CN105480971A - Preparation method of asphalt-based three-dimensional mesoporous graphene material - Google Patents
Preparation method of asphalt-based three-dimensional mesoporous graphene material Download PDFInfo
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- CN105480971A CN105480971A CN201610059718.7A CN201610059718A CN105480971A CN 105480971 A CN105480971 A CN 105480971A CN 201610059718 A CN201610059718 A CN 201610059718A CN 105480971 A CN105480971 A CN 105480971A
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- C01B2204/00—Structure or properties of graphene
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a preparation method of an asphalt-based three-dimensional mesoporous graphene material and belongs to the field of carbon materials. According to the preparation method, asphalt, additives and a dispersing agent are mixed through ball milling, wherein the mass ratio of asphalt to additives is 100: (1-100), the mass fraction of the dispersing agent is 0.1-10%, the volume fraction of a ball milling solvent is 0.1-100%, the purity of the additives, the dispersing agent and the ball milling solvent is larger than 99%, and then the three-dimensional graphene material with the mesoporous structure is prepared through the technologies of drying, carbonizing, acid pickling and the like. The asphalt-based three-dimensional mesoporous graphene material is high in product purity (98-100%), large in specific area (500-2500 m<2>/g) and uniform in size, meanwhile, structural defects are small, the layer number is small (1-5), preparation cost is low, operation is easy, and popularization is easy.
Description
Technical field
The invention belongs to carbon structure Material Field, be specifically related to a kind of preparation method of asphaltic base three-dimensional meso-hole grapheme material.
Background technology
Graphene, as a kind of novel carbon material, has unique Two-dimensional Carbon honeycomb structure and excellent physical and chemical performance.The Graphene of individual layer has the specific surface of superelevation, good thermal conductivity, excellent characteristic electron and superpower mechanical property, therefore has very large utilization potentiality in fields such as electron device, detector, energy storage/conversion, sensor, biological medicine transports.Based on scientific research and the industrial application of Graphene application, progress for energy field opens new development situation and market, particularly require high storing hydrogen, fuel cell, solar cell and the aspect such as lithium ion battery, electrical condenser for storing device, Graphene all has excellent performance.
Porous graphene is as a kind of grapheme material with tridimensional network, there is uniform pore structure, can retain on the intrinsic superperformance basis of Graphene, overcome grapheme material self to reunite and stacking, farthest utilize the performances such as the specific surface area of its super large and electronic mobility.Good mechanical property, excellent electroconductibility and thermal conductivity, make porous graphene more be had an optimistic view of by numerous investigators and enterprise relative to other porous material.In addition, the existence in the hole of different size and shape, for the compound of Graphene and other materials provides great possibility, particularly will have more outstanding application in gas adsorption, separation, storage and support of the catalyst etc.
The method of the three-dimensional porous Graphene of current preparation mainly contains two classes: template and non-template method.Template is divided into hard template method and soft template method.Hard template method comprises chemical Vapor deposition process and epitaxial growth method, such as with inorganic particulates such as mesoporous silicons for template, preparation aperture, morphology controllable mesoporous grapheme material; Soft template aspect mainly prepares porous graphene using the metallic particles of generated in-situ polymkeric substance, porous or oxide compound as template.Non-template mainly refers to that chemical etching method comprises the methods such as activation of potassium hydroxide method, nitric acid oxidation method, catalyst oxidation method, and raw material mainly adopts graphene nanometer sheet, by chemical reaction etching graphene nano lamella, significantly to avoid the reunion of Graphene.But, above-mentioned preparation method exist product defect many, not environmentally, complex process, to yield poorly, the problems such as production cost is high, Difficulty.Therefore, invent a kind of be similar to soft template method low cost and the method can preparing porous graphene material is in a large number necessary and significant.