Patent
US 10,494,263METHOD FOR PREPARING BIOMASS GRAPHENE BY USING CELLULOSE AS RAW MATERIAL
Honggang Fu
US
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Patent
Atlas literature
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US 10,494,263Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a diagram illustrating a method of preparing graphene, in accordance with various embodiments of the disclosure.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Figure 3 is a Raman spectrum of graphene prepared according to
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
- 10. Canceled
Canceled
A method for preparing biomass graphene using cellulose as a raw material, comprising: preparing a catalyst solution, wherein a catalyst is added to distilled water to form a first mixture, the first mixture is stirred for 10 to 30 m in to form a catalyst solution, in which the ratio of catalyst to solvent is within 2:100 to 35:100; preparation a precursor, wherein a biomass cellulose is added to the catalyst solution to form a second mixture, the second mixture is stirred for 1 to 4 hours then deoxidized at a high temperature and dried to obtain a precursor, in which the mass ratio of cellulose to solvent is within 3:100 to 40:100; heat-treating the precursor including a precarbonization step and a secondary carbonization step, wherein the pre-carbonization step includes heating the precursor to within 220 to 650 " C at 10 to 20 " C/min for 1i to 6 hours in an atmosphere including at least one of nitrogen gas, argon gas, and hydrogen gas to obtain a precarbonized precursor, and the secondary carbonization step includes heating the pre-carbonized precursor to within 900 to 1650 " C at 5 to 16 " C/min for 4 to 15 hours to obtain a heat-treated product; and obtaining graphene, wherein the heat-treated product is acid-treated, centrifuged, washed with distilled water to neutral, and dried at 80-110 "0 C to obtain graphene. New
The method of claim 11, wherein the biomass cellulose is at least one of cellulose extracted from corncobs, corn stalks, sorghum stalks, soybean stalks, stems or leaves of cattail, coconut shells, and palm shells. New
The method of claim 11, wherein the catalyst is at least one of FeC 1 2, FeC 1 3, K 3 [Fe(CN) 6], and K 4 [Fe(CN) 6]. New
The method of claim 11, wherein the first mixture is stirred for 13 to 25 minutes, and the ratio of catalyst to solvent being within 3:100 to 25:100. New
The method of claim 11, wherein the second mixture is stirred for 2 to 3 hours, and the deoxidation is conducted at one of 110 to 205 " C for 6 to 16 hours and 110 to 170 " C for 5 minutes to 2 hours at 3-9 kW in microwave strength. New
The method of claim 11, wherein the pre-carbonization step includes heating the precursor to within 300 to 450 " C at 11 to 16 " C/min for 2 to 5 hours, and the secondary carbonization step includes heating the pre-carbonized precursor to within 1000 to 1550 " C at 5 to 12"C/min for to 10 hours. New
The method of claim 11, wherein acid-treating is performed with acid comprising at least sulfuric acid, perchloric acid, and nitric acid, and drying is performed between 90 to 105"C. New
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Preparation of biomass graphene from cellulose: 18 g FeCl₂ dissolved in 100 mL distilled water (ratio 18:100), stirred 25 min to form catalyst solution. Cellulose added to catalyst solution (cellulose:solvent = 26:100), stirred 2 h, reacted at 140°C for 10 h, deoxidized and dried to obtain precursor. Pre-carbonization: heated to 280°C at 10°C/min in N₂/Ar/H₂ atmosphere, held 3 h. Secondary carbonization: heated to 1050°C at 8°C/min, held 6 h. Acid treatment, centrifugation, washing to neutral, drying at 105°C to obtain graphene. Product: uniform size, single- or multi-layer 2D layered structure, size 0.5–2 μm, conductivity 25000–45000 S/cm, yield >99.9%.
2 materials1 process step
Same as Example 1 except the cellulose used is cellulose extracted from soybean straw biomass.
