Fe coated with polydiallyldimethylammonium chloride 1.833 (oh) 0.5 o 2.5 Nitrogen-doped graphene nanocomposite sensing material and preparation method thereof

A technology of polydiallyldimethylammonium chloride and nitrogen-doped graphene, applied in the direction of material electrochemical variables, etc., can solve the problems of large three wastes, cumbersome and complicated operations, and achieve improved dispersion performance and simple process , easy-to-control effects

Active Publication Date: 2019-07-16
NANJING UNIV OF SCI & TECH
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Problems solved by technology

[0006] The present invention aims at the disadvantages of cumbersome and complicated operation and large wastes in the prior art, and provides a polydiallyldimethylammonium chloride (PDDA)-coated Fe 1.833 (OH) 0.5 o 2.5 Nitrogen-doped graphene (NG) nanocomposite sensing material and its preparation method

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  • Fe coated with polydiallyldimethylammonium chloride <sub>1.833</sub> (oh) <sub>0.5</sub> o <sub>2.5</sub> Nitrogen-doped graphene nanocomposite sensing material and preparation method thereof
  • Fe coated with polydiallyldimethylammonium chloride <sub>1.833</sub> (oh) <sub>0.5</sub> o <sub>2.5</sub> Nitrogen-doped graphene nanocomposite sensing material and preparation method thereof
  • Fe coated with polydiallyldimethylammonium chloride <sub>1.833</sub> (oh) <sub>0.5</sub> o <sub>2.5</sub> Nitrogen-doped graphene nanocomposite sensing material and preparation method thereof

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preparation example Construction

[0030] Such as figure 1 As shown, a polydiallyldimethylammonium chloride (PDDA)-coated Fe 1.833 (OH) 0.5 o 2.5 A nitrogen-doped graphene (NG) nanocomposite sensing material and a preparation method thereof, the method comprising the following steps:

[0031] Step 1, adopt the improved Hummers method to prepare graphite oxide solid with natural graphite powder;

[0032] Step 2. Under ultrasonication, prepare an ethanol suspension of graphene oxide, the ratio of graphite oxide to ethanol solvent is 1 ~ 0.2 mg / ml; ultrasonic time is 5 ~ 24 h;

[0033] Step 3, add PDDA to the suspension in step 2 and stir evenly, the ratio of graphite oxide and PDDA is 1:1 ~ 1:10 mg / μl; add FeCl 2 4H 2 O into the suspension and stir well, graphite oxide and FeCl 2 4H 2 The mass ratio of O is 1: 3~2: 1 mg / mg;

[0034] Step 4, mix the mixture of step 3 with NH 3 ·H 2 After O is mixed, it is quickly loaded into a hydrothermal reactor and heated for reaction; graphite oxide and NH 3 ·H 2 T...

Embodiment 1

[0037] The first step, the preparation of graphite oxide solid;

[0038] At 80°C, 20 g of natural graphite was preoxidized with 30 ml of concentrated sulfuric acid, 10 g of potassium persulfate and 10 g of phosphorus pentoxide, washed with water to pH = 7, and dried overnight at room temperature for use;

[0039] Cool 460 ml of concentrated sulfuric acid to about 0 °C, then add 20 g of pre-oxidized graphite into it, slowly add 60 g of potassium permanganate, so that the temperature of the system does not exceed 20 °C, after the addition is completed, heat up to 35 °C, and stir After 2 hours, slowly add 920 ml of deionized water in batches so that the temperature of the system does not exceed 98 °C. After stirring for another 15 minutes, add 2.8 L of deionized water and 50 ml of 30% hydrogen peroxide. The resulting bright yellow suspension was filtered under reduced pressure and washed. Until there is no sulfate ion in the filtrate, and when it is neutral, the product is dried i...

Embodiment 2

[0048] The first step is the same as Step 1 in Example 1.

[0049] In the second step, put 50 mg of graphite oxide powder into a round bottom flask, then add 50 ml of ethanol solvent, and obtain a graphene oxide (GO) suspension after ultrasonication for 24 h;

[0050] In the third step, add 500 μl PDDA to the suspension in step 2 and stir well, then add 0.15 gFeCl 2 4H 2 O into the suspension and stir evenly;

[0051] In the fourth step, mix the mixture from step 3 with 250 μl NH 3 ·H 2 After O was mixed, it was quickly put into a hydrothermal reactor, and heated at 180 °C for 12 h;

[0052] The fifth step is the same as step five in Example 1.

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Abstract

The present invention discloses a polydiallyldimethylammonium chloride-coated Fe1.833(OH)0.5O2.5 supported nitrogen-doped graphene nanometer composite sensing material and a preparation method thereof. The preparation method comprises: under ultrasound, preparing the ethanol suspension of graphene oxide by using a graphite oxide solid; adding PDDA to the suspension, uniformly stirring, continuously adding FeCl2.4H2O, and uniformly stirring; mixing the obtained mixture and NH3.H2O, and immediately carrying out a hydrothermal reaction, wherein a ratio of graphite oxide to NH3.H2O is 1:1-1:5 mg / [mu]l, and the reaction temperature is 160-200 DEG C; and washing, and drying to obtain the sensing material. According to the present invention, the preparation of the sensing material is the one-pothydrothermal assembly method scientifically integrating the in-situ growth of the nanometer metal oxide, the synchronous reduction of the graphene oxide and the polymer coating functionalization; andthe synthesized hybrid material has advantages of simple synthesis steps, high efficiency and easy large-scale preparation, and is particularly suitable for the electrochemical catalytic detection andanalysis of nitrites.

Description

technical field [0001] The invention relates to a functionalized graphene nanomaterial and a preparation method thereof, in particular to a polydiallyldimethylammonium chloride (PDDA)-coated Fe 1.833 (OH) 0.5 o 2.5 The invention relates to a nitrogen-doped graphene (NG) nanocomposite sensing material and a preparation method thereof, belonging to the field of material preparation. Background technique [0002] Nitrite widely exists in the human environment, is the most common nitrogen-containing compound in nature, the nitrogen source of green plants, and is often used as food additives and preservatives in the food industry. Nitrite pollution in drinking water can lead to many diseases such as methemoglobinemia, blue baby syndrome, and gastric cancer. These diseases are all caused by nitrosamines generated by the reaction of nitrite and amines. Due to the harmful effects of nitrite on the environment and human health, the sensitive detection of nitrite has attracted grea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/26
Inventor 张树鹏刘茂祥宋海欧高娟娟钱悦月王霜谢康俊
Owner NANJING UNIV OF SCI & TECH
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