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of asphaltic base three-dimensional meso-hole grapheme material, the specific surface area of obtained asphaltic base three-dimensional meso-hole Graphene is 500 ~ 2500m
2/ g, the number of plies 1 ~ 5 layer, aperture 2nm ~ 50nm, purity 98 ~ 100%; Abundant raw material source, price is low; Processing unit is simple, is easy to scale operation.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for asphaltic base three-dimensional meso-hole grapheme material, concrete steps are as follows:
(1) the ball milling mixing of pitch, additive and dispersion agent
Adding in ball mill by grinding the pitch, additive and the dispersion agent that sieve, then adding ball milling solvent and carrying out ball-milling processing, taking out and carry out drying; The mass ratio of pitch and additive is 100:1 ~ 100; The massfraction of dispersion agent is 0.1%-10%; The volume fraction of ball milling solvent is 0.1%-100%; Additive, dispersion agent and ball milling solvent purity are greater than 99%; Grinding pitch granularity after sieving is 50-300 order; Ball milling parameter is: rotational speed of ball-mill is 60r/min-1200r/min, and Ball-milling Time is 0.1h-12h; Drying temperature is 40 ~ 120 DEG C, and time of drying is 1 ~ 12h;
The pitch adopted is the one in coal-tar pitch, petroleum pitch, rock asphalt, slag oil asphalt, plant asphalt, synthetic asphalts, mesophase pitch, emulsified bitumen, Aqua-mesophase, wood pitch;
The additive adopted is nano alumina particles (2nm-50nm), nano aluminium oxide liquid (the particle size range 2nm-20nm of different-grain diameter, massfraction 5-50%) and nano aluminium oxide water-dispersion slurry (particle size range 5nm-15nm, massfraction 5-50%) in one;
The dispersion agent adopted is polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyvinylacetal, polyvinyl butyral acetal, sodium polyacrylate, triethyl hexyl phosphoric acid, alkyl-sulphate, alkylsulfonate, alkylbenzene sulfonate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester, polyethylene wax, oxidized polyethlene wax, hydrolytic polymaleic anhydride, Sodium glycocholate, glyceryl monostearate, paraffin, phosphotidats, polyoxyethylene, polyacrylate, cellobiose fat, alkyl polyglycoside, the many aldehyde of ring-type, the many ketone of ring-type, quaternary ammonium salt, B oxidation fat alcohol, diglycollic amide, Macrogol Ester, fatty alcohol, one in Soxylat A 25-7 and fat alcohol ethoxyl compound,
The ball milling solvent adopted is water, ethanol, methylene dichloride, acetone, chloroform, methyl alcohol, tetrahydrofuran (THF), tetracol phenixin, hexanaphthene, Virahol, 1,2-trichloroethane, triethylamine, toluene, pyridine, quadrol, butanols, acetic acid, chlorobenzene, p-Xylol, dimethylbenzene, N, dinethylformamide, pimelinketone, hexalin, N, N-N,N-DIMETHYLACETAMIDE, N-METHYLFORMAMIDE, phenol, methyl-sulphoxide, ethylene glycol, N-Methyl pyrrolidone, the one in methane amide, tetramethylene sulfone, glycerine;
(2) carbonize
The raw material that step (1) mixes is put into atmosphere furnace, is incubated after being then warming up to preset temperature, be cooled to room temperature and take out; Charring process parameter is:
Temperature rise rate: 1 DEG C/min ~ 50 DEG C/min
Preset temperature: 1100 DEG C ~ 2000 DEG C
Soaking time: 0.1h ~ 10h
Protective atmosphere: N
2or Ar
2
Gas flow: 25mL/min ~ 300mL/min;
(3) pickling
Step (2) gained carbonizing production is placed in acid solution stir, deionized water fully washs to neutrality, and then put into 40 ~ 100 DEG C of vacuum drying ovens and carry out drying 1 ~ 12h, vacuum tightness is 1.0 × 10
-1~ 1.0 × 10
5pa; Acid cleaning process parameter is:
Acid solution: the one in hydrochloric acid, oxalic acid, sulfuric acid, hydrofluoric acid
Acid solution volumetric molar concentration: 0.05mol/L ~ 6mol/L
Churning time: 1 ~ 5h
Stirring velocity: 25 ~ 200r/min.
