Patent
US 9,790,094Porous Graphene Preparation Method
Yilin TANG
US
Copyright © 2026 Matter42. All rights reserved.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1) in the presence of a catalyst, conducting catalytic treatment on a biomass carbon source, to obtain a first intermediate product, the catalyst comprising one or more selected from the group consisting of chlorides of manganese, iron compounds, cobalt compounds and nickel compounds;
The method ac c ording to Claim 1, wherein a mass ratio of the catalyst to the biomass carbon source in the step 1) is (0.01-2):1.
The method according to Claim 1, wherein the iron compounds in the step
The method ac c ording to Claim 1, wherein the catalyst in the step 1) comprises one or more selected from the group consisting of ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate and nickel acetate.
The method according to Claim 1, wherein the protective gas in the step 2), the protective gas in the step 3), the protective gas in the step 4) and the protective gas in the step 5) are independently one or more selected from the group consisting of nitrogen gas and inert gases.
The method according to Claim 1, wherein heating the first intermediate product from the first temperature to the second temperature in the step 2) is conducted at a heating rate of 5 ° C/min -20° C/min.
The method according to Claim 1, wherein heating the second intermediate product from the second temperature to the third temperature in the step 3) is conducted at a heating rate of 30 C/min -40 C/min.
The method according to Claim 1, wherein heating the third intermediate product from the third temperature to the fourth temperature in the step 4) is conducted at a heating rate of 50 c C/min-60 C/min. 27 PO₁₆₅₀₈₄₈QD Atty Docket No. 586926: 83-16 US
The method a cc ording to Claim 1, wherein cooling the fourth intermediate product from the fourth temperature to the fifth temperature in the step 5) is conducted at a cooling rate of 3 0 C/min -50 C/min. 28 PO₁₆₅₀₈₄₈QD
2) under a condition of a protective gas, heating the first intermediate product from a first temperature to a second temperature, and keeping the second temperature to obtain a second intermediate product, the first temperature being 20 cC~~40c C, and the second temperature being 300 C~3400 C;.
3) under a condition of a protective gas, heating the second intermediate product from the second temperature to a third temperature, and keeping the third temperature to obtain a third intermediate product, the third temperature being 800 C ~ 900 C;
4) under a condition of a protective gas, heating the third intermediate product from the third temperature to a fourth temperature, and keeping the fourth temperature to obtain a fourth intermediate product, the fourth SVG 15322043.12-23-2016.IX₂CFHK₅RXEAPX0.CLM.1.20.1177.1580.1262.1620.svg 0.133 0.283 Chemistry Black and white temperature being 1,1 00 C~1 0C; and
5) under a condition of a protective gas, cooling the fourth intermediate product from the fourth temperature to a fifth temperature, and keeping the fifth temperature to obtain the porous graphene, the fifth temperature being 900 C~1, 000 C.
The method according to Claim 5, wherein the biomass resource in the step A) is the agricultural and forestry residue.
The method according to Claim 5, wherein the acid in the step A) comprises one or more selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, formic acid, sulfurous acid, phosphoric acid and acetic acid.
The method according to Claim 5, wherein a dosage of the acid in the step A) is 3 wt% -20 wt% of the biomass resource.
The method according to Claim 5, wherein the hydrolyzing in the step A) is conducted at a temperature of 9 0C-180 C; and the hydrolyzing in the step A) lasts for 10 min -1O h.
The method according to Claim 5, wherein the salt treatment in the step B) is acidic sulfite treatment or alkaline sulfite treatment.
