WO2023142668A1 - Méthode de préparation d'un matériau composite d'oxyde de graphène réduit-points de carbone dopés à l'azote et son utilisation - Google Patents

Méthode de préparation d'un matériau composite d'oxyde de graphène réduit-points de carbone dopés à l'azote et son utilisation Download PDF

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WO2023142668A1
WO2023142668A1 PCT/CN2022/135783 CN2022135783W WO2023142668A1 WO 2023142668 A1 WO2023142668 A1 WO 2023142668A1 CN 2022135783 W CN2022135783 W CN 2022135783W WO 2023142668 A1 WO2023142668 A1 WO 2023142668A1
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Prior art keywords
nitrogen
graphene oxide
doped carbon
preparation
solution
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PCT/CN2022/135783
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English (en)
Chinese (zh)
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杨剑波
王梦豪
曹凯峰
刘勇奇
巩勤学
李长东
Original Assignee
湖南邦普循环科技有限公司
广东邦普循环科技有限公司
湖南邦普汽车循环有限公司
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Publication of WO2023142668A1 publication Critical patent/WO2023142668A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/198—Graphene oxide
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

Definitions

  • CQDs have a large specific surface area and strong adsorption capacity, and are rich in functional groups, CQDs have a wide range of applications in the adsorption of various heavy metal ions, organic pollutants and biological macromolecules.
  • CQDs due to the electrical conductivity of carbon quantum dots Poor performance limits its application in the field of electrochemical sensing, and the sensitivity and detection limit of electrochemical sensing in the prior art are poor.
  • the present invention adopts the following technical solutions:
  • a preparation method of nitrogen-doped carbon dots-graphene oxide composite material comprising the following steps:
  • the carbon source is mung bean.
  • Melamine not only acts as a nitrogen source but also has an effective synergistic catalytic effect during the reaction.
  • the inner lining of the reactor for hydrothermal reaction is polytetrafluoroethylene.
  • the electrode is a glassy carbon electrode, which is prepared by the following method: wet polishing the glassy carbon electrode, then ultrasonically cleaning, scanning, drying with nitrogen, and sequentially heating the electrode in K 3 [ Fe(CN) 6 ], K 4 [Fe(CN) 6 ] and KCl electrolyte solution are scanned to obtain a glassy carbon electrode with a potential difference between the oxidation peak and the reduction peak below 100mV.
  • the scanning potential of the cyclic voltammetry reduction is -1.5-0V
  • the scanning rate is 0.05-0.1V/s
  • the number of scanning is 30-40 cycles.
  • An electrochemical sensor comprising the nitrogen-doped carbon dot-graphene oxide composite material prepared by the preparation method.
  • Graphene oxide has good electrochemical performance and large specific surface area, and can form coordination compounds with different metal ions through coordination bonds, but the active sites and oxygen-containing functional groups on its surface limit its Applications in the field of electrochemical sensing. Then, chemical modification can be used to increase the active sites.
  • a variety of functional groups can be introduced on the surface of graphene oxide through covalent or non-covalent interactions, so as to modify graphene oxide to make it functional and improve Graphene oxide has the ability to adsorb and enrich analytes.
  • doping other atoms in graphene oxide can adjust the energy band structure of electrons and improve the physical and chemical properties and electrochemical activity of graphene oxide.
  • Fig. 1 is the synthetic schematic diagram of nitrogen-doped carbon dots-reduced graphite oxide composite material of the present invention
  • Fig. 3 is the transmission electron micrograph of the nitrogen-doped carbon dot-reduced graphite oxide composite material of embodiment 1 of the present invention.
  • the nitrogen-doped carbon dot solution and the reduced graphene oxide solution are ultrasonically mixed according to a volume ratio of 2:1 to obtain a nitrogen-doped carbon dot/reduced graphene oxide mixed solution;
