CN105502359B - A kind of preparation method of inexpensive porous graphene - Google Patents
A kind of preparation method of inexpensive porous graphene Download PDFInfo
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- CN105502359B CN105502359B CN201510965997.9A CN201510965997A CN105502359B CN 105502359 B CN105502359 B CN 105502359B CN 201510965997 A CN201510965997 A CN 201510965997A CN 105502359 B CN105502359 B CN 105502359B
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention belongs to high performance carbon cellulosic material field, and in particular to a kind of preparation method of inexpensive porous graphene.By using cheap carbon precursor and additive it is raw material, is mixed by raw material, low-temperature carbonization, acid cleaning process prepare porous graphene.The advantage of the invention is that：Technique is simple, cost is cheap, easy Industry Promotion；Prepared porous graphene purity is high, fault of construction is few, even aperture distribution.
Description
Technical field
The invention belongs to carbon materials field, and in particular to a kind of preparation method of inexpensive porous graphene.
Background technology
Porous graphene, it is a kind of grapheme material with tridimensional network.It is more as a kind of new carbon material
Hole graphene is with its unique three-dimensional structure and excellent physical and chemical performance, in various electrode of electrochemical device materials, catalysis
Agent carrier, gas separation and storage etc. have good application prospect.On the one hand, porous graphene possesses graphene uniqueness
Chemical property, the advantages that thermal conductivity and the specific surface area of superelevation are big；On the other hand, on this basis, its unique three-dimensional
Structure, reunion and the stacking of grapheme material itself can be effectively avoided, make full use of the specific surface area of its super large, good electricity
Sub- migration rate, the premium properties of abundant graphene, further expand the material answering in energy field, electronic applications etc.
With.
At present, it is main that porous graphene is prepared using template and chemical etching method.Template prepares porous graphene,
CVD technology is mainly used, magnesia is that template prepares the controllable porous graphene in aperture.Chemical etching method activates including KOH
Method, nitric acid oxidation method, the methods of agent oxidizing process is facilitated, raw material mainly uses graphene film, and graphene is etched by chemically reacting
Lamella, significantly to avoid the reunion of graphene.But the above method, it is dirty more or less to there is complex process, cost height, environment
Dye, product defect are more and the problem of being difficult to mass production, limit the application and popularization of porous graphene.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of preparation side of inexpensive porous graphene
Method.The preparation technology is simple, cost is low, and Industry Promotion is easy, and prepared porous graphene has good three-dimensional porous knot
Structure, fault of construction are few, and product purity is high.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of inexpensive porous graphene, comprises the following steps：
1）The mixing of raw material：In mass ratio 100:1~100:100 weigh carbon precursor and aluminum contained compound, add solvent,
After 25 DEG C ~ 150 DEG C are stirred 1 ~ 5h, solvent evaporated, solid residue is placed in 40 DEG C~100 DEG C baking ovens and dries 1 ~ 12h；
2）Low-temperature carbonization：By step 1）Dried material is put into atmosphere furnace, then with 1 DEG C/min~50 DEG C/min's
Heating rate keeps the h of 0.1 h~10 after being warming up to 1100 DEG C~2000 DEG C, be cooled to room temperature taking-up；
3）Pickling：By step 2）Gained carbonizing production is placed in 1~5h of stirring, deionized water in acid solution and fully washed into
Property, it is then placed in after being dried in vacuum drying oven, porous graphene is made.
Step 1）The gross mass of middle carbon precursor and aluminum contained compound and the mass values of solvent are：1:1~1:10.
Step 1）Described aluminum contained compound be aluminium chloride, aluminum sulfate, aluminium carbonate, aluminum acetate, aluminum nitrate, aluminium hydroxide,
Sodium metaaluminate, aluminium nitride, aluminum phosphate, alumina silicate, aluminium carbide, ten sulfate dihydrate aluminium ammonia, metasilicic acid aluminium, trifluoromethanesulfonic acid aluminium, three
Alkyl aluminum, dialkylaluminum chloride, an alkyl al dichloride, the aluminium of trialkyl tri-chlorination two, aluminium isopropoxide, butyl aluminium, aluminium acetate, first
Sour aluminium, oxalic acid aluminium, propionic acid aluminium, polyaluminium chloride, alumina silicate, fluoric acid aluminium, aluminium secondary butylate, praseodynium aluminium, triisobutyl aluminium, 8-
Hydroxyquinoline aluminum, aluminum perchlorate, aluminum monostearate, aluminium distearate, oxalic acid aluminium, ethyl aluminum dichloride, second squama aluminium, acetylacetone,2,4-pentanedione
One kind in aluminium, aluminium dihydrogen phosphate, aluminum oleate, aluminium bromide, silver iodide, aluminium ethylate, aluctyl, isooctyl acid aluminium, trioctylaluminum.
