CN102381701A - Method for numerously preparing asphalt-based graphene material with low cost - Google Patents
Method for numerously preparing asphalt-based graphene material with low cost Download PDFInfo
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- CN102381701A CN102381701A CN2011102178217A CN201110217821A CN102381701A CN 102381701 A CN102381701 A CN 102381701A CN 2011102178217 A CN2011102178217 A CN 2011102178217A CN 201110217821 A CN201110217821 A CN 201110217821A CN 102381701 A CN102381701 A CN 102381701A
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Abstract
The invention discloses a method for numerously preparing a graphene material, which takes asphalt as a raw material and comprises the processes of preparing, pyrolyzing and carrying out carbonization. Compared with the conventional preparation of the graphene material, the method disclosed by the invention has low preparation cost, little equipment investment, simplicity for operating, no pollution, and easiness for realizing industrialization; and in addition, the purity of a product is high, the structure defect of the product is little, and the performance of the product is excellent.
Description
Technical field
The invention belongs to raw material of wood-charcoal material field, relate generally to the low-cost asphaltic base grapheme material magnanimity technology of preparing of (comprising individual layer, multi-layer graphene and graphene nano microplate).
Background technology
Graphene is a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape crystalline network, is the elementary cell that makes up other dimension blacking (like zero dimension soccerballene, one dimension carbon nanotube, three-dimensional graphite).Grapheme material (comprising individual layer, multi-layer graphene and graphene nano microplate) has excellent electricity, calorifics and mechanical property, can obtain widespread use in fields such as high-performance nanometer electronic device, matrix material, field emmision material, gas sensor and energy storages.The method for preparing at present grapheme material mainly contains mechanical means and two kinds of methods of chemical process.Mechanical means comprises the method for micromechanics partition method, epitaxy method and heating SiC; Chemical process comprises chemical reduction method and chemical cleavage method.Wherein, chemical reduction method and chemical cleavage method are to prepare the most frequently used method of grapheme material at present.Chemical reduction method is that graphite oxide is mixed with water, with the clear no particulate material of ultra-sonic oscillation to solution, adds an amount of hydrazine and refluxes for some time at a certain temperature, produces the black particle shape deposition, and filtration, oven dry promptly get grapheme material.The chemistry cleavage method is the method that graphite oxide is prepared Graphene through the method for thermal reduction; The oxygen-containing functional group of graphite oxide interlayer reacts at a certain temperature; Emit gas rapidly, make that cleavage was opened when aluminum oxide/graphite layer was reduced, obtain grapheme material.Yet still there are problems such as complex process, cost height, operational hazards, environmental pollution at present in the method for preparing graphite material, and is difficult to prepare in a large number grapheme material, and this greatly hinders the promotion and application of grapheme material.
Summary of the invention
The object of the present invention is to provide a kind of low-cost magnanimity to prepare the method for asphaltic base grapheme material.This method prepares grapheme material and has advantages such as cost is low, technology simple, excellent property, pollution-free, easy industrialization.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
Process step comprises modulation, pyrolytic reaction and the charring process of asphalt stock, and is specific as follows:
(1) modulation of asphalt stock
Raw material comprises one or several mixtures of coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts, mesophase pitch.Put into polymeric kettle after above-mentioned raw materials fully ground, be warming up to the technology that adopts hot melt to stir behind the preset temperature and mix, processing parameter is:
Temperature rise rate: 20 ℃/min of 2 ℃/min –
Preset temperature: 400 ℃ of 200 ℃ –
Churning time: 1h – 5h
Stirring velocity: 50 rpm-1000 rpm
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min
(2) pyrolytic reaction
The raw material that step (1) modulates is put into atmosphere furnace, keep for some time after being warming up to preset temperature with certain temperature rise rate then, cool to room temperature with the furnace and take out, processing parameter is:
Temperature rise rate: 100 ℃/min of 2 ℃/min –
Preset temperature: 1000 ℃ of 500 ℃ –
Soaking time: 1h – 10h
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min
(3) charring process
The resulting pyrolysis product of step (2) is put into vacuum oven, keep for some time after being warming up to preset temperature with certain temperature rise rate then, cool to room temperature with the furnace and take out, processing parameter is:
Temperature rise rate: 50 ℃/min of 2 ℃/min –
Preset temperature: 2200 ℃ of 1200 ℃ –
Soaking time: 0.1 h –, 10 h
Vacuum tightness: 1.0 * 10
-1Pa – 1.0 * 10
3Pa
The present invention reaches the purpose of adjustment grapheme material structure and performance through modulation, pyrolysis and the charring process of control basic raw material.The yield that adopts the prepared grapheme material of preparation method of the present invention is greater than 80%, and the number of plies is that 1～30 layer, carbon content are higher than 98%, specific surface area 10-500m
2/ g.
