CN108455582A - A kind of preparation method of the three-dimensional porous grapheme material of low cost - Google Patents
A kind of preparation method of the three-dimensional porous grapheme material of low cost Download PDFInfo
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- CN108455582A CN108455582A CN201810344732.0A CN201810344732A CN108455582A CN 108455582 A CN108455582 A CN 108455582A CN 201810344732 A CN201810344732 A CN 201810344732A CN 108455582 A CN108455582 A CN 108455582A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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Abstract
The invention discloses a kind of preparation methods of the three-dimensional porous graphene of low cost, belong to carbon materials field.Carbon matrix precursor and a certain amount of solvent are stirred, rear addition additive and template are mixed, and wherein the mass ratio of carbon matrix precursor, additive and template is 1:10:10~10:1:1, the quality of solvent is 1~5 times of carbon matrix precursor, then passes through the techniques such as drying, charing, pickling and the porous graphene material with good three-dimensional structure is prepared.The product specific surface area of the present invention is 300~1600 m2/ g, mesopore content 85 ~ 98%, the number of plies are 1~10 layer, and purity 98~100%, defect is less, and preparation process is simple, at low cost, is easy to industrialized production.
Description
Technical field
The invention belongs to carbon structure Material Fields, and in particular to a kind of preparation of the three-dimensional porous grapheme material of low cost
Method.
Technical background
From graphene from 2004 by since being successfully made, since it is with unique structure and excellent performance, make it
There is huge application potential in each field, therefore become the hot spot studied both at home and abroad in a short time, prepares, characterizes and answer
The extensive concern of the experts and scholars of the multiple fields such as physics, chemistry and material is caused with research.But graphene film interlayer is often
It is easy to reunite there are stronger pi-pi bond and van der Waals interaction, to be difficult to make full use of its specific surface in application process
The performances such as product and electric conductivity, to limit its application to a certain extent.In order to overcome the problems, such as this, structure has three-dimensional more
The graphene of pore structure using its unique porous structure and excellent internal performance, and then promotes the application performance of material, expands
Its big application range has become important one of approach.
The method for preparing three-dimensional porous graphene at present mainly has template, sol-gal process and chemical corrosion method.Template
Method mainly utilizes carbon different solubility in a metal, and by controlling process conditions, oversaturated carbon is precipitated on metal matrix,
Large-size graphene film is obtained, the three-dimensional porous graphene defect obtained is few, and substantially prepared by single layer, and pore-size distribution is equal
It is even, the disadvantage is that process conditions are not easy to control, it is of high cost, it is not suitable with a wide range of production；Sol-gal process is mainly by graphite oxide
Aqueous solution is restored or is assembled, and the Graphene gel system of three-dimensional net structure is obtained to prepare to have, then through dry or
Solidification obtains three-dimensional porous grapheme material, and the three-dimensional porous graphene obtained is had excellent performance, but reaction process is complicated, can not
Control factor is more, and the production cycle is long, and pore size is difficult to control and unsuitable large area production；And chemical corrosion method includes mainly KOH
Two kinds of activation method and nitric acid oxidation etch refer to utilizing chemical activation medium, at a certain temperature, oxidation are made to testing
Graphene film is corroded, and another method of porous activated graphene material is obtained, and this method is relatively simple, the three-dimensional of gained
Porous graphene has higher specific surface area and percent opening, but there are more defects, reduces the mechanical performance of material, aperture point
Cloth and the problem that size is difficult to control and environmental pollution is larger.Generally speaking, the method for preparing three-dimensional porous graphene at present
More or less that there are costs is higher, technique is cumbersome, long preparation period, environmental pollution is big and is difficult to realize industrialization large-scale production
The problems such as.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of low costs to prepare three-dimensional porous graphite
The preparation method of alkene, this method preparation process is simple, and raw material sources are abundant, cheap at low cost, is easy to industrialized production,
It is 300-1600 m that obtained graphene, which has good three-dimensional porous structure, specific surface area,2/ g, mesopore content 85 ~ 98%,
The number of plies is 1~10 layer, 98~100 % of purity.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of asphaltic base three-dimensional meso-hole grapheme material, is as follows：
（1）The mixing of raw material
Carbon matrix precursor and solvent are added in three-necked flask and carry out heating stirring, it is rear that additive and template is added, it is passed through nitrogen,
Solvent is steamed after being uniformly mixed, and takes out drying；Carbon matrix precursor, the mass ratio containing zinc additive and template are 1:10:10
~10:1:1, the quality of solvent is 1~5 times of carbon matrix precursor.