The method according to Claim 5, wherein after the porous cellulose is obtained, the step B) further comprises: conducting bleaching treatment on the porous cellulose.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Corncob hydrolyzed in sulfuric acid (3 wt% of corncob) at 90°C for 10 min to obtain lignocellulose. Acidic sulfite treatment at 70°C for 1 hour (pH 1, sulfuric acid 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in nitric acid (20 wt% of corncob) at 180°C for 10 h to obtain lignocellulose. Acidic sulfite treatment at 180°C for 6 hours (pH 7, sulfuric acid 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (10 wt% of corncob) at 130°C for 5 h to obtain lignocellulose. Acidic sulfite treatment at 120°C for 4 hours (pH 3, sulfuric acid 18 wt% of lignocellulose, ammonium sulfite, liquid-to-solid ratio 10:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (15 wt% of corncob) at 150°C for 1 h to obtain lignocellulose. Alkaline sulfite treatment at 70°C for 1 hour (pH 7, sodium hydroxide 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
3 materials1 process step
Corncob hydrolyzed in hydrochloric acid (8 wt% of corncob) at 120°C for 8 h to obtain lignocellulose. Alkaline sulfite treatment at 180°C for 6 hours (pH 14, magnesium hydroxide 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose.
3 materials1 process step
Porous cellulose from Example 1 stirred with manganese chloride (mass ratio 0.01:1) at 20°C for 2 h for catalytic treatment, dried at 70°C (moisture <10 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (200 mL/min): 25→300°C at 5°C/min, held 4 h (second intermediate); 300→800°C at 20°C/min, held 3.5 h (third intermediate); 800→1100°C at 50°C/min, held 6 h (fourth intermediate); cooled 1100→900°C at 30°C/min, held 2 h, then cooled to 60°C. Washed with 3% NaOH (60°C, 4 h), then 4% HCl (70°C, 4 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 40,000 S/m.
3 materials1 process step
Porous cellulose from Example 2 stirred with ferric nitrate (mass ratio 2:1) at 180°C for 10 h for catalytic treatment, dried at 120°C (moisture <5 wt%) to give first intermediate product. Heated in carbonization furnace under Ar (800 mL/min): 20→400°C at 20°C/min, held 8 h; 400→900°C at 50°C/min, held 7 h; 900→1300°C at 60°C/min, held 8 h; cooled 1300→1000°C at 50°C/min, held 4 h, then cooled to 20°C. Washed with 55% NaOH (120°C, 24 h), then 10% HCl (150°C, 24 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 38,000 S/m.
3 materials1 process step
Porous cellulose from Example 3 stirred with cobalt sulfate (mass ratio 0.1:1) at 50°C for 5 h for catalytic treatment, dried at 90°C (moisture <8 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (400 mL/min): 40→320°C at 10°C/min, held 5 h; 320→820°C at 30°C/min, held 5 h; 820→1150°C at 54°C/min, held 7 h; cooled 1150→920°C at 35°C/min, held 3 h, then cooled to 30°C. Washed with 10% ammonia water (80°C, 8 h), then 6% HCl (90°C, 8 h), then distilled water to neutral, dried. Product: porous graphene.
Materials described outside the worked examples.
biomass carbon source
catalyst (chlorides of manganese, iron compounds, cobalt compounds, nickel compounds)
agricultural and forestry residue
catalyst (ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate, nickel acetate)
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Electrical Conductivity | 40000 S/m | porous graphene |
Electrical Conductivity | 38000 S/m | porous graphene |
Duration | 1–6 hours | — |
Related documents with shared materials, methods, properties, or citations.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1) in the presence of a catalyst, conducting catalytic treatment on a biomass carbon source, to obtain a first intermediate product, the catalyst comprising one or more selected from the group consisting of chlorides of manganese, iron compounds, cobalt compounds and nickel compounds;
The method ac c ording to Claim 1, wherein a mass ratio of the catalyst to the biomass carbon source in the step 1) is (0.01-2):1.
The method according to Claim 1, wherein the iron compounds in the step
The method ac c ording to Claim 1, wherein the catalyst in the step 1) comprises one or more selected from the group consisting of ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate and nickel acetate.
The method according to Claim 1, wherein the protective gas in the step 2), the protective gas in the step 3), the protective gas in the step 4) and the protective gas in the step 5) are independently one or more selected from the group consisting of nitrogen gas and inert gases.
The method according to Claim 1, wherein heating the first intermediate product from the first temperature to the second temperature in the step 2) is conducted at a heating rate of 5 ° C/min -20° C/min.
The method according to Claim 1, wherein heating the second intermediate product from the second temperature to the third temperature in the step 3) is conducted at a heating rate of 30 C/min -40 C/min.
