Patent
US 10,927,009Method for Directly Preparing Expanded Graphite or Graphene Under Normal Temperature and Normal Pressure
Hongbin LU
US
Copyright © 2026 Matter42. All rights reserved.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a contrast graph sh ow ing the volu m e change of graphite before and after expansion, wherein: (a) is raw ma teria l graphite, (b) is expanded graphite;
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 3 shows the Raman spectrum of graphene.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for directly preparing expanded graphite or graphene under normal temperature and normal pressure, wherein, a graphite as a raw material is firstly dispersed in an acidic solution to obtain a suspension, and then the obtained suspension is allowed to stand for a certain period of time under normal temperature and normal pressure to obtain an expanded graphite; the expanded graphite is washed with water and then exfoliated to obtain a graphene dispersion liquid; after the solvent was removed by solid-liquid separation from the graphene dispersion liquid, it can be dispersed in an organic solvent to form a slurry; and the method including steps of: (1) one part by weight of the raw material graphite is added to 1 to 200 parts by weight of the acidic solution to obtain a suspension, the resulting suspension is stirred under normal temperature and normal pressure for 1 minute to 2 hours, and then allowed to stand for 1 to 48 hours to obtain the expanded graphite; the acidic solution is a sulfuric acid solution containing an oxidizing agent, the oxidizing agent is anyone of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide, and the amount of the oxidizing agent is 0.1-20 times the weight of the raw material graphite; (2) the obtained expanded graphite is washed with deionized water and filtered to obtain a wet expanded graphite; the wet expanded graphite is exfoliated in a solution to obtain the graphene dispersion liquid; (3) the graphene dispersion liquid after being exfoliated is spray-dried to obtain a graphene powder, or centrifugated/filtrated to obtian a graphene slurry or a wet graphene solid, and the wet graphene solid is easily re-dispersed in other solvents.
The method of claim 1, wherein the raw material graphite in step (1) refers to anyone of flake graphite, artificial graphite and pyrolytic graphite, and the carbon content is greater than 95%
The method of claim 1, wherein the solution in step (2) is one or more of a pure aqueous solution, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate and chloroform.
The method of claim 1, wherein the exfoliating method in step (2) is water bath ultrasonic, probe ultrasonic, high speed shear, fluid comminution or any combination thereof, wherein, the ultrasonic power of the water bath ultrasonic is 20-5000 W, the ultrasonic power of the probe ultrasonic is 50-5000W; the system temperature is controlled at 80 0 C or less during ultrasonic; the ultrasonic time is 10 minutes- 10 hours; the shear power in high speed 35 shear is 100 W-10 kW, the shear rate is 1000-100,000 revolutions, the operating temperature is controlled at 80 ° C or less, the shear time is from 10 minutes to 10 hours; the fluid pressure is controlled at 200MPa or less during fluid comminution and exfoliation, the flow is controlled at 1.0-500 L/h, and the operating temperature is at 80 ° C or less
The method of claim 1, wherein the spray drying in step (3) employs a conventional aqueous or organic phase spray drying apparatus, and the rotational speed of the separating centrifuge is 1,000 to 20,000 rpm.
The method of claim 1, wherein the graphene oxide or graphene has a radial dimension in the range of 1-10 m.
The method of claim 1, wherein the ratio of monolayer graphene in the graphene oxide or graphene is greater than 75 %.
The method of claim 1, wherein in the step (1), the amount of the oxidizing agent is 1-19 times the weight of the raw material graphite, preferably 1.5-15 times, more preferably 2-10 times.
A graphene material, wherein its radial dimension is in the range of 1-10 m, and the ratio of monolayer graphene in the graphene material is > 75 %.
The graphene material of claim 9, wherein the defect ratio of the graphene material is less than or equal to 0.1.
An article which comprises the graphene material of claim 9 or is prepared from the graphene material of claim 9.