Used carbon matrix precursor be selected from coal tar pitch and petroleum asphalt, bitumen, synthetic asphalts, mesophase pitch, sucrose,
One kind in phenolic resin, epoxy resin, bimaleimide resin.
Used additive is zinc oxide, zinc iodide, zinc bromide, zinc fluoride, zinc sulphide, zinc chloride, naphthalene acid zinc, phthalocyanine
Zinc, zinc sulfate（Seven water）, zinc acetate,（Two water）, zinc nitrate, zinc stearate, one kind in zinc acetylacetonate.
Used template is nano magnesia, light magnesium oxide, magnesium sulfate, magnesium nitrate, magnesium hydroxide, citric acid
One kind in magnesium, magnesium carbonate.
Used solvent be methanol, deionized water, ethyl alcohol, isopropanol, benzene, toluene, dichloromethane, acetone, hexamethylene,
N-Methyl pyrrolidone, ethyl acetate, ethylenediamine, styrene, perchloroethylene, trichloro ethylene, n-butanol, acetic acid, dimethylbenzene, first
One kind in amide, N- methylformamide, n,N-Dimethylformamide, cyclohexanol, ethylene glycol and glycerine.
Raw material whipping temp is 80~160 DEG C, and mixing time is 1~3h；Drying temperature is 25~80 DEG C, and drying time is
2~5h.
（2）Charing
By step（1）The raw material mixed is put into atmosphere furnace, is kept the temperature after then heating to predetermined temperature, is cooled to room temperature and takes
Go out；Charring process parameter is：
Heating rate：1 DEG C/min~25 DEG C/min
Predetermined temperature：1200 DEG C~1900 DEG C
Soaking time：The h of 0.1 h~3
Protective atmosphere：N2Or Ar2
（3）Pickling
By step（2）Gained carbonizing production, which is placed in acid solution, to be stirred, and neutrality is washed till through washing, alcohol, is then put into 40~100 DEG C very
Dry 1~12h in empty baking oven；Acid cleaning process parameter is：
Acid solution：One kind in hydrochloric acid, phosphoric acid, nitric acid, oxalic acid, sulfuric acid
Acid solution molar concentration：The mol/L of 1mol/L~4
Mixing time：2~6h
Mixing speed：25~200 r/min；
The beneficial effects of the present invention are：
（1）The specific surface area of three-dimensional porous graphene produced by the present invention is 300~1600m2/ g, mesoporous contain
Amount 85 ~ 98%, the number of plies are 1~10 layer, and purity 98~100%, fault of construction is few, even aperture distribution；
（2）Three-dimensional porous graphene is prepared using a step charring, reduces processing step, production efficiency is high；
（3）Pore creating material is alternatively arranged as in carbonization process using the template containing magnesium, and the later stage is easy to pickling removal；
（4）Raw material sources are abundant, and cheap, process equipment is simple, easily realizes industrialization.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of the three-dimensional porous graphene prepared using 1 technique of embodiment；
Fig. 2 is the transmission electron microscope picture of the three-dimensional porous graphene prepared using 2 technique of embodiment；
Fig. 3 is the transmission electron microscope picture of the three-dimensional porous graphene prepared using 3 technique of embodiment；
Fig. 4 is the transmission electron microscope picture of the three-dimensional porous graphene prepared using 4 technique of embodiment.
