CN103395776A - Asphalt-based activated graphene sheet and preparation method thereof - Google Patents
Asphalt-based activated graphene sheet and preparation method thereof Download PDFInfo
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- CN103395776A CN103395776A CN2013103323965A CN201310332396A CN103395776A CN 103395776 A CN103395776 A CN 103395776A CN 2013103323965 A CN2013103323965 A CN 2013103323965A CN 201310332396 A CN201310332396 A CN 201310332396A CN 103395776 A CN103395776 A CN 103395776A
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Abstract
The invention belongs to the field of carbon materials, and mainly relates to an asphalt-based activated graphene sheet and a preparation method thereof. The asphalt-based activated graphene sheet is prepared by processes of mixing, carbonizing, reaction milling, activating and pickling with the asphalt and an additive (aluminium powder or aluminium oxide) as raw materials. The preparation method is rich in raw material sources, low in preparation cost and simple in operations and can be industrialized easily. The asphalt-based activated graphene sheet has large specific surface area and high mesopore content.
Description
Technical field
The invention belongs to the carbon materials field, be specifically related to a kind of asphaltic base activation graphene film and preparation method thereof.
Background technology
Graphene film is to be formed by the single-layer graphene stacking, and thickness is the two-dimentional Nano graphite material of nanoscale.Graphene film has individual layer, minority layer and multilayer, and its extreme case is single-layer graphene.The thickness limit of two dimension graphene film should look the electronic structure sudden change and materialization effect suddenlys change and jointly determines, it is generally acknowledged that thickness is no more than 20nm.Due to the difference of dimension, the performance of two-dimentional Graphene is different from carbon nanotube to a great extent, has the character of many uniquenesses.Because graphene film has nontoxic, chemistry and thermal property is excellent, electric conductivity is large, physical strength is large characteristic, make the material take graphene film as basis that industrial applicability widely be arranged, as can be used as sorbent material, drug conveying, support of the catalyst, hot transmission medium, and can be made into the electronic component with fine structure.Especially, along with updating of graphene film performance, graphene film becomes the leading of energy field gradually, at aspects such as storing hydrogen, fuel cell, solar cell, lithium ion battery, ultracapacitors, is widely used.
Therefore compare with graphene film, the activation graphene film has than bigger serface and higher mesopore content, is more suitable for as the stored energy active material, especially as the electrode materials of ultracapacitor.The preparation method that the graphene film of preparation activation at present adopts has physical activation method, chemical activation method and the chemical combined activation method of thing reason –, but all take the graphene film of costliness as raw material, therefore the cost of preparation activation Graphene is high, and prospects for commercial application is dim.
Summary of the invention
The object of the present invention is to provide a kind of asphaltic base activation graphene film and preparation method thereof, raw material sources are abundant, preparation cost is low, simple to operate, easily realize industrialization; The product specific surface area is large, and mesopore content is high.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of asphaltic base activation graphene film comprises mixing, charing, reaction ball milling, activation, the acid cleaning process of raw material.
(1) mixing of raw material
Basic raw material: the mixture of one or several in coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts;
Additive: aluminium powder or aluminum oxide;
Basic raw material and additive are to sieve after 100:20～100:100 fully mixes in mass ratio;
The hybrid technique parameter is:
Raw material granularity: 100-300 order;
Additive purity: greater than 99%;
(2) charing
The raw material that step (1) mixes is put into sintering oven, be incubated after then being warming up to preset temperature, be cooled to room temperature and take out;
The charring process parameter is:
Temperature rise rate: 30 ℃/min of 5 ℃/min –;
Preset temperature: 1,300 1800 ℃ of ℃ –;
Soaking time: 0.1 h – 5 h;
Vacuum tightness: 1.0 * 10
-1Pa – 1.0 * 10
4Pa;
(3) reaction ball milling
Step (2) gained carbonizing production and KOH are carried out reaction ball milling with the rotating speed of 600 rev/mins of 100 – and process 1 – 10h for 1:1～1:4 puts into ball mill in mass ratio;
(4) activation
Step (3) gained ball milling product is put into corundum crucible, be incubated after then being warming up to preset temperature in atmosphere furnace, cool to room temperature with the furnace and take out;
The activating process parameter is:
Temperature rise rate: 10 ℃/min of 2 ℃/min –;
Preset temperature: 700 900 ℃ of ℃ –;
Soaking time: 0.5 h – 5h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50 mL/min – 200 mL/min;
(5) pickling
Step (4) gained activation products are placed in dilute hydrochloric acid stir, it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then puts into 120 ℃ of baking ovens and carries out dry 10 h;
The acid cleaning process parameter is:
Dilute hydrochloric acid pH value: 4 – 6;
The temperature of dilute hydrochloric acid: 25 80 ℃ of ℃ –;
The mass ratio of activation products and dilute hydrochloric acid: 1:2～1:5;
Churning time: 1 h – 5h;
Stirring velocity: 50 500 rev/mins of –.