Step 1）Described carbon precursor is pitch, sucrose, lignin and its derivative, hemicellulose, cellulose, shallow lake
Powder, tannin, rosin, chitin, polyvinyl alcohol, polyethylene glycol, polyethylene, melamine and its derivative, urea, polyvinyl alcohol
Acetal, polyvinyl butyral resin, polystyrene, polyurethane, polyimides, phenolic resin, furfural resin, furfuryl alcohol resin, furan
One kind in furane resins, epoxy resin, bimaleimide resin, cyanate ester resin.
Step 1）Described solvent be water, ethanol, dichloromethane, acetone, chloroform, methanol, tetrahydrofuran, carbon tetrachloride,
Hexamethylene, isopropanol, 1,2- trichloroethanes, triethylamine, toluene, pyridine, ethylenediamine, butanol, acetic acid, chlorobenzene, paraxylene, two
Toluene, N,N-dimethylformamide, cyclohexanone, cyclohexanol, DMAC N,N' dimethyl acetamide, N-METHYLFORMAMIDE, phenol, diformazan are sub-
One kind in sulfone, ethylene glycol, 1-METHYLPYRROLIDONE, formamide, sulfolane, glycerine.
Step 2）It is N in atmosphere furnace2Or argon gas；Gas flow：The mL/min of 25 mL/min~300.
Step 3）Described acid solution is one kind in hydrochloric acid, oxalic acid, sulfuric acid, and the concentration of acid solution is 0.05mol/L~6
Mol/L, mixing speed are 25~200 r/min.
Step 3）The vacuum of middle vacuum drying chamber is 1.0 × 10-1~1.0×105Pa, drying temperature are 40 ~ 100 DEG C.
Beneficial effects of the present invention are：
1）The specific surface area of porous graphene produced by the present invention is 100~1500m2/ g, 1~15 layer of the number of plies, aperture 2nm
~50nm；
2）Raw material raw material sources used in the preparation method of the present invention enrich, and price is low；Process equipment is simple, is easy to big
Large-scale production；Obtained porous graphene specific surface area is high, fault of construction is few, even aperture distribution.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of the porous graphene prepared using the technique of embodiment 1；
Fig. 2 is the scanning electron microscopic picture of the porous graphene prepared using the technique of embodiment 2；
Fig. 3 is the scanning electron microscopic picture of the porous graphene prepared using the technique of embodiment 3；
Fig. 4 is the scanning electron microscopic picture of the porous graphene prepared using the technique of embodiment 4；
Fig. 5 is the scanning electron microscopic picture of the porous graphene prepared using the technique of embodiment 5.
Specific embodiment
It is several specific embodiments of the present invention below, further illustrates the present invention, but the present invention is not limited only to this.
Embodiment 1
1）Raw material mixes：By Aqua-mesophase and aluminum acetate according to mass ratio 100:100 weigh, using deionized water
For solvent, the mass ratio of raw material and solvent is 1:10；Both are well mixed by mechanical agitation, whipping temp is 25 DEG C, is stirred
It is 0.5h to mix the time；It is to be mixed uniformly after, be evaporated under reduced pressure out solvent, be positioned over 60 DEG C of vacuum drying ovens（1.0×10-1Pa）Dry 4
Hour, it is cooled to room temperature；
2）Charing：Drying sample is positioned in atmosphere furnace, is passed through argon gas（Argon flow amount is 100mL/min）, with 10 DEG C/
Min is warming up to 1800 DEG C, is incubated 2h, is cooled to room temperature taking-up；
3）Pickling：Carbonizing production is positioned over hydrochloric acid solution（Acid solution molar concentration is 1mol/L）In, stir 4h, stirring speed
Spend for 120r/min, be washed with deionized water after being separated by filtration to neutrality；It is positioned over vacuum drying chamber（1.0×10-1Pa）Middle drying
60 DEG C of dryings 8 hours, that is, obtain porous graphene；
Prepared porous graphene performance is as follows：The number of plies is 2-10 layers, aperture size 2nm-25nm, and specific surface area is
1500m2/g。
Embodiment 2
1）Raw material mixes：By sucrose and aluminum sulfate according to mass ratio 100:50 weigh, and use acetone as solvent, raw material with it is molten
The mass ratio of agent is 1:3；Both are well mixed by mechanical agitation, whipping temp is 30 DEG C, and mixing time is 1 h；Wait to stir
After mixing uniformly, solvent is evaporated under reduced pressure out, is positioned over 35 DEG C of vacuum drying ovens（1.0×10-1Pa）Dry 2 hours, be cooled to room temperature；
2）Charing：Drying sample is positioned in atmosphere furnace, is passed through nitrogen（Nitrogen flow is 50mL/min）, with 5 DEG C/
