CN103058176A - Method for preparing graphene efficiently - Google Patents
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- CN103058176A CN103058176A CN2012105934969A CN201210593496A CN103058176A CN 103058176 A CN103058176 A CN 103058176A CN 2012105934969 A CN2012105934969 A CN 2012105934969A CN 201210593496 A CN201210593496 A CN 201210593496A CN 103058176 A CN103058176 A CN 103058176A
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Abstract
The invention discloses a method for preparing graphene efficiently. The method comprises the following steps: (1) respectively weighing soluble inorganic salt and/or soluble organic matter and expanded graphite for later use according to the mass ratio of the soluble inorganic salt and/or the soluble organic matter to the expanded graphite of 10:1 to 200:1, wherein the expanded graphite serves as a raw material; (2) adding the soluble inorganic salt and/or the soluble organic matter and the expanded graphite into distilled water, heating, mixing uniformly until the soluble inorganic salt and/or the soluble organic matter are dissolved completely, placing into a drying box until the water is volatilized completely to obtain the mixture of the expanded graphite and the inorganic salt and/or the organic matter, placing the mixture into a ball-milling tank and performing ball milling; and (3) separating ball-milling products, washing with distilled water for 3 to 5 times, performing suction filtration and drying to obtain the graphene. The graphene is prepared according to the physical method. The method is simple and practical, has no specific requirement on equipment, is low in cost, high in efficiency, pollution-free and easy to popularize and use, and solves the problems of high cost, low efficiency, low quality and the like in the conventional preparation technology for the graphene.
Description
Technical field
The present invention relates to the Graphene technical field, particularly relate to a kind of efficient method for preparing Graphene.
Background technology
Graphite is that a kind of two-dimensional nano packing material, particularly individual layer or minority layer graphene with wide application prospect has more very superior electron transfer capacity.
The monatomic thickness two dimensional crystal that Graphene, SP2 carbon atom consist of is because outstanding electronics, mechanics and and thermal property draws and huge application potential and play its extensive concern.The preparation method of existing Graphene mainly is divided into two kinds: mechanically peel method and chemical process.Mechanical means mainly comprises the adhesive tape method, ultrasonic method and ball milled; Chemical process is surperficial epitaxial growth method, graphite oxide reduction method and chemical Vapor deposition process.
At present, the graphite oxide reduction method is the main method of preparation Graphene, and the method is that graphite is carried out strong oxide treatment, obtain graphite oxide after, again it is peeled off the preparation graphene oxide, process and obtain Graphene finally by crossing reduction.Because the structure of meeting havoc graphene sheet layer in strong oxidising process, although process through reduction, the electron conjugated structure of graphene sheet layer obtains part and recovers, and still there is larger gap in the property indices of gained grapheme material with high-quality Graphene.In addition, the oxidising process of graphite needs a large amount of strongly-acid oxygenants such as the vitriol oil, concentrated nitric acid, potassium permanganate etc. usually; And have in the reduction process and need pyroprocessing or use the poisonous chemical substances such as hydrazine hydrate, sodium borohydride, not only energy consumption is large, and efficient is low, cost height and contaminate environment.
Epitaxial growth method prepares Graphene, needs at high temperature, is filled with carbon-source gas (methane, ethane, acetylene etc.), decomposing gas also forms Graphene in substrate, and the method needs the above high temperature of 1000K, and is strict to working condition, productive rate is lower, so the application of restriction Graphene.
Wherein, the guest knows the human hairs such as bud, a Gao Jun and understands the method for utilizing high-energy ball milling to prepare graphite nano-sheets, and the method is to carry out ball milling after adopting the soluble powder grinding element and expanded graphite mixing again, and the product that obtains is water or dilute hydrochloric acid washing again.Among the above-mentioned preparation method, adopt the planetary ball mill power consumption large, cost is higher during large-scale commercial production; Simultaneously, adopt dilute hydrochloric acid as solvent wash soluble powder foot couple environment certain pollution to be arranged.
Therefore, simple in the urgent need to developing a kind of method, without particular requirement, cost is low, efficient is high to equipment, pollutes littlely, easily promotes the use of, and has solved the method for the problems such as the cost that exists in the existing Graphene technology of preparing is high, efficient is low, of poor quality.
Summary of the invention
The purpose of this invention is to provide a kind of efficient, a large amount of, low-cost method for preparing Graphene, to solve high, the problems such as efficient is low, contaminate environment of the cost that exists in the prior art.