The method according to Claim 1, wherein heating the third intermediate product from the third temperature to the fourth temperature in the step 4) is conducted at a heating rate of 50 c C/min-60 C/min. 27 PO₁₆₅₀₈₄₈QD Atty Docket No. 586926: 83-16 US
The method a cc ording to Claim 1, wherein cooling the fourth intermediate product from the fourth temperature to the fifth temperature in the step 5) is conducted at a cooling rate of 3 0 C/min -50 C/min. 28 PO₁₆₅₀₈₄₈QD
2) under a condition of a protective gas, heating the first intermediate product from a first temperature to a second temperature, and keeping the second temperature to obtain a second intermediate product, the first temperature being 20 cC~~40c C, and the second temperature being 300 C~3400 C;.
3) under a condition of a protective gas, heating the second intermediate product from the second temperature to a third temperature, and keeping the third temperature to obtain a third intermediate product, the third temperature being 800 C ~ 900 C;
4) under a condition of a protective gas, heating the third intermediate product from the third temperature to a fourth temperature, and keeping the fourth temperature to obtain a fourth intermediate product, the fourth SVG 15322043.12-23-2016.IX₂CFHK₅RXEAPX0.CLM.1.20.1177.1580.1262.1620.svg 0.133 0.283 Chemistry Black and white temperature being 1,1 00 C~1 0C; and
5) under a condition of a protective gas, cooling the fourth intermediate product from the fourth temperature to a fifth temperature, and keeping the fifth temperature to obtain the porous graphene, the fifth temperature being 900 C~1, 000 C.
The method according to Claim 5, wherein the biomass resource in the step A) is the agricultural and forestry residue.
The method according to Claim 5, wherein the acid in the step A) comprises one or more selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, formic acid, sulfurous acid, phosphoric acid and acetic acid.
The method according to Claim 5, wherein a dosage of the acid in the step A) is 3 wt% -20 wt% of the biomass resource.
The method according to Claim 5, wherein the hydrolyzing in the step A) is conducted at a temperature of 9 0C-180 C; and the hydrolyzing in the step A) lasts for 10 min -1O h.
The method according to Claim 5, wherein the salt treatment in the step B) is acidic sulfite treatment or alkaline sulfite treatment.
The method according to Claim 5, wherein after the porous cellulose is obtained, the step B) further comprises: conducting bleaching treatment on the porous cellulose.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Corncob hydrolyzed in sulfuric acid (3 wt% of corncob) at 90°C for 10 min to obtain lignocellulose. Acidic sulfite treatment at 70°C for 1 hour (pH 1, sulfuric acid 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in nitric acid (20 wt% of corncob) at 180°C for 10 h to obtain lignocellulose. Acidic sulfite treatment at 180°C for 6 hours (pH 7, sulfuric acid 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (10 wt% of corncob) at 130°C for 5 h to obtain lignocellulose. Acidic sulfite treatment at 120°C for 4 hours (pH 3, sulfuric acid 18 wt% of lignocellulose, ammonium sulfite, liquid-to-solid ratio 10:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (15 wt% of corncob) at 150°C for 1 h to obtain lignocellulose. Alkaline sulfite treatment at 70°C for 1 hour (pH 7, sodium hydroxide 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
3 materials1 process step
Corncob hydrolyzed in hydrochloric acid (8 wt% of corncob) at 120°C for 8 h to obtain lignocellulose. Alkaline sulfite treatment at 180°C for 6 hours (pH 14, magnesium hydroxide 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose.
3 materials1 process step
Porous cellulose from Example 1 stirred with manganese chloride (mass ratio 0.01:1) at 20°C for 2 h for catalytic treatment, dried at 70°C (moisture <10 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (200 mL/min): 25→300°C at 5°C/min, held 4 h (second intermediate); 300→800°C at 20°C/min, held 3.5 h (third intermediate); 800→1100°C at 50°C/min, held 6 h (fourth intermediate); cooled 1100→900°C at 30°C/min, held 2 h, then cooled to 60°C. Washed with 3% NaOH (60°C, 4 h), then 4% HCl (70°C, 4 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 40,000 S/m.
