CN103771415A - High-specific surface area graphene hybridized active carbon material, and preparation method and application thereof - Google Patents
High-specific surface area graphene hybridized active carbon material, and preparation method and application thereof Download PDFInfo
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- CN103771415A CN103771415A CN201410067615.6A CN201410067615A CN103771415A CN 103771415 A CN103771415 A CN 103771415A CN 201410067615 A CN201410067615 A CN 201410067615A CN 103771415 A CN103771415 A CN 103771415A
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Abstract
The invention relates to a high-specific surface area graphene hybridized active carbon material, and a preparation method and an application thereof, and belongs to the technical field of preparation methods of the active carbon materials. The preparation method comprises the steps of mixing a mixture of graphene powder which is obtained through heat treatment or microwave irradiation and a coconut shell carbonized material with a strong base in a weight ratio of 1: (1-50), loading the mixture obtained in a reactor, increasing the temperature to 700-900 DEG C under the protection of nitrogen gas, starting activating, keeping the temperature constant for 120 minutes, reducing the temperature to the room temperature under the protection of nitrogen gas after the reaction is finished, taking out the product and recovering and washing with water, and then drying to obtain the finished product. In the meantime, the graphene can be further deoxidized through high-temperature treatment, so that high conductivity of the obtained active carbon material can be guaranteed. The high-specific surface area graphene hybridized active carbon material is safe and reliable, the security in the production process is improved, the production process is more continuous, the production efficiency is improved, the production cost is reduced and the quality of the active carbon material is stable, and therefore, the high-specific surface area graphene hybridized active carbon material has a wide application prospect.
Description
Technical field
The present invention relates to a kind of Graphene hydridization preparing high-specific surface area graphene material and its preparation method and application, belong to absorbent charcoal material preparation method technical field.
Background technology
The active carbon with high specific surface area of preparation activates amorphous carbon preparation by highly basic at present, and its conductivity is very poor, needs additional conductive agent in the time preparing ultracapacitor, affects its application in electrical condenser.The present invention activates by KOH after a certain amount of Graphene is mixed with carbonized stock.The active carbon with high specific surface area of preparing by controlling the electroconductibility of addition control gac of Graphene.Graphene provides high conduction performance and high-specific surface area simultaneously, compares with Activated Graphite alkene, and cost reduces greatly.Expection has fabulous application prospect on ultracapacitor.
Summary of the invention
The continuous preparation method that the object of this invention is to provide a kind of Graphene doping active carbon with high specific surface area, adopts dry mixed raw material and continuously carbonizing reactor to produce active carbon with high specific surface area.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of active carbon with high specific surface area, the specific surface area of described gac is 2000～3000m
2/ g.
A preparation method for gac as described in the present invention, it comprises the steps:
After graphene powder and carbonized stock are mixed and highly basic solid according to 1: after the mass ratio of (1～50) is dry mixed, in the inert atmosphere of 500～1500 ℃, carry out priming reaction, obtain active carbon with high specific surface area.
As a kind of preferred version, the addition of described graphene powder is 1～50% of carbonized stock quality.
As a kind of preferred version, described Graphene is prepared through stripping method with graphene oxide.
As a kind of preferred version, described highly basic is at least two kinds in potassium hydroxide, sodium hydroxide, calcium hydroxide.
As a kind of preferred version, described inert atmosphere is realized by passing into nitrogen or argon gas.
As a kind of preferred version, the temperature of described priming reaction is 700～1200 ℃.
As a kind of preferred version, described stripping method is selected from that microwave is peeled off, thermal reduction is peeled off and the one of ball milled in peeling off.
As a kind of preferred version, described highly basic is selected from least one in potassium hydroxide, sodium hydroxide.
A kind of as the present invention states activated carbon application in hydrogen storage material, lithium ion battery, ultracapacitor or fuel cell, and the manufacture of nanometer electronic device, high frequency circuit, photon sensor, the order-checking of gene electronics and minimizing noise device.
The present invention has following beneficial effect compared with existing technique:
1, safe and reliable: to adopt dry mixed raw material, avoided the process for preparation etching apparatus of KOH solution, improved the security in production process.
2, produce continuously: whole reaction process is all carried out under solid state shape, the problem of having avoided whole process to bring in the transformation of liquid, solid two-phase, makes to produce more continuous.
3, increase rate production efficiency, has reduced production cost; Adopt full-automatic charing reactor, from being fed to discharging unattended operation, increase rate production efficiency, has reduced production cost.
