Method for preparing oxygen reduction catalyst from cobalt sulfide

A technology of sulfide and catalyst, which is applied in the field of preparation of cobalt sulfide to prepare oxygen reduction catalyst, can solve the problems such as cost and scarcity hindering wide implementation, poor methanol resistance, poor stability, etc., and achieve high product quality and good stability. good performance

Inactive Publication Date: 2018-08-17
SHANDONG SUNRISE NEW MATERIAL TECH CO LTD
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Problems solved by technology

However, cost and scarcity have severely hindered its widespread implementation in such clean energy applications
In addition, Pt-based catalysts usually have poor methanol resistance and poor stability

Method used

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  • Method for preparing oxygen reduction catalyst from cobalt sulfide
  • Method for preparing oxygen reduction catalyst from cobalt sulfide
  • Method for preparing oxygen reduction catalyst from cobalt sulfide

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[0019] A method for preparing an oxygen reduction catalyst from a cobalt sulfide of the present invention, especially for preparing an oxygen reduction catalyst from a cobalt sulfide derived from a cobalt-based metal organic framework, the preparation process includes the following steps:

[0020] 1) Cobalt nitrate hexahydrate (52.4 mg, 0.2 mmol) and 4,4'-bpdc (48.4 mg, 0.2 mmol) were dissolved in 23 mL of DMF. 1,3-bib (31.5 mg, 0.15 mmol) was dissolved in 2 mL DMF respectively.

[0021] 2) After the samples obtained in step 1 were ultrasonically treated for 1 minute, the solutions were mixed, transferred to a reaction kettle (50cm3), and heated at 1.2°C min -1 The heating rate was heated to 120°C; kept at 120°C for 48 hours, then slowly cooled to room temperature (0.4°C min -1 ); after cooling to room temperature, the purple crystals were separated by decanting the mother liquor and washed with DMF, and then dried to obtain a cobalt-based metal-organic framework.

[0022] 3...

Embodiment 1

[0026] Cobalt nitrate hexahydrate (52.4 mg, 0.2 mmol) and 4,4'-bpdc (48.4 mg, 0.2 mmol) were dissolved in 23 mL of DMF. 1,3-Bis(imidazol-1-yl)benzene (1,3-bib) (31.5 mg, 0.15 mmol) was dissolved in 2 mL of DMF respectively. After sonication for 1 min, the solutions were mixed, transferred to a reaction kettle (50 cm3), and heated at 1.2 °C min -1 The heating rate is heated to 120 °C. Keep at 120°C for 48 hours, then slowly cool to room temperature (0.4°C min -1 ). After cooling to room temperature, the purple crystals were separated by decanting the mother liquor and washed with DMF, and then dried to obtain a cobalt-based metal-organic framework.

[0027] The prepared crystals (2.0 g) were weighed into a ceramic vessel and transferred to the outlet port of the tube furnace. Thioacetamide (1.0 g) was weighed into a ceramic vessel and transferred to the inlet port of the tube furnace. Pyrolysis at 700°C for 2 hours under nitrogen with a heating rate of 5°C min -1 , to obt...

Embodiment 2

[0031] Cobalt nitrate hexahydrate (52.4 mg, 0.2 mmol) and 4,4'-bpdc (48.4 mg, 0.2 mmol) were dissolved in 23 mL of DMF. 1,3-Bis(imidazol-1-yl)benzene (1,3-bib) (31.5 mg, 0.15 mmol) was dissolved in 2 mL of DMF respectively. After sonication for 1 min, the solutions were mixed, transferred to a reaction kettle (50 cm3), and heated at 1.2 °C min -1 Heating rate Heat up to 120°C. Keep at 120°C for 48 hours, then slowly cool to room temperature (0.4°C min -1 ). After cooling to room temperature, the purple crystals were separated by decanting the mother liquor and washed with DMF, and then dried to obtain a cobalt-based metal-organic framework.

[0032] The prepared crystals (2.0 g) were weighed into a ceramic vessel and transferred to the outlet port of the tube furnace. Thioacetamide (1.0 g) was weighed into a ceramic vessel and transferred to the inlet port of the tube furnace. Pyrolysis at 600°C for 2 hours under nitrogen with a heating rate of 5°C min -1 , to obtain nit...

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Abstract

The invention provides a method for preparing an oxygen reduction catalyst from cobalt sulfide. The method comprises the following steps: (1) dissolving 52.4 mg of cobalt nitrate hexahydrate (with a molar mass of 0.2 mmol) and 48.4 mg of 4,4'-bpdc (with a molar mass of 0.2 mmol) in 23 mL of DMF and dissolving 31.5mg of 1,3-bib (with a molar mass of 0.15 mmol) in 2mL of DMF, respectively; (2) afterrespective ultrasonic treatment of solution samples obtained in step (1) for 1 minute, mixing the obtained solutions, transferring the obtained mixture to a reactor with a volume of 50 cm<3>, carrying out heating to 120 DEG C at a heating rate of 1.2 DEG C / min, keeping the mixture at 120 DEG C for 48 hours, then carrying out slow cooling to room temperature at a rate of 0.4 DEG C / min, after cooling to room temperature, separating purple crystals by decanting mother liquor, carrying out washing with DMF, and carrying out drying after cleaning so as to obtain a cobalt-based metal organic framework; (3) weighing a part of a sample prepared in the step (2) and thioacetamide, putting the weighed sample and thioacetamide into ceramic vessels respectively transferring the weighed sample and thioacetamide to the outlet end and the inlet end of a tube furnace, and carrying out pyrolysis in a nitrogen atmosphere at a heating rate of 5 DEG C / min to obtain black powder; and (4) testing the ORR performance of the produced black powder by using an electrochemical workstation and a rotating disk electrode.

Description

technical field [0001] The invention relates to the field of fuel cells, in particular to a method for preparing an oxygen reduction catalyst from cobalt sulfide. Background technique [0002] Pt-based materials are known as the most efficient ORR electrocatalysts. However, cost and scarcity have severely hindered their widespread implementation in such clean energy applications. In addition, Pt-based catalysts usually have poor methanol resistance and poor stability. Recent extensive research efforts to replace Pt-based electrodes in fuel cells have led to the exploration of various Pt-free materials as potential alternative catalysts for ORR. N- or S-doped carbons have recently shown promising electrocatalytic activity attributed to charge polarization and asymmetric electron spin density due to differences in electronegativity and electron spin density between carbon and heteroatoms . Especially the participation of transition metals will be able to significantly impr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/88H01M4/90Y02E60/50
Inventor 王晓东
Owner SHANDONG SUNRISE NEW MATERIAL TECH CO LTD
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