Materials described outside the worked examples.
iron-based catalyst
acid mixture (sulfuric acid, perchloric acid, nitric acid)
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
electrical conductivity of biomass graphene (claimed range) | 25000–45000 S/m | biomass graphene |
lateral dimension of biomass graphene (claimed range) | 0.5–2 μm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,494,263Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a diagram illustrating a method of preparing graphene, in accordance with various embodiments of the disclosure.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Figure 3 is a Raman spectrum of graphene prepared according to
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
- 10. Canceled
Canceled
A method for preparing biomass graphene using cellulose as a raw material, comprising: preparing a catalyst solution, wherein a catalyst is added to distilled water to form a first mixture, the first mixture is stirred for 10 to 30 m in to form a catalyst solution, in which the ratio of catalyst to solvent is within 2:100 to 35:100; preparation a precursor, wherein a biomass cellulose is added to the catalyst solution to form a second mixture, the second mixture is stirred for 1 to 4 hours then deoxidized at a high temperature and dried to obtain a precursor, in which the mass ratio of cellulose to solvent is within 3:100 to 40:100; heat-treating the precursor including a precarbonization step and a secondary carbonization step, wherein the pre-carbonization step includes heating the precursor to within 220 to 650 " C at 10 to 20 " C/min for 1i to 6 hours in an atmosphere including at least one of nitrogen gas, argon gas, and hydrogen gas to obtain a precarbonized precursor, and the secondary carbonization step includes heating the pre-carbonized precursor to within 900 to 1650 " C at 5 to 16 " C/min for 4 to 15 hours to obtain a heat-treated product; and obtaining graphene, wherein the heat-treated product is acid-treated, centrifuged, washed with distilled water to neutral, and dried at 80-110 "0 C to obtain graphene. New
The method of claim 11, wherein the biomass cellulose is at least one of cellulose extracted from corncobs, corn stalks, sorghum stalks, soybean stalks, stems or leaves of cattail, coconut shells, and palm shells. New
The method of claim 11, wherein the catalyst is at least one of FeC 1 2, FeC 1 3, K 3 [Fe(CN) 6], and K 4 [Fe(CN) 6]. New
The method of claim 11, wherein the first mixture is stirred for 13 to 25 minutes, and the ratio of catalyst to solvent being within 3:100 to 25:100. New
The method of claim 11, wherein the second mixture is stirred for 2 to 3 hours, and the deoxidation is conducted at one of 110 to 205 " C for 6 to 16 hours and 110 to 170 " C for 5 minutes to 2 hours at 3-9 kW in microwave strength. New
The method of claim 11, wherein the pre-carbonization step includes heating the precursor to within 300 to 450 " C at 11 to 16 " C/min for 2 to 5 hours, and the secondary carbonization step includes heating the pre-carbonized precursor to within 1000 to 1550 " C at 5 to 12"C/min for to 10 hours. New
The method of claim 11, wherein acid-treating is performed with acid comprising at least sulfuric acid, perchloric acid, and nitric acid, and drying is performed between 90 to 105"C. New
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Preparation of biomass graphene from cellulose: 18 g FeCl₂ dissolved in 100 mL distilled water (ratio 18:100), stirred 25 min to form catalyst solution. Cellulose added to catalyst solution (cellulose:solvent = 26:100), stirred 2 h, reacted at 140°C for 10 h, deoxidized and dried to obtain precursor. Pre-carbonization: heated to 280°C at 10°C/min in N₂/Ar/H₂ atmosphere, held 3 h. Secondary carbonization: heated to 1050°C at 8°C/min, held 6 h. Acid treatment, centrifugation, washing to neutral, drying at 105°C to obtain graphene. Product: uniform size, single- or multi-layer 2D layered structure, size 0.5–2 μm, conductivity 25000–45000 S/cm, yield >99.9%.
2 materials1 process step
Same as Example 1 except the cellulose used is cellulose extracted from soybean straw biomass.
Materials described outside the worked examples.
