Chlorine-doped graphene and preparation method and application thereof

A graphene and chlorine doping technology, applied in chemical instruments and methods, electrical components, circuits, etc., can solve the problems of high cost of noble metal catalysts, lack of resources, etc., and achieve the improvement of oxygen reduction catalytic activity and stability, and good catalytic activity , the effect of simple process

Active Publication Date: 2013-05-22
永嘉跃龙密封件有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing an oxygen-reducing non-noble metal (i.e., chlorine-doped graphene) catalyst for the disadvantages of high cost and lack of resources of the noble metal catalyst of the current fuel cell. The chlorine-doped graphene catalyst prepared by the method has electrical High chemical catalytic activity, good stability, low cost, long life, etc.

Method used

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  • Chlorine-doped graphene and preparation method and application thereof
  • Chlorine-doped graphene and preparation method and application thereof
  • Chlorine-doped graphene and preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0026] Take 10ml of carbon tetrachloride and add it to a 250ml three-necked flask, reflux at 130°C for 30 minutes, then take 1g of magnesium strips and ignite them in the air and quickly put them into the three-necked flask, a large amount of black matter will be produced instantaneously, filter , to obtain a filter cake.

[0027] The resulting filter cake was rinsed with absolute ethanol to remove excess carbon tetrachloride, and centrifuged (7000 rpm, 5 min) to obtain a black solid substance, that is, precipitate a. Immerse the precipitate a in aqueous hydrochloric acid solution with a mass concentration of 15%, fully stir at 25°C for 30 minutes, and centrifuge (7000rpm, 5min). Take the precipitate b and wash it twice with pure water and absolute ethanol, and then centrifuge again (7000rpm , 5min), to obtain the precipitate c, freeze-dry the precipitate c at -80℃ for 10h, and obtain 50mg of chlorine-doped graphene material, the area of ​​chlorine-doped graphene sheet is 10~4...

Embodiment 2

[0029] Take 10ml of chloroform and add it to a 250ml three-necked flask, reflux at 80°C for 30 minutes to obtain a chloroform reflux liquid, then take 1g of magnesium strips and ignite them in the air and quickly put them into the three-necked flask to generate instantaneous A large amount of black matter was filtered to obtain a filter cake.

[0030]Wash the resulting filter cake with absolute ethanol to remove excess chloroform, and centrifuge (7000rpm, 5min) to obtain precipitate a. Soak the above precipitate a in aqueous hydrochloric acid solution with a mass concentration of 15%, fully stir at 25°C for 30 minutes, centrifuge (7000rpm, 5min), take the precipitate b, wash it twice with pure water and absolute ethanol, and centrifuge again ( 7000rpm, 5min), obtained precipitate c, freeze-dried the precipitate c at -80°C for 10h, obtained 30mg of chlorine-doped graphene material, and the area of ​​chlorine-doped graphene sheet was 10-40μm 2 .

Embodiment 3

[0032] Take 20ml of carbon tetrachloride and add it to a 250ml three-necked flask, reflux at 120°C for 20 minutes to obtain a carbon tetrachloride reflux liquid, then take 1g of magnesium strips and ignite them in the air and quickly put them into the three-necked flask. A large amount of black matter is produced instantaneously, and filtered to obtain a filter cake.

[0033] Wash the resulting filter cake with absolute ethanol to remove excess carbon tetrachloride, and centrifuge (7000rpm, 5min) to obtain precipitate a. Add the above precipitate a into the hydrochloric acid aqueous solution with a mass concentration of 15%, fully stir at 25°C for 30 minutes, centrifuge (7000rpm, 5min), take the precipitate b, wash them twice with pure water and absolute ethanol, and centrifuge again (7000rpm , 5min), to obtain the precipitate c, freeze-dry the precipitate c at 80℃ for 10h, and obtain 40mg of chlorine-doped graphene material, the area of ​​chlorine-doped graphene sheet is 10~4...

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Abstract

The invention discloses a chlorine-doped graphene and a preparation method and an application thereof in preparation of an oxygen reduction electrode. The preparation method of the chlorine-doped graphene comprises the following steps of: refluxing methyl chloride at 65-160 DEG C for 10-30 minutes to obtain a methyl chloride reflux, combusting a magnesium rod in air and rapidly placing in the methyl chloride reflux, and filtering after reaction, so as to obtain a filter cake; flushing the filter cake with absolute ethyl alcohol, and carrying out centrifugal separation to obtain sediment a; adding the sediment a in hydrochloric acid, stirring completely for 10-30 minutes, and carrying out centrifugal separation to obtain sediment b, washing the sediment b successively with purified water and absolute ethyl alcohol, carrying out centrifugal separation on the washing liquid to obtain sediment c, and carrying out freeze drying on the sediment c to obtain the chlorine-doped graphene. The chlorine-doped graphene is high in catalytic activity, and the oxygen reduction catalytic activity and stability are obviously improved. The method is simple in process, convenient to operate, short in reaction time and low in equipment request, and is easy to implement.

Description

(1) Technical field [0001] The invention relates to the preparation of nanometer materials and fuel cells, in particular to a chlorine-doped graphene and its preparation method, and the application of the chlorine-doped graphene as a cathode catalyst material in oxygen reduction. (2) Background technology [0002] A fuel cell is an efficient and clean electrochemical power generation device. In recent years, it has received widespread attention at home and abroad. At present, the cathode catalysts of fuel cells mainly use Pt or Pt-based alloy catalysts. Due to the scarcity of Pt resources and the high price, the large-scale commercial development of fuel cells is seriously hindered. In addition, the commercialized direct methanol fuel cell has poor poisoning resistance of the cathode Pt catalyst. Therefore, developing a non-precious metal catalyst with high catalytic activity, long life and low cost is one of the difficulties in current fuel cell research. [0003] Graphe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/06H01M4/90
CPCY02E60/50
Inventor 金辉乐王舜卜永峰李蔚王健
Owner 永嘉跃龙密封件有限公司
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