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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, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc. problems such as the speed of nanoparticle nucleation, to achieve the effect of convenient operation and prevention of overlapping

Inactive Publication Date: 2011-09-28
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Abstract
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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

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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

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Example Embodiment

[0031] Example 1

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

[0033] 1. In a round-bottom flask, add 50 mL of concentrated sulfuric acid (92 g), heat it to 80-90°C in an oil bath, and then add 10 g of potassium persulfate and 10 g of phosphorus pentoxide. 10g of natural graphite powder was slowly added to the above solution. This 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, the solid was dried under vacuum for more than one day, and finally pre-oxidized graphite powder was obtained;

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

Example Embodiment

[0038] Example 2

[0039] 1. In a round-bottom flask, add 50 mL of concentrated sulfuric acid (92 g), heat it to 80-90°C in an oil bath, and then add 16 g of potassium persulfate and 16 g of phosphorus pentoxide. 20g of natural graphite powder was slowly added to the above solution. This 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, the solid was dried under vacuum for more than one day, and finally pre-oxidized graphite powder was obtained;

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

Example Embodiment

[0044] Example 3

[0045] In a 50 mL round bottom flask, add 20 mL of N-methylpyrrolidone solution. Under nitrogen protection, add a certain amount of palladium acetylacetonate to the above solution. Under fully stirring, use a heating mantle to heat it After reaching the optimal reaction temperature of 180-200°C, after reacting for 2 hours and cooling to room temperature, add 20 mL of ethanol to obtain a black precipitate. After washing with a large amount of ethanol and acetone, dry to obtain palladium nanoparticles. figure 2 (C), the result shows 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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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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