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Preparation and application of a porous hollow carbon nanosphere material

A carbon nanosphere and hollow technology, applied in the field of electrochemical detection and nanomaterials, can solve the problems of reagent toxicity, time-consuming operation, complex instruments, etc.

Active Publication Date: 2022-01-28
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of them have some unavoidable disadvantages, such as the toxicity of reagents, complicated instruments, time-consuming operations

Method used

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  • Preparation and application of a porous hollow carbon nanosphere material
  • Preparation and application of a porous hollow carbon nanosphere material
  • Preparation and application of a porous hollow carbon nanosphere material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1, the preparation of porous hollow carbon nanosphere material PHCNs

[0035] Take 0.38 ml (4.17 mmol) of aniline and 0.29 ml (4.17 mmol) of pyrrole, add them to 60 ml of an aqueous solution containing amphoteric surfactant (60 mg (0.24 mmol)), stir and sonicate until the dispersion is uniform to obtain a mixed solution; then The mixed solution was placed in an ice-water bath and stirred for 20-60 min, then 15 ml of an aqueous solution containing 1.9 g of ammonium persulfate was added, stirred vigorously for 20-50 s, and then slowly stirred for 24-36 h under an ice-water bath environment, and the obtained product was mixed with deionized water and Washing with ethanol and filtering under reduced pressure until the filtrate is neutral and dried to obtain the precursor of the hollow carbon nanosphere material;

[0036] The above-mentioned hollow carbon nanosphere material precursor was placed in a tube furnace, and the temperature was raised to 800 °C at a heat...

Embodiment 2

[0037] Embodiment 2, the preparation of modified electrode PHCNs / GCE

[0038] (1) Pretreatment of the glassy carbon electrode: the glassy carbon electrode is polished into a mirror surface with 0.30 μm and 0.05 μm Al2O3 suspension in sequence, and then ultrasonically cleaned with 95% ethanol and double distilled water in sequence , to obtain the treated glassy carbon electrode; then use the glassy carbon electrode as the working electrode, the platinum column as the counter electrode, and the saturated calomel electrode as the reference electrode in a three-electrode system. M potassium chloride electrolyte solution, carry out cyclic voltammetry scanning (scanning speed is 50mV / s), finally take out the electrode and rinse with twice distilled water and dry;

[0039] (2) Preparation of the modified electrode PHCNs / GCE: take 0.005 g of the porous hollow carbon nanosphere material PHCNs prepared in Example 1, and disperse it in 5 ml of water to make a concentration of 1.0 mg·mL ...

Embodiment 3

[0040] Embodiment 3, modified electrode PHCNs / GCE detects NO in the solution 2 -

[0041] (1) Preparation of sample solution: Weigh 0.276 mg of sodium nitrite and dissolve it in 4 ml of ultrapure water to obtain a concentration of 10 -3 M's NO 2 - aqueous solution.

[0042] (2) NO 2 - Concentration detection: use the modified electrode PHCNs / GCE as the working electrode, the platinum column as the counter electrode, and the saturated calomel electrode as the reference electrode to form a three-electrode system, use 0.2M phosphate buffer solution with pH=7.0 as the electrolyte, measure The sample solution prepared in step (1) with a volume of 4 ~ 400 μl was added dropwise to the electrolyte solution, and scanned by chronoamperometry at a working potential of 1.0V. According to the response current Ip and NO 2 - Concentration linear regression equation: Ip (μA) = 13.249[NO 2 − ] (mM) - 0.709 (R 2 = 0.999). Calculate NO 2 - The concentration is 1.014×10 -3 M.

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Abstract

The invention provides a preparation of a porous hollow carbon nanosphere material, which uses aniline and pyrrole as a homopolymerization monomer, ammonium persulfate as an oxidant, and uses a surfactant Triton X-100 to self-assemble into micelles in an aqueous solution, polymerize The monomers are polymerized at the micellar interface to prepare the hollow nanosphere precursor, and then the precursor is carbonized under the protection of an inert gas to obtain the porous hollow carbon nanosphere material PHCNs. Electrochemically modified electrode PHCNs / GCE constructed with PHCNs as NO 2 ‑ sensor, for NO 2 ‑ It has sensitive electrochemical response, and has the characteristics of wide detection range, low detection limit, simple detection process, high sensitivity, strong anti-interference performance, good stability and reproducibility. Very good results, and can be directly used to detect nitrite in pickles.

Description

technical field [0001] The invention relates to a preparation method of a porous hollow carbon nanosphere material, which is mainly used as an electrochemical sensor for detecting nitrite in a solution, and belongs to the technical field of nanometer materials and the technical field of electrochemical detection. Background technique [0002] In recent years, hollow carbon nanospheres, as an important spherical nanomaterial, not only maintain the characteristics of large specific surface area, low density, high strength and good chemical stability of nanoporous carbon materials, but also have a unique carbon shell structure and its surrounding The resulting spherical nano-hollow cavity has received extensive attention in many fields. So far, the template method is the most used method for preparing hollow carbon nanosphere materials. The specific steps of the template method include coating or polymerizing the carbon shell precursor on the surface of predetermined template ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30G01N27/32
CPCG01N27/30G01N27/32
Inventor 刘秀辉张彬雁李琳刘福鑫
Owner NORTHWEST NORMAL UNIVERSITY