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Preparation method of nano carbon based loaded two-dimensional noble metal cluster composite material

A technology of composite materials and noble metal ions, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. Large-scale batch preparation of graphene composite materials, cumbersome preparation of graphite oxide, etc., to achieve the effect of enhancing synergy, strong application value, and enriching preparation methods

Inactive Publication Date: 2016-02-03
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the graphene composite material invented by this patent has very high catalytic activity for methanol oxidation, the invention has the following disadvantages: first, the preparation of graphite oxide is very cumbersome and the preparation cost is high; more importantly, in the preparation process of the invention Three-step electrochemical reduction of Pb 2+ During the process, graphite oxide will peel off and dissociate part of the sheets under this voltage and melt into the solution. Therefore, only a small part of the graphene-two-dimensional noble metal composite material can be obtained in the preparation process, and most of the Graphene oxide re-dissociates in solution, so this method cannot prepare graphene composites on a large scale and in batches, and its commercial application prospects are greatly affected
However, the currently widely used solution chemical reduction method, microwave reduction and other methods can only prepare composite materials of noble metal nanoparticles such as three-dimensional Pt, and the improvement of the performance of the composite material is far less than that of the two-dimensional Pt atomic cluster composite material.

Method used

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  • Preparation method of nano carbon based loaded two-dimensional noble metal cluster composite material

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Embodiment 1

[0021] The first step is the preparation of oxidized carbon black. 50mg of nano-carbon black (Vulcan, XC-72) was soaked in a mixed solution of 1M sulfuric acid and saturated ammonium persulfate for 24 hours at room temperature, and the oxidized carbon black particles were taken out, and washed 3 times with distilled water to remove sulfuric acid on the surface of carbon black Salt and other sundries should be dried in an oven at 50°C for 12 hours, and stored in a desiccator.

[0022] In the second step, put 50mg of oxidized carbon black into 50ml of distilled water, ultrasonically disperse for 30 minutes, take the dispersed oxidized carbon black suspension and drop it on the glass carbon electrode, let it dry naturally and slowly.

[0023] In the third step, immerse the glass electrode in a lead nitrate solution with a concentration of 2mM, and adjust its pH value to 11 with a 1M NaOH solution, and the immersion reaction time is 2h.

[0024] The fourth step is to take out the...

Embodiment 2

[0027] The first and second steps of this implementation are the same as in Embodiment 1.

[0028] The third step is to immerse the glass electrode in 2mM lead nitrate solution and adjust its pH value to 12 with 1M NaOH solution for 4 hours.

[0029] The fourth step is to take out the glass carbon electrode and insert 0.1M NaClO 4 solution, in N 2 In the atmosphere, the electrochemical reduction was carried out at the potential of –1V for 5min. (The reference electrode is Ag / AgCl, 3MCl ? electrode).

[0030] In the fifth step, after reduction, the glassy carbon electrode was placed in N 2 Immerse in 0.5mM K under gas protection 2 PtCl 4 and 0.5mM RuCl 3 In the mixed solution, react for 10 minutes, take out the glass carbon electrode and wash it with distilled water. Its methanol oxidation reaction is about 14 times the catalytic activity of commercial E-TEKPtRu / C (carbon black-based). (Catalytic activity test conditions: the reference electrode is Ag / AgCl, 3MCl ? Ele...

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Abstract

The invention discloses a preparation method of a nano carbon based loaded two-dimensional noble metal cluster composite material. According to the invention, nano carbon refers to nano carbon black. The method comprises the following steps: immersing the carbon black into a mixed solution of sulfuric acid and ammonium persulfate, and oxidizing the surface of the carbon black to carry an oxygen-containing radical; carrying out ultrasonic dispersion on a carbon black water solution subjected to oxidization treatment to form a carbon black suspension solution; dripping the carbon black suspension solution to the surface of a glass electrode and slowly drying; immersing the glass electrode into a Pb<2+> solution for a period of time and carrying out exchange reaction on Pb<2+> and the oxygen-containing radical on the surface of the carbon black; adsorbing the Pb<2+> to the surface of the carbon black through the oxygen-containing radical on the surface of the carbon black; carrying out electrochemical reduction on the glass electrode and reducing the Pb<2+> into PbO; immersing the glass electrode into a solution of noble metal ions so as to carry out replacement reaction on the noble metal ions and the PbO; and finally, depositing a two-dimensional noble metal cluster on the surface of the carbon black. The nano carbon based loaded two-dimensional PtRu cluster composite material prepared by the invention has ultrahigh catalytic activity on methanol oxidation reaction; and according to the invention, preparation methods of the nano carbon based composite material are hopeful to enrich, the structure of the material is optimized and the performance of the material is improved.

Description

technical field [0001] The invention relates to a preparation method for depositing a two-dimensional precious metal atomic cluster composite material on the surface of nano carbon black. The carbon black-based two-dimensional PtRu composite material prepared by the method has super high catalytic activity for methanol oxidation reaction. It belongs to the technical field of carbon materials. Background technique [0002] Direct methanol fuel cell (DMFC) has the advantages of high cell efficiency and energy density, low operating temperature, quick start-up, etc., and has no fuel storage, transportation and other safety problems that hydrogen ion membrane fuel cells have, so it is considered as a portable electronic device, Ideal power sources for mobile phones, video cameras and electric vehicles, fuel cells are the most likely to achieve commercial application. At present, one of the main obstacles to the commercial application of DMFC is the low activity of the catalyst ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J37/34H01M4/92
CPCY02E60/50
Inventor 胡忠良胡舜钦席柳江秦士林黄志
Owner HUNAN UNIV OF TECH
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