Patent
US 10,899,621System and Method for Preparing Graphene Oxide and Reduced Graphene Oxide
Anthony B. Taves
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,899,621Patent 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.
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed KMn O 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed KMn O 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; and separating colloidal graphene oxide from reaction products within the vessel contents [[.]]; and wherein the method further comprises one or more of the following: (a) adding the first volume of warm distilled water to the reaction vessel at a controlled rate between 2m l/min and 5m l/min so as to maintain the temperature of contents of the reaction vessel between 80 and 90 degrees C; and (b) wherein the second volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Currently amended
The method of Claim 1, further comprising reducing the graphene oxide by: adding ascorbic acid to the colloidal graphene oxide while agitating and maintaining the colloidal graphene oxide/ascorbic acid mixture at a predetermined reduction temperature; and allowing the colloidal graphene oxide/ascorbic acid mixture to cool to an ambient temperature for a determined reduction period. Currently amended
The method of Claim 1, wherein the predetermined chill temperature is approximately 0 degrees C. Original
The method of Claim 1, wherein the two or more acid reactants include a quantity of H 2 S O 4 and a quantity of H 3 P O 4. Original
The method of Claim 1, wherein the intermixed acid mixture comprises sulfuric acid and phosphoric acid in a ratio of approximately 75/25 by volume, respectively. Original
The method of Claim 1, wherein a ratio of the quantity of KMn O 4 and the quantity of graphite is 3 to 1 by weight, respectively. Original
The method of Claim 1, wherein graphite suspension placed into the chilled reaction vessel is in gaseous communication with atmospheric oxygen. Original
The method of Claim 1, wherein the predetermined period of cool agitation comprises a period of four to eight hours. Original
The method of Claim 1, wherein the predetermined cool temperature profile comprises one or more of: maintaining a temperature of the graphite suspension below 50 degrees C over the first 90 minutes of the predetermined period of cool agitation; providing a continuously rising temperature profile of the graphite suspension from about zero degrees C to about 45 degrees C, over an initial 60 to 90 minutes of the predetermined period of cool agitation; maintaining a temperature profile of the graphite suspension to prevent temperatures from plateauing for more than five minutes during the predetermined period of cool agitation; [[and]] maintaining temperature of the graphite suspension between 40 and 45 degrees C with a PID thermal control loop; and cooling the graphite suspension during a first 15 to 30 minutes of the predetermined period of cool agitation and thereafter allowing the temperature the graphite suspension to rise to between 40 to 45 degrees C over about 90 minutes of the predetermined period of cool agitation and then remain at a temperature between 40 to 45 degrees C a remainder of the predetermined period of cool agitation. Currently amended
The method of Claim 1, wherein the first volume of warm distilled water is heated to 50 to degrees C. Original
The method of Claim 1, wherein the first period of warm agitation comprises a period of time from 45 to 60 minutes. Original
The method of Claim 1, wherein the first volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Original
The method of Claim 1, wherein the reaction vessel further comprises a PID thermal control loop and a heating and/or cooling apparatus interface. Currently amended
The method of Claim 1, wherein the second volume of warm distilled water is heated to approximately 90 degrees C. Original
The method of Claim 1, wherein the predetermined pre-peroxide temperature is approximately 50 degrees C. Original
The method of Claim 1, wherein a concentration of the hydrogen peroxide is 35% by volume Original
The method of Claim 1, wherein a volume of the hydrogen peroxide is approximately equal to one half an initial volume of H 2 S O 4 used in the intermixed acid mixture. Original
The method of Claim 1, wherein the agitation further comprises a stainless steel multi-wire whip rotating within the reaction vessel at a predetermined speed. Original
The method of Claim 1, wherein the settling period is within the range of 12 to 14 hours. Original
Canceled
Canceled
(Cu rr ently Amended) A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 300 ml of 98 % H 2 S O 4 and 100 ml of 85% H 3 P O 4; the KMn O 4 comprises approximately 30 grams of potassium permanganate; the graphite comprises approximately 10 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 400 ml of distilled [[H20;]] H₂ O; the second volume of warm distilled water comprises approximately 400 ml H20; and the predetermined amount of hydrogen peroxide comprises approximately 150 ml of 35% H 202. Currently amended
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 900 ml of 98 % H 2 S O 4 and 300 ml of 85% H₃P O 4; the KMn O 4 comprises approximately 90 grams of potassium permanganate; the graphite comprises approximately 30 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 1200 ml of distilled H 2 0; the second volume of warm distilled water comprises approximately 1200 ml H 2 0; and the predetermined amount of hydrogen peroxide comprises approximately 450 ml of 35 % H 2 0 2. Currently amended
Materials described outside the worked examples.
potassium permanganate
KMnO₄
graphite
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 60–90 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,899,621Patent 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.
