# US 10,766,774 B2 · Oxidized graphite derivative and method for producing same

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- Number: US 10,766,774 B2
- Document ID: US10766774B2
- Status: Granted
- Kind: B2
- Application number: 15/775,526
- Filed: 2016-11-08
- Published: 2018-11-15
- Granted: 2020-09-08
- Earliest claimed: 2015-11-12
- Assignees: Nippon Shokubai Co., Ltd.
- Applicants: Nippon Shokubai Co., Ltd.
- Inventors: Syun Gohda; Hironobu Ono; Osamu Konosu; Shin-ichi Okuoka
- Web page: https://patentgrep.com/patent/US10766774B2

## CPC

- C01B 32/23: Oxidation
- C01B 32/198: Graphene oxide
- C01B 32/21: After-treatment
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/82: by IR- or Raman-data
- C10M 103/02: Carbon; Graphite
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C10M: LUBRICATING COMPOSITIONS (well drilling compositions C09K8/02); USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION (mould release, i.e. separating, agents for metals B22C3/00, for plastics or substances in a plastic state, in general B29C33/56, for glass C03B40/02; textile lubricating compositions D06M11/00, D06M13/00, D06M15/00; immersion oils for microscopy G02B21/33)

## Abstract

Provided are a method for producing a graphite oxide derivative capable of simply producing a high-quality graphite oxide derivative, and a high-quality graphite oxide derivative. The present invention relates to a method for producing a graphite oxide derivative, the method including the steps of oxidizing graphite; and preparing a graphite oxide derivative by reacting graphite oxide in a reaction liquid containing graphite oxide obtained in the oxidation step or graphite oxide in a graphite oxide-containing composition that is separated from the reaction liquid with a compound reactive with an oxygen-containing functional group of the graphite oxide, the method not including the step of purifying and drying the graphite oxide-containing reaction liquid between the oxidation step and the graphite oxide derivative preparation step.

## Claims

### Claim 1

A method for producing a graphite oxide derivative, the method comprising the steps of:
oxidizing graphite using sulfuric acid; and
preparing a graphite oxide derivative by reacting graphite oxide in a graphite oxide-containing composition obtained in the oxidation step and a compound reactive with an oxygen-containing functional group of the graphite oxide,
the method not comprising a step of purifying the graphite oxide-containing composition between the oxidation step and the graphite oxide derivative preparation step,
wherein a sulfuric acid concentration is 1% by mass or more of the mass of the graphite oxide during the oxidation step and the graphite oxide derivative preparation step.

### Claim 2 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1, the method further comprising, between the oxidation step and the graphite oxide derivative preparation step:
the steps of adding a solvent that has a solubility in water of 0.01% or higher and is not arbitrarily miscible with water to the graphite oxide-containing composition and then separating the graphite oxide-containing composition.

### Claim 3 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1,
wherein the compound reactive with an oxygen-containing functional group of the graphite oxide is an alcohol and/or an amine.

### Claim 4 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1,
wherein the graphite oxide derivative preparation step includes the step of reacting the graphite oxide and the compound reactive with an oxygen-containing functional group of the graphite oxide at a reaction temperature of 120° C. or higher.

### Claim 5 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1,
wherein the graphite oxide-containing composition for use in the reaction in the graphite oxide derivative preparation step contains sulfuric acid in an amount of 1% by mass or more and 1000% by mass or less for 100% by mass of the graphite oxide in the composition.

### Claim 6 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1,
wherein the graphite oxide-containing composition for use in the reaction in the graphite oxide derivative preparation step contains water in an amount of 3% by mass or more and 10000% by mass or less for 100% by mass of the graphite oxide in the composition.

### Claim 7 (depends on 3)

The method for producing a graphite oxide derivative according to claim 3,
wherein the alcohol is an aliphatic alcohol and the amine is an aliphatic amine.

### Claim 8 (depends on 2)

The method for producing a graphite oxide derivative according to claim 2,
wherein the solvent has a solubility in water of 0.5% or higher.

### Claim 9 (depends on 2)

The method for producing a graphite oxide derivative according to claim 2,
wherein the solvent is added in an amount of 1% to 1000% by mass for 100% by mass of the graphite oxide in the graphite oxide-containing composition.

### Claim 10 (depends on 2)

The method for producing a graphite oxide derivative according to claim 2,
wherein the graphite oxide-containing composition is separated by any of filtration, decantation, centrifugation, and separation extraction.

### Claim 11 (depends on 10)

The method for producing a graphite oxide derivative according to claim 10,
wherein the graphite oxide-containing composition is separated by filtration.

### Claim 12 (depends on 1)

The method for producing a graphite oxide derivative according to claim 1,
wherein the oxidation step is a step of adding a permanganate to a liquid mixture containing graphite and sulfuric acid.
