Nano-grade composite catalyst, and preparation method and application thereof

A nanocomposite and nanocluster technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. Strong, low precious metal loading efficiency and other issues

Active Publication Date: 2016-02-10
无锡盛鑫氢能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ordinary conductive carbon black, carbon nanotubes, graphene and other materials have poor adsorption capacity for metal nanoclusters in colloidal solutions, ...

Method used

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  • Nano-grade composite catalyst, and preparation method and application thereof
  • Nano-grade composite catalyst, and preparation method and application thereof
  • Nano-grade composite catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] Embodiment 1, the preparation metal content is the Pt-Cu alloy nano-cluster composite catalyst Pt-Cu / MDC1-1 of 16wt% (method one)

[0095] Dissolve 0.1g of melamine in 100mL of water to make a melamine solution. Conductive carbon black (commercially available XC-72R, 0.4g, specific surface area 254m 2 / g) was added to the above-mentioned melamine solution, ultrasonically treated for 20 minutes, and heated in an oil bath at 150° C. to evaporate the solvent water to obtain a melamine-carbon material ( XC-72R) mixture. Under the air atmosphere, the mixture was heated to 613K in a muffle furnace, kept for 1 h and then cooled to room temperature to obtain a carbon material MDC1-1 modified by melamine polycondensate. Elemental analysis showed that the nitrogen content in MDC1-1 was 4.4%. BET specific surface area test shows that the specific surface area of ​​MDC1-1 is 100m 2 / g.

[0096] attached figure 1 The N1sXPS spectra of the raw material Melamine (a), the melam...

Embodiment 2

[0106] Example 2, the preparation of a Pt-Cu alloy nanocluster composite catalyst Pt-Cu / MDC1-2 with a metal content of 41wt%

[0107] (method one)

[0108] The carbon material MDC1-1 modified by melamine condensation polymer was prepared according to the method described in Example 1.

[0109] Dissolve 1 g of chloroplatinic acid hexahydrate in 50 mL of ethylene glycol for later use. Under stirring condition at 313K, 7.6mL chloroplatinic acid hexahydrate (0.31mmol) ethylene glycol solution was added in the ethylene glycol solution (227mL) that was dissolved with 150mg copper acetate monohydrate, the ethylene glycol solution (0.25mol) of NaOH / L) adjust the pH of the above solution to 10, and stir for 30 minutes. The above mixture was added dropwise to 324 mL of ethylene glycol solution in which MDC1-1 (350 mg) was dispersed, heated to reflux at 471K for 4 hours under a nitrogen atmosphere, cooled to room temperature, filtered, washed, and vacuum-dried at 343K for 5 hours. Ta...

Embodiment 3

[0110] Example 3, the preparation of a Pt-Cu alloy nanocluster composite catalyst Pt-Cu / MDC1-3 with a metal content of 27.8wt%

[0111] The Pt-Cu / MDC1-2 catalyst (50mg) prepared in Example 2 was ultrasonically dispersed in 1M nitric acid (20mL), stirred at 298K for 20 hours, centrifuged and washed with water to remove residual acid, the resulting solid product Vacuum drying at 298K for 3 hours to prepare Pt-Cu alloy nano-cluster composite catalyst Pt-Cu / MDC1-3. ICP-AES analysis showed that the Pt / Cu atomic ratio in Pt-Cu / MDC1-3 was 72:28, and the Pt metal loading was 24.7wt%.

[0112] The TEM photo of the PtCu / MDC1-3 catalyst is attached Figure 5 shown. In Pt-Cu / MDC1-3, the average particle size of metal nanoparticles is 2.1 nm, and the particle size distribution is 1.5-3.5 nm.

[0113] Test the Pt-Cu / MDC1-3 catalyst prepared by embodiment 3 and commercially available Pt / C-JM catalyst (platinum content: 52wt%) to the electrocatalytic activity of oxygen reduction reaction b...

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Abstract

The invention discloses a nano-grade composition, a preparation method thereof, and an application thereof as an electrochemical catalyst. The nano-grade composition provided by the invention is basically composed of a melamine derivative, a carbon material, and transition metal or transition metal alloy nano-cluster. The carbon material comprises at least one selected from conductive carbon black, activated carbon, carbon nano-horn, N-doped carbon nano-horn, carbon nano-tube, graphene, graphite and carbon fiber material. The metal nano-cluster is at least one selected from Pt, Ru, Pd, Rh and Ir nano-clusters. The alloy nano-cluster is nano-cluster formed by more than two elements selected from Pt, Ru, Pd, Rh, Ir, Fe, Cu and Ni. The mass percentage content of the transition metal or alloy nano-cluster is 0.1-90%. The size of the transition metal or alloy nano-cluster is 0.5-10nm. As a fuel cell catalyst, the nano-grade composition provided by the invention has excellent electrocatalytic activity upon reactions such as oxygen reduction and methanol oxidation.

Description

technical field [0001] The invention relates to a nanocomposite catalyst and its preparation method and application. Background technique [0002] Nanoclusters of transition metals and their alloys are a class of nanomaterials with important application value, which can be used to develop a variety of functional materials and devices (Y.Wang, Y.Wei, "Metal Nanoclusters" (Chapter) in H.S.Nalwa, Ed. , EncyclopediaofNanoscienceandNanotechnology, Vol.5,337-367,2004AmericanScientificPublishers), in catalysis, energy conversion, environmental protection (tail gas treatment, air purification, etc.) has a very broad application prospects. The inventors of the present invention have invented a class of "non-protected" precious metals and their alloy nanoclusters and their manufacturing methods. This type of metal nanoclusters only uses simple ions and organic solvent molecules as stabilizers, and not only has a small size and a narrow particle size distribution , can be synthesized ...

Claims

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Application Information

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IPC IPC(8): B01J31/28B01J31/06B01J31/02H01M4/92
CPCY02E60/50
Inventor 王远刘岩高昂朱春梅
Owner 无锡盛鑫氢能科技有限公司
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