# US 2014/0154164 A1 · Nitrate salt-based process for manufacture of graphite oxide

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- Number: US 2014/0154164 A1
- Document ID: US20140154164A1
- Status: Published application
- Kind: A1
- Application number: 14/172,124
- Filed: 2014-02-04
- Published: 2014-06-05
- Earliest claimed: 2009-01-26
- Assignees: Dow Global Technologies LLC
- Applicants: Dow Global Technologies LLC
- Inventors: Shu T. Chen; Michael S. Paquette; Mary Anne Leugers
- Web page: https://patentgrep.com/patent/US20140154164A1

## CPC

- C01B 32/23: Oxidation
- C01B 32/225: Expansion; Exfoliation
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

The present invention relates to a nitrate salt-based process for preparing a graphite oxide. The invention nitrate salt-based process employs starting materials comprising a sulfuric acid, an inorganic nitrate salt, an amount of water, a first amount of chlorate salt, and a graphite.

## Claims

### Claim 1

A nitrate salt-based process for manufacturing graphite oxide, the process comprising steps of:
(a) mixing in a reaction vessel a reaction mixture comprising the following starting materials: a sulfuric acid, an inorganic nitrate salt, an amount of water, a first amount of a chlorate salt, and a graphite;
(b) allowing the reaction mixture to react to form graphite oxide; and
(c) separating the graphite oxide from the reaction mixture to give an isolated graphite oxide.

### Claim 2 (depends on 1)

The process as in claim 1, the process further comprising forming the reaction mixture by steps of:
(i) premixing in the reaction vessel the following starting materials: the sulfuric acid, the inorganic nitrate salt, water, and graphite to give a first sulfuric acid/inorganic nitrate salt/water/graphite mixture; and
(ii) adding the first amount of the chlorate salt to the first sulfuric acid/inorganic nitrate salt/graphite mixture to give the reaction mixture.

### Claim 3 (depends on 1)

The process as in claim 1, the process further comprising forming the reaction mixture by steps of:
(i) premixing in the reaction vessel the following starting materials: the sulfuric acid, water and inorganic nitrate salt to give a sulfuric acid/inorganic nitrate salt/water mixture;
(ii) adding the graphite to the sulfuric acid/inorganic nitrate salt/water mixture to give a second sulfuric acid/inorganic nitrate salt/water/graphite mixture; and
(iii) adding the first amount of the chlorate salt to the second sulfuric acid/inorganic nitrate salt/graphite mixture to give the reaction mixture.

### Claim 4 (depends on 1)

The process as in claim 1, wherein the inorganic nitrate salt comprises ammonium nitrate or a metal nitrate salt of the formula M(NO3)y, wherein M is a metal of any one of Groups 1, 2, and 3 of the Periodic Table of the Elements, the metal M being in a formal oxidation state of +1, +2, or +3, respectively, and y is an integer of 1, 2, or 3 and is selected such that M(NO3)y is, in aggregate, neutral.

### Claim 5 (depends on 4)

The process as in claim 4, wherein the inorganic nitrate salt comprises an aqueous inorganic nitrate salt.

### Claim 6 (depends on 5)

The process as in claim 5, wherein the inorganic nitrate salt comprises aqueous aluminum nitrate, aqueous ammonium nitrate, or aqueous sodium nitrate.

### Claim 7 (depends on 4)

The process as in claim 4, wherein the inorganic nitrate salt comprises solid inorganic nitrate salt.

### Claim 8 (depends on 7)

The process as in claim 7, wherein the solid inorganic nitrate salt is solid ammonium nitrate, solid aluminum nitrate, solid potassium nitrate, solid lithium nitrate, solid calcium nitrate, solid magnesium nitrate, or solid sodium nitrate.

### Claim 9 (depends on 1)

The process as in claim 1, wherein the chlorate salt comprises calcium chlorate, magnesium chlorate, barium chlorate, lithium chlorate, potassium chlorate, or sodium chlorate.

### Claim 10 (depends on 9)

The process as in claim 9, wherein the chlorate salt comprises solid potassium chlorate.

### Claim 11 (depends on 1)

The process as in claim 1, wherein the chlorate salt comprises aqueous sodium chlorate.

### Claim 12 (depends on 1)

The process as in claim 1, wherein temperature of the reaction mixture is 0 degrees Celsius or higher and 55 degrees Celsius or lower.

### Claim 13 (depends on 1)

The process as in claim 1, wherein the graphite consists essentially of particles having sizes characterized as being −10 mesh number or a higher mesh number, wherein the “−” designation before the mesh number indicates particles pass through a sieve having the mesh number.

### Claim 14 (depends on 1)

The process as in claim 1, the process further comprising a step of subjecting the isolated graphite oxide to an exfoliation step to produce an exfoliated graphite.

### Claim 15 (depends on 15)

The process as in claim 15, wherein the exfoliated graphite comprises a highly exfoliated graphite, which is characterized as having a Brunauer-Emmett-Teller surface area of from about 200 square meters per gram to about 1500 square meters per gram.