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed KMn O 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed KMn O 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; and separating colloidal graphene oxide from reaction products within the vessel contents [[.]]; and wherein the method further comprises one or more of the following: (a) adding the first volume of warm distilled water to the reaction vessel at a controlled rate between 2m l/min and 5m l/min so as to maintain the temperature of contents of the reaction vessel between 80 and 90 degrees C; and (b) wherein the second volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Currently amended
The method of Claim 1, further comprising reducing the graphene oxide by: adding ascorbic acid to the colloidal graphene oxide while agitating and maintaining the colloidal graphene oxide/ascorbic acid mixture at a predetermined reduction temperature; and allowing the colloidal graphene oxide/ascorbic acid mixture to cool to an ambient temperature for a determined reduction period. Currently amended
The method of Claim 1, wherein the predetermined chill temperature is approximately 0 degrees C. Original
The method of Claim 1, wherein the two or more acid reactants include a quantity of H 2 S O 4 and a quantity of H 3 P O 4. Original
The method of Claim 1, wherein the intermixed acid mixture comprises sulfuric acid and phosphoric acid in a ratio of approximately 75/25 by volume, respectively. Original
The method of Claim 1, wherein a ratio of the quantity of KMn O 4 and the quantity of graphite is 3 to 1 by weight, respectively. Original
The method of Claim 1, wherein graphite suspension placed into the chilled reaction vessel is in gaseous communication with atmospheric oxygen. Original
The method of Claim 1, wherein the predetermined period of cool agitation comprises a period of four to eight hours. Original
The method of Claim 1, wherein the predetermined cool temperature profile comprises one or more of: maintaining a temperature of the graphite suspension below 50 degrees C over the first 90 minutes of the predetermined period of cool agitation; providing a continuously rising temperature profile of the graphite suspension from about zero degrees C to about 45 degrees C, over an initial 60 to 90 minutes of the predetermined period of cool agitation; maintaining a temperature profile of the graphite suspension to prevent temperatures from plateauing for more than five minutes during the predetermined period of cool agitation; [[and]] maintaining temperature of the graphite suspension between 40 and 45 degrees C with a PID thermal control loop; and cooling the graphite suspension during a first 15 to 30 minutes of the predetermined period of cool agitation and thereafter allowing the temperature the graphite suspension to rise to between 40 to 45 degrees C over about 90 minutes of the predetermined period of cool agitation and then remain at a temperature between 40 to 45 degrees C a remainder of the predetermined period of cool agitation. Currently amended
The method of Claim 1, wherein the first volume of warm distilled water is heated to 50 to degrees C. Original
The method of Claim 1, wherein the first period of warm agitation comprises a period of time from 45 to 60 minutes. Original
The method of Claim 1, wherein the first volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Original
The method of Claim 1, wherein the reaction vessel further comprises a PID thermal control loop and a heating and/or cooling apparatus interface. Currently amended
The method of Claim 1, wherein the second volume of warm distilled water is heated to approximately 90 degrees C. Original
The method of Claim 1, wherein the predetermined pre-peroxide temperature is approximately 50 degrees C. Original
The method of Claim 1, wherein a concentration of the hydrogen peroxide is 35% by volume Original
The method of Claim 1, wherein a volume of the hydrogen peroxide is approximately equal to one half an initial volume of H 2 S O 4 used in the intermixed acid mixture. Original
The method of Claim 1, wherein the agitation further comprises a stainless steel multi-wire whip rotating within the reaction vessel at a predetermined speed. Original
The method of Claim 1, wherein the settling period is within the range of 12 to 14 hours. Original
Canceled
Canceled
(Cu rr ently Amended) A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 300 ml of 98 % H 2 S O 4 and 100 ml of 85% H 3 P O 4; the KMn O 4 comprises approximately 30 grams of potassium permanganate; the graphite comprises approximately 10 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 400 ml of distilled [[H20;]] H₂ O; the second volume of warm distilled water comprises approximately 400 ml H20; and the predetermined amount of hydrogen peroxide comprises approximately 150 ml of 35% H 202. Currently amended
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 900 ml of 98 % H 2 S O 4 and 300 ml of 85% H₃P O 4; the KMn O 4 comprises approximately 90 grams of potassium permanganate; the graphite comprises approximately 30 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 1200 ml of distilled H 2 0; the second volume of warm distilled water comprises approximately 1200 ml H 2 0; and the predetermined amount of hydrogen peroxide comprises approximately 450 ml of 35 % H 2 0 2. Currently amended
Materials described outside the worked examples.
potassium permanganate
KMnO₄
graphite
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 60–90 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,899,621Patent 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.