iron-based catalyst
acid mixture (sulfuric acid, perchloric acid, nitric acid)
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
electrical conductivity of biomass graphene (claimed range) | 25000–45000 S/m | biomass graphene |
lateral dimension of biomass graphene (claimed range) | 0.5–2 μm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,494,263Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a diagram illustrating a method of preparing graphene, in accordance with various embodiments of the disclosure.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Figure 3 is a Raman spectrum of graphene prepared according to
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
- 10. Canceled
Canceled
A method for preparing biomass graphene using cellulose as a raw material, comprising: preparing a catalyst solution, wherein a catalyst is added to distilled water to form a first mixture, the first mixture is stirred for 10 to 30 m in to form a catalyst solution, in which the ratio of catalyst to solvent is within 2:100 to 35:100; preparation a precursor, wherein a biomass cellulose is added to the catalyst solution to form a second mixture, the second mixture is stirred for 1 to 4 hours then deoxidized at a high temperature and dried to obtain a precursor, in which the mass ratio of cellulose to solvent is within 3:100 to 40:100; heat-treating the precursor including a precarbonization step and a secondary carbonization step, wherein the pre-carbonization step includes heating the precursor to within 220 to 650 " C at 10 to 20 " C/min for 1i to 6 hours in an atmosphere including at least one of nitrogen gas, argon gas, and hydrogen gas to obtain a precarbonized precursor, and the secondary carbonization step includes heating the pre-carbonized precursor to within 900 to 1650 " C at 5 to 16 " C/min for 4 to 15 hours to obtain a heat-treated product; and obtaining graphene, wherein the heat-treated product is acid-treated, centrifuged, washed with distilled water to neutral, and dried at 80-110 "0 C to obtain graphene. New
The method of claim 11, wherein the biomass cellulose is at least one of cellulose extracted from corncobs, corn stalks, sorghum stalks, soybean stalks, stems or leaves of cattail, coconut shells, and palm shells. New
The method of claim 11, wherein the catalyst is at least one of FeC 1 2, FeC 1 3, K 3 [Fe(CN) 6], and K 4 [Fe(CN) 6]. New
The method of claim 11, wherein the first mixture is stirred for 13 to 25 minutes, and the ratio of catalyst to solvent being within 3:100 to 25:100. New
The method of claim 11, wherein the second mixture is stirred for 2 to 3 hours, and the deoxidation is conducted at one of 110 to 205 " C for 6 to 16 hours and 110 to 170 " C for 5 minutes to 2 hours at 3-9 kW in microwave strength. New
The method of claim 11, wherein the pre-carbonization step includes heating the precursor to within 300 to 450 " C at 11 to 16 " C/min for 2 to 5 hours, and the secondary carbonization step includes heating the pre-carbonized precursor to within 1000 to 1550 " C at 5 to 12"C/min for to 10 hours. New
The method of claim 11, wherein acid-treating is performed with acid comprising at least sulfuric acid, perchloric acid, and nitric acid, and drying is performed between 90 to 105"C. New
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Preparation of biomass graphene from cellulose: 18 g FeCl₂ dissolved in 100 mL distilled water (ratio 18:100), stirred 25 min to form catalyst solution. Cellulose added to catalyst solution (cellulose:solvent = 26:100), stirred 2 h, reacted at 140°C for 10 h, deoxidized and dried to obtain precursor. Pre-carbonization: heated to 280°C at 10°C/min in N₂/Ar/H₂ atmosphere, held 3 h. Secondary carbonization: heated to 1050°C at 8°C/min, held 6 h. Acid treatment, centrifugation, washing to neutral, drying at 105°C to obtain graphene. Product: uniform size, single- or multi-layer 2D layered structure, size 0.5–2 μm, conductivity 25000–45000 S/cm, yield >99.9%.
2 materials1 process step
Same as Example 1 except the cellulose used is cellulose extracted from soybean straw biomass.
Materials described outside the worked examples.