Beneficial effect of the present invention is:
1) specific surface area of asphaltic base three-dimensional meso-hole grapheme material that the present invention obtains is 500 ~ 2500m
2/ g, the number of plies 1 ~ 5 layer, aperture 2nm ~ 50nm, high purity 98 ~ 100%;
2) abundant raw material source that uses of preparation method of the present invention, price is low; Processing unit is simple, is easy to scale operation.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the asphaltic base three-dimensional meso-hole grapheme material adopting embodiment 1 technique to prepare;
Fig. 2 is the transmission electron microscope picture of the asphaltic base three-dimensional meso-hole grapheme material adopting embodiment 2 technique to prepare;
Fig. 3 is the transmission electron microscope picture of the asphaltic base three-dimensional meso-hole grapheme material adopting embodiment 3 technique to prepare;
Fig. 4 is the transmission electron microscope picture of the asphaltic base three-dimensional meso-hole grapheme material adopting embodiment 4 technique to prepare;
Fig. 5 is the transmission electron microscope picture of the asphaltic base three-dimensional meso-hole grapheme material adopting embodiment 5 technique to prepare.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
Be that 2nm nano aluminium oxide liquid (massfraction 30%) adds in ball grinder with particle diameter after coal-tar pitch being ground to 180 orders, the mass ratio of coal-tar pitch and nano aluminium oxide is 1:1; Select polyvinylpyrrolidone as dispersion agent, massfraction is 10%; Ball milling solvent is DMF, and volume fraction is 20%; Be 600r/min at rotational speed of ball-mill, after ball milling 3h, be positioned in 80 DEG C of loft drier, dry 8h removes ball milling solvent.Dry sample is positioned in atmosphere furnace, passes into argon gas (argon flow amount is 100mL/min), be warming up to 1800 DEG C with 15 DEG C/min, insulation 2h, be cooled to room temperature and take out.Be positioned over by carbonizing production in hydrochloric acid soln (acid solution volumetric molar concentration is 1mol/L), stir 5h, stirring velocity is 120 revs/min, filters and is washed till neutrality with deionized water.Be positioned over vacuum drying oven (1.0 × 10
-1pa) in, dry 60 DEG C of dryings 12 hours, namely obtain asphaltic base three-dimensional meso-hole Graphene.Prepared mesoporous grapheme material performance is as follows: the number of plies is 1-3 layer, and aperture size is 2nm-5nm, and specific surface area is 2500m
2/ g, purity 98.2%.
Embodiment 2
Be that 15nm nano alumina particles adds in ball grinder with particle diameter after mesophase pitch being ground to 100 orders, the mass ratio of mesophase pitch and nano aluminium oxide is 2:1; Select sodium polyacrylate as dispersion agent, massfraction is 5%; Ball milling solvent is methylene dichloride, and volume fraction is 10%; Be 900r/min at rotational speed of ball-mill, after ball milling 1h, be positioned in 40 DEG C of loft drier, dry 4h removes ball milling solvent.Dry sample is positioned in atmosphere furnace, passes into nitrogen (nitrogen flow is 50mL/min), be warming up to 1600 DEG C with 20 DEG C/min, insulation 8h, be cooled to room temperature and take out.Be positioned over by carbonizing production in oxalic acid solution (acid solution volumetric molar concentration is 2mol/L), stir 4h, stirring velocity is 60 revs/min, filters and is washed till neutrality with deionized water.Be positioned over vacuum drying oven (1.0 × 10
-1pa) in, dry 80 DEG C of dryings 4 hours, namely obtain asphaltic base three-dimensional meso-hole Graphene.Prepared mesoporous grapheme material performance is as follows: the number of plies is 1-4 layer, and aperture size is 10nm-15nm, and specific surface area is 1000m
2/ g, purity 99.5%.
