US 11,939,221 B2
Method for the manufacture of reduced graphene oxide from electrode graphite scrap
Thi Tan Vu, Oviedo (ES); Abel Alvarez-Alvarez, Asturias (ES); and Roberto Suarez Sanchez, Aviles Asturias (ES)
Assigned to ArcelorMittal, Luxembourg (LU)
Appl. No. 17/055,780
Filed by ArcelorMittal, Luxembourg (LU)
PCT Filed Apr. 10, 2019, PCT No. PCT/IB2019/052942
§ 371(c)(1), (2) Date Nov. 16, 2020,
PCT Pub. No. WO2019/224620, PCT Pub. Date Nov. 28, 2019.
Claims priority of application No. PCT/IB2018/053643 (WO), filed on May 23, 2018.
Prior Publication US 2021/0230003 A1, Jul. 29, 2021
Int. Cl. C01B 32/198 (2017.01)
CPC C01B 32/198 (2017.08) 16 Claims
 
1. A method for manufacture of reduced graphene oxide from a graphite electrode scrap used in an electric arc furnace comprising:
A. providing the graphite electrode scrap,
B. grinding the electrode graphite scrap to obtain ground graphite electrode,
C. oxidizing the ground graphite electrode to obtain graphene oxide including the following successive sub-steps:
i. preparing a mixture including the ground graphite electrode, an acid and a nitrate salt, the mixture being kept at a temperature below 5° C., the acid being chosen from at least one of the group consisting of: H2SO4, HCl, HNO3, H3PO4, C2H2Cl2O2 (dichloroacetic acid), HSO2OH (alkylsulfonic acid) and mixtures thereof,
ii. adding an oxidizing agent into the mixture obtained in step C.i) to obtain graphite oxide in an oxidation reaction, the oxidizing agent being chosen from at least one of the group consisting of: potassium permanganate, H2O2, O3, H2S2O8, H2SO5, KNO3, NaClO and mixtures thereof,
iii. after a targeted level of oxidation of at least 45% by weight of oxygen functional groups is reached, adding a chemical element to stop the oxidation reaction, the chemical element being chosen from at least one of the group consisting of: an acid, non-deionized water, deionized water, H2O2 and mixtures thereof,
iv. separating of the graphite oxide from the mixture obtained in step C.iii),
v. exfoliating the graphite oxide into graphene oxide and
D. reducing the graphene oxide into reduced graphene oxide.