US 11,701,621 B2
Method for directly growing ultrathin porous graphene separation membrane
Xie Quan, Dalian (CN); Gaoliang Wei, Dalian (CN); Shuo Chen, Dalian (CN); and Hongtao Yu, Dalian (CN)
Assigned to DALIAN UNIVERSITY OF TECHNOLOGY, Dalian (CN)
Appl. No. 16/325,168
Filed by DALIAN UNIVERSITY OF TECHNOLOGY, Dalian (CN)
PCT Filed Jun. 2, 2017, PCT No. PCT/CN2017/086957
§ 371(c)(1), (2) Date Feb. 12, 2019,
PCT Pub. No. WO2018/218644, PCT Pub. Date Dec. 6, 2018.
Prior Publication US 2019/0176094 A1, Jun. 13, 2019
Int. Cl. B01D 67/00 (2006.01); B01D 71/02 (2006.01); B01D 69/12 (2006.01); C01B 32/184 (2017.01); B01D 69/02 (2006.01)
CPC B01D 67/0062 (2013.01) [B01D 67/0067 (2013.01); B01D 69/02 (2013.01); B01D 69/122 (2013.01); B01D 71/021 (2013.01); C01B 32/184 (2017.08); B01D 67/0011 (2013.01); B01D 2325/04 (2013.01); C01B 2204/02 (2013.01); C01B 2204/04 (2013.01)] 1 Claim
OG exemplary drawing
 
1. A method for direct growth of porous graphene separation membrane on a metal foil, comprising:
(1) directly coating mixture of an etching agent, an organic solvent A and a polymer on a metal foil, and calcining the mixture and the metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to the organic solvent A is 1:0.5-50:100-1000,
alternatively, coating a dispersion or solution of the etching agent on a metal foil, on which a polymer film is overlaid; calcining the obtained metal foil at high temperature in absence of oxygen; wherein a mass ratio of the etching agent to the polymer to a solvent B or a dispersion B is 1:0.5-50:100-1000; the calcination is performed at 400-1200° C. for 0.17-4 hours;
wherein the solvent B or the dispersion B is used for dissolution or dispersion of the etching agent,
wherein the etching agent is polyoxometalate, metal nitrates, metal oxide, or a mixture of thereof, and a mass concentration of the etching agent solution or dispersion is 0.1%-20%,
wherein the polymer is polyvinyl butyral or/and polymethylmethacrylate,
wherein the organic solvent A is methanol, ethanol, isopropyl alcohol, acetone, chloroform, or a mixture thereof, the solvent B or the dispersion B is ethanol or/and water,
wherein the metal foil is copper foil or nickel foil, and
wherein the oxygen-free condition is inert gas protection or vacuum,
(2) removing the metal foil and reaction products to obtain the porous graphene separation membranes; wherein the porous graphene separation membranes consist of single-layered, double-layered or multi-layered graphene.