Specific implementation mode
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
A kind of preparation method of three-dimensional porous graphene, includes the following steps：
Asphalt is added in three-necked flask, uses dichloromethane for solvent, the mass ratio of asphalt and dichloromethane is
1:2, carry out heating stirring, whipping temp is 80 DEG C, is then added zinc oxide and nano magnesia, asphalt, zinc oxide and
The mass ratio of nano magnesia is 1:2:1.5, and it is passed through nitrogen, mixing time 2h.It is to be mixed uniformly after, be evaporated under reduced pressure out molten
Agent is positioned over 50 DEG C of vacuum drying ovens and dries 4 hours, is cooled to room temperature.Drying sample is positioned in atmosphere furnace, nitrogen is passed through,
800 DEG C are warming up to 10 DEG C/min, 1h is kept the temperature, then 1300 DEG C are warming up to 4 DEG C/min, keeps the temperature 2h, be cooled to room temperature taking-up.It will
Carbonizing production is positioned over sulfuric acid solution（Acid solution molar concentration is 2mol/L）In, 2h is stirred, mixing speed is 60 r/min, filtering
After separation neutrality is washed till with deionized water and ethyl alcohol.Dry 80 DEG C of dryings 10 hours are positioned in drying box, that is, are obtained three-dimensional more
Hole graphene.Prepared three-dimensional porous graphene performance is as follows：Specific surface area is 1600 m2/ g, mesopore content 85%, the number of plies
It is 1~5 layer, purity 98.2%.
Embodiment 2
Sucrose is added in three-necked flask, uses deionized water for solvent, the mass ratio of sucrose and deionized water is 1:3, it carries out
Heating stirring, whipping temp are 70 DEG C, are then added zinc chloride and magnesium citrate, sucrose, zinc chloride and magnesium citrate quality
Than being 1:3:3, and it is passed through nitrogen, mixing time 3h.It is to be mixed uniformly after, be evaporated under reduced pressure out solvent, be positioned over 60 DEG C of vacuum
Oven drying 3.5 hours, is cooled to room temperature.Drying sample is positioned in atmosphere furnace, nitrogen is passed through, is warming up to 4 DEG C/min
800 DEG C, 2h is kept the temperature, then 1800 DEG C are warming up to 2 DEG C/min, keep the temperature 2h, be cooled to room temperature taking-up.Carbonizing production is positioned over salt
Acid solution（Acid solution molar concentration is 1mol/L）In, 4h is stirred, mixing speed is 80 r/min, and deionized water is used after being separated by filtration
And ethyl alcohol is washed till neutrality.Dry 90 DEG C of dryings 12 hours are positioned in drying box, that is, obtain three-dimensional porous graphene.It is prepared
Three-dimensional porous graphene performance it is as follows：Specific surface area is 500 m2/ g, mesopore content 91%, the number of plies are 5~10 layers, purity
98%。
Embodiment 3
Epoxy resin is added in three-necked flask, uses ethyl acetate for solvent, the mass ratio of epoxy resin and ethyl acetate is
1:4, carry out heating stirring, whipping temp is 120 DEG C, is then added Phthalocyanine Zinc and nano magnesia, epoxy resin, Phthalocyanine Zinc and
The mass ratio of nano magnesia is 1:3:4, and it is passed through nitrogen, mixing time 1.5h.It is to be mixed uniformly after, be evaporated under reduced pressure out molten
Agent is positioned over 80 DEG C of vacuum drying ovens and dries 3 hours, is cooled to room temperature.Drying sample is positioned in atmosphere furnace, nitrogen is passed through,
800 DEG C are warming up to 5 DEG C/min, 2h is kept the temperature, then 1500 DEG C are warming up to 3 DEG C/min, keeps the temperature 2h, be cooled to room temperature taking-up.It will
Carbonizing production is positioned over hydrochloric acid solution（Acid solution molar concentration is 1mol/L）In, 3h is stirred, mixing speed is 100 r/min, mistake
After filter separation neutrality is washed till with deionized water and ethyl alcohol.Dry 100 DEG C of dryings 8 hours are positioned in drying box, that is, are obtained three-dimensional
Porous graphene.Prepared three-dimensional porous graphene performance is as follows：Specific surface area is 650 m2/ g, mesopore content 95%, the number of plies