4, the activated carbon product steady quality that adopts the present invention to prepare, specific surface area reaches 2000～3000m
2/ g, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
Graphite oxide microwave is peeled off and obtained Graphene, take 30g Graphene; After 100:1 mixes by weight with Graphene by coconut carbon material, join fast-crushing in pulverizer with KOH solid by the mass ratio of 1: 4 and mix; Then the raw material after mixing is packed in nickel reactant device, after closed reactor, pass into nitrogen, the air in metathesis reactor heats up under nitrogen protection, 10～12 ℃/min of heat-up rate, and to 450 ℃, constant temperature dehydration in 2 hours; Continue, with 10～12 ℃/min of heat-up rate, to be warmed up to 850 ℃ again, start activation, constant temperature 120min, arrives room temperature at nitrogen protection borehole cooling after reaction finishes, and takes out product washing, dries and makes product, and its BET surface-area is 2540m
2/ g.
Embodiment 2
Utilize the activation of KOH activator to prepare the method for active carbon with high specific surface area material, comprise following preparation process:
Graphite oxide microwave is peeled off and obtained Graphene, take 40g Graphene; After coconut carbon material is mixed in mass ratio with Graphene at 2: 1, join fast-crushing in pulverizer with KOH solid by the weight ratio of 1: 1 and mix; Then the raw material after mixing is packed in nickel reactant device, after closed reactor, pass into nitrogen, the air in metathesis reactor heats up under nitrogen protection, 10～12 ℃/min of heat-up rate, and to 450 ℃, constant temperature dehydration in 2 hours; Continue, with 10～12 ℃/min of heat-up rate, to be warmed up to 800 ℃ again, start activation, constant temperature 120min, arrives room temperature at nitrogen protection borehole cooling after reaction finishes, and takes out product washing, dries and makes product, and its BET surface-area is 2540m
2/ g.。
Embodiment 3
Utilize the activation of KOH activator to prepare the method for active carbon with high specific surface area material, comprise following preparation process:
Graphite oxide microwave is peeled off and obtained Graphene, take 40g Graphene; After coconut carbon material is mixed in mass ratio with Graphene at 4: 1, join fast-crushing in pulverizer with KOH solid by the mass ratio of 1: 50 and mix; Then the raw material after mixing is packed in nickel reactant device, after closed reactor, pass into nitrogen, the air in metathesis reactor heats up under nitrogen protection, 10～12 ℃/min of heat-up rate, and to 450 ℃, constant temperature dehydration in 2 hours; Continue, with 10～12 ℃/min of heat-up rate, to be warmed up to 800 ℃ again, start activation, constant temperature 120min, arrives room temperature at nitrogen protection borehole cooling after reaction finishes, and takes out product washing, dries and makes product, and its BET surface-area is 2540m
2/ g.
Embodiment 4
Utilize KOH, the activation of NaOH hybrid activator to prepare the method for active carbon with high specific surface area material, comprise following preparation process:
Graphite oxide thermal reduction is peeled off and obtained Graphene, take 20g Graphene; KOH and NaOH are mixed into mixed base for 5: 1 in molar ratio, after coconut carbon material is mixed in mass ratio with Graphene at 10: 3, join fast-crushing in pulverizer with mixed base by the mass ratio of 1: 25 and mix; Then the raw material after mixing is packed in nickel reactant device, after closed reactor, pass into nitrogen, the air in metathesis reactor heats up under nitrogen protection, 10～12 ℃/min of heat-up rate, and to 450 ℃, constant temperature dehydration in 2 hours; Continue, with 10～12 ℃/min of heat-up rate, to be warmed up to 800 ℃ again, start activation, constant temperature 120min, arrives room temperature at nitrogen protection borehole cooling after reaction finishes, and takes out product washing, dries and makes product, and its BET surface-area is 2390m
2/ g.
The active carbon with high specific surface area material that the embodiment of the present invention 1～4 prepares, specific surface area is 2000～3000m
2/ g, compared with prior art, safe and reliable, produce continuously, increase rate production efficiency, reduced production cost; Adopt full-automatic charing reactor, from being fed to discharging unattended operation, increase rate production efficiency, has reduced production cost.The active carbon with high specific surface area material that the embodiment of the present invention 1～4 prepares, in guaranteeing high-specific surface area, has kept the height electricity of grapheme material to lead.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (10)
1. a Graphene doping active carbon with high specific surface area, is characterized in that, the specific surface area of described gac is 2000～3000m
2/ g.
2. a preparation method for Graphene doping active carbon with high specific surface area as claimed in claim 1, is characterized in that, comprises the steps:
After graphene powder and carbonized stock are mixed with highly basic solid according to 1: after the mass ratio of (1～50) is dry mixed, in the inert atmosphere of 500～1500 ℃, carry out priming reaction, obtain the Graphene active carbon with high specific surface area that adulterates.
3. preparation method as claimed in claim 2, is characterized in that, the addition of described graphene powder is 1～50% of carbonized stock quality.
4. preparation method as claimed in claim 2, is characterized in that, described Graphene is prepared through stripping method with graphene oxide.