Embodiment 3
Be that the water-dispersion of 10nm nano aluminium oxide is starched (massfraction 20wt%) and added in ball grinder by liquid emulsion pitch and median size, the mass ratio of emulsified bitumen and nano aluminium oxide aqueous dispersions is 4:1; Select Soxylat A 25-7 as dispersion agent, massfraction is 2%; Ball milling solvent is deionized water, and volume fraction is 3%; Be 300r/min at rotational speed of ball-mill, after ball milling 12h, be positioned in 60 DEG C of loft drier, dry 10h removes ball milling solvent.Dry sample is positioned in atmosphere furnace, passes into argon gas (argon flow amount is 150mL/min), be warming up to 1700 DEG C with 10 DEG C/min, insulation 3h, be cooled to room temperature and take out.Be positioned over by carbonizing production in hydrochloric acid soln (acid solution volumetric molar concentration is 2mol/L), stir 1h, stirring velocity is 80 revs/min, filters and is washed till neutrality with deionized water.Be positioned over vacuum drying oven (1.0 × 10
-1pa) in, dry 60 DEG C of dryings 10 hours, namely obtain asphaltic base three-dimensional meso-hole Graphene.Prepared mesoporous grapheme material performance is as follows: the number of plies is 1-5 layer, and aperture size is 5nm-10nm, and specific surface area is 1350m
2/ g, purity 98.9%.
Embodiment 4
Be that 10nm nano alumina particles adds in ball grinder with median size after rock asphalt being ground 300 orders, the mass ratio of rock asphalt and nano aluminium oxide is 5:1; Select polyvinyl alcohol-400 as dispersion agent, massfraction is 0.1%; Ball milling solvent is ethanol, and volume fraction is 50%; Be 800r/min at rotational speed of ball-mill, after ball milling 2h, be positioned in 50 DEG C of loft drier, dry 12h removes ball milling solvent.Dry sample is positioned in atmosphere furnace, passes into argon gas (argon flow amount is 200mL/min), be warming up to 1900 DEG C with 30 DEG C/min, insulation 0.5h, be cooled to room temperature and take out.Be positioned over by carbonizing production in hydrofluoric acid solution (acid solution volumetric molar concentration is 0.5mol/L), stir 2.5h, stirring velocity is 100 revs/min, filters and is washed till neutrality with deionized water.Be positioned over vacuum drying oven (1.0 × 10
-1pa) in, dry 80 DEG C of dryings 12 hours, namely obtain asphaltic base three-dimensional meso-hole Graphene.Prepared mesoporous grapheme material performance is as follows: the number of plies is 1-5 layer, and aperture size is 4nm-10nm, and specific surface area is 1100m
2/ g, purity 99.6%.
Embodiment 5
Be that the water-dispersion of 15nm nano aluminium oxide is starched (massfraction 50%) and added in ball grinder with median size after petroleum pitch being ground 50 orders, the mass ratio of petroleum pitch and nano aluminium oxide water-dispersion slurry is 10:1; Select sodium lauryl sulphate as dispersion agent, massfraction is 2.5%; Ball milling solvent is hexanaphthene, and volume fraction is 25%; Be 300r/min at rotational speed of ball-mill, after ball milling 6h, be positioned in 70 DEG C of loft drier, dry 6h removes ball milling solvent.Dry sample is positioned in atmosphere furnace, passes into argon gas (argon flow amount is 120mL/min), be warming up to 2000 DEG C with 5 DEG C/min, insulation 0.5h, be cooled to room temperature and take out.Be positioned over by carbonizing production in sulphuric acid soln (acid solution volumetric molar concentration is 5mol/L), stir 3h, stirring velocity is 60 revs/min, filters and is washed till neutrality with deionized water.Be positioned over vacuum drying oven (1.0 × 10
-1pa) in, dry 80 DEG C of dryings 12 hours, namely obtain asphaltic base three-dimensional meso-hole Graphene.Prepared mesoporous grapheme material performance is as follows: the number of plies is 2-5 layer, and aperture size is 10nm-15nm, and specific surface area is 900m