Compared with prior art, advantage that the present invention had and effect are:
(1) abundant raw material, cheap.
(2) processing unit is simple, and is pollution-free, is easy to scale operation.
(3) the product structure defective is few, need not reduction and handles, and is of many uses.
(4) modulation, pyrolysis and the charring process through the control basic raw material reaches the purpose of adjusting grapheme material structure and performance.
Description of drawings
Fig. 1 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 1 prepared.
Fig. 2 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 2 prepared.
Fig. 3 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 3 prepared.
Fig. 4 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 4 prepared.
Fig. 5 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 5 prepared.
Fig. 6 is the field emission scanning electron microscope picture of the grapheme material of employing embodiment 6 prepared.
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Embodiment
Embodiment 1
Coal-tar pitch is ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 100 ℃, 100 ℃ afterwards with the speed intensification of 20 ℃/min, and begins to feed N from intensification
2, N
2Flow is 50mL/min.When temperature rose to 300 ℃, rotating speed transferred to 1000rpm and stirs 5h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50 mL/min), be incubated 10h after being warming up to 500 ℃ with 2 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 100 Pa), keep 5 h after being warming up to 2200 ℃ with 2 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 91%, the number of plies are 1～3 layer, carbon content 99.5%, specific surface area 462m
2/ g.
Embodiment 2
Mesophase pitch is ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 200 ℃, 200 ℃ afterwards with the speed intensification of 10 ℃/min, and begins to feed Ar from intensification
2, Ar
2Flow is 100mL/min.When temperature rose to 400 ℃, rotating speed transferred to 50rpm and stirs 1h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50mL/min), be incubated 5h after being warming up to 1000 ℃ with 100 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 1.0 * 10
3Pa), keep 0.1 h after being warming up to 1900 ℃ with 20 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 95%, the number of plies are 25～30 layers, carbon content 98.1%, specific surface area 12.4m
2/ g.
Embodiment 3
Coal-tar pitch and petroleum pitch are taken by weighing by 50:50 (weight ratio), be ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 100 ℃, 100 ℃ afterwards with the speed intensification of 5 ℃/min, and begins to feed N from intensification
2, N
2Flow is 200mL/min.When temperature rose to 200 ℃, rotating speed transferred to 500rpm and stirs 4h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (Ar
2Flow is 200mL/min), be incubated 10h after being warming up to 500 ℃ with 2 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 10 Pa), keep 10 h after being warming up to 2000 ℃ with 50 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 94%, the number of plies are 2～6 layers, carbon content 99%, specific surface area 220m
2/ g.
Embodiment 4
Coal-tar pitch and mesophase pitch are taken by weighing by 80:20 (weight ratio), be ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 100 ℃, 100 ℃ afterwards with the speed intensification of 20 ℃/min, and begins to feed N from intensification
2, N
2Flow is 50mL/min.When temperature rose to 300 ℃, rotating speed transferred to 200rpm and stirs 2h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 100 mL/min), be incubated 1h after being warming up to 600 ℃ with 20 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 1.0 * 10
-1Pa), keep 4 h after being warming up to 1600 ℃ with 5 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 96%, the number of plies are 10～16 layers, carbon content 99.2%, specific surface area 105m
2/ g.
Embodiment 5
Slag oil asphalt is ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 80 ℃, 80 ℃ afterwards with the speed intensification of 2 ℃/min, and begins to feed N from intensification
2, N
2Flow is 150mL/min.When temperature rose to 300 ℃, rotating speed transferred to 380rpm and stirs 1h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (Ar
2Flow is 100 mL/min), be incubated 3h after being warming up to 900 ℃ with 60 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 1Pa), keep 6h after being warming up to 1600 ℃ with 50 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 87.2%, the number of plies are 2～6 layers, carbon content 99.3%, specific surface area 480m
2/ g.