3 materials1 process step
Porous cellulose from Example 2 stirred with ferric nitrate (mass ratio 2:1) at 180°C for 10 h for catalytic treatment, dried at 120°C (moisture <5 wt%) to give first intermediate product. Heated in carbonization furnace under Ar (800 mL/min): 20→400°C at 20°C/min, held 8 h; 400→900°C at 50°C/min, held 7 h; 900→1300°C at 60°C/min, held 8 h; cooled 1300→1000°C at 50°C/min, held 4 h, then cooled to 20°C. Washed with 55% NaOH (120°C, 24 h), then 10% HCl (150°C, 24 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 38,000 S/m.
3 materials1 process step
Porous cellulose from Example 3 stirred with cobalt sulfate (mass ratio 0.1:1) at 50°C for 5 h for catalytic treatment, dried at 90°C (moisture <8 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (400 mL/min): 40→320°C at 10°C/min, held 5 h; 320→820°C at 30°C/min, held 5 h; 820→1150°C at 54°C/min, held 7 h; cooled 1150→920°C at 35°C/min, held 3 h, then cooled to 30°C. Washed with 10% ammonia water (80°C, 8 h), then 6% HCl (90°C, 8 h), then distilled water to neutral, dried. Product: porous graphene.
Materials described outside the worked examples.
biomass carbon source
catalyst (chlorides of manganese, iron compounds, cobalt compounds, nickel compounds)
agricultural and forestry residue
catalyst (ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate, nickel acetate)
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Electrical Conductivity | 40000 S/m | porous graphene |
Electrical Conductivity | 38000 S/m | porous graphene |
Duration | 1–6 hours | — |
Related documents with shared materials, methods, properties, or citations.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1) in the presence of a catalyst, conducting catalytic treatment on a biomass carbon source, to obtain a first intermediate product, the catalyst comprising one or more selected from the group consisting of chlorides of manganese, iron compounds, cobalt compounds and nickel compounds;
The method ac c ording to Claim 1, wherein a mass ratio of the catalyst to the biomass carbon source in the step 1) is (0.01-2):1.
The method according to Claim 1, wherein the iron compounds in the step
The method ac c ording to Claim 1, wherein the catalyst in the step 1) comprises one or more selected from the group consisting of ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate and nickel acetate.
The method according to Claim 1, wherein the protective gas in the step 2), the protective gas in the step 3), the protective gas in the step 4) and the protective gas in the step 5) are independently one or more selected from the group consisting of nitrogen gas and inert gases.
The method according to Claim 1, wherein heating the first intermediate product from the first temperature to the second temperature in the step 2) is conducted at a heating rate of 5 ° C/min -20° C/min.
The method according to Claim 1, wherein heating the second intermediate product from the second temperature to the third temperature in the step 3) is conducted at a heating rate of 30 C/min -40 C/min.
The method according to Claim 1, wherein heating the third intermediate product from the third temperature to the fourth temperature in the step 4) is conducted at a heating rate of 50 c C/min-60 C/min. 27 PO₁₆₅₀₈₄₈QD Atty Docket No. 586926: 83-16 US
The method a cc ording to Claim 1, wherein cooling the fourth intermediate product from the fourth temperature to the fifth temperature in the step 5) is conducted at a cooling rate of 3 0 C/min -50 C/min. 28 PO₁₆₅₀₈₄₈QD
2) under a condition of a protective gas, heating the first intermediate product from a first temperature to a second temperature, and keeping the second temperature to obtain a second intermediate product, the first temperature being 20 cC~~40c C, and the second temperature being 300 C~3400 C;.
3) under a condition of a protective gas, heating the second intermediate product from the second temperature to a third temperature, and keeping the third temperature to obtain a third intermediate product, the third temperature being 800 C ~ 900 C;
4) under a condition of a protective gas, heating the third intermediate product from the third temperature to a fourth temperature, and keeping the fourth temperature to obtain a fourth intermediate product, the fourth SVG 15322043.12-23-2016.IX₂CFHK₅RXEAPX0.CLM.1.20.1177.1580.1262.1620.svg 0.133 0.283 Chemistry Black and white temperature being 1,1 00 C~1 0C; and
5) under a condition of a protective gas, cooling the fourth intermediate product from the fourth temperature to a fifth temperature, and keeping the fifth temperature to obtain the porous graphene, the fifth temperature being 900 C~1, 000 C.