The specific surface area of the asphaltic base activation graphene film that makes is 1500 ~ 3000m
2/ g, mesopore content are 30 ~ 60%.
Compared with prior art, the advantage and the effect that have of the present invention is:
(1) abundant raw material, cheap.
(2) processing unit is simple, is easy to scale operation.
(3) specific surface area is high, and mesopore content is high.
Embodiment
Embodiment 1
With coal-tar pitch and aluminium powder 100:20(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 100 mesh sieves
3Pa), be incubated 2h after being warming up to 1800 ℃ with 30 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 100 rev/mins of ball mill reaction ball milling 1h(rotational speed of ball-mill after 1:1 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into N
2, N
2Flow is 50mL/min, keeps 2h after being warming up to 800 ℃ with 5 ℃/min, cools to room temperature with the furnace and takes out.It is 4 hydrochloric acid (the mass ratio 1:2 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 500 rev/mins of 1h(stirring velocitys in 25 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 6～10nm, specific surface area 1500m
2/ g, mesopore content 42%.
Embodiment 2
With coal-tar pitch and aluminum oxide powder 100:50(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 150 mesh sieves
4Pa), be incubated 2h after being warming up to 1600 ℃ with 5 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 600 rev/mins of ball mill reaction ball milling 5h(rotational speed of ball-mill after 1:3 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into Ar, the Ar flow is 200mL/min, keeps 0.5h after being warming up to 900 ℃ with 2 ℃/min, cools to room temperature with the furnace and takes out.It is 6 hydrochloric acid (the mass ratio 1:3 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 200 rev/mins of 3h(stirring velocitys in 80 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 3～5nm, specific surface area 2208m
2/ g, mesopore content 30%.
Embodiment 3
With petroleum pitch and aluminium powder 100:100(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 300 mesh sieves
-1Pa), be incubated 5h after being warming up to 1300 ℃ with 10 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 300 rev/mins of ball mill reaction ball milling 2.5h(rotational speed of ball-mill after 1:3 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into Ar, the Ar flow is 150mL/min, keeps 5h after being warming up to 800 ℃ with 10 ℃/min, cools to room temperature with the furnace and takes out.It is 4 hydrochloric acid (the mass ratio 1:5 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 200 rev/mins of 2h(stirring velocitys in 60 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 1～3nm, specific surface area 2530m
2/ g, mesopore content 60%.
Embodiment 4
With slag oil asphalt and aluminium powder 100:50(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 150 mesh sieves
2Pa), be incubated 3h after being warming up to 1600 ℃ with 15 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 500 rev/mins of ball mill reaction ball milling 10h(rotational speed of ball-mill after 1:4 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into N
2, N
2Flow is 50mL/min, keeps 2.5h after being warming up to 700 ℃ with 10 ℃/min, cools to room temperature with the furnace and takes out.It is 5 hydrochloric acid (the mass ratio 1:4 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 250 rev/mins of 2h(stirring velocitys in 50 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 1～3nm, specific surface area 2980m
2/ g, mesopore content 45%.
Embodiment 5
With synthetic asphalts and aluminum oxide powder 100:40(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 200 mesh sieves
3Pa), be incubated 2h after being warming up to 1800 ℃ with 8 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 300 rev/mins of ball mill reaction ball milling 6h(rotational speed of ball-mill after 1:4 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into N
2, N
2Flow is 200mL/min, keeps 1.5h after being warming up to 850 ℃ with 5 ℃/min, cools to room temperature with the furnace and takes out.It is 4 hydrochloric acid (the mass ratio 1:3 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 200 rev/mins of 2h(stirring velocitys in 60 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 2～5nm, specific surface area 2060m
2/ g, mesopore content 35%.
Embodiment 6
With coal-tar pitch and aluminium powder 100:100(mass ratio in mass ratio) take, put into sintering oven (vacuum tightness 1.0 * 10 after fully mixing 300 mesh sieves
1Pa), be incubated 5h after being warming up to 1700 ℃ with 5 ℃/min, be cooled to room temperature and take out carbonizing production.Put into 600 rev/mins of ball mill reaction ball milling 10h(rotational speed of ball-mill after 1:3 mixes in mass ratio with KOH with carbonizing production).The ball milling product is put into corundum crucible, then be placed in atmosphere furnace, and pass into N
2, N
2Flow is 100mL/min, keeps 1h after being warming up to 800 ℃ with 2 ℃/min, cools to room temperature with the furnace and takes out.It is 4 hydrochloric acid (the mass ratio 1:4 of activation products and hydrochloric acid) that activation products are placed in the pH value, stir 50 rev/mins of 2h(stirring velocitys in 25 ℃), it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then be placed in 120 ℃ of baking ovens and carry out dry 10 h, namely obtain the activation graphene film.Prepared activation graphene film has following performance: graphene film thickness 2～3nm, specific surface area 2550m
2/ g, mesopore content 52%.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing 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 (3)
1. the preparation method of an asphaltic base activation graphene film, is characterized in that: the mixing, charing, reaction ball milling, activation, the acid cleaning process that comprise raw material.