2/ g, purity 98%.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (6)
1. a preparation method for asphaltic base three-dimensional meso-hole grapheme material, is characterized in that: concrete steps are as follows:
(1) the ball milling mixing of pitch, additive and dispersion agent
Adding in ball mill by grinding the pitch, additive and the dispersion agent that sieve, then adding ball milling solvent and carrying out ball-milling processing, taking out and carry out drying; The mass ratio of pitch and additive is 100:1 ~ 100; The massfraction of dispersion agent is 0.1%-10%; The volume fraction of ball milling solvent is 0.1%-100%; Additive, dispersion agent and ball milling solvent purity are greater than 99%;
(2) carbonize
The raw material that step (1) mixes is put into atmosphere furnace, is incubated after being then warming up to preset temperature, be cooled to room temperature and take out; Charring process parameter is:
Temperature rise rate: 1 DEG C/min ~ 50 DEG C/min
Preset temperature: 1100 DEG C ~ 2000 DEG C
Soaking time: 0.1h ~ 10h
Protective atmosphere: N
2or Ar
2
Gas flow: 25mL/min ~ 300mL/min;
(3) pickling
Step (2) gained carbonizing production is placed in acid solution stir, deionized water fully washs to neutrality, and then put into 40 ~ 100 DEG C of vacuum drying ovens and carry out drying 1 ~ 12h, vacuum tightness is 1.0 × 10
-1~ 1.0 × 10
5pa; Acid cleaning process parameter is:
Acid solution: the one in hydrochloric acid, oxalic acid, sulfuric acid
Acid solution volumetric molar concentration: 0.05mol/L ~ 6mol/L
Churning time: 1 ~ 5h
Stirring velocity: 25 ~ 200r/min.
2. the preparation method of a kind of asphaltic base three-dimensional meso-hole grapheme material according to claim 1, is characterized in that: described pitch is the one in coal-tar pitch, petroleum pitch, rock asphalt, slag oil asphalt, plant asphalt, synthetic asphalts, mesophase pitch, emulsified bitumen, Aqua-mesophase and wood pitch.
3. method according to claim 1, is characterized in that: described additive is the one in nano alumina particles, nano aluminium oxide liquid and nano aluminium oxide water-dispersion slurry; Described nano alumina particles particle size range 2nm-50nm; Described nano aluminium oxide liquid particle size range 2nm-20nm, massfraction 5-50%; Described nano aluminium oxide water-dispersion slurry particle size range 5nm-15nm, massfraction 5-50%.
4. method according to claim 1, it is characterized in that: described dispersion agent is polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polyvinylacetal, polyvinyl butyral acetal, sodium polyacrylate, triethyl hexyl phosphoric acid, alkyl-sulphate, alkylsulfonate, alkylbenzene sulfonate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester, polyethylene wax, oxidized polyethlene wax, hydrolytic polymaleic anhydride, Sodium glycocholate, glyceryl monostearate, paraffin, phosphotidats, polyoxyethylene, polyacrylate, cellobiose fat, alkyl polyglycoside, the many aldehyde of ring-type, the many ketone of ring-type, quaternary ammonium salt, B oxidation fat alcohol, diglycollic amide, Macrogol Ester, fatty alcohol, one in Soxylat A 25-7 and fat alcohol ethoxyl compound.
5. method according to claim 1, it is characterized in that: described ball milling solvent is water, ethanol, methylene dichloride, acetone, chloroform, methyl alcohol, tetrahydrofuran (THF), tetracol phenixin, hexanaphthene, Virahol, 1,2-trichloroethane, triethylamine, toluene, pyridine, quadrol, butanols, acetic acid, chlorobenzene, p-Xylol, dimethylbenzene, N, one in dinethylformamide, pimelinketone, hexalin, N,N-dimethylacetamide, N-METHYLFORMAMIDE, phenol, methyl-sulphoxide, ethylene glycol, N-Methyl pyrrolidone, methane amide, tetramethylene sulfone and glycerine.