The method according to Claim 5, wherein the biomass resource in the step A) is the agricultural and forestry residue.
The method according to Claim 5, wherein the acid in the step A) comprises one or more selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, formic acid, sulfurous acid, phosphoric acid and acetic acid.
The method according to Claim 5, wherein a dosage of the acid in the step A) is 3 wt% -20 wt% of the biomass resource.
The method according to Claim 5, wherein the hydrolyzing in the step A) is conducted at a temperature of 9 0C-180 C; and the hydrolyzing in the step A) lasts for 10 min -1O h.
The method according to Claim 5, wherein the salt treatment in the step B) is acidic sulfite treatment or alkaline sulfite treatment.
The method according to Claim 5, wherein after the porous cellulose is obtained, the step B) further comprises: conducting bleaching treatment on the porous cellulose.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Corncob hydrolyzed in sulfuric acid (3 wt% of corncob) at 90°C for 10 min to obtain lignocellulose. Acidic sulfite treatment at 70°C for 1 hour (pH 1, sulfuric acid 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in nitric acid (20 wt% of corncob) at 180°C for 10 h to obtain lignocellulose. Acidic sulfite treatment at 180°C for 6 hours (pH 7, sulfuric acid 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (10 wt% of corncob) at 130°C for 5 h to obtain lignocellulose. Acidic sulfite treatment at 120°C for 4 hours (pH 3, sulfuric acid 18 wt% of lignocellulose, ammonium sulfite, liquid-to-solid ratio 10:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (15 wt% of corncob) at 150°C for 1 h to obtain lignocellulose. Alkaline sulfite treatment at 70°C for 1 hour (pH 7, sodium hydroxide 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
3 materials1 process step
Corncob hydrolyzed in hydrochloric acid (8 wt% of corncob) at 120°C for 8 h to obtain lignocellulose. Alkaline sulfite treatment at 180°C for 6 hours (pH 14, magnesium hydroxide 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose.
3 materials1 process step
Porous cellulose from Example 1 stirred with manganese chloride (mass ratio 0.01:1) at 20°C for 2 h for catalytic treatment, dried at 70°C (moisture <10 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (200 mL/min): 25→300°C at 5°C/min, held 4 h (second intermediate); 300→800°C at 20°C/min, held 3.5 h (third intermediate); 800→1100°C at 50°C/min, held 6 h (fourth intermediate); cooled 1100→900°C at 30°C/min, held 2 h, then cooled to 60°C. Washed with 3% NaOH (60°C, 4 h), then 4% HCl (70°C, 4 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 40,000 S/m.
3 materials1 process step
Porous cellulose from Example 2 stirred with ferric nitrate (mass ratio 2:1) at 180°C for 10 h for catalytic treatment, dried at 120°C (moisture <5 wt%) to give first intermediate product. Heated in carbonization furnace under Ar (800 mL/min): 20→400°C at 20°C/min, held 8 h; 400→900°C at 50°C/min, held 7 h; 900→1300°C at 60°C/min, held 8 h; cooled 1300→1000°C at 50°C/min, held 4 h, then cooled to 20°C. Washed with 55% NaOH (120°C, 24 h), then 10% HCl (150°C, 24 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 38,000 S/m.
3 materials1 process step
Porous cellulose from Example 3 stirred with cobalt sulfate (mass ratio 0.1:1) at 50°C for 5 h for catalytic treatment, dried at 90°C (moisture <8 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (400 mL/min): 40→320°C at 10°C/min, held 5 h; 320→820°C at 30°C/min, held 5 h; 820→1150°C at 54°C/min, held 7 h; cooled 1150→920°C at 35°C/min, held 3 h, then cooled to 30°C. Washed with 10% ammonia water (80°C, 8 h), then 6% HCl (90°C, 8 h), then distilled water to neutral, dried. Product: porous graphene.