To achieve these goals, the present invention adopts following technical scheme:
A kind of efficient method for preparing Graphene is characterized in that, realizes as follows:
(1) take expanded graphite as raw material, according to soluble inorganic salt or/and the mass ratio of dissolved organic matter and expanded graphite be 10:1-200:1 respectively the weighing soluble inorganic salt or/and dissolved organic matter, expanded graphite are for subsequent use;
(2) heating mixes to soluble inorganic salt or/and dissolved organic matter all dissolves in the distilled water or/and dissolved organic matter and expanded graphite join with soluble inorganic salt, make expanded graphite and soluble inorganic salt or/and dissolved organic matter mixes, then placing loft drier to be dried to moisture all volatilizees, obtain expanded graphite and inorganic salt or/and organic mixture, again with expanded graphite and inorganic salt or/and organic mixture was put into the ball grinder stirring ball-milling 5 minutes-48 hours;
(3) the ball milling product that step (2) is obtained distilled water wash 3-5 time, suction filtration, oven dry obtains Graphene.
Described soluble inorganic salt is a kind of in soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, the phosphoric acid salt, or two kinds or two or more mixtures in the soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, sulfonate, phosphoric acid salt; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
Described dissolved organic matter is to be solid dissolvable under the normal temperature in the organic compound of water.
Described organic compound is one or more the mixture in urea, sucrose, acetate, acetic acid pyridinium salt, tartrate, the benzoate; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
The material of described ball grinder is tetrafluoroethylene, stainless steel or pottery, and the material that employed mill is situated between is zirconia ball, pottery, steel ball, glass or agate ball.
After adopting such scheme, compared with prior art, the invention has the beneficial effects as follows:
1, the present invention prepares the method for Graphene, owing to adopt ball grinding technique technique, single prepares output can be larger, and preparation cycle can be as short as 5 minutes, and production efficiency is higher, goes for large-scale industrial production;
2, the preparation technology to Graphene involved in the present invention has overcome the chemical preparation process such as graphite oxide reduction method to the graphene sheet layer structural damage, can make preferably Graphene of electroconductibility;
3, the selected soluble inorganic salt of the present invention or dissolved organic matter such as sodium-chlor, SODIUMNITRATE, urea, sucrose etc. are with low cost, wide material sources;
4, soluble inorganic salt involved in the present invention can recycling, and environmental pollution is less, and preparation technology has environment friendly.
Description of drawings
Fig. 1 is the field emission scanning electron microscope photo of the prepared Graphene of the present invention.
Embodiment
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
A kind of efficient method for preparing Graphene of the present invention is characterized in that, realizes as follows:
(1) take expanded graphite as raw material, according to soluble inorganic salt or/and the mass ratio of dissolved organic matter and expanded graphite be 10:1-200:1 respectively the weighing soluble inorganic salt or/and dissolved organic matter, expanded graphite are for subsequent use;
(2) heating mixes to soluble inorganic salt or/and dissolved organic matter all dissolves in the distilled water or/and dissolved organic matter and expanded graphite join with soluble inorganic salt, make expanded graphite and soluble inorganic salt or/and dissolved organic matter mixes, then placing loft drier to be dried to moisture all volatilizees, obtain expanded graphite and inorganic salt or/and organic mixture, again with expanded graphite and inorganic salt or/and organic mixture was put into the ball grinder stirring ball-milling 5 minutes-48 hours;
(3) the ball milling product that step (2) is obtained distilled water wash 3-5 time, suction filtration, oven dry obtains Graphene.
Described soluble inorganic salt is a kind of in soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, the phosphoric acid salt, or two kinds or two or more mixtures in the soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, sulfonate, phosphoric acid salt; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
Described dissolved organic matter is to be solid dissolvable under the normal temperature in the organic compound of water.
Described organic compound is one or more the mixture in urea, sucrose, acetate, acetic acid pyridinium salt, tartrate, the benzoate; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
The material of described ball grinder is tetrafluoroethylene, stainless steel or pottery, and the material that employed mill is situated between is zirconia ball, pottery, steel ball, glass or agate ball.
