# US 10,865,111 B2 · Method of making nanomaterials from a renewable carbon source

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- Number: US 10,865,111 B2
- Document ID: US10865111B2
- Status: Granted
- Kind: B2
- Application number: 16/182,506
- Filed: 2018-11-06
- Published: 2019-05-16
- Granted: 2020-12-15
- Earliest claimed: 2017-11-07
- Applicants: Michael Kwabena Opoku
- Inventors: Michael Kwabena Opoku
- Web page: https://patentgrep.com/patent/US10865111B2

## CPC

- C01B 32/15: Nano-sized carbon materials
- C01B 32/382: {Making shaped products, e.g. fibres, spheres, membranes or foam}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2004/03: obtained by SEM
- C01P 2006/12: Surface area
- C01P 2006/14: Pore volume
- C01P 2006/17: Pore diameter distribution
- 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
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

This patent disclosure includes a process that uniquely and unexpectedly results in the production of extremely high specific surface area and large pore volume carbon nanomaterial with high content of sp2 hybridized carbon-carbon in the form of nanosheets from a renewable carbonaceous raw material. The resulting nanomaterial is in particulate form or porous nanomaterial or dispersed in solvent. This process can also be used to produce carbon nanosheet on substrates or form a nanocomposite with other materials that results in exceptional properties.

## Claims

### Claim 1

A process for making carbon nanosheet material, said process comprising the steps of:
providing a renewable carbohydrate source to a reactor comprising a solvent to obtain a soaked or dissolved carbohydrate source;
adding a dehydration solution and a catalyst to the reactor comprising the soaked or dissolved carbohydrate source to obtain a reaction mixture, where
the dehydration solution has a hydrogen ions concentration of at least approximately 1%, and
the catalyst is chosen from the group consisting of platinum, palladium, LiAlH4, nickel, yeast, aluminum-nickel alloy, cobalt, B2H6, zinc, NaBH4, and copper;
charging said reactor with air or inert gas;
heating the reaction mixture to remove glycosidic linkages and water molecules from the carbohydrate thereby producing an intermediate mixture with sheet-like morphology; and
further heating the intermediate mixture in inert gas to form a network of the carbon nanosheet material, wherein the carbon nanosheet material is in a particulate form, porous foam form, or dispersed in a solvent.

### Claim 2 (depends on 1)

The process of claim 1, wherein said carbohydrate source comprises yam root extract or potatoes root extract.

### Claim 3 (depends on 1)

The process of claim 1, wherein the carbohydrate source comprises cassava root extract, cassava root flour, tapioca flour, dried cassava root pulp, or dried and fried cassava root flakes.

### Claim 4 (depends on 1)

The process of claim 1, wherein the carbohydrate source comprises sugarcane extract, sugar beet root extract, or sucrose.

### Claim 5 (depends on 1)

The process of claim 1, wherein the carbohydrate source comprises rice grain, corn, or wheat grain.

### Claim 6 (depends on 1)

The process of claim 1, wherein the solvent is chosen from the group consisting of distilled water, deionized water, ethanol, and ethylene glycol.

### Claim 7 (depends on 1)

The process of claim 1, wherein said dehydration solution is chosen from the group consisting of sodium hydroxide, hydrochloric acid, phosphoric acid, phosphorous acid, and nitric acid.

### Claim 8 (depends on 1)

The process of claim 1, further comprising the step of removing the dehydration solution by washing and diluting with excess distilled or deionized water prior to further heating of the intermediate mixture.

### Claim 9 (depends on 1)

The process of claim 1, further comprising the step of removing said catalyst by washing, filtering, magnetic separation, sonication, sieving, or centrifugation prior to further heating of the intermediate mixture.

### Claim 10 (depends on 1)

The process of claim 1, wherein the heating of the reaction mixture is carried out in air or inert gas at approximately 45 to 1050° C.

### Claim 11 (depends on 1)

The process of claim 1, further comprising, prior to further heating the intermediate mixture, drying the intermediate mixture to produce an intermediate mixture in form of a powder, foam, or film on a substrate; wherein the intermediate mixture in form of powder, foam, or film on a substrate is heated in the inert gas at approximately 500 to 1500° C. to produce the carbon nanosheet material.

### Claim 12 (depends on 1)

The process of claim 1, wherein said inert gas comprises argon, helium, or nitrogen.

### Claim 13 (depends on 12)

The process of claim 12, wherein said inert gas further comprises a partial pressure of hydrogen gas.

### Claim 14 (depends on 1)

The process of claim 1, wherein heating the reaction mixture or the intermediate mixture is carried out using a resistive element source, laser irradiation, or microwave irradiation.

### Claim 15 (depends on 1)

The process of claim 1, further comprising the steps of:
washing the carbon nanosheet material with hydrogen peroxide or hydrochloric acid to obtain washed carbon nanosheet material;
rinsing the washed carbon nanosheet material with distilled or deionized water to obtain rinsed carbon nanosheet material;
heating the rinsed carbon nanosheet material in a third inert gas at approximately 700 to 1500° C., thereby producing a high surface area carbon nanomaterial.

### Claim 16 (depends on 15)

The process of claim 15, wherein the third inert gas comprises argon, helium, or nitrogen.

### Claim 17 (depends on 15)

The process of claim 15, wherein the third inert gas further comprises a partial pressure of hydrogen gas.

### Claim 18 (depends on 15)

The process of claim 15, wherein said heating is carried out using a resistive element source, laser irradiation, or microwave irradiation.

### Claim 19 (depends on 1)

The process of claim 1, wherein the intermediate mixture is heated to a temperature of approximately 45 to 1050° C.