Materials described outside the worked examples.
biomass carbon source
catalyst (chlorides of manganese, iron compounds, cobalt compounds, nickel compounds)
agricultural and forestry residue
catalyst (ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate, nickel acetate)
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Electrical Conductivity | 40000 S/m | porous graphene |
Electrical Conductivity | 38000 S/m | porous graphene |
Duration | 1–6 hours | — |
Related documents with shared materials, methods, properties, or citations.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1) in the presence of a catalyst, conducting catalytic treatment on a biomass carbon source, to obtain a first intermediate product, the catalyst comprising one or more selected from the group consisting of chlorides of manganese, iron compounds, cobalt compounds and nickel compounds;
The method ac c ording to Claim 1, wherein a mass ratio of the catalyst to the biomass carbon source in the step 1) is (0.01-2):1.
The method according to Claim 1, wherein the iron compounds in the step
The method ac c ording to Claim 1, wherein the catalyst in the step 1) comprises one or more selected from the group consisting of ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate and nickel acetate.
The method according to Claim 1, wherein the protective gas in the step 2), the protective gas in the step 3), the protective gas in the step 4) and the protective gas in the step 5) are independently one or more selected from the group consisting of nitrogen gas and inert gases.
The method according to Claim 1, wherein heating the first intermediate product from the first temperature to the second temperature in the step 2) is conducted at a heating rate of 5 ° C/min -20° C/min.
The method according to Claim 1, wherein heating the second intermediate product from the second temperature to the third temperature in the step 3) is conducted at a heating rate of 30 C/min -40 C/min.
The method according to Claim 1, wherein heating the third intermediate product from the third temperature to the fourth temperature in the step 4) is conducted at a heating rate of 50 c C/min-60 C/min. 27 PO₁₆₅₀₈₄₈QD Atty Docket No. 586926: 83-16 US
The method a cc ording to Claim 1, wherein cooling the fourth intermediate product from the fourth temperature to the fifth temperature in the step 5) is conducted at a cooling rate of 3 0 C/min -50 C/min. 28 PO₁₆₅₀₈₄₈QD
2) under a condition of a protective gas, heating the first intermediate product from a first temperature to a second temperature, and keeping the second temperature to obtain a second intermediate product, the first temperature being 20 cC~~40c C, and the second temperature being 300 C~3400 C;.
3) under a condition of a protective gas, heating the second intermediate product from the second temperature to a third temperature, and keeping the third temperature to obtain a third intermediate product, the third temperature being 800 C ~ 900 C;
4) under a condition of a protective gas, heating the third intermediate product from the third temperature to a fourth temperature, and keeping the fourth temperature to obtain a fourth intermediate product, the fourth SVG 15322043.12-23-2016.IX₂CFHK₅RXEAPX0.CLM.1.20.1177.1580.1262.1620.svg 0.133 0.283 Chemistry Black and white temperature being 1,1 00 C~1 0C; and
5) under a condition of a protective gas, cooling the fourth intermediate product from the fourth temperature to a fifth temperature, and keeping the fifth temperature to obtain the porous graphene, the fifth temperature being 900 C~1, 000 C.
The method according to Claim 5, wherein the biomass resource in the step A) is the agricultural and forestry residue.
The method according to Claim 5, wherein the acid in the step A) comprises one or more selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, formic acid, sulfurous acid, phosphoric acid and acetic acid.
The method according to Claim 5, wherein a dosage of the acid in the step A) is 3 wt% -20 wt% of the biomass resource.
The method according to Claim 5, wherein the hydrolyzing in the step A) is conducted at a temperature of 9 0C-180 C; and the hydrolyzing in the step A) lasts for 10 min -1O h.
The method according to Claim 5, wherein the salt treatment in the step B) is acidic sulfite treatment or alkaline sulfite treatment.