iron-based catalyst
acid mixture (sulfuric acid, perchloric acid, nitric acid)
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
electrical conductivity of biomass graphene (claimed range) | 25000–45000 S/m | biomass graphene |
lateral dimension of biomass graphene (claimed range) | 0.5–2 μm |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,494,263Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a diagram illustrating a method of preparing graphene, in accordance with various embodiments of the disclosure.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Figure 3 is a Raman spectrum of graphene prepared according to
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
- 10. Canceled
Canceled
A method for preparing biomass graphene using cellulose as a raw material, comprising: preparing a catalyst solution, wherein a catalyst is added to distilled water to form a first mixture, the first mixture is stirred for 10 to 30 m in to form a catalyst solution, in which the ratio of catalyst to solvent is within 2:100 to 35:100; preparation a precursor, wherein a biomass cellulose is added to the catalyst solution to form a second mixture, the second mixture is stirred for 1 to 4 hours then deoxidized at a high temperature and dried to obtain a precursor, in which the mass ratio of cellulose to solvent is within 3:100 to 40:100; heat-treating the precursor including a precarbonization step and a secondary carbonization step, wherein the pre-carbonization step includes heating the precursor to within 220 to 650 " C at 10 to 20 " C/min for 1i to 6 hours in an atmosphere including at least one of nitrogen gas, argon gas, and hydrogen gas to obtain a precarbonized precursor, and the secondary carbonization step includes heating the pre-carbonized precursor to within 900 to 1650 " C at 5 to 16 " C/min for 4 to 15 hours to obtain a heat-treated product; and obtaining graphene, wherein the heat-treated product is acid-treated, centrifuged, washed with distilled water to neutral, and dried at 80-110 "0 C to obtain graphene. New
The method of claim 11, wherein the biomass cellulose is at least one of cellulose extracted from corncobs, corn stalks, sorghum stalks, soybean stalks, stems or leaves of cattail, coconut shells, and palm shells. New
The method of claim 11, wherein the catalyst is at least one of FeC 1 2, FeC 1 3, K 3 [Fe(CN) 6], and K 4 [Fe(CN) 6]. New
The method of claim 11, wherein the first mixture is stirred for 13 to 25 minutes, and the ratio of catalyst to solvent being within 3:100 to 25:100. New
The method of claim 11, wherein the second mixture is stirred for 2 to 3 hours, and the deoxidation is conducted at one of 110 to 205 " C for 6 to 16 hours and 110 to 170 " C for 5 minutes to 2 hours at 3-9 kW in microwave strength. New
The method of claim 11, wherein the pre-carbonization step includes heating the precursor to within 300 to 450 " C at 11 to 16 " C/min for 2 to 5 hours, and the secondary carbonization step includes heating the pre-carbonized precursor to within 1000 to 1550 " C at 5 to 12"C/min for to 10 hours. New
The method of claim 11, wherein acid-treating is performed with acid comprising at least sulfuric acid, perchloric acid, and nitric acid, and drying is performed between 90 to 105"C. New
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Preparation of biomass graphene from cellulose: 18 g FeCl₂ dissolved in 100 mL distilled water (ratio 18:100), stirred 25 min to form catalyst solution. Cellulose added to catalyst solution (cellulose:solvent = 26:100), stirred 2 h, reacted at 140°C for 10 h, deoxidized and dried to obtain precursor. Pre-carbonization: heated to 280°C at 10°C/min in N₂/Ar/H₂ atmosphere, held 3 h. Secondary carbonization: heated to 1050°C at 8°C/min, held 6 h. Acid treatment, centrifugation, washing to neutral, drying at 105°C to obtain graphene. Product: uniform size, single- or multi-layer 2D layered structure, size 0.5–2 μm, conductivity 25000–45000 S/cm, yield >99.9%.
2 materials1 process step
Same as Example 1 except the cellulose used is cellulose extracted from soybean straw biomass.
Materials described outside the worked examples.
iron-based catalyst
acid mixture (sulfuric acid, perchloric acid, nitric acid)
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 is a transmission electron micrograph of graphene prepared according to Example 12.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
electrical conductivity of biomass graphene (claimed range) | 25000–45000 S/m | biomass graphene |
lateral dimension of biomass graphene (claimed range) | 0.5–2 μm |
Related documents with shared materials, methods, properties, or citations.