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed KMn O 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed KMn O 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; and separating colloidal graphene oxide from reaction products within the vessel contents [[.]]; and wherein the method further comprises one or more of the following: (a) adding the first volume of warm distilled water to the reaction vessel at a controlled rate between 2m l/min and 5m l/min so as to maintain the temperature of contents of the reaction vessel between 80 and 90 degrees C; and (b) wherein the second volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Currently amended
The method of Claim 1, further comprising reducing the graphene oxide by: adding ascorbic acid to the colloidal graphene oxide while agitating and maintaining the colloidal graphene oxide/ascorbic acid mixture at a predetermined reduction temperature; and allowing the colloidal graphene oxide/ascorbic acid mixture to cool to an ambient temperature for a determined reduction period. Currently amended
The method of Claim 1, wherein the predetermined chill temperature is approximately 0 degrees C. Original
The method of Claim 1, wherein the two or more acid reactants include a quantity of H 2 S O 4 and a quantity of H 3 P O 4. Original
The method of Claim 1, wherein the intermixed acid mixture comprises sulfuric acid and phosphoric acid in a ratio of approximately 75/25 by volume, respectively. Original
The method of Claim 1, wherein a ratio of the quantity of KMn O 4 and the quantity of graphite is 3 to 1 by weight, respectively. Original
The method of Claim 1, wherein graphite suspension placed into the chilled reaction vessel is in gaseous communication with atmospheric oxygen. Original
The method of Claim 1, wherein the predetermined period of cool agitation comprises a period of four to eight hours. Original
The method of Claim 1, wherein the predetermined cool temperature profile comprises one or more of: maintaining a temperature of the graphite suspension below 50 degrees C over the first 90 minutes of the predetermined period of cool agitation; providing a continuously rising temperature profile of the graphite suspension from about zero degrees C to about 45 degrees C, over an initial 60 to 90 minutes of the predetermined period of cool agitation; maintaining a temperature profile of the graphite suspension to prevent temperatures from plateauing for more than five minutes during the predetermined period of cool agitation; [[and]] maintaining temperature of the graphite suspension between 40 and 45 degrees C with a PID thermal control loop; and cooling the graphite suspension during a first 15 to 30 minutes of the predetermined period of cool agitation and thereafter allowing the temperature the graphite suspension to rise to between 40 to 45 degrees C over about 90 minutes of the predetermined period of cool agitation and then remain at a temperature between 40 to 45 degrees C a remainder of the predetermined period of cool agitation. Currently amended
The method of Claim 1, wherein the first volume of warm distilled water is heated to 50 to degrees C. Original
The method of Claim 1, wherein the first period of warm agitation comprises a period of time from 45 to 60 minutes. Original
The method of Claim 1, wherein the first volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Original
The method of Claim 1, wherein the reaction vessel further comprises a PID thermal control loop and a heating and/or cooling apparatus interface. Currently amended
The method of Claim 1, wherein the second volume of warm distilled water is heated to approximately 90 degrees C. Original
The method of Claim 1, wherein the predetermined pre-peroxide temperature is approximately 50 degrees C. Original
The method of Claim 1, wherein a concentration of the hydrogen peroxide is 35% by volume Original
The method of Claim 1, wherein a volume of the hydrogen peroxide is approximately equal to one half an initial volume of H 2 S O 4 used in the intermixed acid mixture. Original
The method of Claim 1, wherein the agitation further comprises a stainless steel multi-wire whip rotating within the reaction vessel at a predetermined speed. Original
The method of Claim 1, wherein the settling period is within the range of 12 to 14 hours. Original
Canceled
Canceled
(Cu rr ently Amended) A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 300 ml of 98 % H 2 S O 4 and 100 ml of 85% H 3 P O 4; the KMn O 4 comprises approximately 30 grams of potassium permanganate; the graphite comprises approximately 10 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 400 ml of distilled [[H20;]] H₂ O; the second volume of warm distilled water comprises approximately 400 ml H20; and the predetermined amount of hydrogen peroxide comprises approximately 150 ml of 35% H 202. Currently amended
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 900 ml of 98 % H 2 S O 4 and 300 ml of 85% H₃P O 4; the KMn O 4 comprises approximately 90 grams of potassium permanganate; the graphite comprises approximately 30 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 1200 ml of distilled H 2 0; the second volume of warm distilled water comprises approximately 1200 ml H 2 0; and the predetermined amount of hydrogen peroxide comprises approximately 450 ml of 35 % H 2 0 2. Currently amended
Materials described outside the worked examples.
