Supported nickel-copper alloy nano-catalyst and preparation method thereof and application to catalytic hydrogenation

A nano-catalyst, nickel-copper alloy technology, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of low purity and crystallinity of supported catalysts, metal and Weak carrier interaction, complex catalyst preparation process and other issues, to achieve the effect of green production process, high catalytic activity and stability, simple magnetic separation and recovery

Inactive Publication Date: 2016-12-07
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

Literature (Ding Weiping, Liu Hong, Guan Chengyue, Xue Nianhua, etc. Chinese patent, 201210567980.4, 2012-12-24) obtained alumina carrier by hydrothermal method with oleic acid as surfactant, and after roasting, mixed with copper nitrate solution and nickel nitrate Solution, sodium hydroxide solution and hydrazine hydrate solution are mixed, and a large amount of organic solvents are added to form a microemulsion, and the product is roasted at a high temperature in a reducing atmosphere to obtain a supported nickel-copper alloy nanocatalyst; the method has complex production processes and high costs. Moreover, the obtained catalyst has poor dispersion and large particle size, which is difficult to apply to industrial production
The literature (Zhengdong Liu, Zongyou Yin, Zehui Du, Yang Yang, etal.Nanoscale, 2014, 6, 5110-5115) uses a solid carbon source through a chemical vapor deposition process to coat graphene on the surface of nickel-copper oxide nanoparticles. And reduce under hydrogen atmosphere to obtain nickel-copper alloy / carbon nanocomposite catalyst; the preparation process of the catalyst is complicated and the production cost is high
Documents (Hao Fang, Ming wen, Hanxing Chen, Qingsheng Wu, et al.Nanoscale, 2016, 8, 536-542) firstly synthesized graphene oxide by Hummers method, and then dispersed it into a mixture containing copper chloride, nickel chloride and reducing agent. In the solution, the nickel-copper alloy / carbon nanocomposite catalyst is obtained by hydrothermal synthesis; although the catalyst exhibits high hydrogenation performance, the yield is low and the production cost is high, and the purity and crystallinity of the obtained supported catalyst are low. Carrier-carrier interactions are weak

Method used

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  • Supported nickel-copper alloy nano-catalyst and preparation method thereof and application to catalytic hydrogenation
  • Supported nickel-copper alloy nano-catalyst and preparation method thereof and application to catalytic hydrogenation
  • Supported nickel-copper alloy nano-catalyst and preparation method thereof and application to catalytic hydrogenation

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Experimental program
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Effect test

Embodiment 1

[0029] 1) Make 50mL concentration 0.15mol L -1 Nickel nitrate, 50mL concentration is 0.05mol L -1 Copper nitrate aqueous solution and 50mL concentration is 0.4mol L -1 The aqueous solution of sodium salicylate was evenly mixed, and after stirring for 10 minutes, slowly added 50 mL of -1 The urea aqueous solution was reacted in a nitrogen atmosphere at 95°C for 36 hours. The product was centrifuged, washed and dried to obtain a layered nickel hydroxide precursor with a large amount of organic anion intercalation. The scanning electron microscope photo is shown in figure 2 ;

[0030] 2) The precursor prepared in the above steps was calcined at 500°C for 1 hour in a nitrogen atmosphere to obtain a nickel-copper alloy / carbon nanocomposite catalyst, which was denoted as NiCu / C. For the characterization results, see Figure 2-6 , the product was used to evaluate the catalytic hydrogenation performance of p-nitrophenol.

Embodiment 2

[0032] 1) Make 50mL concentration 0.12mol L -1 Nickel nitrate, 50mL concentration is 0.08mol L -1 Copper nitrate aqueous solution and 50mL concentration is 0.4mol L -1 The aqueous solution of sodium salicylate was evenly mixed, and after stirring for 10 minutes, slowly added 50 mL of -1 The urea aqueous solution was reacted in an argon atmosphere at 95°C for 36 hours, and the product was centrifuged, washed and dried to obtain a layered nickel hydroxide precursor with a large amount of organic anion intercalation;

[0033] 2) The precursor prepared in the above steps was calcined at 700°C for 2 hours in a nitrogen atmosphere to obtain a nickel-copper alloy / carbon nanocomposite catalyst, denoted as NiCu / C-1, and the characterization results are as follows Figure 4 with Figure 5 , the product was used to evaluate the catalytic hydrogenation performance of p-nitrophenol.

Embodiment 3

[0035] 1) Make 50mL concentration 0.1mol·L -1 Nickel nitrate, 50mL concentration is 0.1mol L -1 Copper nitrate aqueous solution and 50mL concentration is 0.4mol L -1 The aqueous solution of sodium salicylate was evenly mixed, and after stirring for 10 minutes, slowly added 50 mL of -1 The urea aqueous solution was reacted in a nitrogen atmosphere at 95°C for 48 hours, and the product was centrifuged, washed and dried to obtain a layered nickel hydroxide precursor with a large amount of organic anion intercalation;

[0036] 2) The precursor prepared in the above steps was calcined at 600°C for 1 hour in a nitrogen atmosphere to obtain a nickel-copper alloy / carbon nanocomposite catalyst, which was denoted as NiCu / C-2. For the characterization results, see Figure 4 with Figure 5 , the product was used to evaluate the catalytic hydrogenation performance of p-nitrophenol.

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Abstract

The invention discloses a supported nickel-copper alloy nano-catalyst, a preparation method thereof and application of catalytic hydrogenation. The invention utilizes a simple co-precipitation synthesis technique to self-assemble in an aqueous solution to obtain a large amount of layered nickel-copper hydroxide intercalated with organic anions as a precursor, and obtains nickel with high catalytic activity and stability through one-step in-situ solid-state pyrolysis under an inert atmosphere. Copper alloy/carbon nanocomposite catalyst. This method realizes the uniform dispersion of highly crystalline nickel-copper alloy nanoparticles in the graphitized carbon matrix, and there is a strong interaction between the metal and the support. The invention does not use additional reducing agent, surface active agent and organic solvent, reduces production cost and improves product purity. In the catalytic hydrogenation reaction performance test, the nickel-copper alloy/carbon nanocomposite catalyst prepared by the present invention showed higher catalytic activity and stability than the commercial platinum/carbon catalyst, and it still had High catalytic efficiency.

Description

technical field [0001] The invention belongs to the technical field of chemical catalyst preparation, and in particular relates to a supported nickel-copper alloy nano catalyst, a preparation method thereof and the application of catalytic hydrogenation. Background technique [0002] Nickel-copper alloy has been widely used in industrial production as an important catalyst. In order to improve its catalytic activity and stability, carbon materials, alumina, silicon oxide, etc. are often used as its carrier. method, sol-gel method, etc.) with high cost and complex process, requiring a large amount of reducing agent and organic solvent, and the obtained nano-catalyst is easily oxidized and agglomerated, greatly reducing its catalytic performance, and it is difficult to meet the requirements of modern production. Therefore, it is of great significance to prepare green catalysts with high catalytic performance and low cost. [0003] In recent years, reports on the synthesis of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J35/10C07C213/02C07C215/76
CPCB01J23/755B01J35/023B01J35/1004C07C213/02
Inventor 王连英刘欣欣郭晓迪高文奇耿红帅
Owner BEIJING UNIV OF CHEM TECH
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