CN111825086A - Graphene preparation method - Google Patents
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- CN111825086A CN111825086A CN202010788108.7A CN202010788108A CN111825086A CN 111825086 A CN111825086 A CN 111825086A CN 202010788108 A CN202010788108 A CN 202010788108A CN 111825086 A CN111825086 A CN 111825086A
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- asphalt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention provides a graphene preparation method, which comprises the following steps: crushing and primary screening the waste asphalt, mixing the waste asphalt with a solvent to obtain a mixture, performing secondary screening on the mixture to obtain a slurry mixture, centrifuging the slurry mixture to obtain a supernatant slurry, separating the supernatant slurry to obtain asphalt, mixing the asphalt and an auxiliary agent to obtain an asphalt preprocessing base material, preparing carbon powder, and performing high-temperature baking and washing treatment, oscillation dispersion treatment and atomization drying treatment on the carbon powder to obtain graphene; according to the method, the waste asphalt is favorable for preparing the graphene, the problem that the waste asphalt cannot be reused is solved, the waste asphalt is low in price and easy to obtain, the preparation cost of the graphene can be reduced when the waste asphalt is used for preparing the graphene, the economic benefit is improved, meanwhile, the method for preparing the graphene by using the waste asphalt is simple and easy to operate, is suitable for mass production, and the prepared graphene is high in physical and chemical properties.
Description
Technical Field
The invention relates to the field of graphene, in particular to a graphene preparation method.
Background
Graphene (Graphene) is a polymer made of carbon atoms in sp2The graphene is regarded as a revolutionary material in the future, and a common powder production method of the graphene is an oxidation-reduction method, wherein the oxidation-reduction method is to carry out strong oxidation treatment on graphite to obtain graphene oxide, then strip the graphene oxide to prepare the graphene oxide, and finally carry out reduction treatment to obtain the graphene.
In recent years, asphalt highway construction in China is in a period of comprehensive development, a large amount of asphalt is used every year, asphalt roads with long service life are refitted and re-paved, a large amount of waste gas asphalt cannot be well reused, a large amount of resources are wasted, a large amount of resources are consumed in subsequent treatment projects of the waste gas asphalt, a certain harm is caused to the environment, the carbon content in the asphalt is up to 70%, economic loss is caused if rich carbon resources cannot be reasonably utilized, and the residual value of the waste asphalt can be effectively improved by using the waste asphalt as a raw material to prepare graphene. Therefore, the invention provides a preparation method of graphene, which aims to overcome the defects in the prior art.
Disclosure of Invention
Aiming at the problems, the graphene is prepared by using the waste asphalt, so that the problem that the waste asphalt cannot be reused is solved, the waste asphalt is low in price and easy to obtain, the graphene preparation cost can be reduced when the waste asphalt is used for preparing graphene, the economic benefit is improved, meanwhile, the method for preparing the graphene by using the waste asphalt is simple and easy to operate, is suitable for mass production, and the prepared graphene is high in physical and chemical properties.
The invention provides a graphene preparation method, which comprises the following steps:
the method comprises the following steps: crushing the waste asphalt and performing primary screening treatment, and mixing and stirring the screened waste asphalt blocks and the solvent to obtain a mixture;
step two: performing secondary screening treatment on the mixture obtained in the first step, removing particulate filter residues, and reserving a slurry mixture for later use;
step three: centrifuging the slurry mixture obtained in the second step, removing residual particles of the slurry mixture to obtain supernatant slurry, separating the supernatant slurry, and recovering the solution to obtain asphalt;
step four: adding the asphalt obtained in the third step and the auxiliary agent into a mixing and stirring container according to the mass ratio of 100:1-100:5 for stirring reaction to obtain an asphalt preprocessing base material;
step five: introducing the asphalt preprocessing base material obtained in the fourth step into a vacuum drier for high-temperature carbonization, and grinding the carbonized asphalt preprocessing base material to obtain carbon powder;
step six: c, baking the carbon powder obtained in the fifth step at a high temperature, mixing and stirring the baked carbon powder and an acetone solution to obtain a carbon powder mixed solution, and washing the carbon powder mixed solution;
step seven: and introducing the carbon powder mixed solution subjected to the washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment, and finally carrying out atomization drying on the carbon powder mixed solution subjected to the oscillation dispersion treatment to obtain the graphene.