A method for preparing graphene, comprising the steps of: (a) reacting a graphite with an acidic solution under normal temperature and normal pressure to obtain an expanded graphite, the acidic solution is a sulfuric acid solution containing an oxidizing agent, and the oxidizing agent is selected form the group consisting of ammonium persulfate, potassium persulfate, sodium persulfate, hydrogen peroxide and a combination thereof; (b) after mixing the obtained expanded graphite with a solution, the mixture is subjected exfoliation to obtain a graphene dispension liquid; (c) drying the graphene dispension liquid obtained in step (b) to obtain a graphene slurry or a wet graphene solid; and (d) optionally, dispersing the graphene slurry or wet graphene solid obtained in step (c) to other solvent, and said other solvent is selected from the group consisting of N-methylpyrrolidone, N,N-dimethyl formamide, N,N-dimethyl sulfoxide, benzyl benzoate, alcohols, water, and a combination thereof.
Materials described outside the worked examples.
graphite (raw material)
C
expanded graphite
graphene
ammonium persulfate
(NH₄)2S₂O₈
potassium persulfate
K₂S₂O₈
sodium persulfate
Na₂S₂O₈
hydrogen peroxide
H₂O₂
exfoliation solvents (NMP, DMF, DMAc, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate, chloroform, water)
graphene oxide
sulfuric acid solution
H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
expanded graphite volume expansion | 50–1500 times | expanded graphite |
graphene radial dimension | 1–10 μm | graphene |
ratio of monolayer graphene | ≥ 75 % | graphene |
defect ratio (ID/IG or equivalent) | ≤ 0.1 | graphene |
Thickness | 5–10 µm | — |
Temperature | 5–50 °C | — |
Temperature | 5–40 °C | — |
Duration | 60–7200 s | — |
Duration | 600–36000 s | — |
Pressure | 1–200 pa | — |
Duration | 1–48 hours | — |
— | 20–5000 W | — |
— | 50–5000 W | — |
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a contrast graph sh ow ing the volu m e change of graphite before and after expansion, wherein: (a) is raw ma teria l graphite, (b) is expanded graphite;
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 3 shows the Raman spectrum of graphene.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for directly preparing expanded graphite or graphene under normal temperature and normal pressure, wherein, a graphite as a raw material is firstly dispersed in an acidic solution to obtain a suspension, and then the obtained suspension is allowed to stand for a certain period of time under normal temperature and normal pressure to obtain an expanded graphite; the expanded graphite is washed with water and then exfoliated to obtain a graphene dispersion liquid; after the solvent was removed by solid-liquid separation from the graphene dispersion liquid, it can be dispersed in an organic solvent to form a slurry; and the method including steps of: (1) one part by weight of the raw material graphite is added to 1 to 200 parts by weight of the acidic solution to obtain a suspension, the resulting suspension is stirred under normal temperature and normal pressure for 1 minute to 2 hours, and then allowed to stand for 1 to 48 hours to obtain the expanded graphite; the acidic solution is a sulfuric acid solution containing an oxidizing agent, the oxidizing agent is anyone of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide, and the amount of the oxidizing agent is 0.1-20 times the weight of the raw material graphite; (2) the obtained expanded graphite is washed with deionized water and filtered to obtain a wet expanded graphite; the wet expanded graphite is exfoliated in a solution to obtain the graphene dispersion liquid; (3) the graphene dispersion liquid after being exfoliated is spray-dried to obtain a graphene powder, or centrifugated/filtrated to obtian a graphene slurry or a wet graphene solid, and the wet graphene solid is easily re-dispersed in other solvents.
The method of claim 1, wherein the raw material graphite in step (1) refers to anyone of flake graphite, artificial graphite and pyrolytic graphite, and the carbon content is greater than 95%
The method of claim 1, wherein the solution in step (2) is one or more of a pure aqueous solution, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate and chloroform.