  • the preparation method of the nitrogen-doped carbon dots-reduced graphene oxide composite material (Er-NCQD/rGO) of the present embodiment comprises the following steps:
  • the preparation method of the nitrogen-doped carbon dot-reduced graphene oxide composite material of this comparative example comprises the steps:
  • the nitrogen-doped carbon dot solution and the reduced graphene oxide solution are ultrasonically mixed at a volume ratio of 2:1 to obtain a nitrogen-doped carbon dot/reduced graphene oxide mixed solution.
  • the nitrogen-doped carbon dot-graphene oxide (Er-NCQD/rGO) composite material prepared by electroreduction using specific implementation 1, specific implementation 2 and specific implementation 3 is prepared into an electrochemical sensor, and then The soil in the experimental farmland is used as a sample to detect heavy metal ions.
  • the amount of Cd 2+ added in Example 1 is 100.00 ⁇ g/L, and the total detection amount can reach 106.91 ⁇ g/L, which reduces the detection limit and improves the recovery rate. .
  • Fig. 2 is the transmission electron microscope picture of the nitrogen-doped carbon dot of embodiment 1 of the present invention; , the dispersion is good, and the size is relatively uniform and uniformly dispersed without aggregation.
  • Fig. 4 is the scanning electron micrograph of the nitrogen-doped carbon dot-reduced graphite oxide composite material of embodiment 1 of the present invention.
  • the pre-reduced graphene oxide is stacked in sheets and has a certain three-dimensional shape on the surface, which provides a larger specific surface area, while NCQDs cannot be shown in the figure because of their small particle size.
  • NCQDs For individual NCQDs, the FT-IR spectrum shows an absorption peak between 3263-3712 cm -1 indicating the presence of hydroxyl (-OH), and NCQDs contain various oxygen-containing functional groups, such as hydroxyl, carbonyl, ether or ring Oxygen, these oxygen-containing functional groups provide a large number of lone pairs of electrons, which can provide electron donors when electrochemically detecting heavy metal ions, which is conducive to the enrichment of heavy metal ions to enhance the sensitivity of detection.
  • oxygen-containing functional groups such as hydroxyl, carbonyl, ether or ring Oxygen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Nanotechnology (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne une méthode de préparation d'un matériau composite d'oxyde de graphène-points de carbone dopés à l'azote et son utilisation. La méthode comprend les étapes suivantes consistant à : mélanger une source de carbone et une source d'azote, réaliser une réaction hydrothermique, et réaliser une séparation solide-liquide pour donner une solution de points de carbone dopés à l'azote ; mélanger de l'oxyde de graphène et un agent réducteur, agiter, réaliser une séparation solide-liquide, et dissoudre la phase solide pour donner une solution d'oxyde de graphène pré-réduite ; et mélanger la solution de points de carbone dopés à l'azote et la solution d'oxyde de graphène pré-réduite par sonication, ajouter goutte à goutte le mélange sur une électrode, et réaliser une voltampérométrie cyclique pour réduction pour donner le matériau composite d'oxyde de graphène-points de carbone dopés à l'azote.
PCT/CN2022/135783 2022-01-28 2022-12-01 Méthode de préparation d'un matériau composite d'oxyde de graphène réduit-points de carbone dopés à l'azote et son utilisation WO2023142668A1 (fr)

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CN202210105592.8 2022-01-28
CN202210105592.8A CN114538409A (zh) 2022-01-28 2022-01-28 氮掺杂碳点-还原氧化石墨烯复合材料的制备方法和应用

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CN117088361A (zh) * 2023-10-20 2023-11-21 北京化工大学 一种针状焦基碳点及其水凝胶复合材料的制备方法和应用

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CN114538409A (zh) * 2022-01-28 2022-05-27 湖南邦普循环科技有限公司 氮掺杂碳点-还原氧化石墨烯复合材料的制备方法和应用
CN115616050B (zh) * 2022-12-02 2023-04-07 杭州德海艾科能源科技有限公司 一种钒电池电解液离子浓度传感器材料的制备方法及应用
CN115888811A (zh) * 2022-12-29 2023-04-04 云南省烟草质量监督检测站 纳米酶材料及其制备方法和应用、Pb2+离子的检测方法
CN116588917B (zh) * 2023-06-30 2024-05-14 苏州擎动动力科技有限公司 一种载体及其制备方法和应用

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Publication number Priority date Publication date Assignee Title
CN117088361A (zh) * 2023-10-20 2023-11-21 北京化工大学 一种针状焦基碳点及其水凝胶复合材料的制备方法和应用

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