# US 10,500,547 B2 · Graphene membrane film for solvent purification, method for producing same, and solvent purification system using same

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- Number: US 10,500,547 B2
- Document ID: US10500547B2
- Status: Granted
- Kind: B2
- Application number: 15/539,941
- Filed: 2015-08-12
- Published: 2018-01-04
- Granted: 2019-12-10
- Earliest claimed: 2014-12-26
- Applicants: Soulbrain Co., Ltd.
- Inventors: Seung hyun Lee; Seok joo Kim
- Web page: https://patentgrep.com/patent/US10500547B2

## CPC

- B01D 67/0069: {by deposition from the liquid phase, e.g. electrochemical deposition (B01D67/0046 takes precedence)}
- B01D 67/0067: {by carbonisation or pyrolysis}
- B01D 69/02: characterised by their properties
- B01D 69/06: Flat membranes
- B01D 71/0211: {Graphene or derivates thereof}
- C01B 32/182: Graphene
- C01B 32/192: starting from graphitic oxides
- B01D 2313/143: on the feed side
- B01D 2313/146: on the permeate side
- B01D 2313/243: Pumps
- B01D 2313/501: Permeate storage tanks
- B01D 2313/502: Concentrate storage tanks
- B01D 2323/081: Heating
- B01D 2323/10: Specific pressure applied
- B01D 2323/30: Cross-linking
- B01D 2323/50: Control of the membrane preparation process
- B01D 2323/52: Use of a mould
- B01D 2325/04: Characteristic thickness
- B01D 2325/20: Specific permeability or cut-off range
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 2204/04: Specific amount of layers or specific thickness
- Y10S 977/734: Fullerenes, i.e. graphene-based structures, such as nanohorns, nanococoons, nanoscrolls or fullerene-like structures, e.g. WS2 or MoS2 chalcogenide nanotubes, planar C3N4, etc.
- Y10S 977/842: for carbon nanotubes or fullerenes
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

Described embodiments include a graphene membrane film for solvent purification and related method, and a solvent purification system using same. The graphene membrane film for solvent purification is formed having a plurality of stacked graphene plate-shaped flakes, and at least one pair of the plurality of stacked graphene plate-shaped flakes comprises a physical bond or a chemical bond connecting layers. The graphene membrane film for solvent purification is produced by preparing a graphene oxide dispersion liquid by dispersing graphene oxide in distilled water; confining the graphene oxide dispersion liquid between a pair of substrates; and applying heat and pressure to the graphene oxide dispersion liquid between the substrates to perform a hydrothermal reaction to concurrently thermally reduce the graphene oxide and bind graphenes. Due to lipophilic surface property and fine pores, size exclusion separation and hydrophilic-lipophilic component separation through polarity may be realized, and thus is usable in fine chemistry fields.

## Claims

### Claim 1

A method for producing a graphene membrane film for solvent purification, the method comprising:
preparing a graphene oxide dispersion liquid by dispersing graphene oxide in dispersion medium;
confining the graphene oxide dispersion liquid between a pair of substrates; and
applying heat and pressure to the graphene oxide dispersion liquid between the substrates to perform a hydrothermal reaction to concurrently thermally reduce the graphene oxide and bind graphenes,
wherein the graphene oxide dispersion liquid has a concentration of about 0.1 mg/ml to about 200 mg/ml,
wherein the applying heat and pressure comprises positioning the substrates, between which the graphene oxide dispersion liquid is confined, into an airtight pressure container and applying heat and pressure,
wherein a temperature of the applying heat and pressure is in a range of about 140° C. to about 200° C.,
wherein a time of the applying heat and pressure is in a range of about 1 hour to about 24 hours, and
wherein a pressure of the applying heat and pressure is in a range of about 5 bar and about 15 bar.

### Claim 2 (depends on 1)

The method of claim 1, wherein the graphene oxide comprises graphene oxide plate-shaped flakes.

### Claim 3 (depends on 2)

The method of claim 2, wherein the graphene oxide plate-shaped flakes has a size of about 0.1 μm to about 10 μm.

### Claim 4 (depends on 1)

The method of claim 1, wherein a thickness of the film is about 1 nm to about 10 μm.

### Claim 5 (depends on 1)

The method of claim 1, wherein the pair of substrates comprises a borosilicate glass, a soda lime glass, a silicon wafer, and a sapphire wafer.

### Claim 6 (depends on 1)

The method of claim 1, wherein the film comprises a plurality of stacked graphene plate-shaped flakes.

### Claim 7 (depends on 5)

The method of claim 5, wherein at least one pair of the plurality of stacked graphene-shaped flakes comprises a physical bond or a chemical bond connecting layers.

### Claim 8 (depends on 6)

The method of claim 6, wherein the film has a carbon/oxygen weight ratio (C/O ratio, unit: wt % of carbon/wt % of oxygen) of about 3 to about 99.9.

### Claim 9 (depends on 7)

The method of claim 7, wherein a d-spacing between the at least one pair of stacked graphene plate-shaped flakes is in a range of about 1 Å to about 10 Å.

### Claim 10 (depends on 8)

The method of claim 8, wherein the chemical bond connecting the layers is a —C—O—C— bond by oxygen or a π-π bond.