2. asphaltic base according to claim 1 activates the preparation method of graphene film, it is characterized in that: comprise the following steps:
(1) mixing of raw material
Basic raw material: the mixture of one or several in coal-tar pitch, petroleum pitch, slag oil asphalt, synthetic asphalts;
Additive: aluminium powder or aluminum oxide;
Basic raw material and additive are to sieve after 100:20～100:100 fully mixes in mass ratio;
The hybrid technique parameter is:
Raw material granularity: 100-300 order;
Additive purity: greater than 99%;
(2) charing
The raw material that step (1) mixes is put into sintering oven, be incubated after then being warming up to preset temperature, be cooled to room temperature and take out;
The charring process parameter is:
Temperature rise rate: 30 ℃/min of 5 ℃/min –;
Preset temperature: 1,300 1800 ℃ of ℃ –;
Soaking time: 0.1 h – 5 h;
Vacuum tightness: 1.0 * 10
-1Pa – 1.0 * 10
4Pa;
(3) reaction ball milling
Step (2) gained carbonizing production and KOH are carried out reaction ball milling with the rotating speed of 600 rev/mins of 100 – and process 1 – 10h for 1:1～1:4 puts into ball mill in mass ratio;
(4) activation
Step (3) gained ball milling product is put into corundum crucible, be incubated after then being warming up to preset temperature in atmosphere furnace, cool to room temperature with the furnace and take out;
The activating process parameter is:
Temperature rise rate: 10 ℃/min of 2 ℃/min –;
Preset temperature: 700 900 ℃ of ℃ –;
Soaking time: 0.5 h – 5h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50 mL/min – 200 mL/min;
(5) pickling
Step (4) gained activation products are placed in dilute hydrochloric acid stir, it is neutral being separated by filtration rear with deionized water, fully the washing to filtrate pH value, then puts into 120 ℃ of baking ovens and carries out dry 10 h;
The acid cleaning process parameter is:
Dilute hydrochloric acid pH value: 4 – 6;
The temperature of dilute hydrochloric acid: 25 80 ℃ of ℃ –;
The mass ratio of activation products and dilute hydrochloric acid: 1:2～1:5;
Churning time: 1 h – 5h;
Stirring velocity: 50 500 rev/mins of –.
3. the asphaltic base activation graphene film that makes of the method for claim 1, it is characterized in that: the specific surface area of the asphaltic base activation graphene film that makes is 1500 ~ 3000m
2/ g, mesopore content are 30 ~ 60%.
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| CN103641111A (en) * | 2013-12-26 | 2014-03-19 | 安徽工业大学 | Preparation method of graded porous graphene material for super-capacitor |
| CN105480971A (en) * | 2016-01-29 | 2016-04-13 | 福州大学 | Preparation method of asphalt-based three-dimensional mesoporous graphene material |
| CN105502363A (en) * | 2015-12-25 | 2016-04-20 | 安徽工业大学 | Method for preparing corrugated graphene nanosheets for supercapacitor |
| CN105752970A (en) * | 2016-03-30 | 2016-07-13 | 福州大学 | Method for preparing carbon nanotube/graphene compound |
| CN107108219A (en) * | 2014-08-08 | 2017-08-29 | 奥兰雷瓦朱·W·塔尼莫拉 | From asphaltene, Graphene derivative, the method for 2D materials synthesis paraffin derivatives and application |
| 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 |
| CN108976618A (en) * | 2018-08-08 | 2018-12-11 | 南通迅达橡塑制造有限公司 | A kind of graphene modified EPT rubber composite material and preparation method thereof |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107108219A (en) * | 2014-08-08 | 2017-08-29 | 奥兰雷瓦朱·W·塔尼莫拉 | From asphaltene, Graphene derivative, the method for 2D materials synthesis paraffin derivatives and application |
| CN105502363A (en) * | 2015-12-25 | 2016-04-20 | 安徽工业大学 | Method for preparing corrugated graphene nanosheets for supercapacitor |
| CN105502363B (en) * | 2015-12-25 | 2018-02-09 | 安徽工业大学 | A kind of preparation method of the graphene nanometer sheet of ultracapacitor fold |
| CN105480971A (en) * | 2016-01-29 | 2016-04-13 | 福州大学 | Preparation method of asphalt-based three-dimensional mesoporous graphene material |
| CN105752970A (en) * | 2016-03-30 | 2016-07-13 | 福州大学 | Method for preparing carbon nanotube/graphene compound |
| 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 |
| CN108976618A (en) * | 2018-08-08 | 2018-12-11 | 南通迅达橡塑制造有限公司 | A kind of graphene modified EPT rubber composite material and preparation method thereof |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
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