Zr-MOF structure based CO selective methanation Ni/ZrO2 catalyst and preparation method thereof

A catalyst and selective technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of insufficient activity and selectivity stability, and achieve the effects of excellent CO methanation activity, low price and simple operation.

Inactive Publication Date: 2017-05-31
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a CO-selective methanation Ni / ZrO based on the Zr-MOF structure for the shortcomings of existing Ni-based catalysts with insufficient activity, selectivity and stability. 2 catalyst

Method used

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  • Zr-MOF structure based CO selective methanation Ni/ZrO2 catalyst and preparation method thereof
  • Zr-MOF structure based CO selective methanation Ni/ZrO2 catalyst and preparation method thereof
  • Zr-MOF structure based CO selective methanation Ni/ZrO2 catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0044] (1) Preparation of metal-organic framework material Zr-MOF: ZrCl 4 , BDC and DMF were uniformly mixed at a molar ratio of 1:1:180, crystallized at 120°C for 24 h, centrifuged, washed with DMF and methanol three times in turn, and dried at 65°C to obtain a white powder; the obtained white powder was washed with methanol solvent Soak for three days, and change the methanol every day to replace the remaining ligands and solvent molecules in the sample, and dry the resulting white powder at 65°C to obtain the metal-organic framework material Zr-MOF;

[0045] The XRD pattern of the prepared metal-organic framework material Zr-MOF and the XRD pattern obtained from its single crystal data simulation are as follows figure 1 and figure 2 As shown, it can be seen from the figure that the main diffraction peaks of the synthesized Zr-MOF are basically consistent with the XRD diffraction peaks obtained by the single crystal data simulation, indicating that the Zr-MOF was successfu...

Embodiment 2

[0053] (1) ZrCl 4 , BDC and DMF were uniformly mixed at a molar ratio of 1:1:150, crystallized at 110°C for 36 h, centrifuged, washed with DMF and methanol three times in turn, and dried at 70°C to obtain a white powder; the obtained white powder was washed with methanol solvent Soak for three days, and change methanol every day to replace the remaining ligands and solvent molecules in the sample, and dry the resulting white powder at 70°C to obtain the metal-organic framework material Zr-MOF;

[0054] (2) Take 8 ml concentration to be 6×10 -4 g / ml NiCl 2 ·6H 2 The aqueous solution of O was stirred evenly, and 0.2 g of pretreated Zr-MOF was added, stirred vigorously at room temperature for 12 h, centrifuged, dried at 70 °C, and then calcined in a muffle furnace at 550 °C for 2 h, 20% H 2 -N 2 Methanated Ni / ZrO can be obtained after reduction at 450°C for 2 hours in a mixed gas atmosphere 2 catalyst.

[0055] Prepared Ni / ZrO 2 The specific surface area of ​​the catalyst...

Embodiment 3

[0058] (1) ZrCl 4 , BDC and DMF were uniformly mixed at a molar ratio of 1:1:250, crystallized at 130°C for 72 h, centrifuged, washed with DMF and methanol three times in turn, and dried at 65°C to obtain a white powder; the obtained white powder was washed with methanol solvent Soak for three days, and change the methanol every day to replace the remaining ligands and solvent molecules in the sample, and dry the resulting white powder at 75°C to obtain the metal-organic framework material Zr-MOF;

[0059] (2) Take 8 ml concentration to be 6×10 -3 g / ml NiCl 2 ·6H 2 O in ethanol solution, stirred evenly, added 0.2 g of pretreated Zr-MOF, stirred vigorously for 5 h, centrifuged, dried at 75 °C, and roasted in a muffle furnace at 450 °C for 4 h, 20% H 2 -N 2 After reduction at 350°C for 1 h in a mixed gas atmosphere, the methanated Ni / ZrO 2 catalyst.

[0060] Prepared Ni / ZrO 2 The specific surface area of ​​the catalyst is 73.8 m 2 / g, the pore size is 15.9 nm, and the l...

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Abstract

The invention discloses a Zr-MOF structure based CO selective methanation Ni / ZrO2 catalyst and a preparation method of the Zr-MOF structure based CO selective methanation Ni / ZrO2 catalyst. The main active ingredient of the Ni / ZrO2 catalyst is Ni, the carrier is ZrO2, the specific surface area of the catalyst is 55-98 m<2> / g, the pore diameter is 9.0-16.2 nm, and the Ni capacity is 5-15wt%. The method comprises the following steps: (1) preparing a metal-organic framework Zr-MOF; and (2) preparing the Ni / ZrO2 catalyst. The Ni / ZrO2 catalyst is excellent in CO selective methanation, the content of CO, which is 1 vol%, in a reformed gas is reduced to be lower than 10 ppm under the conditions of wide reaction temperature interval (210-350) and reactant gas space velocity (4,000-20,000 h<-1>), and the selectivity is higher than 50%.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a catalyst for selective methanation of CO in hydrogen-rich gas and a preparation method thereof. Background technique [0002] Proton exchange membrane fuel cell (PEMFC) has become one of the most competitive power sources to replace gasoline internal combustion engine vehicles due to its advantages of high efficiency, low pollution, low operating temperature, fast start-up, and high power density. PEMFC uses hydrogen-rich reformed gas as fuel, but the Pt electrode in PEMFC is extremely sensitive to CO, and a small amount of CO can poison it and reduce the performance of the battery. Therefore, a small amount of CO in the hydrogen-rich gas must be removed to reduce its concentration to Tolerance level (below 10 ppm) for fuel cell Pt electrodes. CO selective methanation does not need to add additional reactants, and the raw material H can be directly used 2 The rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/8825H01M4/8885H01M4/9041H01M4/9075Y02E60/50
Inventor 董新法平丹耿建铭封啸
Owner SOUTH CHINA UNIV OF TECH
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