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Preparation method for synthesizing graphene loaded noble metal catalyst in organic phase

A precious metal catalyst, a technology for synthesizing graphite, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve uneven dispersion, large size of metal nanoparticles, and affect the speed of metal nanoparticles nucleation and other problems to achieve the effect of preventing overlapping and convenient operation

Inactive Publication Date: 2012-12-12
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

(See: (a) Y.J. Li, W. Gao, L.J. Ci, C.M. Wang, P.M. Ajayan, Carbon, 2010, 48, 1124-1130. (b) N.G. Shang, P. Papakonstantinou, P. Wang, S. Ravi. P. Silva, J. Phys. Chem. C, 2010, 114, 15837-15841. (c) S.J. Guo, S.J. Dong, and E.K. Wang, ACS Nano. 2010, 4, 4559-64. (d) Y.C. Si, and E. T.Samulski, Chem. Mater. 2008, 20, 6792-6797.) Especially when sodium borohydride and hydrazine hydrate are used as reducing agents, adding the reducing agent solution slowly can also reduce metal ions to metal nanoparticles and finally adsorb on the surface of graphene, but Since the reducing agent is added in addition, it is very easy to produce a local reducing agent concentration greater than that at other locations, which affects the nucleation speed of metal nanoparticles, so the metal nanoparticles obtained by this method are large in size and unevenly dispersed.

Method used

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  • Preparation method for synthesizing graphene loaded noble metal catalyst in organic phase
  • Preparation method for synthesizing graphene loaded noble metal catalyst in organic phase
  • Preparation method for synthesizing graphene loaded noble metal catalyst in organic phase

Examples

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Embodiment 1

[0032] Such as figure 1 As shown, the preparation method described in this example includes the following steps (precious metal precursor palladium acetylacetonate, stabilizer oleylamine and trioctylphosphine are particularly preferred):

[0033] 1. In a round bottom flask, add 50 mL of concentrated sulfuric acid (92 g), heat to 80-90°C in an oil bath, then add 10 g of potassium persulfate and 10 g of phosphorus pentoxide. 10 g of natural graphite powder was slowly added to the above solution. The mixture was kept in an oil bath at 80-90°C for 4 hours. After cooling to room temperature, the mixture was diluted with deionized water, then vacuum filtered, washed with 3 L of deionized water, and the solid was dried under vacuum for more than one day to finally obtain pre-oxidized graphite powder;

[0034] 2. In a 2L beaker, add 230 mL (4.3 mol) of concentrated sulfuric acid, cool to 0°C, then add 5 g (0.42 mol) of pre-oxidized graphite powder in the first step, and then divide...

Embodiment 2

[0039] 1. In a round bottom flask, add 50 mL of concentrated sulfuric acid (92 g), heat to 80-90°C in an oil bath, then add 16 g of potassium persulfate and 16 g of phosphorus pentoxide. Slowly add 20 g of natural graphite powder into the above solution. The mixture was kept in an oil bath at 80-90°C for 4 hours. After cooling to room temperature, the mixture was diluted with deionized water, then vacuum filtered, washed with 3 L of deionized water, and the solid was dried under vacuum for more than one day to finally obtain pre-oxidized graphite powder;

[0040] 2. In a beaker, add 421 mL (2.15 mol) of concentrated sulfuric acid, cool to 0°C, then add 6 g (0.5 mol) of pre-oxidized graphite powder in the first step, and then add 60 g (0.19 mol) of potassium permanganate in batches Add to the beaker while keeping the temperature below 10°C, then keep in a water bath at 38°C for an optimal time of 2 hours. This mixture was diluted with 0.6L of deionized water, stirred for 2 ho...

Embodiment 3

[0045] In a 50 mL round bottom flask, add 20ml of N-methylpyrrolidone solution, under the condition of nitrogen protection, add a certain amount of palladium acetylacetonate to the above solution, and heat it with a heating mantle under the condition of sufficient stirring The optimal reaction temperature is 180-200°C. After 2 hours of reaction, after cooling to room temperature, add 20mL of ethanol to obtain a black precipitate, wash with a large amount of ethanol and acetone, and dry to obtain palladium nanoparticles. For XRD results, see figure 2 (c), the results show that the simple substance of palladium was successfully obtained.

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Abstract

The invention discloses a preparation method for synthesizing a graphene loaded noble metal catalyst in an organic phase, and belongs to the technical field of catalysts and preparation thereof. The method mainly comprises the following steps of: preparing pre-oxidized graphite powder; preparing glassy yellow oxidized graphite solution; preparing an oxidized graphite solid; dispersing oxidized graphite in N-methylpyrrolidone solution, and stripping the oxidized graphite by ultrasonic processing to prepare the N-methylpyrrolidone solution of oxidized graphene; and adding a stabilizing agent and a precursor of noble metal into the N-methylpyrrolidone solution of oxidized graphene, mixing fully, and heating to obtain the graphene loaded monodisperse noble metal catalyst in one step. The graphene loaded noble metal nano particle catalyst prepared by the method has high structural stability, dispersibility, stability and activity and large specific surface area.

Description

technical field [0001] The invention belongs to the technical field of catalysts and their preparation, in particular to a method for preparing graphene-loaded noble metal catalysts. Background technique [0002] Graphene, that is, single-layer graphite, is made of sp 2 A new type of carbon material with a two-dimensional honeycomb structure of monomolecular layer thickness composed of hybridized carbon atoms connected to each other. Due to its special structure, graphene has many special physical properties and extraordinary electrical, thermal, optical and mechanical properties, and has great potential in nanoelectronic devices, composite materials, energy storage materials, catalytic materials, sensing materials, etc. application prospects. Since its discovery before 2004 (see: K. S. Novoselov, A. K. Geim, S. V. Morozov, D. Jiang, Y. Zhang, S. V. Dubonos, I. V. Grigorieva, and A. A. Firsov Science, 2004, 306, 666-669), there has been a lot of research on graphene Basic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J37/16B82Y40/00
Inventor 张校刚杨苏东申承民高鸿钧
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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