It is 4~8 layers, purity 99.5%
Embodiment 4
Mesophase pitch is added in three-necked flask, uses n-butanol for solvent, the mass ratio of mesophase pitch and n-butanol is
1:5, heating stirring is carried out, whipping temp is 150 DEG C, and zinc acetylacetonate and light magnesium oxide, mesophase pitch, second is then added
The mass ratio of acyl acetone zinc and light magnesium oxide is 1:2:4, and it is passed through argon gas, mixing time 1h.It is to be mixed uniformly after, decompression
Distilling off solvent is positioned over 65 DEG C of vacuum drying ovens and dries 4 hours, is cooled to room temperature.Drying sample is positioned in atmosphere furnace,
It is passed through nitrogen, 800 DEG C are warming up to 5 DEG C/min, 1.5h is kept the temperature, then 1400 DEG C are warming up to 3 DEG C/min, keeps the temperature 2h, be cooled to
Room temperature is taken out.Carbonizing production is positioned over sulfuric acid solution（Acid solution molar concentration is 2mol/L）In, 3h is stirred, mixing speed is
100 r/min, neutrality is washed till after being separated by filtration with deionized water and ethyl alcohol.It is small that dry 100 DEG C of dryings 8 are positioned in drying box
When, that is, obtain three-dimensional porous graphene.Prepared three-dimensional porous graphene performance is as follows：Specific surface area is 800 m2/ g, in
Hole content 98%, the number of plies are 3~6 layers, purity 99.3%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of preparation method of the three-dimensional porous grapheme material of low cost, it is characterised in that：It is as follows：
（1）The mixing of raw material
Progress heating stirring dissolving in three-necked flask is added in carbon matrix precursor and solvent in mass ratio, rear that additive and template is added
Agent is passed through nitrogen, is uniformly mixed and steams solvent, takes out drying；The mass ratio of carbon matrix precursor, additive and template is
1:10:10~10:1:1, the quality of solvent is 1~5 times of carbon matrix precursor quality；
（2）Charing
By step（1）The raw material mixed is put into atmosphere furnace, is kept the temperature after then heating to predetermined temperature, is cooled to room temperature and takes
Go out；Charring process parameter is：
Heating rate：1 DEG C/min~25 DEG C/min；
Predetermined temperature：1200 DEG C~1900 DEG C；
Soaking time：The h of 0.1 h~3；
Protective atmosphere：N2Or Ar2；
（3）Pickling
By step（2）Gained carbonizing production, which is placed in acid solution, to be stirred, and neutrality is washed till through washing, alcohol, is then put into 40~100 DEG C very
1~12h is dried in empty baking oven；Acid cleaning process parameter is：
Acid solution：One kind in hydrochloric acid, phosphoric acid, nitric acid, oxalic acid, sulfuric acid；
Acid solution molar concentration：The mol/L of 1mol/L~4；
Mixing time：2~6h；
Mixing speed：25~200 r/min.
2. preparation method according to claim 1, it is characterised in that：Step（1）Employed in carbon matrix precursor be coal drip
Blueness, asphalt, bitumen, synthetic asphalts, mesophase pitch, sucrose, phenolic resin, epoxy resin, bismaleimide
One kind in resin.
3. preparation method according to claim 1, it is characterised in that：Step（1）Employed in additive be zinc oxide,
Zinc iodide, zinc bromide, zinc fluoride, zinc sulphide, zinc chloride, naphthalene acid zinc, Phthalocyanine Zinc, zinc sulfate, zinc acetate, zinc nitrate, stearic acid
One kind in zinc, zinc acetylacetonate.
4. preparation method according to claim 1, it is characterised in that：Step（1）Employed in template be nano oxygen
Change one kind in magnesium, light magnesium oxide, magnesium sulfate, magnesium nitrate, magnesium hydroxide, magnesium citrate, magnesium carbonate.
5. preparation method according to claim 1, it is characterised in that：Step（1）Employed in solvent
For methanol, deionized water, ethyl alcohol, isopropanol, benzene, toluene, dichloromethane, acetone, hexamethylene, N-Methyl pyrrolidone,
Ethyl acetate, ethylenediamine, styrene, perchloroethylene, trichloro ethylene, n-butanol, acetic acid, dimethylbenzene, formamide, N- methyl first
One kind in amide, n,N-Dimethylformamide, cyclohexanol, ethylene glycol and glycerine.
