N-doped porous carbon electrocatalyst and process for preparation thereof

Patent metadata

Field	Value
Publication number	US-10170770-B2
Application number	US-201415022767-A
Country	US
Kind code	B2
Filing date	Sep 19, 2014
Priority date	Sep 19, 2013
Publication date	Jan 1, 2019
Grant date	Jan 1, 2019

Abstract

The present invention relates to an efficient, non-metal, N-doped porous carbon electrocatalyst for oxygen reduction reaction and a process for the preparation of using g-C 3 N 4 as a nitrogen precursor, metal organic frameworks (MOF) as a carbon template having high specific surface area, large number of active sites and large pore volume.

First claim

We claim:

1. A process for the preparation of an N-doped porous carbon electrocatalysts comprising carbon in the range of 90 to 93% and nitrogen in the range of 7 to 10%:
a. pyrolysing of metal organic frameworks (MOF) to obtain mesoporous carbon (MOFC);
b. mixing and grinding the mesoporous carbon as obtained in step (a) and melamine to get a uniform mixture;
c. dispersing the uniform mixture of step (b) in alcohol in order to get a homogeneous mixture;
d. evaporating solvent by simultaneous heating and stirring the homogeneous mixture as obtained in step (c) till a solid material obtained;
e. heating the solid material as obtained in step (d) in a flow of argon atmosphere to obtain a composite;
f. pyrolysing the composite as obtained in step (e) under argon atmosphere to obtain N-doped porous carbon electrocatalyst;
wherein in step (b) the ratio of the mesoporous carbon and melamine ranges between 1:2 to 1:5.

2. The process as claimed in claim 1 , wherein the MOF is selected from the group consisting of MOF-2, MOF-5.

3. The process as claimed in claim 1 , wherein in step (a) pyrolysis is done at temperature in the range of 900 to 1000° C. at a heating rate of 3 to 5° C./min for period in the range of 2 to 3 h.

4. The process as claimed in claim 1 , wherein in step (c) alcohol is selected from methanol, ethanol, propanol.

5. The process as claimed in claim 1 , wherein in step (c) the dispersion is sonicated for period in the range of 20 to 30 min in a bath type sonicator followed by stirring for period in the range of 6 to 12 h at room temperature in the range of 25 to 30° C.

6. The process as claimed in claim 1 , wherein in step (d) evaporation is performed at temperature in the range of 50 to 60° C.

7. The process as claimed in claim 1 , wherein in step (e) heating is performed at temperature in the range of 300 to 550° C. and flow of argon at a rate of 3 to 5° C./min for period in the range of 2 to 3 h followed by natural cooling to room temperature in the range of 25 to 30° C.

8. The process as claimed in claim 1 , wherein in step (f) pyrolysing at a rate of 3 to 5° C./min for period in the range of 2 to 3 h.

9. The process as claimed in claim 1 , wherein in step (f) heating is carried out at 700-1000° C.

Assignees

• Council Scient Ind Res

Inventors

• Kurungot Sreekumar
• Banerjee Rahul
• Pandiaraj Sekar
• Aiyappa Harshitha Barike

Classifications

• H01M4/88

  Processes of manufacture · CPC title

• H01M4/96

  Carbon-based electrodes · CPC title

• H01M4/86 Primary

  Inert electrodes with catalytic activity, e.g. for fuel cells · CPC title

• H01M4/8605

  Porous electrodes · CPC title

• H01M4/90 Primary

  Selection of catalytic material · CPC title