Min is warming up to 1400 DEG C, is incubated 1h, is cooled to room temperature taking-up；
3）Pickling：Carbonizing production is positioned over sulfuric acid solution（Acid solution molar concentration is 0.5mol/L）In, stir 2h, stirring
Speed is 60r/min, is washed with deionized water after being separated by filtration to neutrality；It is positioned over vacuum drying chamber（1.0×10-1Pa）Middle drying
80 DEG C of dryings 4 hours, that is, obtain porous graphene；
Prepared porous graphene performance is as follows：The number of plies is 5-15 layers, aperture size 10nm-50nm, specific surface area
For 400m2/g。
Embodiment 3
1）Raw material mixes：By polystyrene and aluminium isopropoxide according to mass ratio 100:70 weigh, using N, N- dimethyl methyls
Acid amides is solvent, and the mass ratio of raw material and solvent is 1:5；Both are well mixed by mechanical agitation, whipping temp 120
DEG C, mixing time 1.5h.It is to be mixed uniformly after, be evaporated under reduced pressure out solvent, be positioned over 80 DEG C of vacuum drying ovens（1.0×10-1Pa）
Dry 10 hours, be cooled to room temperature；
2）Charing：Drying sample is positioned in atmosphere furnace, is passed through argon gas（Argon flow amount is 120mL/min）, with 15 DEG C/
Min is warming up to 2000 DEG C, is incubated 0.5h, is cooled to room temperature taking-up；
3）Pickling：Carbonizing production is positioned over oxalic acid solution（Acid solution molar concentration is 2mol/L）In, stir 3h, stirring speed
Spend for 80 revs/min, be washed with deionized water after being separated by filtration to neutrality；It is positioned over vacuum drying chamber（1.0×10-1Pa）Middle drying 70
DEG C dry 8 hours, that is, obtain porous graphene；
Prepared porous graphene piece performance is as follows：The number of plies is 5-10 layers, aperture size 20nm-35nm, compares surface
Product is 350m2/g。
Embodiment 4
1）Raw material mixes：By lignin and anhydrous Aluminum chloride according to mass ratio 100:80 weigh, and use toluene as solvent, former
The mass ratio of material and solvent is 1:9；Both are well mixed by mechanical agitation, whipping temp is 80 DEG C, mixing time 4h；
It is to be mixed uniformly after, be evaporated under reduced pressure out solvent, be positioned over 60 DEG C of vacuum drying ovens（1.0×10-1Pa）Dry 3 hours, be cooled to room
Temperature；
2）Charing：Drying sample is positioned in atmosphere furnace, is passed through nitrogen（Nitrogen flow is 80mL/min）, with 2 DEG C/
Min is warming up to 1100 DEG C, is incubated 5h, is cooled to room temperature taking-up；
3）Pickling：Carbonizing production is positioned over hydrochloric acid solution（Acid solution molar concentration is 0.05mol/L）In, 5h is stirred, is stirred
Speed is mixed as 40 revs/min, is washed with deionized water after being separated by filtration to neutrality；It is positioned over vacuum drying chamber（1.0×105Pa）In do
Dry 100 DEG C of dryings 2 hours, that is, obtain porous graphene；
Prepared porous graphene performance is as follows：The number of plies is 2-12 layers, aperture size 30nm-40nm, specific surface area
For 500m2/g。
Embodiment 5
1）Raw material mixes：By thermoplastic phenolic resin and aluminum nitrate according to mass ratio 100:30 weigh, using N- methyl first
Acid amides is solvent, and the mass ratio of raw material and solvent is 1:4；Both are well mixed by mechanical agitation, whipping temp 100
DEG C, mixing time 3.5h.It is to be mixed uniformly after, be evaporated under reduced pressure out solvent, be positioned over 70 DEG C of vacuum drying ovens（1.0×102Pa）
Dry 5 hours, be cooled to room temperature；
2）Charing：Drying sample is positioned in atmosphere furnace, is passed through argon gas（Argon flow amount is 200mL/min）, with 20 DEG C/
Min is warming up to 1700 DEG C, is incubated 6h, is cooled to room temperature taking-up；
3）Pickling：Carbonizing production is positioned over hydrochloric acid solution（Acid solution molar concentration is 4mol/L）In, stir 5h, stirring speed
Spend for 90 revs/min, be washed with deionized water after being separated by filtration to neutrality.It is positioned over vacuum drying chamber（1.0×10-1Pa）Middle drying 60
DEG C dry 10 hours, that is, obtain porous graphene.Prepared porous graphene performance is as follows：The number of plies is 3-9 layers, aperture size
For 5nm-25nm, specific surface area 800m2/g。
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (6)
