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Silver-Prussian-blue-loaded nitrogen-doped graphene composite material and preparation method and application thereof

A nitrogen-doped graphene and Prussian blue technology is applied in the field of electrochemical detection, which can solve the problems of high detection limit and low detection limit of sodium nitrite, and achieves low detection limit, good storage stability, and high detection limit. wide range of effects

Active Publication Date: 2019-11-08
湖南角山米业有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The primary technical problem to be solved by the present invention is to provide a silver-Prussian blue-loaded nitrogen-doped graphene composite in order to overcome the problem that the chemically modified electrode used to detect sodium nitrite in the prior art has a high detection limit. The preparation method of the material; the modified electrode prepared by the material has a lower detection limit for the detection of sodium nitrite

Method used

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  • Silver-Prussian-blue-loaded nitrogen-doped graphene composite material and preparation method and application thereof
  • Silver-Prussian-blue-loaded nitrogen-doped graphene composite material and preparation method and application thereof
  • Silver-Prussian-blue-loaded nitrogen-doped graphene composite material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] The preparation of the nitrogen-doped graphene composite material of embodiment 1 silver-Prussian blue load

[0047] (1) Synthesis of Prussian blue: to 0.016g K 3 [Fe(CN) 6 ], add 2.5mL of concentrated hydrochloric acid, 10mL of deionized water, 5mL of N-N-dimethylformamide (DMF), react in the reaction kettle for 24h, the reaction temperature is 80°C, and then the reaction solution is centrifuged and washed. get Prussian blue;

[0048] (2) Prepare the Prussian blue dispersion: disperse the obtained Prussian blue in 20 mL of deionized water, add 0.75 g of glucose and stir for 30 minutes to obtain the Prussian blue dispersion;

[0049] (3) Configure silver ammonia solution: take 0.102g AgNO 3 Disperse in 10mL deionized water, add ammonia water until the precipitate disappears to obtain silver ammonia solution;

[0050] (4) Add 1mL min to the Prussian blue dispersion -1 Add the silver ammonia solution at a high speed, heat in a water bath at 35°C for 30 minutes, and l...

Embodiment 2

[0062] Example 2 Preparation of silver-Prussian blue-loaded nitrogen-doped graphene composite modified electrode

[0063] Using 0.3μm and 0.05μm Al 2 o 3 Polish the glassy carbon electrode (diameter 3mm) on sandpaper to a smooth mirror surface, then use 1:1 dilute nitric acid, acetone and distilled water to ultrasonically clean the glassy carbon electrode for 5 minutes, and then dry it under an infrared lamp for later use. Good glassy carbon electrode. Then, take 1 mg of the silver-Prussian blue-loaded nitrogen-doped graphene composite material prepared in Example 1 and add it to 2 mL of N,N-dimethylformamide, and ultrasonically disperse it for 5 minutes to obtain the silver-Prussian blue-loaded nitrogen-doped graphene composite. The dispersion liquid of heterographene composite material, drop 6 μL of the dispersion liquid on the surface of the treated glassy carbon electrode, and dry it under the irradiation of infrared light to prepare the nitrogen-doped graphene composite...

Embodiment 3

[0065] Example 3 Detection performance of silver-Prussian blue loaded nitrogen-doped graphene composite modified electrode

[0066] In this example, each modified electrode prepared in Example 2 was used as the experimental object, and a three-electrode system was formed with it, a platinum auxiliary electrode, and a saturated calomel reference electrode, and it was connected to a CHI660 electrochemical workstation (Shanghai Chenhua Instrument Co., Ltd.) Electrochemical performance testing.

[0067] (1) Comparison of electrocatalytic oxidation performance of different electrodes for sodium nitrite

[0068] Use glassy carbon electrode, nitrogen-doped graphene modified electrode, Prussian blue-loaded nitrogen-doped graphene modified electrode and the silver-Prussian blue-loaded nitrogen-doped graphene composite modified electrode electrode prepared in Example 2, measure 1mmol Cyclic voltammogram of / L sodium nitrite in the phosphoric acid bottom solution of pH=6.9. And the chr...

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Abstract

The invention discloses a silver-Prussian-blue-loaded nitrogen-doped graphene composite material and a preparation method and application thereof. The preparation method comprises the following stepsof adding concentrated hydrochloric acid, deionized water and N-N-dimethylformamide into K3[Fe(CN)6] for a reaction in a reaction kettle to obtain Prussian blue; dispersing the Prussian blue in deionized water, adding glucose, and stirring the mixture to obtain a Prussian blue dispersion; adding a silver ammonia solution into the Prussian blue dispersion, heating the mixture through a water bath,and performing standing; separating and washing products to obtain a silver-Prussian blue material; adding the silver-Prussian blue material into N,N-dimethylformamide-dispersed nitrogen-doped graphene to obtain the silver-Prussian-blue-loaded nitrogen-doped graphene composite material. A chemically modified electrode prepared from the silver-Prussian-blue-loaded nitrogen-doped graphene compositematerial can be used for quickly detecting sodium nitrite in food and has the advantages of wide detection range, low detection limit, simple operation and the like.

Description

technical field [0001] The invention relates to the technical field of electrochemical detection, in particular to a nitrogen-doped graphene composite material supported by silver-Prussian blue and its preparation method and application. Background technique [0002] Sodium nitrite is commonly known as nitrite, and its chemical formula is NaNO 2 , is a potential carcinogen mainly found in food, medicine, agriculture and biological samples. Sodium nitrite is not only deliquescent, but also soluble in water and liquid ammonia, and easily converted into sodium nitrate when exposed to air. Sodium nitrite is a strong oxidant and also has reducing properties; sodium nitrite has a salty taste, and is often used by unscrupulous people to make fake table salt or as a substitute for table salt in illegal food production. High levels of nitrite can cause great harm to health and disrupt the balance of the ecosystem. Therefore, the development of rapid and highly sensitive detection ...

Claims

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Application Information

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IPC IPC(8): G01N27/30G01N27/48B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00G01N27/308G01N27/48
Inventor 李俊华贺译婵李娟许志锋刘梦琴易正戟
Owner 湖南角山米业有限责任公司
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