The method of claim 1, wherein the exfoliating method in step (2) is water bath ultrasonic, probe ultrasonic, high speed shear, fluid comminution or any combination thereof, wherein, the ultrasonic power of the water bath ultrasonic is 20-5000 W, the ultrasonic power of the probe ultrasonic is 50-5000W; the system temperature is controlled at 80 0 C or less during ultrasonic; the ultrasonic time is 10 minutes- 10 hours; the shear power in high speed 35 shear is 100 W-10 kW, the shear rate is 1000-100,000 revolutions, the operating temperature is controlled at 80 ° C or less, the shear time is from 10 minutes to 10 hours; the fluid pressure is controlled at 200MPa or less during fluid comminution and exfoliation, the flow is controlled at 1.0-500 L/h, and the operating temperature is at 80 ° C or less
The method of claim 1, wherein the spray drying in step (3) employs a conventional aqueous or organic phase spray drying apparatus, and the rotational speed of the separating centrifuge is 1,000 to 20,000 rpm.
The method of claim 1, wherein the graphene oxide or graphene has a radial dimension in the range of 1-10 m.
The method of claim 1, wherein the ratio of monolayer graphene in the graphene oxide or graphene is greater than 75 %.
The method of claim 1, wherein in the step (1), the amount of the oxidizing agent is 1-19 times the weight of the raw material graphite, preferably 1.5-15 times, more preferably 2-10 times.
A graphene material, wherein its radial dimension is in the range of 1-10 m, and the ratio of monolayer graphene in the graphene material is > 75 %.
The graphene material of claim 9, wherein the defect ratio of the graphene material is less than or equal to 0.1.
An article which comprises the graphene material of claim 9 or is prepared from the graphene material of claim 9.
A method for preparing graphene, comprising the steps of: (a) reacting a graphite with an acidic solution under normal temperature and normal pressure to obtain an expanded graphite, the acidic solution is a sulfuric acid solution containing an oxidizing agent, and the oxidizing agent is selected form the group consisting of ammonium persulfate, potassium persulfate, sodium persulfate, hydrogen peroxide and a combination thereof; (b) after mixing the obtained expanded graphite with a solution, the mixture is subjected exfoliation to obtain a graphene dispension liquid; (c) drying the graphene dispension liquid obtained in step (b) to obtain a graphene slurry or a wet graphene solid; and (d) optionally, dispersing the graphene slurry or wet graphene solid obtained in step (c) to other solvent, and said other solvent is selected from the group consisting of N-methylpyrrolidone, N,N-dimethyl formamide, N,N-dimethyl sulfoxide, benzyl benzoate, alcohols, water, and a combination thereof.
Materials described outside the worked examples.
graphite (raw material)
C
expanded graphite
graphene
ammonium persulfate
(NH₄)2S₂O₈
potassium persulfate
K₂S₂O₈
sodium persulfate
Na₂S₂O₈
hydrogen peroxide
H₂O₂
exfoliation solvents (NMP, DMF, DMAc, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate, chloroform, water)
graphene oxide
sulfuric acid solution
H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
expanded graphite volume expansion | 50–1500 times | expanded graphite |
graphene radial dimension | 1–10 μm | graphene |
ratio of monolayer graphene | ≥ 75 % | graphene |
defect ratio (ID/IG or equivalent) | ≤ 0.1 | graphene |
Thickness | 5–10 µm | — |
Temperature | 5–50 °C | — |
Temperature | 5–40 °C | — |
Duration | 60–7200 s | — |
Duration | 600–36000 s | — |
Pressure | 1–200 pa | — |
Duration | 1–48 hours | — |
— | 20–5000 W | — |
— | 50–5000 W | — |
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a contrast graph sh ow ing the volu m e change of graphite before and after expansion, wherein: (a) is raw ma teria l graphite, (b) is expanded graphite;