Embodiment 1:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 4g, take by weighing saltpetre 40g, the mass ratio of saltpetre and expanded graphite is 10:1;
(2) saltpetre and expanded graphite being joined in the beaker that 80mL distilled water is housed heating mixes to saltpetre and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and saltpetre, then the mixture of expanded graphite and saltpetre is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 2 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 70 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 2:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 2g, take by weighing Repone K 40g, the mass ratio of Repone K and expanded graphite is 20:1;
(2) Repone K and expanded graphite being joined in the beaker that 100mL distilled water is housed heating mixes to Repone K and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and Repone K, then the mixture of expanded graphite and Repone K is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 3 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 90 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 3:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 1.5g, take by weighing sodium sulfate 45g, the mass ratio of sodium sulfate and expanded graphite is 30:1;
(2) sodium sulfate and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to sodium sulfate and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sodium sulfate, then the mixture of expanded graphite and sodium sulfate is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 50:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 8 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 90 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 4:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 1.1g, take by weighing sodium-chlor 44g, the mass ratio of sodium-chlor and expanded graphite is 40:1;
(2) sodium-chlor and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to sodium-chlor and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sodium-chlor, then the mixture of expanded graphite and sodium-chlor is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 40:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 24 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 90 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 5:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.9g, take by weighing SODIUMNITRATE 45g, the mass ratio of SODIUMNITRATE and expanded graphite is 50:1;
(2) SODIUMNITRATE and expanded graphite being joined in the beaker that 100mL distilled water is housed heating mixes to SODIUMNITRATE and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and SODIUMNITRATE, then the mixture of expanded graphite and SODIUMNITRATE is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 36 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 6:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.8g, take by weighing vitriolate of tartar 48g, the mass ratio of vitriolate of tartar and expanded graphite is 60:1;
(2) vitriolate of tartar and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to vitriolate of tartar and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and vitriolate of tartar, then the mixture of expanded graphite and vitriolate of tartar is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 48 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 7:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.8g, take by weighing sucrose 48g, the mass ratio of sucrose and expanded graphite is 60:1;
(2) sucrose and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to sucrose and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sucrose, then the mixture of expanded graphite and sucrose is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 5 minutes, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 8:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.8g, take by weighing urea 48g, the mass ratio of urea and expanded graphite is 60:1;
(2) urea and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to urea and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and urea, then the mixture of expanded graphite and sucrose is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 10 minutes, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 9:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.8g, take by weighing sucrose 24g, sodium-chlor 24g, the mass ratio of sucrose, sodium-chlor and expanded graphite are 60:1;
(2) sucrose, sodium-chlor and expanded graphite being joined in the beaker that 120mL distilled water is housed heating mixes to sucrose, sodium-chlor and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sucrose, sodium-chlor, then the mixture of expanded graphite and sucrose, sodium-chlor is put into the ball grinder that volume is 1000mL, add the zirconium ball according to the ball material mass ratio of 25:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 20 minutes hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 10:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 4g, take by weighing saltpetre 600g, the mass ratio of saltpetre and expanded graphite is 150:1;
(2) saltpetre and expanded graphite being joined in the beaker that 500mL distilled water is housed heating mixes to saltpetre and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and saltpetre, then the mixture of expanded graphite and saltpetre is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 5:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 2 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 2500mL and stir in this ball milling product, vacuum filtration adds 2500mL, about 70 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 11:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 4g, take by weighing saltpetre 800g, the mass ratio of saltpetre and expanded graphite is 200:1;
(2) saltpetre and expanded graphite being joined in the beaker that 2000mL distilled water is housed heating mixes to saltpetre and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and saltpetre, then the mixture of expanded graphite and saltpetre is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 5:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 2 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 2500mL and stir in this ball milling product, vacuum filtration adds 2500mL, about 70 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 12:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 1.1g, take by weighing sodium-chlor 88g, the mass ratio of sodium-chlor and expanded graphite is 80:1;
(2) sodium-chlor and expanded graphite being joined in the beaker that 320mL distilled water is housed heating mixes to sodium-chlor and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sodium-chlor, then the mixture of expanded graphite and sodium-chlor is put into the ball grinder that volume is 1000mL, according to the ball material mass ratio adding zirconium ball of 10:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 24 hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 1500mL and stir in this ball milling product, vacuum filtration adds 1500mL, about 90 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Embodiment 13:
A kind of efficient method for preparing Graphene, realize as follows:
(1) take by weighing expanded graphite 0.8g, take by weighing sucrose 72g, sodium-chlor 72g, the mass ratio of sucrose, sodium-chlor and expanded graphite are 180:1;
(2) sucrose, sodium-chlor and expanded graphite being joined in the beaker that 2000mL distilled water is housed heating mixes to sucrose, sodium-chlor and all dissolves, again beaker is placed loft drier to moisture all to volatilize, obtain the mixture of expanded graphite and sucrose, sodium-chlor, then the mixture of expanded graphite and sucrose, sodium-chlor is put into the ball grinder that volume is 2000mL, add the zirconium ball according to the ball material mass ratio of 10:1;
(3) then ball grinder is installed on the agitating ball mill, with 70 rev/mins rotating speed ball millings 30 minutes hours, in ball grinder, pours out ball milling product and zirconium ball;
(4) the ball milling product of step (3) being poured out and zirconium ball distilled water flushing, sieve, the ball milling product is separated with the zirconium ball, obtain the ball milling product, add distilled water 2500mL and stir in this ball milling product, vacuum filtration adds 2500mL, about 100 ℃ distilled water wash again, vacuum filtration, twice so repeatedly; At last the 100 ℃ of lower dryings in electric drying oven with forced convection of the product behind the suction filtration were just obtained Graphene in 12 hours.