The further improvement lies in that: in the first step, the waste asphalt is firstly added into a crusher to be crushed to obtain waste asphalt blocks, then the waste asphalt blocks are added into a vibration screening machine to be screened to remove impurities, the screened waste asphalt blocks and a solvent are mixed and stirred for 20-30 minutes, solvent extraction treatment is carried out to dissolve the asphalt in the waste asphalt blocks into the solvent to obtain a mixture, and the mixing and stirring speed is controlled to be 150-200 revolutions per minute.
The further improvement lies in that: in the first step, the solvent is one or more of dichlorohydrocarbon of C2-C5, alkane of C6-C9 or monocyclic aromatic hydrocarbon of C9-C10.
The further improvement lies in that: and in the third step, the slurry mixture left in the second step is firstly added into an ultrahigh speed centrifuge for centrifugal treatment to remove residual particles of the slurry mixture to obtain supernatant slurry, the rotating speed of the ultrahigh speed centrifuge is controlled to be 2000-3000 r/min, then the supernatant slurry is poured into a reaction container for sedimentation treatment for 5-7 hours, and then the supernatant slurry in the reaction container is heated to 150-200 ℃ for distillation separation to obtain asphalt and recover the solvent.
The further improvement lies in that: in the fourth step, the asphalt and the auxiliary agent obtained in the third step are added into a mixing and stirring container according to the mass ratio of 100:1-100:5 to carry out stirring reaction for 40-50 minutes, the temperature in the mixing and stirring container is controlled to be 80-110 ℃, the stirring reaction speed is controlled to be 300-.
The further improvement lies in that: and the auxiliary agent in the fourth step is a mixture of polyethylene glycol dimethyl ether, calcium carbonate and molybdenum sulfide.
The further improvement lies in that: in the fifth step, the pressure in the vacuum dryer is 26-32Mpa, the high-temperature carbonization treatment temperature is 300-450 ℃, and the powder grade of the grinding treatment is 600-800-mesh sieve.
The further improvement lies in that: in the sixth step, the carbon powder obtained in the fifth step is baked at high temperature for 20-25 minutes, the baking temperature is controlled at 500-600 ℃, the baked carbon powder and the acetone solution are mixed and stirred for 15-20 minutes to obtain a carbon powder mixed solution, and the carbon powder mixed solution is washed by deionized water.
The further improvement lies in that: and seventhly, guiding the carbon powder mixed solution subjected to washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment for 20 minutes, finally guiding the carbon powder mixed solution subjected to oscillation dispersion treatment into a centrifugal spray dryer for atomization drying for 3-8 hours, and controlling the temperature in the centrifugal spray dryer to be 55-75 ℃ to obtain the graphene.
The invention has the beneficial effects that: the graphene is prepared by the waste asphalt, so that the problem that the waste asphalt cannot be reused is solved, the waste asphalt is low in price and easy to obtain, the graphene preparation cost can be reduced when the waste asphalt is used for preparing graphene, the economic benefit is improved, meanwhile, the method for preparing the graphene by the waste asphalt is simple, easy to operate and suitable for large-batch production and preparation, the carbon content of the prepared carbon powder can be improved by performing high-temperature carbonization treatment in a vacuum drier, the prepared graphene is better in conductivity, the drying speed can be improved by atomization drying treatment, the drying is more comprehensive and uniform, the arrangement uniformity of carbon atoms in the prepared graphene can be improved by ultrasonic oscillation dispersion treatment adopted in the preparation method, and the prepared graphene is strong in physical and chemical properties.
Detailed Description
In order to make the technical means, objectives and functions of the invention easy to understand, the invention will be further described with reference to the following embodiments.
