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Preparation method of graphite oxide phase carbon nitride modified electrode and its application to detection of heavy metal ions

A graphite-phase carbon nitride and modified electrode technology, which is applied in the direction of material electrochemical variables, can solve the problems of easy stacking of sheets, difficulty in compounding, and film formation problems, and achieve large specific surface area, ultra-high sensitivity, and improved compatibility. sexual effect

Active Publication Date: 2017-03-15
YANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

but in g - C 3 N 4 There is a problem in the application process, due to g -C 3 N 4 High chemical stability, each sheet has a strong force, and the surface is in an inert state, which makes the sheets easy to stack together and difficult to disperse, difficult to dissolve in solvents, and even more difficult to combine with other inorganic materials or Organic materials are evenly compounded
This gives g - C 3 N 4 The film formation caused certain problems

Method used

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  • Preparation method of graphite oxide phase carbon nitride modified electrode and its application to detection of heavy metal ions
  • Preparation method of graphite oxide phase carbon nitride modified electrode and its application to detection of heavy metal ions
  • Preparation method of graphite oxide phase carbon nitride modified electrode and its application to detection of heavy metal ions

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preparation example Construction

[0032] The preparation method of graphite oxide phase carbon nitride modified electrode comprises the following steps:

[0033] First, the preparation of graphite oxide phase carbon nitride:

[0034] (1) Add concentrated sulfuric acid under the condition of ice-water bath, add graphite phase carbon nitride under magnetic stirrer, the solution turns yellow, then slowly add potassium permanganate, time after adding, and react 2-3 under stirring Hour, the solution becomes dark brown, and the controlled reaction temperature is no more than 5°C;

[0035] (2) The dark brown solution obtained in step (1) continued to stir and react in a water bath at 35-45 °C, and a large number of bubbles were generated. After reacting for 1 hour, slowly add deionized water to dilute;

[0036] (3) Add 1-2 mol / L hydrogen peroxide to the diluent obtained in step (2) for reduction, and strictly control the reduction temperature at 35-45 °C until the solution is milky white;

[0037](4) Continue to fi...

Embodiment 1

[0049] 1. Synthesis steps of graphite oxide phase carbon nitride:

[0050] (1) A certain amount of melamine was weighed and placed in a tube furnace, calcined at 550 °C for 2 h at a heating rate of 5 °C / min, and ground to obtain powdery carbon nitride with light yellow graphite structure (g - C 3 N 4 ).

[0051] (2) Add 46 ml of concentrated sulfuric acid in an ice-water bath, and add 2 g of graphite-phase carbon nitride under a magnetic stirrer.

[0052] (3), slowly add 6 g KMnO in step 2 4 , Timing after addition, reacted for 3 hours under stirring, the solution was dark brown.

[0053] (4) Transfer the beaker in step 3 to a water bath at a temperature of 35 °C, continue magnetic stirring, slowly add 200 ml of deionized water for dilution, control the temperature not to exceed 40 °C, and react for 1 h.

[0054] (5), slowly add 5% hydrogen peroxide to the beaker in step 4 for reduction, the solution is milky white. Strain while hot. Wash thoroughly with 5% HCl and deion...

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Abstract

The preparation method of graphite oxide phase carbon nitride modified electrode comprises: (1) preparation of graphite oxide phase carbon nitride; (2) preparation of graphite oxide phase carbon nitride sensor. The application of the above electrodes in the detection of heavy metal ions. Graphite oxide phase carbon nitride has a three-dimensional pore structure, large specific surface area, and the surface contains hydrophilic groups such as hydroxyl, carboxyl, and epoxy groups. Applying graphite oxide phase carbon nitride to electrochemical sensors uses differential pulse The stripping voltammetry was used to detect the heavy metal ion Cu2+, and the influence of enrichment time, enrichment potential, solution pH value, modification amount and other factors on the stripping peak current was optimized. Under the experimental conditions of enrichment time 300s, enrichment potential ‑0.6 V, solution pH 4.68, modification volume 12 μL, the standard curve showed a good linear relationship, and the linear range was 1.60×10‑15 mol / L~6.31× 10‑5 mol / L, the linear equation is ip (μA)=1.2533 C(μmol / L)+6.2232, the correlation coefficient (R) is 0.9989, and the detection limit (S / N=3) reaches 1×10‑16 mol / L, which has ultra-high sensitivity for the detection of heavy metal ions.

Description

technical field [0001] The invention relates to the use of new material oxide graphite phase carbon nitride as an electrochemical sensor for detecting heavy metal ions. Background technique [0002] With the rapid development of industry, heavy metal pollution has become one of the increasingly serious environmental pollution problems. Because heavy metals are not easily metabolized by organisms, they are easy to accumulate in organisms, causing heavy metal poisoning. Therefore, the detection of heavy metals is particularly important. Traditional heavy metal detection methods mainly include atomic absorption spectrometry, atomic emission spectrometry, inductively coupled plasma mass spectrometry, etc., but these methods often have the disadvantages of large and expensive equipment, complicated experimental operations, and the need for experienced operators. Stripping voltammetry has the advantages of simple equipment, high sensitivity, and good selectivity, and is widely us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/26G01N27/30
Inventor 王赪胤吕红映陈敬平王春霞
Owner YANGZHOU UNIV