Figure 3 is a Raman spectrum of graphene prepared according to
graphene yield (Example 1) | ≥ 99.9 % | biomass graphene |
electrical conductivity of graphene (Example 1) | 25000–45000 S/cm | biomass graphene |
Duration | 300–7200 s | — |
Duration | 1200–5400 s | — |
Duration | 1–4 hours | — |
Duration | 4–15 hours | — |
Duration | 13–25 minutes | — |
Duration | 15–20 minutes | — |
Duration | 2–3 hours | — |
Duration | 6–16 hours | — |
Duration | 2–5 hours | — |
Duration | 5–10 hours | — |
Duration | 2–4 hours | — |
Duration | 5–8 hours | — |
Temperature | 900–1650 °C | — |
Temperature | 5–16 °C | — |
Temperature | 80–110 °C | — |
Temperature | 110–170 °C | — |
Temperature | 120–180 °C | — |
Temperature | 130–160 °C | — |
Temperature | 300–450 °C | — |
Temperature | 11–16 °C | — |
Temperature | 1000–1550 °C | — |
Temperature | 5–12 °C | — |
Temperature | 330–420 °C | — |
Temperature | 12–16 °C | — |
Temperature | 1050–1450 °C | — |
Temperature | 6–10 °C | — |
METHOD OF PREPARING GRAPHENE SHELL AND GRAPHENE SHELL PREPARED USING THE METHOD
Figure 3 is a Raman spectrum of graphene prepared according to
graphene yield (Example 1) | ≥ 99.9 % | biomass graphene |
electrical conductivity of graphene (Example 1) | 25000–45000 S/cm | biomass graphene |
Duration | 300–7200 s | — |
Duration | 1200–5400 s | — |
Duration | 1–4 hours | — |
Duration | 4–15 hours | — |
Duration | 13–25 minutes | — |
Duration | 15–20 minutes | — |
Duration | 2–3 hours | — |
Duration | 6–16 hours | — |
Duration | 2–5 hours | — |
Duration | 5–10 hours | — |
Duration | 2–4 hours | — |
Duration | 5–8 hours | — |
Temperature | 900–1650 °C | — |
Temperature | 5–16 °C | — |
Temperature | 80–110 °C | — |
Temperature | 110–170 °C | — |
Temperature | 120–180 °C | — |
Temperature | 130–160 °C | — |
Temperature | 300–450 °C | — |
Temperature | 11–16 °C | — |
Temperature | 1000–1550 °C | — |
Temperature | 5–12 °C | — |
Temperature | 330–420 °C | — |
Temperature | 12–16 °C | — |
Temperature | 1050–1450 °C | — |
Temperature | 6–10 °C | — |
METHOD OF PREPARING GRAPHENE SHELL AND GRAPHENE SHELL PREPARED USING THE METHOD
Figure 3 is a Raman spectrum of graphene prepared according to
graphene yield (Example 1) | ≥ 99.9 % | biomass graphene |
electrical conductivity of graphene (Example 1) | 25000–45000 S/cm | biomass graphene |
Duration | 300–7200 s | — |
Duration | 1200–5400 s | — |
Duration | 1–4 hours | — |
Duration | 4–15 hours | — |
Duration | 13–25 minutes | — |
Duration | 15–20 minutes | — |
Duration | 2–3 hours | — |
Duration | 6–16 hours | — |
Duration | 2–5 hours | — |
Duration | 5–10 hours | — |
Duration | 2–4 hours | — |
Duration | 5–8 hours | — |
Temperature | 900–1650 °C | — |
Temperature | 5–16 °C | — |
Temperature | 80–110 °C | — |
Temperature | 110–170 °C | — |
Temperature | 120–180 °C | — |
Temperature | 130–160 °C | — |
Temperature | 300–450 °C | — |
Temperature | 11–16 °C | — |
Temperature | 1000–1550 °C | — |
Temperature | 5–12 °C | — |
Temperature | 330–420 °C | — |
Temperature | 12–16 °C | — |
Temperature | 1050–1450 °C | — |
Temperature | 6–10 °C | — |
METHOD OF PREPARING GRAPHENE SHELL AND GRAPHENE SHELL PREPARED USING THE METHOD
Figure 3 is a Raman spectrum of graphene prepared according to
graphene yield (Example 1) | ≥ 99.9 % | biomass graphene |
electrical conductivity of graphene (Example 1) | 25000–45000 S/cm | biomass graphene |
Duration | 300–7200 s | — |
Duration | 1200–5400 s | — |
Duration | 1–4 hours | — |
Duration | 4–15 hours | — |
Duration | 13–25 minutes | — |
Duration | 15–20 minutes | — |
Duration | 2–3 hours | — |
Duration | 6–16 hours | — |
Duration | 2–5 hours | — |
Duration | 5–10 hours | — |
Duration | 2–4 hours | — |
Duration | 5–8 hours | — |
Temperature | 900–1650 °C | — |
Temperature | 5–16 °C | — |
Temperature | 80–110 °C | — |
Temperature | 110–170 °C | — |
Temperature | 120–180 °C | — |
Temperature | 130–160 °C | — |
Temperature | 300–450 °C | — |
Temperature | 11–16 °C | — |
Temperature | 1000–1550 °C | — |
Temperature | 5–12 °C | — |
Temperature | 330–420 °C | — |
Temperature | 12–16 °C | — |
Temperature | 1050–1450 °C | — |
Temperature | 6–10 °C | — |
METHOD OF PREPARING GRAPHENE SHELL AND GRAPHENE SHELL PREPARED USING THE METHOD