Purification and drying of graphene oxide

Patent metadata

Field	Value
Publication number	US-10988383-B2
Application number	US-201815970968-A
Country	US
Kind code	B2
Filing date	May 4, 2018
Priority date	May 5, 2017
Publication date	Apr 27, 2021
Grant date	Apr 27, 2021

Abstract

Provided herein are graphene materials, fabrication processes, and devices with improved performance and a high throughput. In some embodiments, the present disclosure provides graphene oxide (GO) materials and methods for forming GO materials. Such methods for forming GO materials avoid the shortcomings of current forming methods, to facilitate facile, high-throughput production of GO materials.

First claim

What is claimed is:

1. A method of forming a purified graphene oxide (GO) material comprising:
forming a GO suspension comprising GO;
dewatering the GO suspension with a first filter to form a dewatered GO suspension;
forming a GO solution comprising the dewatered GO suspension and a solvent solution comprising a polar organic solvent; and
filtering the GO solution through a second filter to form the purified GO material.

2. The method of claim 1 , wherein filtering the GO solution comprises centrifugal filtering, dead-end filtering, cross-flow filtering, stationary phase filtering, dynamic phase filtering, surface filtering, depth filtering, vacuum filtering, recirculation filtering, or any combination thereof.

3. The method of claim 2 , wherein filtering the GO solution comprises dead-end filtering and vacuum filtering, and wherein a hydraulic pressure exerted upon the GO suspension is about 1 pound per square inch (psi) to about 5 psi.

4. The method of claim 2 , wherein filtering the GO solution comprises cross-flow recirculation filtering the GO solution to form a retentate and a permeate, wherein the retentate is added to the GO solution.

5. The method of claim 4 , further comprising continually adding a volume of the solvent solution to the GO solution during the cross-flow recirculation filtering of the GO solution.

6. The method of claim 5 , wherein the volume of the solvent solution is added to the GO solution at a solvent solution flow rate approximately equal to a flow rate of the permeate.

7. The method of claim 5 , wherein for a first period of time the solvent solution comprises at least one of water and the polar organic solvent, and for a second period of time the solvent solution comprises water or the polar organic solvent.

8. The method of claim 1 , wherein a percent by mass of the GO in the GO suspension is about 0.05% to about 2%.

9. The method of claim 1 , wherein dewatering the GO suspension comprises centrifugal filtering, dead-end filtering, cross-flow filtering, stationary phase filtering, dynamic phase filtering, surface filtering, depth filtering, vacuum filtering, recirculation filtering, or any combination thereof.

10. The method of claim 1 , wherein the polar organic solvent solution comprises a protic solvent.

11. The method of claim 1 , wherein a percent by mass of the GO suspension in the GO suspension and the solvent solution is about 10% to about 60%.

12. The method of claim 1 , wherein a mass of the GO suspension per an area of the second filter is about 3 kilograms per meter squared (kg/m 2 ) to about 30 kg/m 2 .

13. The method of claim 1 , wherein filtering the dewatered GO suspension and the solvent solution comprises depositing the dewatered GO suspension onto the second filter and then depositing the solvent solution onto the dewatered GO suspension on the second filter.

14. The method of claim 1 , wherein at least one of the first filter and the second filter comprises a Buchner funnel, a surface filter, a sieve, a filter paper, a belt filter, a drum filter, a cross-flow filter, a screen filter, a depth filter, a polymeric membrane, a ceramic membrane, a stainless steel filter, a stainless steel mesh, a carbon fiber mesh, a microfilter, an ultrafilter, a membrane, or any combination thereof.

15. The method of claim 1 , wherein the second filter is the first filter.

16. The method of claim 1 , further comprising drying the GO suspension and the solvent solution.

17. The method of claim 16 , wherein drying the GO suspension is performed by air blowing, dry evaporation, heating, oven heating, freeze-drying, or any combination thereof.

18. The method of claim 17 , wherein the air blowing is performed with a dry gas stream at a pressure of about 10 psi to about 30 psi.

19. The method of claim 17 , wherein the heating is performed at a temperature of about 10° C. to about 50° C.

20. The method of claim 1 , wherein the GO material comprises GO powder, an anhydrous GO powder, an intercalated GO powder, an exfoliated GO powder, a single layer GO material, a water dispersible GO material, a polar solvent dispersible GO material, an aqueous GO material, a GO ink, a GO paste, a GO solution, a GO fluid, a GO liquid, a GO paint, a GO dye, a GO coating, a GO compound, or any combination thereof.

21. The method of claim 1 , wherein the purified GO material has a surface area of about 800 m 2 /g to about 2,400 m 2 /g.

22. The method of claim 1 , wherein the purified GO material has a conductivity of about 0.1 siemens per meter (S/m) to about 5 S/m.

23. The method of claim 1 , wherein the purified GO material has an oxidation percentage of about 15% to about 60%.

24. The method of claim 1 , wherein the polar organic solvent comprises ethyl acetate, tetrahydrofuran, dichloromethane, acetone, acetonitrile, dimethylformamide, dimethyl sulfoxide, acetic acid, n-butanol, isopropanol, n-propanol, ethanol, methanol, formic acid, or any combination thereof.

25. The method of claim 1 , wherein the polar organic solvent comprises an alcohol.

26. The method of claim 25 , wherein the alcohol comprises methanol, ethanol, propan-2-ol, butan-1-ol, pentan-1-ol, hexadecan-1-ol, ethane-1,2-diol, propane-1,2-diol, propane-1,2,3-triol, butane-1,2,3,4-tetraol, pentane-1,2,3,4,5-pentol, hexane-1,2,3,4,5,6-hexol, heptane-1,2,3,4,5,6,7-heptol, prop-2-ene-1-ol, 3,7-dimethylocta-2,6-dien-1-ol, prop-2-yn-1-ol, cyclohexane-1,2,3,4,5,6-hexol, 2-(2-propyl)-5-methyl-cyclohexane-1-ol, or any combination thereof.

Assignees

• Univ California

Inventors

• Kaner Richard B
• Kowal Matthew
• Jun Dukwoo

Classifications

• C01P2006/80

  Compositional purity · CPC title

• C01B2204/32

  Size or surface area · CPC title

• C01B2204/22

  Electronic properties · CPC title

• C01B32/198 Primary

  Graphene oxide · CPC title

• C01B32/196

  Purification · CPC title