The method according to Claim 5, wherein after the porous cellulose is obtained, the step B) further comprises: conducting bleaching treatment on the porous cellulose.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Corncob hydrolyzed in sulfuric acid (3 wt% of corncob) at 90°C for 10 min to obtain lignocellulose. Acidic sulfite treatment at 70°C for 1 hour (pH 1, sulfuric acid 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in nitric acid (20 wt% of corncob) at 180°C for 10 h to obtain lignocellulose. Acidic sulfite treatment at 180°C for 6 hours (pH 7, sulfuric acid 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (10 wt% of corncob) at 130°C for 5 h to obtain lignocellulose. Acidic sulfite treatment at 120°C for 4 hours (pH 3, sulfuric acid 18 wt% of lignocellulose, ammonium sulfite, liquid-to-solid ratio 10:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
4 materials1 process step
Corncob hydrolyzed in hydrochloric acid (15 wt% of corncob) at 150°C for 1 h to obtain lignocellulose. Alkaline sulfite treatment at 70°C for 1 hour (pH 7, sodium hydroxide 4 wt% of lignocellulose, magnesium sulfite, liquid-to-solid ratio 2:1) to obtain porous cellulose. Hydrogen peroxide bleaching (5 wt% H₂O2, 100°C, 5 h).
3 materials1 process step
Corncob hydrolyzed in hydrochloric acid (8 wt% of corncob) at 120°C for 8 h to obtain lignocellulose. Alkaline sulfite treatment at 180°C for 6 hours (pH 14, magnesium hydroxide 30 wt% of lignocellulose, sodium sulfite, liquid-to-solid ratio 20:1) to obtain porous cellulose.
3 materials1 process step
Porous cellulose from Example 1 stirred with manganese chloride (mass ratio 0.01:1) at 20°C for 2 h for catalytic treatment, dried at 70°C (moisture <10 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (200 mL/min): 25→300°C at 5°C/min, held 4 h (second intermediate); 300→800°C at 20°C/min, held 3.5 h (third intermediate); 800→1100°C at 50°C/min, held 6 h (fourth intermediate); cooled 1100→900°C at 30°C/min, held 2 h, then cooled to 60°C. Washed with 3% NaOH (60°C, 4 h), then 4% HCl (70°C, 4 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 40,000 S/m.
3 materials1 process step
Porous cellulose from Example 2 stirred with ferric nitrate (mass ratio 2:1) at 180°C for 10 h for catalytic treatment, dried at 120°C (moisture <5 wt%) to give first intermediate product. Heated in carbonization furnace under Ar (800 mL/min): 20→400°C at 20°C/min, held 8 h; 400→900°C at 50°C/min, held 7 h; 900→1300°C at 60°C/min, held 8 h; cooled 1300→1000°C at 50°C/min, held 4 h, then cooled to 20°C. Washed with 55% NaOH (120°C, 24 h), then 10% HCl (150°C, 24 h), then distilled water to neutral, dried. Product: porous graphene with electrical conductivity 38,000 S/m.
3 materials1 process step
Porous cellulose from Example 3 stirred with cobalt sulfate (mass ratio 0.1:1) at 50°C for 5 h for catalytic treatment, dried at 90°C (moisture <8 wt%) to give first intermediate product. Heated in carbonization furnace under N₂ (400 mL/min): 40→320°C at 10°C/min, held 5 h; 320→820°C at 30°C/min, held 5 h; 820→1150°C at 54°C/min, held 7 h; cooled 1150→920°C at 35°C/min, held 3 h, then cooled to 30°C. Washed with 10% ammonia water (80°C, 8 h), then 6% HCl (90°C, 8 h), then distilled water to neutral, dried. Product: porous graphene.
Materials described outside the worked examples.
biomass carbon source
catalyst (chlorides of manganese, iron compounds, cobalt compounds, nickel compounds)
agricultural and forestry residue
catalyst (ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate, ferrous sulfate, potassium ferricyanide, potassium ferrocyanide, potassium trioxalatoferrate, cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate, nickel chloride, nickel nitrate, nickel sulfate, nickel acetate)
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Electrical Conductivity | 40000 S/m | porous graphene |
Electrical Conductivity | 38000 S/m | porous graphene |
Duration | 1–6 hours | — |
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