Continuous manufacture of graphenic compounds

Patent metadata

Field	Value
Publication number	US-11713249-B2
Application number	US-201816755394-A
Country	US
Kind code	B2
Filing date	Oct 10, 2018
Priority date	Oct 11, 2017
Publication date	Aug 1, 2023
Grant date	Aug 1, 2023

Abstract

Provided herein are high throughput continuous or semi-continuous reactors and processes for manufacturing graphenic materials, such as graphene oxide. Such processes are suitable for manufacturing graphenic materials at rates that are up to hundreds of times faster than conventional techniques, have little batch-to-batch variation, have a high degree of tunability, and have excellent performance characteristics.

First claim

What is claimed is:

1. A process for manufacturing a graphenic compound, the process comprising:
a. injecting a first stock into a first inlet of a continuous or semi-continuous reactor, the first stock comprising graphite;
b. optionally injecting a second stock into a second inlet of the continuous reactor or semi-continuous reactor, the second stock comprising potassium permanganate;
c. optionally injecting a third stock into a third inlet of the continuous or semi-continuous reactor, the third stock comprising an oxidizing or quenching agent and being injected downstream from the injection point of the first and/or second stock(s);
d. optionally injecting a fourth stock into a fourth inlet of the continuous reactor or semi-continuous reactor, the fourth stock comprising water and being injected downstream from the injection point of the first, second, and third stocks; and
e. collecting the graphenic compound from an outlet of the continuous reactor or semi-continuous reactor, the graphenic compound being collected downstream from the injection points of the first, second, third, and fourth stocks,

wherein the continuous reactor or semi-continuous reactor comprises a reactor chamber into which the first, second, third, and fourth stocks are injected; the reactor chamber being configured between an outer wall of a first cylindrical body and the inner wall of a second cylindrical body or bore, one or both of the first and/or second cylindrical bodies rotating around the axis thereof; and the first and second cylindrical bodies are rotating in opposite directions.

2. The process of claim 1 , wherein the continuous reactor has a flow from the first inlet to the outlet, the flow being a vortex flow.

3. The process of claim 2 , wherein the vortex flow is a toroidal vortex flow.

4. The process of claim 1 , wherein the continuous reactor is configured to produce a toroidal vortex flow.

5. The process of claim 4 , wherein the toroidal vortex flow comprises a plurality of non-axisymmetric toroidal vortices.

6. The process of claim 1 , wherein the continuous reactor is a continuous Taylor-Couette reactor.

7. The process of claim 1 , wherein the first fluid stock further comprising phosphoric acid and wherein the quenching agent is hydrogen peroxide.

8. The process of claim 1 , wherein the graphite is intercalated with sulfuric acid, bisulfate, sulfate, or a combination thereof upstream of injection of the third stock.

9. The process of claim 1 , wherein the graphite is converted to graphite oxide upstream of injection of the fourth stock.

10. The process of claim 9 , wherein the graphene oxide is in the form of a particle comprising more than one graphene oxide sheet, on average, or a particle comprising about 2 to about 20 graphene oxide sheets, on average.

11. The process of claim 1 , wherein the first stock comprises graphite in a concentration of about 0.1 wt. % to about 50 wt. %.

12. The method of claim 1 , wherein the graphenic compound is graphene oxide.

Assignees

• Univ Cornell
• Axium Ip Llc

Inventors

• Joo Yong Lak
• Alamer Mohammed
• Williams Brian

Classifications

• C01B32/198 Primary

  Graphene oxide · CPC title

• B01J8/10

  moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title

• B01J19/1843

  Concentric tube · CPC title

• B01J2219/0009

  Coils · CPC title

• B01J2219/00094

  Jackets · CPC title