- A kind of 1. preparation method of inexpensive porous graphene, it is characterised in that：Comprise the following steps：1）The mixing of raw material：In mass ratio 100:1~100:100 weigh carbon precursor and aluminum contained compound, solvent are added, 25 DEG C ~ 150 DEG C stirring 1 ~ 5h after, solvent evaporated, by solid residue be placed in 40 DEG C~100 DEG C baking ovens dry 1 ~ 12h；Described Aluminum contained compound is aluminium chloride, aluminum sulfate, aluminium carbonate, aluminum nitrate, aluminium hydroxide, sodium metaaluminate, aluminium nitride, aluminum phosphate, carbonization Aluminium, ten sulfate dihydrate aluminium ammonia, metasilicic acid aluminium, trifluoromethanesulfonic acid aluminium, trialkylaluminium, dialkylaluminum chloride, an alkyl al dichloride, The aluminium of trialkyl tri-chlorination two, aluminium isopropoxide, butyl aluminium, aluminium acetate, aluminium triformate, oxalic acid aluminium, propionic acid aluminium, polyaluminium chloride, alumina silicate, It is fluoric acid aluminium, aluminium secondary butylate, praseodynium aluminium, triisobutyl aluminium, 8-hydroxyquinoline aluminium, aluminum perchlorate, aluminum monostearate, two hard Resin acid aluminium, oxalic acid aluminium, ethyl aluminum dichloride, aluminium acetylacetonate, aluminium dihydrogen phosphate, aluminum oleate, aluminium bromide, silver iodide, aluminium ethylate, One kind in aluctyl, isooctyl acid aluminium;2）Low-temperature carbonization：By step 1）Dried material is put into atmosphere furnace, then with 1 DEG C/min~50 DEG C/min heating Speed keeps the h of 0.1 h~10 after being warming up to 1100 DEG C~2000 DEG C, be cooled to room temperature taking-up；It is N in described atmosphere furnace2Or Person's argon gas；Gas flow：The mL/min of 25 mL/min~300；3）Pickling：By step 2）Gained carbonizing production is placed in acid solution 1~5h of stirring, and deionized water is fully washed to neutrality, so After be put into and be dried in vacuum drying oven after, porous graphene is made.
- 2. the preparation method of inexpensive porous graphene according to claim 1, it is characterised in that：Step 1）Middle charcoal forerunner The mass values of the gross mass and solvent of body and aluminum contained compound are：1:1~1:10.
- 3. the preparation method of inexpensive porous graphene according to claim 1, it is characterised in that：Step 1）Described charcoal Presoma is pitch, sucrose, lignin and its derivative, hemicellulose, cellulose, starch, tannin, rosin, chitin, poly- second It is enol, polyethylene glycol, polyethylene, melamine and its derivative, urea, polyvinyl acetal, polyvinyl butyral resin, poly- Styrene, polyurethane, polyimides, phenolic resin, furfural resin, furfuryl alcohol resin, furane resins, epoxy resin, span carry out acyl One kind in imide resin, cyanate ester resin.
- 4. the preparation method of inexpensive porous graphene according to claim 1, it is characterised in that：Step 1）Described is molten Agent is water, ethanol, dichloromethane, acetone, chloroform, methanol, tetrahydrofuran, carbon tetrachloride, hexamethylene, isopropanol, 1,2- trichlorines Ethane, triethylamine, toluene, pyridine, ethylenediamine, butanol, acetic acid, chlorobenzene, dimethylbenzene, N,N-dimethylformamide, cyclohexanone, ring Hexanol, DMAC N,N' dimethyl acetamide, N-METHYLFORMAMIDE, phenol, dimethyl sulfoxide, ethylene glycol, 1-METHYLPYRROLIDONE, formyl One kind in amine, sulfolane, glycerine.
- 5. the preparation method of inexpensive porous graphene according to claim 1, it is characterised in that：Step 3）Described acid Liquid is hydrochloric acid, oxalic acid, one kind in sulfuric acid, and the concentration of acid solution is the mol/L of 0.05mol/L~6, and mixing speed is 25~200 r/min。
- 6. the preparation method of inexpensive porous graphene according to claim 1, it is characterised in that：Step 3）Middle vacuum is dried The vacuum of case is 1.0 × 10-1~1.0×105Pa, drying temperature are 40 ~ 100 DEG C.
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| CN102115069B (en) * | 2010-12-20 | 2012-09-05 | 中国石油大学(北京) | Graphene with porous structure and preparation method of graphene |
| CN103072982B (en) * | 2013-02-28 | 2015-02-04 | 福州大学 | Low-cost asphalt-based graphene sheet and preparation method thereof |
| CN104108709A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Porous graphene and preparation method thereof |
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