Example one
A graphene preparation method comprises the following steps:
the method comprises the following steps: adding waste asphalt into a crusher to perform crushing treatment to obtain waste asphalt blocks, then adding the waste asphalt blocks into a vibration screening machine to perform screening treatment to remove impurities, mixing and stirring the screened waste asphalt blocks and dichlorohydrocarbon of C2-C5 for 25 minutes, performing solvent extraction treatment to dissolve the asphalt in the waste asphalt blocks into a solvent to obtain a mixture, and controlling the mixing and stirring speed to be 180 r/min;
step two: performing secondary screening treatment on the mixture obtained in the first step, removing particulate filter residues, and reserving a slurry mixture for later use;
step three: adding the slurry mixture left in the second step into an ultrahigh speed centrifuge for centrifugal treatment, removing residual particles of the slurry mixture to obtain a supernatant slurry, controlling the rotating speed of the ultrahigh speed centrifuge to 2800 revolutions per minute, pouring the supernatant slurry into a reaction vessel for settling treatment for 6 hours, heating the supernatant slurry in the reaction vessel to 180 ℃ for distillation separation to obtain asphalt and recovering a solvent;
step four: firstly, adding the mixture of the asphalt, the polyethylene glycol dimethyl ether, the calcium carbonate and the molybdenum sulfide obtained in the third step into a mixing and stirring container according to the mass ratio of 100:1, stirring and reacting for 45 minutes, controlling the temperature in the mixing and stirring container to be 100 ℃, controlling the stirring and reacting rotating speed to be 400 revolutions per minute, and carrying out heat preservation treatment for 30 minutes after stirring and reacting to obtain an asphalt preprocessing base material;
step five: introducing the asphalt preprocessing bed charge obtained in the fourth step into a vacuum drier for high-temperature carbonization treatment, wherein the pressure in the vacuum drier is 30Mpa, the high-temperature carbonization treatment temperature is 420 ℃, then grinding the carbonized asphalt preprocessing bed charge to obtain carbon powder, and the powder grade of the ground powder is 800 meshes;
step six: c, baking the carbon powder obtained in the fifth step for 20 minutes at a high temperature, controlling the baking temperature to be 550 ℃, mixing and stirring the baked carbon powder and an acetone solution for 20 minutes to obtain a carbon powder mixed solution, and washing the carbon powder mixed solution by using deionized water;
step seven: and (3) firstly introducing the carbon powder mixed solution subjected to washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment for 20 minutes, finally introducing the carbon powder mixed solution subjected to oscillation dispersion treatment into a centrifugal spray dryer for atomization drying for 5 hours, and controlling the temperature in the centrifugal spray dryer to be 70 ℃ to obtain the graphene.
Example two
A graphene preparation method comprises the following steps:
the method comprises the following steps: adding waste asphalt into a crusher to perform crushing treatment to obtain waste asphalt blocks, then adding the waste asphalt blocks into a vibration screening machine to perform screening treatment to remove impurities, mixing and stirring the screened waste asphalt blocks and dichlorohydrocarbon of C2-C5 for 25 minutes, performing solvent extraction treatment to dissolve the asphalt in the waste asphalt blocks into a solvent to obtain a mixture, and controlling the mixing and stirring speed to be 180 r/min;
step two: performing secondary screening treatment on the mixture obtained in the first step, removing particulate filter residues, and reserving a slurry mixture for later use;
step three: adding the slurry mixture left in the second step into an ultrahigh speed centrifuge for centrifugal treatment, removing residual particles of the slurry mixture to obtain a supernatant slurry, controlling the rotating speed of the ultrahigh speed centrifuge to 2800 revolutions per minute, pouring the supernatant slurry into a reaction vessel for settling treatment for 6 hours, heating the supernatant slurry in the reaction vessel to 180 ℃ for distillation separation to obtain asphalt and recovering a solvent;
step four: firstly, adding the mixture of the asphalt, the polyethylene glycol dimethyl ether, the calcium carbonate and the molybdenum sulfide obtained in the third step into a mixing and stirring container according to the mass ratio of 100:2.5, stirring and reacting for 45 minutes, controlling the temperature in the mixing and stirring container to be 100 ℃, controlling the stirring and reacting rotating speed to be 400 revolutions per minute, and carrying out heat preservation treatment for 30 minutes after stirring and reacting to obtain an asphalt preprocessing base material;
step five: introducing the asphalt preprocessing bed charge obtained in the fourth step into a vacuum drier for high-temperature carbonization treatment, wherein the pressure in the vacuum drier is 30Mpa, the high-temperature carbonization treatment temperature is 420 ℃, then grinding the carbonized asphalt preprocessing bed charge to obtain carbon powder, and the powder grade of the ground powder is 800 meshes;
step six: c, baking the carbon powder obtained in the fifth step for 20 minutes at a high temperature, controlling the baking temperature to be 550 ℃, mixing and stirring the baked carbon powder and an acetone solution for 20 minutes to obtain a carbon powder mixed solution, and washing the carbon powder mixed solution by using deionized water;
step seven: and (3) firstly introducing the carbon powder mixed solution subjected to washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment for 20 minutes, finally introducing the carbon powder mixed solution subjected to oscillation dispersion treatment into a centrifugal spray dryer for atomization drying for 5 hours, and controlling the temperature in the centrifugal spray dryer to be 70 ℃ to obtain the graphene.