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 3 shows the Raman spectrum of graphene.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for directly preparing expanded graphite or graphene under normal temperature and normal pressure, wherein, a graphite as a raw material is firstly dispersed in an acidic solution to obtain a suspension, and then the obtained suspension is allowed to stand for a certain period of time under normal temperature and normal pressure to obtain an expanded graphite; the expanded graphite is washed with water and then exfoliated to obtain a graphene dispersion liquid; after the solvent was removed by solid-liquid separation from the graphene dispersion liquid, it can be dispersed in an organic solvent to form a slurry; and the method including steps of: (1) one part by weight of the raw material graphite is added to 1 to 200 parts by weight of the acidic solution to obtain a suspension, the resulting suspension is stirred under normal temperature and normal pressure for 1 minute to 2 hours, and then allowed to stand for 1 to 48 hours to obtain the expanded graphite; the acidic solution is a sulfuric acid solution containing an oxidizing agent, the oxidizing agent is anyone of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide, and the amount of the oxidizing agent is 0.1-20 times the weight of the raw material graphite; (2) the obtained expanded graphite is washed with deionized water and filtered to obtain a wet expanded graphite; the wet expanded graphite is exfoliated in a solution to obtain the graphene dispersion liquid; (3) the graphene dispersion liquid after being exfoliated is spray-dried to obtain a graphene powder, or centrifugated/filtrated to obtian a graphene slurry or a wet graphene solid, and the wet graphene solid is easily re-dispersed in other solvents.
The method of claim 1, wherein the raw material graphite in step (1) refers to anyone of flake graphite, artificial graphite and pyrolytic graphite, and the carbon content is greater than 95%
The method of claim 1, wherein the solution in step (2) is one or more of a pure aqueous solution, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate and chloroform.
The method of claim 1, wherein the exfoliating method in step (2) is water bath ultrasonic, probe ultrasonic, high speed shear, fluid comminution or any combination thereof, wherein, the ultrasonic power of the water bath ultrasonic is 20-5000 W, the ultrasonic power of the probe ultrasonic is 50-5000W; the system temperature is controlled at 80 0 C or less during ultrasonic; the ultrasonic time is 10 minutes- 10 hours; the shear power in high speed 35 shear is 100 W-10 kW, the shear rate is 1000-100,000 revolutions, the operating temperature is controlled at 80 ° C or less, the shear time is from 10 minutes to 10 hours; the fluid pressure is controlled at 200MPa or less during fluid comminution and exfoliation, the flow is controlled at 1.0-500 L/h, and the operating temperature is at 80 ° C or less
The method of claim 1, wherein the spray drying in step (3) employs a conventional aqueous or organic phase spray drying apparatus, and the rotational speed of the separating centrifuge is 1,000 to 20,000 rpm.
The method of claim 1, wherein the graphene oxide or graphene has a radial dimension in the range of 1-10 m.
The method of claim 1, wherein the ratio of monolayer graphene in the graphene oxide or graphene is greater than 75 %.
The method of claim 1, wherein in the step (1), the amount of the oxidizing agent is 1-19 times the weight of the raw material graphite, preferably 1.5-15 times, more preferably 2-10 times.
A graphene material, wherein its radial dimension is in the range of 1-10 m, and the ratio of monolayer graphene in the graphene material is > 75 %.
The graphene material of claim 9, wherein the defect ratio of the graphene material is less than or equal to 0.1.
An article which comprises the graphene material of claim 9 or is prepared from the graphene material of claim 9.
A method for preparing graphene, comprising the steps of: (a) reacting a graphite with an acidic solution under normal temperature and normal pressure to obtain an expanded graphite, the acidic solution is a sulfuric acid solution containing an oxidizing agent, and the oxidizing agent is selected form the group consisting of ammonium persulfate, potassium persulfate, sodium persulfate, hydrogen peroxide and a combination thereof; (b) after mixing the obtained expanded graphite with a solution, the mixture is subjected exfoliation to obtain a graphene dispension liquid; (c) drying the graphene dispension liquid obtained in step (b) to obtain a graphene slurry or a wet graphene solid; and (d) optionally, dispersing the graphene slurry or wet graphene solid obtained in step (c) to other solvent, and said other solvent is selected from the group consisting of N-methylpyrrolidone, N,N-dimethyl formamide, N,N-dimethyl sulfoxide, benzyl benzoate, alcohols, water, and a combination thereof.