Embodiment 6
Synthetic asphalts is ground to the polymeric kettle of packing into behind 200 orders, freely heated up before 150 ℃, 150 ℃ afterwards with the speed intensification of 5 ℃/min, and begins to feed N from intensification
2, N
2Flow is 50mL/min.When temperature rose to 380 ℃, rotating speed transferred to 200rpm and stirs 1h, promptly obtained the pitch that modulates.The pitch that modulates is put into atmosphere furnace (N
2Flow is 50mL/min), be incubated 2h after being warming up to 800 ℃ with 25 ℃/min then, cool to room temperature with the furnace and take out pyrolysis product.Pyrolysis product is put into vacuum oven (vacuum tightness 1.0 * 10
2Pa), keep 5h after being warming up to 1200 ℃ with 30 ℃/min then, cool to room temperature with the furnace and take out, promptly obtain grapheme material.The prepared graphene material has following performance: yield 82%, the number of plies are 20～30 layers, carbon content 98.5%, specific surface area 10.1m
2/ g.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (6)
1. a low-cost magnanimity prepares the method for asphaltic base grapheme material, and it is characterized in that: its technical process comprises modulation, pyrolytic reaction and the charring process of asphalt stock.
2. a kind of low-cost magnanimity according to claim 1 prepares the method for asphaltic base grapheme material, it is characterized in that: described asphalt stock comprises one or several mixtures of coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts, mesophase pitch.
3. according to claim 1; 2 described a kind of low-cost magnanimities prepare the method for asphaltic base grapheme material; It is characterized in that: the modulation of described asphalt stock is that asphalt stock is fully ground through putting into polymeric kettle behind 200 mesh sieves; Be warming up to the technology that adopts hot melt to stir behind the preset temperature and mix the asphalt stock that obtains modulating, processing parameter is:
Temperature rise rate: 20 ℃/min of 2 ℃/min –
Preset temperature: 400 ℃ of 200 ℃ –
Churning time: 1h – 5h
Stirring velocity: 50 rpm-1000 rpm
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min.
4. a kind of low-cost magnanimity according to claim 1 prepares the method for asphaltic base grapheme material; It is characterized in that: described pyrolytic reaction is that the asphalt stock that modulates is put into atmosphere furnace; Keep for some time after being warming up to preset temperature with certain temperature rise rate then; Cool to the room temperature taking-up with the furnace and obtain pyrolysis product, processing parameter is:
Temperature rise rate: 100 ℃/min of 2 ℃/min –
Preset temperature: 1000 ℃ of 500 ℃ –
Soaking time: 1h – 10h
Protective atmosphere: N
2Perhaps Ar
2
Gas flow: 50 mL/min –, 200 mL/min.
5. a kind of low-cost magnanimity according to claim 1 prepares the method for asphaltic base grapheme material; It is characterized in that: described charring process is that pyrolysis product is put into vacuum oven; Keep for some time after being warming up to preset temperature with certain temperature rise rate then; Cool to the room temperature taking-up with the furnace and obtain the asphaltic base grapheme material, processing parameter is:
Temperature rise rate: 50 ℃/min of 2 ℃/min –
Preset temperature: 2200 ℃ of 1200 ℃ –
Soaking time: 0.1 h –, 10 h
Vacuum tightness: 1.0 * 10
-1Pa – 1.0 * 10
3Pa.
6. according to claim 1,5 described a kind of low-cost magnanimities prepare the method for asphaltic base grapheme material, and it is characterized in that: described asphaltic base grapheme material comprises individual layer, multi-layer graphene and graphene nano microplate.