EXAMPLE III
A graphene preparation method comprises the following steps:
the method comprises the following steps: adding waste asphalt into a crusher to perform crushing treatment to obtain waste asphalt blocks, then adding the waste asphalt blocks into a vibration screening machine to perform screening treatment to remove impurities, mixing and stirring the screened waste asphalt blocks and dichlorohydrocarbon of C2-C5 for 25 minutes, performing solvent extraction treatment to dissolve the asphalt in the waste asphalt blocks into a solvent to obtain a mixture, and controlling the mixing and stirring speed to be 180 r/min;
step two: performing secondary screening treatment on the mixture obtained in the first step, removing particulate filter residues, and reserving a slurry mixture for later use;
step three: adding the slurry mixture left in the second step into an ultrahigh speed centrifuge for centrifugal treatment, removing residual particles of the slurry mixture to obtain a supernatant slurry, controlling the rotating speed of the ultrahigh speed centrifuge to 2800 revolutions per minute, pouring the supernatant slurry into a reaction vessel for settling treatment for 6 hours, heating the supernatant slurry in the reaction vessel to 180 ℃ for distillation separation to obtain asphalt and recovering a solvent;
step four: firstly, adding the mixture of the asphalt, the polyethylene glycol dimethyl ether, the calcium carbonate and the molybdenum sulfide obtained in the third step into a mixing and stirring container according to the mass ratio of 100:5, stirring and reacting for 45 minutes, controlling the temperature in the mixing and stirring container to be 100 ℃, controlling the stirring and reacting rotating speed to be 400 revolutions per minute, and carrying out heat preservation treatment for 30 minutes after stirring and reacting to obtain an asphalt preprocessing base material;
step five: introducing the asphalt preprocessing bed charge obtained in the fourth step into a vacuum drier for high-temperature carbonization treatment, wherein the pressure in the vacuum drier is 30Mpa, the high-temperature carbonization treatment temperature is 420 ℃, then grinding the carbonized asphalt preprocessing bed charge to obtain carbon powder, and the powder grade of the ground powder is 800 meshes;
step six: c, baking the carbon powder obtained in the fifth step for 20 minutes at a high temperature, controlling the baking temperature to be 550 ℃, mixing and stirring the baked carbon powder and an acetone solution for 20 minutes to obtain a carbon powder mixed solution, and washing the carbon powder mixed solution by using deionized water;
step seven: and (3) firstly introducing the carbon powder mixed solution subjected to washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment for 20 minutes, finally introducing the carbon powder mixed solution subjected to oscillation dispersion treatment into a centrifugal spray dryer for atomization drying for 5 hours, and controlling the temperature in the centrifugal spray dryer to be 70 ℃ to obtain the graphene.
According to the first embodiment, the second embodiment and the third embodiment, the graphene prepared by the asphalt preprocessing base material obtained by mixing, stirring and carrying out heat preservation treatment on the auxiliary agent consisting of the mixture of the asphalt, the polyethylene glycol dimethyl ether, the calcium carbonate and the molybdenum sulfide according to the mass ratio of 100:1-100:5 is the best in physicochemical property.
The graphene is prepared by the waste asphalt, so that the problem that the waste asphalt cannot be reused is solved, the waste asphalt is low in price and easy to obtain, the graphene preparation cost can be reduced when the waste asphalt is used for preparing graphene, the economic benefit is improved, meanwhile, the method for preparing the graphene by the waste asphalt is simple, easy to operate and suitable for large-batch production and preparation, the carbon content of the prepared carbon powder can be improved by performing high-temperature carbonization treatment in a vacuum drier, the prepared graphene is better in conductivity, the drying speed can be improved by atomization drying treatment, the drying is more comprehensive and uniform, the arrangement uniformity of carbon atoms in the prepared graphene can be improved by ultrasonic oscillation dispersion treatment adopted in the preparation method, and the prepared graphene is strong in physical and chemical properties.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A graphene preparation method is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: crushing the waste asphalt and performing primary screening treatment, and mixing and stirring the screened waste asphalt blocks and the solvent to obtain a mixture;
step two: performing secondary screening treatment on the mixture obtained in the first step, removing particulate filter residues, and reserving a slurry mixture for later use;
step three: centrifuging the slurry mixture obtained in the second step, removing residual particles of the slurry mixture to obtain supernatant slurry, separating the supernatant slurry, and recovering the solution to obtain asphalt;
step four: adding the asphalt obtained in the third step and the auxiliary agent into a mixing and stirring container according to the mass ratio of 100:1-100:5 for stirring reaction to obtain an asphalt preprocessing base material;
step five: introducing the asphalt preprocessing base material obtained in the fourth step into a vacuum drier for high-temperature carbonization, and grinding the carbonized asphalt preprocessing base material to obtain carbon powder;
step six: c, baking the carbon powder obtained in the fifth step at a high temperature, mixing and stirring the baked carbon powder and an acetone solution to obtain a carbon powder mixed solution, and washing the carbon powder mixed solution;
step seven: and introducing the carbon powder mixed solution subjected to the washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment, and finally carrying out atomization drying on the carbon powder mixed solution subjected to the oscillation dispersion treatment to obtain the graphene.
