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

A technology of graphite phase carbon nitride and electrode modification, applied in the direction of electrochemical variables of materials, etc., can solve the problems of film formation, easy stacking of lamellae, difficult compounding, etc., and achieves improved compatibility, large specific surface area, and improved dispersion. sexual effect

Active Publication Date: 2015-05-20
YANGZHOU UNIV
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Problems solved by technology

But there is a problem in the application of g - C3N4, because g - C3N4 >The chemical stability is high, each layer has a strong force, and the surface is in an inert state, which makes the layers 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 has caused some difficulties in the film formation of g - C3N4

Method used

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  • Preparation method of graphite oxide phase carbon nitride modified electrode and application of electrode in detection of heavy metal ions
  • Preparation method of graphite oxide phase carbon nitride modified electrode and application of electrode in detection of heavy metal ions
  • Preparation method of graphite oxide phase carbon nitride modified electrode and application of electrode in 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 in an ice-water bath, add graphite phase carbon nitride under a magnetic stirrer, the solution turns yellow, then slowly add potassium permanganate, time after the addition, and react for 2-3 hours 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 f...

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. Fully washed with 5% HCl and deionize...

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Abstract

The invention relates to a preparation method of a graphite oxide phase carbon nitride modified electrode. The preparation method comprises the following steps: (1) preparing graphite oxide phase carbon nitride; and (2) preparing a graphite oxide phase carbon nitride sensor. The electrode is applied to detecting heavy metal ions. Graphite oxide phase carbon is of a three-dimensional hole structure which is large in specific surface area and contains hydrophilic groups such as hydroxyl, carboxyl, and epoxy groups. The graphite oxide phase carbon is applied to an electrochemical sensor. The heavy metal ions Cu<2+> are detected by virtue of a different pulse stripping voltammetry, and influence of factors such as enriching time, enriching potential, the pH value of a solution, and modification amount on stripping peak current can be optimized. Under an experimental condition that the enriching time is 300s, the enriching potential is -0.6V, the pH value of the solution is 4.68 and the modification amount is 12 microliters, a standard curve represents a good linear relationship, wherein the linear range is (1.60*10<-15>-6.31*10<-15>mol/L, the linear equation is ip(microA)=1.2533C(micro mol/L)+6.2232, the correlation coefficient (R) is 0.9989, and the limit of detection (S/N=3) reaches 1*10<-16>mol/l. The electrode has ultrahigh sensitivity to heavy metal ion detection.

Description

Technical field [0001] The present invention involves the use of new material oxide galcotte nitride as an electrochemical sensor for detecting heavy metal ions. Background technique [0002] With the rapid development of the industry, heavy metal pollution has become one of the increasingly serious environmental pollution problems. Because heavy metals are not easy to be metabolized by biology, it is easy to accumulate in biology, causing heavy metal poisoning.Therefore, the detection of heavy metals is particularly important.Traditional detection of heavy metal methods mainly include atom absorption spectral method, atomic launch spectrum method, inductive coupling plasma mass spectrometry method, etc., but these methods often have shortcomings and equipment instruments, complicated experimental operations, and experienced operators.The solubility of the amphibious method has the advantages of simple instrument equipment, high sensitivity, and good selectivity. It is widely use...

Claims

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Application Information

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