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|---|---|---|---|
| CN2011102178217A CN102381701A (en) | 2011-08-01 | 2011-08-01 | Method for numerously preparing asphalt-based graphene material with low cost |
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| CN2011102178217A CN102381701A (en) | 2011-08-01 | 2011-08-01 | Method for numerously preparing asphalt-based graphene material with low cost |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103072982A (en) * | 2013-02-28 | 2013-05-01 | 福州大学 | Low-cost asphalt-based graphene sheet and preparation method thereof |
| CN103395776A (en) * | 2013-08-02 | 2013-11-20 | 福州大学 | Asphalt-based activated graphene sheet and preparation method thereof |
| CN103539103A (en) * | 2013-10-25 | 2014-01-29 | 福州大学 | Low-cost carbon graphene sheet and preparation method thereof |
| CN103613096A (en) * | 2013-12-06 | 2014-03-05 | 福州大学 | Low-cost method for preparing graphene macroform |
| CN103641111A (en) * | 2013-12-26 | 2014-03-19 | 安徽工业大学 | Preparation method of graded porous graphene material for super-capacitor |
| CN104319116A (en) * | 2014-09-28 | 2015-01-28 | 安徽工业大学 | Preparation method of microporous carbon/graphene composite electrode material for super capacitor |
| CN105668558A (en) * | 2016-01-28 | 2016-06-15 | 成都新柯力化工科技有限公司 | Method for preparing graphene from waste asphalt reclaimed materials |
| 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 |
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| CN107417965A (en) * | 2017-09-14 | 2017-12-01 | 南通迅达橡塑制造有限公司 | A kind of preparation method of rubber-plastics material graphene composite flame-retardant agent |
| GB2568499A (en) * | 2017-11-17 | 2019-05-22 | Graphene Star Ltd | Improvements in or relating to organic material |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103072982B (en) * | 2013-02-28 | 2015-02-04 | 福州大学 | Low-cost asphalt-based graphene sheet and preparation method thereof |
| CN103072982A (en) * | 2013-02-28 | 2013-05-01 | 福州大学 | Low-cost asphalt-based graphene sheet and preparation method thereof |
| CN103395776A (en) * | 2013-08-02 | 2013-11-20 | 福州大学 | Asphalt-based activated graphene sheet and preparation method thereof |
| CN103395776B (en) * | 2013-08-02 | 2015-07-01 | 福州大学 | Asphalt-based activated graphene sheet and preparation method thereof |
| CN103539103A (en) * | 2013-10-25 | 2014-01-29 | 福州大学 | Low-cost carbon graphene sheet and preparation method thereof |
| CN103539103B (en) * | 2013-10-25 | 2015-10-14 | 福州大学 | A kind of Low-cost carbon graphene sheet and preparation method thereof |
| CN103613096A (en) * | 2013-12-06 | 2014-03-05 | 福州大学 | Low-cost method for preparing graphene macroform |
| CN103641111A (en) * | 2013-12-26 | 2014-03-19 | 安徽工业大学 | Preparation method of graded porous graphene material for super-capacitor |
| CN103641111B (en) * | 2013-12-26 | 2015-12-30 | 安徽工业大学 | A kind of ultracapacitor preparation method of classifying porous grapheme material |
| CN104319116B (en) * | 2014-09-28 | 2017-01-25 | 安徽工业大学 | Preparation method of microporous carbon/graphene composite electrode material for super capacitor |
| CN104319116A (en) * | 2014-09-28 | 2015-01-28 | 安徽工业大学 | Preparation method of microporous carbon/graphene composite electrode material for super capacitor |
| CN105668558A (en) * | 2016-01-28 | 2016-06-15 | 成都新柯力化工科技有限公司 | Method for preparing graphene from waste asphalt reclaimed materials |
| CN106159624A (en) * | 2016-06-29 | 2016-11-23 | 佛山市盈通黑金碳材料股份有限公司 | A kind of metal-graphite brush and preparation method thereof |
| 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 |
| CN106159624B (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 metal-graphite brush and preparation method thereof |
| 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 |
| CN107417965A (en) * | 2017-09-14 | 2017-12-01 | 南通迅达橡塑制造有限公司 | A kind of preparation method of rubber-plastics material graphene composite flame-retardant agent |
| GB2568499A (en) * | 2017-11-17 | 2019-05-22 | Graphene Star Ltd | Improvements in or relating to organic material |
| GB2568499B (en) * | 2017-11-17 | 2019-12-18 | Graphene Star Ltd | A method for producing graphene |
| CN110104638A (en) * | 2019-04-29 | 2019-08-09 | 广东煤基碳材料研究有限公司 | A kind of graphene and preparation method thereof |
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Application publication date: 20120321 |