2. The method for preparing graphene according to claim 1, wherein: in the first step, the waste asphalt is firstly added into a crusher to be crushed to obtain waste asphalt blocks, then the waste asphalt blocks are added into a vibration screening machine to be screened to remove impurities, the screened waste asphalt blocks and a solvent are mixed and stirred for 20-30 minutes, solvent extraction treatment is carried out to dissolve the asphalt in the waste asphalt blocks into the solvent to obtain a mixture, and the mixing and stirring speed is controlled to be 150-200 revolutions per minute.
3. The method for preparing graphene according to claim 1, wherein: in the first step, the solvent is one or more of dichlorohydrocarbon of C2-C5, alkane of C6-C9 or monocyclic aromatic hydrocarbon of C9-C10.
4. The method for preparing graphene according to claim 1, wherein: and in the third step, the slurry mixture left in the second step is firstly added into an ultrahigh speed centrifuge for centrifugal treatment to remove residual particles of the slurry mixture to obtain supernatant slurry, the rotating speed of the ultrahigh speed centrifuge is controlled to be 2000-3000 r/min, then the supernatant slurry is poured into a reaction container for sedimentation treatment for 5-7 hours, and then the supernatant slurry in the reaction container is heated to 150-200 ℃ for distillation separation to obtain asphalt and recover the solvent.
5. The method for preparing graphene according to claim 1, wherein: in the fourth step, the asphalt and the auxiliary agent obtained in the third step are added into a mixing and stirring container according to the mass ratio of 100:1-100:5 to carry out stirring reaction for 40-50 minutes, the temperature in the mixing and stirring container is controlled to be 80-110 ℃, the stirring reaction speed is controlled to be 300-.
6. The method for preparing graphene according to claim 1, wherein: and the auxiliary agent in the fourth step is a mixture of polyethylene glycol dimethyl ether, calcium carbonate and molybdenum sulfide.
7. The method for preparing graphene according to claim 1, wherein: in the fifth step, the pressure in the vacuum dryer is 26-32Mpa, the high-temperature carbonization treatment temperature is 300-450 ℃, and the powder grade of the grinding treatment is 600-800-mesh sieve.
8. The method for preparing graphene according to claim 1, wherein: in the sixth step, the carbon powder obtained in the fifth step is baked at high temperature for 20-25 minutes, the baking temperature is controlled at 500-600 ℃, the baked carbon powder and the acetone solution are mixed and stirred for 15-20 minutes to obtain a carbon powder mixed solution, and the carbon powder mixed solution is washed by deionized water.
9. The method for preparing graphene according to claim 1, wherein: and seventhly, guiding the carbon powder mixed solution subjected to washing treatment in the sixth step into an ultrasonic oscillator for oscillation dispersion treatment for 20 minutes, finally guiding the carbon powder mixed solution subjected to oscillation dispersion treatment into a centrifugal spray dryer for atomization drying for 3-8 hours, and controlling the temperature in the centrifugal spray dryer to be 55-75 ℃ to obtain the graphene.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113213453A (en) * | 2021-07-08 | 2021-08-06 | 长沙理工大学 | Preparation method of ion battery negative electrode material based on waste asphalt |
| CN114258166A (en) * | 2021-12-31 | 2022-03-29 | 甘肃暖季新能源科技有限公司 | Preparation method of graphene integrated heating decorative plate |
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