potassium permanganate
KMnO₄
graphite
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 60–90 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,899,621Patent 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.
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed KMn O 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed KMn O 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; and separating colloidal graphene oxide from reaction products within the vessel contents [[.]]; and wherein the method further comprises one or more of the following: (a) adding the first volume of warm distilled water to the reaction vessel at a controlled rate between 2m l/min and 5m l/min so as to maintain the temperature of contents of the reaction vessel between 80 and 90 degrees C; and (b) wherein the second volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Currently amended
The method of Claim 1, further comprising reducing the graphene oxide by: adding ascorbic acid to the colloidal graphene oxide while agitating and maintaining the colloidal graphene oxide/ascorbic acid mixture at a predetermined reduction temperature; and allowing the colloidal graphene oxide/ascorbic acid mixture to cool to an ambient temperature for a determined reduction period. Currently amended
The method of Claim 1, wherein the predetermined chill temperature is approximately 0 degrees C. Original
The method of Claim 1, wherein the two or more acid reactants include a quantity of H 2 S O 4 and a quantity of H 3 P O 4. Original
The method of Claim 1, wherein the intermixed acid mixture comprises sulfuric acid and phosphoric acid in a ratio of approximately 75/25 by volume, respectively. Original
The method of Claim 1, wherein a ratio of the quantity of KMn O 4 and the quantity of graphite is 3 to 1 by weight, respectively. Original
The method of Claim 1, wherein graphite suspension placed into the chilled reaction vessel is in gaseous communication with atmospheric oxygen. Original
The method of Claim 1, wherein the predetermined period of cool agitation comprises a period of four to eight hours. Original
The method of Claim 1, wherein the predetermined cool temperature profile comprises one or more of: maintaining a temperature of the graphite suspension below 50 degrees C over the first 90 minutes of the predetermined period of cool agitation; providing a continuously rising temperature profile of the graphite suspension from about zero degrees C to about 45 degrees C, over an initial 60 to 90 minutes of the predetermined period of cool agitation; maintaining a temperature profile of the graphite suspension to prevent temperatures from plateauing for more than five minutes during the predetermined period of cool agitation; [[and]] maintaining temperature of the graphite suspension between 40 and 45 degrees C with a PID thermal control loop; and cooling the graphite suspension during a first 15 to 30 minutes of the predetermined period of cool agitation and thereafter allowing the temperature the graphite suspension to rise to between 40 to 45 degrees C over about 90 minutes of the predetermined period of cool agitation and then remain at a temperature between 40 to 45 degrees C a remainder of the predetermined period of cool agitation. Currently amended
The method of Claim 1, wherein the first volume of warm distilled water is heated to 50 to degrees C. Original
The method of Claim 1, wherein the first period of warm agitation comprises a period of time from 45 to 60 minutes. Original
The method of Claim 1, wherein the first volume of warm distilled water is approximately equal to a volume of the intermixed acid mixture. Original
The method of Claim 1, wherein the reaction vessel further comprises a PID thermal control loop and a heating and/or cooling apparatus interface. Currently amended
The method of Claim 1, wherein the second volume of warm distilled water is heated to approximately 90 degrees C. Original
The method of Claim 1, wherein the predetermined pre-peroxide temperature is approximately 50 degrees C. Original
The method of Claim 1, wherein a concentration of the hydrogen peroxide is 35% by volume Original
The method of Claim 1, wherein a volume of the hydrogen peroxide is approximately equal to one half an initial volume of H 2 S O 4 used in the intermixed acid mixture. Original