5. preparation method as claimed in claim 2, is characterized in that, described highly basic is at least two kinds in potassium hydroxide, sodium hydroxide, calcium hydroxide.
6. preparation method as claimed in claim 2, is characterized in that, described inert atmosphere is realized by passing into nitrogen or argon gas.
7. preparation method as claimed in claim 2, is characterized in that, the temperature of described priming reaction is 700～1200 ℃.
8. preparation method as claimed in claim 4, is characterized in that, described stripping method is selected from that microwave is peeled off, thermal reduction is peeled off and the one of ball milled in peeling off.
9. preparation method as claimed in claim 5, is characterized in that, described highly basic is selected from least one in potassium hydroxide, sodium hydroxide.
As claimed in claim 1 activated carbon application in hydrogen storage material, lithium ion battery, ultracapacitor or a fuel cell, and nanometer electronic device, high frequency circuit, photon sensor, the order-checking of gene electronics and reduce the manufacture of noise device.
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Cited By (10)
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|---|---|---|---|---|
| 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 |
| CN105261488A (en) * | 2015-11-05 | 2016-01-20 | 宁波南车新能源科技有限公司 | Core composite carbon electrode material for double-electric-layer capacitor |
| CN105374572A (en) * | 2015-12-16 | 2016-03-02 | 天津工业大学 | Low cost high specific energy long-acting capacitor electrode material and preparation method for the same |
| CN105575674A (en) * | 2014-10-13 | 2016-05-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene/active carbon composite material, preparation method thereof, and supercapacitor |
| WO2016080910A1 (en) * | 2014-11-17 | 2016-05-26 | Nanyang Technological University | A composite material and method of preparation thereof |
| CN106587049A (en) * | 2016-12-06 | 2017-04-26 | 南京九致信息科技有限公司 | Method for preparing active carbon with apricot pit as carbon source through microwave heating |
| CN107500292A (en) * | 2017-09-25 | 2017-12-22 | 江苏苏利精细化工股份有限公司 | A kind of method that graphene oxide is modified cocoanut active charcoal |
| CN108807014A (en) * | 2018-06-14 | 2018-11-13 | 西南科技大学 | The method for preparing electrode material for super capacitor using discarded cigarette butt |
| CN109354018A (en) * | 2018-12-04 | 2019-02-19 | 中国人民解放军军事科学院防化研究院 | A kind of preparation method of High surface area carbon microbeads |
| CN110970603A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Multifunctional activated carbon composite material for negative electrode of lead-carbon battery, preparation method of multifunctional activated carbon composite material and lead-carbon battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN105575674A (en) * | 2014-10-13 | 2016-05-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene/active carbon composite material, preparation method thereof, and supercapacitor |
| CN105575674B (en) * | 2014-10-13 | 2018-04-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene/absorbent charcoal composite material and preparation method, ultracapacitor |
| WO2016080910A1 (en) * | 2014-11-17 | 2016-05-26 | Nanyang Technological University | A composite material and method of preparation thereof |
| CN105261488B (en) * | 2015-11-05 | 2016-08-24 | 宁波中车新能源科技有限公司 | A kind of sandwich composite carbon electrode material being applied to double layer capacitor |
| CN105261488A (en) * | 2015-11-05 | 2016-01-20 | 宁波南车新能源科技有限公司 | Core composite carbon electrode material for double-electric-layer capacitor |
| CN105374572A (en) * | 2015-12-16 | 2016-03-02 | 天津工业大学 | Low cost high specific energy long-acting capacitor electrode material and preparation method for the same |
| CN106587049A (en) * | 2016-12-06 | 2017-04-26 | 南京九致信息科技有限公司 | Method for preparing active carbon with apricot pit as carbon source through microwave heating |
| CN107500292A (en) * | 2017-09-25 | 2017-12-22 | 江苏苏利精细化工股份有限公司 | A kind of method that graphene oxide is modified cocoanut active charcoal |
| CN108807014A (en) * | 2018-06-14 | 2018-11-13 | 西南科技大学 | The method for preparing electrode material for super capacitor using discarded cigarette butt |
| CN108807014B (en) * | 2018-06-14 | 2020-03-24 | 西南科技大学 | Method for preparing supercapacitor electrode material by using waste cigarette ends |
| CN110970603A (en) * | 2018-09-30 | 2020-04-07 | 山东欧铂新材料有限公司 | Multifunctional activated carbon composite material for negative electrode of lead-carbon battery, preparation method of multifunctional activated carbon composite material and lead-carbon battery |
| CN109354018A (en) * | 2018-12-04 | 2019-02-19 | 中国人民解放军军事科学院防化研究院 | A kind of preparation method of High surface area carbon microbeads |
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