Among the present invention, the mass ratio of soluble inorganic salt and/or dissolved organic matter and expanded graphite is satisfying the requirement of 10:1-200:1, and Ball-milling Time can both be realized the present invention in 5 minutes-48 hours; This does not enumerate embodiment one by one again.
Claims (5)
1. a method that efficiently prepares Graphene is characterized in that, realizes as follows:
(1) take expanded graphite as raw material, according to soluble inorganic salt or/and the mass ratio of dissolved organic matter and expanded graphite be 10:1-200:1 respectively the weighing soluble inorganic salt or/and dissolved organic matter, expanded graphite are for subsequent use;
(2) heating mixes to soluble inorganic salt or/and dissolved organic matter all dissolves in the distilled water or/and dissolved organic matter and expanded graphite join with soluble inorganic salt, make expanded graphite and soluble inorganic salt or/and dissolved organic matter mixes, then placing loft drier to be dried to moisture all volatilizees, obtain expanded graphite and inorganic salt or/and organic mixture, again with expanded graphite and inorganic salt or/and organic mixture was put into the ball grinder stirring ball-milling 5 minutes-48 hours;
(3) the ball milling product that step (2) is obtained distilled water wash 3-5 time, suction filtration, oven dry obtains Graphene.
2. a kind of efficient method for preparing Graphene according to claim 1, it is characterized in that: described soluble inorganic salt is a kind of in soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, the phosphoric acid salt, or two kinds or two or more mixtures in the soluble chloride, nitrate, vitriol, carbonate, chromic salt, sulfonate, sulfonate, phosphoric acid salt; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
3. a kind of efficient method for preparing Graphene according to claim 1, it is characterized in that: described dissolved organic matter is to be solid dissolvable under the normal temperature in the organic compound of water.
4. a kind of efficient method for preparing Graphene according to claim 3 is characterized in that: described organic compound is one or more the mixture in urea, sucrose, acetate, acetic acid pyridinium salt, tartrate, the benzoate; When adopting mixture, the ratio of mixture of the each component in the described mixture is any proportioning.
5. a kind of efficient method for preparing Graphene according to claim 1, it is characterized in that: the material of described ball grinder is tetrafluoroethylene, stainless steel or pottery, the material that employed mill is situated between is zirconia ball, pottery, steel ball, glass or agate ball.
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| CN105480965A (en) * | 2015-11-26 | 2016-04-13 | 中国第一汽车股份有限公司 | Preparation method of graphene |
| CN105800603A (en) * | 2016-04-22 | 2016-07-27 | 华侨大学 | Method for quickly preparing high-quality graphene |
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| CN105800603A (en) * | 2016-04-22 | 2016-07-27 | 华侨大学 | Method for quickly preparing high-quality graphene |
| CN105800603B (en) * | 2016-04-22 | 2018-01-09 | 华侨大学 | A kind of quick method for preparing high-quality graphene |
| WO2017190571A1 (en) * | 2016-05-06 | 2017-11-09 | 成都新柯力化工科技有限公司 | Method for preparing organic graphene by milling and organic graphene |
| CN110117006A (en) * | 2019-06-26 | 2019-08-13 | 武汉中科先进技术研究院有限公司 | A kind of method that high-efficiency environment friendly prepares grapheme material |
| US10836641B1 (en) | 2019-07-12 | 2020-11-17 | King Abdulaziz University | Process for forming graphene-coated particles |
| US11053125B2 (en) | 2019-07-12 | 2021-07-06 | King Abdulaziz University | Graphene from fly ash |
| US11111149B2 (en) | 2019-07-12 | 2021-09-07 | King Abdulaziz University | Fly ash-catalyzed method for making graphene |
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| CN113823787A (en) * | 2021-08-17 | 2021-12-21 | 华南理工大学 | Porous sulfur composite cathode material and preparation method and application thereof |
| CN114195138A (en) * | 2021-12-14 | 2022-03-18 | 安徽大学绿色产业创新研究院 | Mechanical stripping method for preparing high-concentration graphene slurry from graphite and application of mechanical stripping method in preparation of pole plate material |
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