6. preparation method according to claim 1, it is characterised in that：Step（1）Middle raw material whipping temp is 80~160
DEG C, mixing time is 1~3h；Drying temperature is 25~80 DEG C, and drying time is 2~5h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126776A (en) * | 2018-09-06 | 2019-01-04 | 青岛科技大学 | A kind of preparation method and application of low reaction object diffusion steric hindrance hydrogenation catalyst |
| CN109305669A (en) * | 2018-11-22 | 2019-02-05 | 陕西延长石油（集团）有限责任公司 | It is a kind of to utilize the clay standby three-dimensional porous graphene and preparation method thereof of coal base oil |
| CN109321211A (en) * | 2018-10-19 | 2019-02-12 | 福州大学 | A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof |
| CN109686990A (en) * | 2019-01-29 | 2019-04-26 | 东北大学 | A kind of preparation method and application of Ni-Zn/ nitrogen sulphur codope three-dimensional graphene electrode material |
| CN111484002A (en) * | 2020-04-17 | 2020-08-04 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene membrane |
| CN113716546A (en) * | 2021-08-31 | 2021-11-30 | 青岛海洋科学与技术国家实验室发展中心 | Graphene/mesoporous carbon/ZIF-derived carbon composite three-dimensional graded porous carbon material, and preparation method and application thereof |
| CN114195128A (en) * | 2021-11-26 | 2022-03-18 | 北方民族大学 | Nitrogen-oxygen co-doped carbon nanosheet, preparation method and application thereof, and supercapacitor |
| CN115043400A (en) * | 2022-05-18 | 2022-09-13 | 黄河科技学院 | Nitrogen-doped hierarchical pore carbon nanoflower material taking ZnO/coal pitch as raw material, and preparation method and application thereof |
| CN115991469A (en) * | 2021-10-18 | 2023-04-21 | 中国石油天然气股份有限公司 | Method for preparing graphene material by catalytic slurry oil |
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| CN109126776B (en) * | 2018-09-06 | 2021-05-28 | 青岛科技大学 | Preparation method and application of hydrogenation catalyst with low reactant diffusion steric hindrance |
| CN109126776A (en) * | 2018-09-06 | 2019-01-04 | 青岛科技大学 | A kind of preparation method and application of low reaction object diffusion steric hindrance hydrogenation catalyst |
| CN109321211A (en) * | 2018-10-19 | 2019-02-12 | 福州大学 | A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof |
| CN109305669A (en) * | 2018-11-22 | 2019-02-05 | 陕西延长石油（集团）有限责任公司 | It is a kind of to utilize the clay standby three-dimensional porous graphene and preparation method thereof of coal base oil |
| CN109686990A (en) * | 2019-01-29 | 2019-04-26 | 东北大学 | A kind of preparation method and application of Ni-Zn/ nitrogen sulphur codope three-dimensional graphene electrode material |
| CN109686990B (en) * | 2019-01-29 | 2020-11-24 | 东北大学 | Preparation method and application of Ni-Zn/nitrogen-sulfur double-doped three-dimensional graphene electrode material |
| CN111484002A (en) * | 2020-04-17 | 2020-08-04 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene membrane |
| CN113716546A (en) * | 2021-08-31 | 2021-11-30 | 青岛海洋科学与技术国家实验室发展中心 | Graphene/mesoporous carbon/ZIF-derived carbon composite three-dimensional graded porous carbon material, and preparation method and application thereof |
| CN115991469A (en) * | 2021-10-18 | 2023-04-21 | 中国石油天然气股份有限公司 | Method for preparing graphene material by catalytic slurry oil |
| CN114195128A (en) * | 2021-11-26 | 2022-03-18 | 北方民族大学 | Nitrogen-oxygen co-doped carbon nanosheet, preparation method and application thereof, and supercapacitor |
| CN114195128B (en) * | 2021-11-26 | 2023-03-10 | 北方民族大学 | Nitrogen-oxygen co-doped carbon nanosheet, preparation method and application thereof, and supercapacitor |
| CN115043400A (en) * | 2022-05-18 | 2022-09-13 | 黄河科技学院 | Nitrogen-doped hierarchical pore carbon nanoflower material taking ZnO/coal pitch as raw material, and preparation method and application thereof |
| CN115043400B (en) * | 2022-05-18 | 2024-01-12 | 黄河科技学院 | Nitrogen-doped hierarchical pore carbon nanoflower material with ZnO/coal tar pitch as raw material, and preparation method and application thereof |
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