Materials described outside the worked examples.
graphite (raw material)
C
expanded graphite
graphene
ammonium persulfate
(NH₄)2S₂O₈
potassium persulfate
K₂S₂O₈
sodium persulfate
Na₂S₂O₈
hydrogen peroxide
H₂O₂
exfoliation solvents (NMP, DMF, DMAc, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate, chloroform, water)
graphene oxide
sulfuric acid solution
H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
expanded graphite volume expansion | 50–1500 times | expanded graphite |
graphene radial dimension | 1–10 μm | graphene |
ratio of monolayer graphene | ≥ 75 % | graphene |
defect ratio (ID/IG or equivalent) | ≤ 0.1 | graphene |
Thickness | 5–10 µm | — |
Temperature | 5–50 °C | — |
Temperature | 5–40 °C | — |
Duration | 60–7200 s | — |
Duration | 600–36000 s | — |
Pressure | 1–200 pa | — |
Duration | 1–48 hours | — |
— | 20–5000 W | — |
— | 50–5000 W | — |
Related documents with shared materials, methods, properties, or citations.
GRAPHENE OXIDE MODIFIED THERMOSET MONOMER AND SYNTHESIS THEREOF
METHOD FOR THE PREPARATION OF POLYANILINE/REDUCED GRAPHENE OXIDE COMPOSITES
HIGH-THROUGHPUT IMAGING OF GRAPHENE BASED SHEETS BY FLUORESCENCE QUENCHING MICROSCOPY AND APPLICATIONS OF SAME
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a contrast graph sh ow ing the volu m e change of graphite before and after expansion, wherein: (a) is raw ma teria l graphite, (b) is expanded graphite;
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 3 shows the Raman spectrum of graphene.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for directly preparing expanded graphite or graphene under normal temperature and normal pressure, wherein, a graphite as a raw material is firstly dispersed in an acidic solution to obtain a suspension, and then the obtained suspension is allowed to stand for a certain period of time under normal temperature and normal pressure to obtain an expanded graphite; the expanded graphite is washed with water and then exfoliated to obtain a graphene dispersion liquid; after the solvent was removed by solid-liquid separation from the graphene dispersion liquid, it can be dispersed in an organic solvent to form a slurry; and the method including steps of: (1) one part by weight of the raw material graphite is added to 1 to 200 parts by weight of the acidic solution to obtain a suspension, the resulting suspension is stirred under normal temperature and normal pressure for 1 minute to 2 hours, and then allowed to stand for 1 to 48 hours to obtain the expanded graphite; the acidic solution is a sulfuric acid solution containing an oxidizing agent, the oxidizing agent is anyone of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide, and the amount of the oxidizing agent is 0.1-20 times the weight of the raw material graphite; (2) the obtained expanded graphite is washed with deionized water and filtered to obtain a wet expanded graphite; the wet expanded graphite is exfoliated in a solution to obtain the graphene dispersion liquid; (3) the graphene dispersion liquid after being exfoliated is spray-dried to obtain a graphene powder, or centrifugated/filtrated to obtian a graphene slurry or a wet graphene solid, and the wet graphene solid is easily re-dispersed in other solvents.
The method of claim 1, wherein the raw material graphite in step (1) refers to anyone of flake graphite, artificial graphite and pyrolytic graphite, and the carbon content is greater than 95%
The method of claim 1, wherein the solution in step (2) is one or more of a pure aqueous solution, N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate and chloroform.
