Preparation method for edge-fluorinated graphite via mechanic-chemical process
View Patent ↗Disclosed is a method for producing edge-functionalized graphite or graphene with fluoro groups. According to the method, graphite is pulverized into smaller pieces and is then allowed to react with a surrounding material containing fluorine or a fluorocarbon compound. The method enables the production of graphite or graphene functionalized with fluoro groups, which could not be achieved by conventional mechanochemical methods. In addition, the method is carried out in a very simple and economical manner and is suitable for large-scale production.
1. A method for producing edge-functionalized graphite or graphene with fluoro groups, comprising (i) mechanically pulverizing graphite under an inert atmosphere in a closed container; (ii) then, evacuating the inert atmosphere, and (iii) reacting the pulverized graphite with fluorine or a fluorocarbon compound at a pressure of 2 to 20 bar, wherein the fluorocarbon compound is trifluoromethane, tetrafluoromethane, trifluoroethane, tetrafluoroethane, chlorotrifluoroethane, dichlorodifluoroethane, pentafluoroethane, hexafluoroethane or a mixture thereof.
2. The method according to claim 1 , wherein the pulverization of graphite and the reaction with fluorine or a fluorocarbon compound are carried out in an atmosphere isolated from the external environment.
3. The method according to claim 1 , wherein step (iii) further comprises introducing an inert gas and the pulverized graphite is allowed to react with a mixture of the fluorine or fluorocarbon compound in the presence of the inert gas.
4. The method according to claim 1 , wherein the inert atmosphere is created by at least one inert gas selected from the group consisting of argon, helium, and neon.
5. The method according to claim 1 , wherein the graphite is pulverized at a rate of 100 to 10,000 rpm for 1 to 100 hours.
6. The method according to claim 1 , wherein the pulverized graphite is allowed to react with the fluorine or fluorocarbon compound for 1 to 100 hours.
7. The method according to claim 1 , wherein the pulverized graphite is 50 nm or more in average diameter.
8. The method according to claim 1 , wherein the fluoro groups are present in an amount of 0.01 to 50% by weight, based on the total weight of the edge-functionalized graphite.
9. The method according to claim 1 , wherein the edge-functionalized graphite or graphene with fluoro groups is a graphene nanoplate having a laminate structure of 1 to 20 graphene sheets.
10. The method according to claim 1 , comprising reacting the pulverized graphite with fluorine or a fluorocarbon compound at a pressure of 2 to 15 bar.