The method of Claim 1, wherein the agitation further comprises a stainless steel multi-wire whip rotating within the reaction vessel at a predetermined speed. Original
The method of Claim 1, wherein the settling period is within the range of 12 to 14 hours. Original
Canceled
Canceled
(Cu rr ently Amended) A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 300 ml of 98 % H 2 S O 4 and 100 ml of 85% H 3 P O 4; the KMn O 4 comprises approximately 30 grams of potassium permanganate; the graphite comprises approximately 10 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 400 ml of distilled [[H20;]] H₂ O; the second volume of warm distilled water comprises approximately 400 ml H20; and the predetermined amount of hydrogen peroxide comprises approximately 150 ml of 35% H 202. Currently amended
A method comprising: chilling a reaction vessel to a predetermined chill temperature; intermixing a quantity of two or more acid reactants to form an intermixed acid mixture; chilling the intermixed acid mixture to the predetermined chill temperature; intermixing a quantity of KMn O 4 and a quantity of graphite; chilling the intermixed K MnO 4 and graphite to the predetermined chill temperature; placing the chilled intermixed acid mixture into the chilled reaction vessel and initiating a low speed agitation of the acid mixture; adding the chilled intermixed K MnO 4 and graphite to the chilled reaction vessel to form a graphite suspension; continuing agitation of the reaction vessel for a predetermined period of cool agitation while maintaining the reaction vessel within a predetermined cool temperature profile; adding a first volume of warm distilled water during a first period of warm agitation while the graphite suspension is agitated; adding a second volume of distilled water during a second period of warm agitation while the graphite suspension is agitated; while agitating, cooling the graphite suspension to a predetermined pre- peroxide temperature; adding a predetermined amount of hydrogen peroxide to the reaction vessel; allowing contents of the reaction vessel to cool and se tt le over a se tt ling period; separating colloidal graphene oxide from reaction products within the vessel contents; and wherein: the intermixed acid mixture comprises approximately 900 ml of 98 % H 2 S O 4 and 300 ml of 85% H₃P O 4; the KMn O 4 comprises approximately 90 grams of potassium permanganate; the graphite comprises approximately 30 grams of flake graphite between about 50 and 250 mesh in size; the first volume of warm distilled water comprises approximately 1200 ml of distilled H 2 0; the second volume of warm distilled water comprises approximately 1200 ml H 2 0; and the predetermined amount of hydrogen peroxide comprises approximately 450 ml of 35 % H 2 0 2. Currently amended
Materials described outside the worked examples.
potassium permanganate
KMnO₄
graphite
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Duration | 60–90 minutes | — |
Duration |
Related documents with shared materials, methods, properties, or citations.
sulfuric acid
H₂SO₄
phosphoric acid
H₃PO₄
hydrogen peroxide
H₂O₂
graphene oxide
ascorbic acid
reduced graphene oxide
flake graphite (50-250 mesh)
| 15–30 minutes |
| — |
Duration | 4–8 hours | — |
Duration | 45–60 minutes | — |
Thickness | 45–100 µm | — |
Duration | 12–14 hours | — |
Duration | 1–10 hours | — |
PROCESS FOR THE PREPARATION OF GRAPHENE
sulfuric acid
H₂SO₄
phosphoric acid
H₃PO₄
hydrogen peroxide
H₂O₂
graphene oxide
ascorbic acid
reduced graphene oxide
flake graphite (50-250 mesh)
| 15–30 minutes |
| — |
Duration | 4–8 hours | — |
Duration | 45–60 minutes | — |
Thickness | 45–100 µm | — |
Duration | 12–14 hours | — |
Duration | 1–10 hours | — |
PROCESS FOR THE PREPARATION OF GRAPHENE
sulfuric acid
H₂SO₄
phosphoric acid
H₃PO₄
hydrogen peroxide
H₂O₂
graphene oxide
ascorbic acid
reduced graphene oxide
flake graphite (50-250 mesh)
| 15–30 minutes |
| — |
Duration | 4–8 hours | — |
Duration | 45–60 minutes | — |
Thickness | 45–100 µm | — |
Duration | 12–14 hours | — |
Duration | 1–10 hours | — |
PROCESS FOR THE PREPARATION OF GRAPHENE
sulfuric acid
H₂SO₄
phosphoric acid
H₃PO₄
hydrogen peroxide
H₂O₂
graphene oxide
ascorbic acid
reduced graphene oxide
flake graphite (50-250 mesh)
| 15–30 minutes |
| — |
Duration | 4–8 hours | — |
Duration | 45–60 minutes | — |
Thickness | 45–100 µm | — |
Duration | 12–14 hours | — |
Duration | 1–10 hours | — |
PROCESS FOR THE PREPARATION OF GRAPHENE