The method of claim 1, wherein the exfoliating method in step (2) is water bath ultrasonic, probe ultrasonic, high speed shear, fluid comminution or any combination thereof, wherein, the ultrasonic power of the water bath ultrasonic is 20-5000 W, the ultrasonic power of the probe ultrasonic is 50-5000W; the system temperature is controlled at 80 0 C or less during ultrasonic; the ultrasonic time is 10 minutes- 10 hours; the shear power in high speed 35 shear is 100 W-10 kW, the shear rate is 1000-100,000 revolutions, the operating temperature is controlled at 80 ° C or less, the shear time is from 10 minutes to 10 hours; the fluid pressure is controlled at 200MPa or less during fluid comminution and exfoliation, the flow is controlled at 1.0-500 L/h, and the operating temperature is at 80 ° C or less
The method of claim 1, wherein the spray drying in step (3) employs a conventional aqueous or organic phase spray drying apparatus, and the rotational speed of the separating centrifuge is 1,000 to 20,000 rpm.
The method of claim 1, wherein the graphene oxide or graphene has a radial dimension in the range of 1-10 m.
The method of claim 1, wherein the ratio of monolayer graphene in the graphene oxide or graphene is greater than 75 %.
The method of claim 1, wherein in the step (1), the amount of the oxidizing agent is 1-19 times the weight of the raw material graphite, preferably 1.5-15 times, more preferably 2-10 times.
A graphene material, wherein its radial dimension is in the range of 1-10 m, and the ratio of monolayer graphene in the graphene material is > 75 %.
The graphene material of claim 9, wherein the defect ratio of the graphene material is less than or equal to 0.1.
An article which comprises the graphene material of claim 9 or is prepared from the graphene material of claim 9.
A method for preparing graphene, comprising the steps of: (a) reacting a graphite with an acidic solution under normal temperature and normal pressure to obtain an expanded graphite, the acidic solution is a sulfuric acid solution containing an oxidizing agent, and the oxidizing agent is selected form the group consisting of ammonium persulfate, potassium persulfate, sodium persulfate, hydrogen peroxide and a combination thereof; (b) after mixing the obtained expanded graphite with a solution, the mixture is subjected exfoliation to obtain a graphene dispension liquid; (c) drying the graphene dispension liquid obtained in step (b) to obtain a graphene slurry or a wet graphene solid; and (d) optionally, dispersing the graphene slurry or wet graphene solid obtained in step (c) to other solvent, and said other solvent is selected from the group consisting of N-methylpyrrolidone, N,N-dimethyl formamide, N,N-dimethyl sulfoxide, benzyl benzoate, alcohols, water, and a combination thereof.
Materials described outside the worked examples.
graphite (raw material)
C
expanded graphite
graphene
ammonium persulfate
(NH₄)2S₂O₈
potassium persulfate
K₂S₂O₈
sodium persulfate
Na₂S₂O₈
hydrogen peroxide
H₂O₂
exfoliation solvents (NMP, DMF, DMAc, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, methanol, ethanol, propanol, isopropanol, butanol, pentanol, benzyl benzoate, ethyl acetate, butyl acetate, chloroform, water)
graphene oxide
sulfuric acid solution
H₂SO₄
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Figure 2 shows TEM micrograph of the exfoliated graphene and the ultraviolet absorption spectrum of the graphene suspens io n, wherein (a) i s a TEM i mage of graphene, and (b) is an ultraviolet absorption spectrum of the graphene dispersion liquid.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
expanded graphite volume expansion | 50–1500 times | expanded graphite |
graphene radial dimension | 1–10 μm | graphene |
ratio of monolayer graphene | ≥ 75 % | graphene |
defect ratio (ID/IG or equivalent) | ≤ 0.1 | graphene |
Thickness | 5–10 µm | — |
Temperature | 5–50 °C | — |
Temperature | 5–40 °C | — |
Duration | 60–7200 s | — |
Duration | 600–36000 s | — |
Pressure | 1–200 pa | — |
Duration | 1–48 hours | — |
— | 20–5000 W | — |
— | 50–5000 W | — |
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