6. method according to claim 1, is characterized in that: grinding pitch granularity after sieving in step (1) is 50-300 order; Ball milling parameter is: rotational speed of ball-mill is 60r/min-1200r/min, and Ball-milling Time is 0.1h-12h; Drying temperature is 40 ~ 120 DEG C, and time of drying is 1 ~ 12h.
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Cited By (12)
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| CN106025745A (en) * | 2016-06-29 | 2016-10-12 | 佛山市盈通黑金碳材料股份有限公司 | Graphite brush and preparation method thereof |
| CN106185890A (en) * | 2016-07-04 | 2016-12-07 | 石河子大学 | A kind of preparation method of porous class Graphene |
| CN108793137A (en) * | 2018-08-29 | 2018-11-13 | 中国科学院半导体研究所 | The method for preparing single-layer graphene using Parylene |
| CN109179363A (en) * | 2018-08-01 | 2019-01-11 | 湖南工业大学 | A kind of charcoal and preparation method thereof of Screw Extrusion processing |
| CN108163844B (en) * | 2018-03-19 | 2020-02-11 | 程贤甦 | Preparation method for preparing graphene by using waste tire rubber powder |
| CN111269329A (en) * | 2020-02-28 | 2020-06-12 | 王春林 | Novel asphalt emulsifier and preparation method thereof |
| CN111825086A (en) * | 2020-08-07 | 2020-10-27 | 河南墨特石墨烯科技有限公司 | Graphene preparation method |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
| CN112885895A (en) * | 2021-01-25 | 2021-06-01 | 北海惠科光电技术有限公司 | Preparation method of graphene conductive film, thin film transistor and display device |
| WO2021212407A1 (en) * | 2020-04-23 | 2021-10-28 | 浙江华彩新材料有限公司 | Super-leveling acid rain-resistant powder coating for aluminum profile |
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| CN106025745B (en) * | 2016-06-29 | 2019-03-05 | 佛山市盈通黑金碳材料股份有限公司 | A kind of electrographite brush and preparation method thereof |
| CN106185890A (en) * | 2016-07-04 | 2016-12-07 | 石河子大学 | A kind of preparation method of porous class Graphene |
| CN108163844B (en) * | 2018-03-19 | 2020-02-11 | 程贤甦 | Preparation method for preparing graphene by using waste tire rubber powder |
| CN109179363A (en) * | 2018-08-01 | 2019-01-11 | 湖南工业大学 | A kind of charcoal and preparation method thereof of Screw Extrusion processing |
| CN108793137A (en) * | 2018-08-29 | 2018-11-13 | 中国科学院半导体研究所 | The method for preparing single-layer graphene using Parylene |
| CN111269329A (en) * | 2020-02-28 | 2020-06-12 | 王春林 | Novel asphalt emulsifier and preparation method thereof |
| WO2021212407A1 (en) * | 2020-04-23 | 2021-10-28 | 浙江华彩新材料有限公司 | Super-leveling acid rain-resistant powder coating for aluminum profile |
| CN111825086A (en) * | 2020-08-07 | 2020-10-27 | 河南墨特石墨烯科技有限公司 | Graphene preparation method |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
| CN112885895A (en) * | 2021-01-25 | 2021-06-01 | 北海惠科光电技术有限公司 | Preparation method of graphene conductive film, thin film transistor and display device |
| CN114408903A (en) * | 2022-01-12 | 2022-04-29 | 华南理工大学 | Method for preparing in-plane porous few-layer graphene material at low temperature in environment-friendly manner |
| CN115010118A (en) * | 2022-06-06 | 2022-09-06 | 武汉理工大学 | Nitrogen and sulfur doped hierarchical macroporous/mesoporous graphene, and preparation method and application thereof |
| CN115010118B (en) * | 2022-06-06 | 2024-01-23 | 武汉理工大学 | Nitrogen and sulfur doped hierarchical macroporous/mesoporous graphene and preparation method and application thereof |
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