyl parathion (MP) is the most commonly used organophosphorus pesticide in agricultural pest control, but its The pollution to the environment cannot be ignored. Even a small amount of MP residues can pollute water and soil. In addition, MP may penetrate into plant tissues and stay in plants, such as fruits and vegetables. Once ingested by the human body, even a small amount can cause The denaturation of human acetylcholinesterase (AChE) leads to interruption of nerve signal transmission, which can cause serious consequences such ...

Claims

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Application Information

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IPC IPC(8): C01B32/19C01B32/194G01N27/30
CPCC01B32/19C01B32/194G01N27/308
Inventor 杨永强张艳陈振斐章路王勤生
Owner SPECIAL EQUIP SAFETY SUPERVISION INSPECTION INST OF JIANGSU PROVINCE
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