US 12,485,410 B1
Porous carbon catalyst loaded with metal sulfides based on high-sulfur petroleum coke and preparation method therefor and application thereof
Jingcai Chang, Qingdao (CN); Yulin Huang, Qingdao (CN); Xin'an Zhang, Qingdao (CN); Lianhai Zhang, Qingdao (CN); Yong Shi, Qingdao (CN); Haoran Wu, Qingdao (CN); Yifan Li, Qingdao (CN); Yiming Wang, Qingdao (CN); Jiahao Zhang, Qingdao (CN); Taiyang Liu, Qingdao (CN); Yang Zhang, Qingdao (CN); and Chen Huang, Qingdao (CN)
Assigned to SHANDONG UNIVERSITY, Shandong (CN); and QINGDA LOW CARBON GREEN HYDROGEN INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE (QINGDAO) CO., LTD., Shandong (CN)
Filed by SHANDONG UNIVERSITY, Shandong (CN); and QINGDA LOW CARBON GREEN HYDROGEN INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE (QINGDAO) CO., LTD., Shandong (CN)
Filed on Oct. 28, 2024, as Appl. No. 18/928,876.
Claims priority of application No. 202410705034.4 (CN), filed on Jun. 3, 2024.
Int. Cl. B01J 37/20 (2006.01); B01J 27/04 (2006.01); B01J 27/043 (2006.01); B01J 37/00 (2006.01); B01J 37/04 (2006.01); B01J 37/06 (2006.01); B01J 37/08 (2006.01); C01B 3/04 (2006.01)
CPC B01J 37/20 (2013.01) [B01J 27/04 (2013.01); B01J 27/043 (2013.01); B01J 37/0036 (2013.01); B01J 37/04 (2013.01); B01J 37/06 (2013.01); B01J 37/088 (2013.01); C01B 3/04 (2013.01)] 5 Claims
OG exemplary drawing
 
1. A method for preparing a porous carbon catalyst loaded with a transition metal sulfide based on high-sulfur petroleum coke, comprising:
(1) preparing an in-situ activated precursor:
mixing a high-sulfur petroleum coke having a content of sulfur of 3-10 wt % with a transition metal salt in an ethanol aqueous solution thoroughly, and then evaporating and drying to obtain the in-situ activated precursor;
the transition metal of the salt is nickel or niobium;
(2) destabilizing bulk sulfur:
grinding and mixing the in-situ activated precursor obtained from step (1) with an alkaline activator in a mass ratio of the alkaline activator to the high-sulfur petroleum coke of (1-5):(1-2), followed by placement in a tube furnace, heating from room temperature to a specified temperature of 600-800° C. at a controlled rate under an argon inert atmosphere, bulk sulfur is destabilized under the joint action of the specified temperature and alkaline activator;
the alkaline activator is potassium hydroxide or sodium hydroxide;
(3) conducting an in-situ the transition metal-sulfur bonding reaction:
maintaining the specified temperature from step (2), switching the argon atmosphere to hydrogen at a flow rate of 10-60 mL/min, and conducting the in-situ the transition metal-sulfur bonding reaction for 1-2 hours, followed by cooling down to room temperature under an argon atmosphere;
(4) washing and drying:
washing the product obtained from step (3) with a washing solution, drying and grinding to obtain the porous carbon catalyst loaded with the transition metal sulfide based on high-sulfur petroleum coke.