CN103771415B - A kind of Graphene hydridization active carbon with high specific surface area material and its preparation method and application - Google Patents
A kind of Graphene hydridization active carbon with high specific surface area material and its preparation method and application Download PDFInfo
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- CN103771415B CN103771415B CN201410067615.6A CN201410067615A CN103771415B CN 103771415 B CN103771415 B CN 103771415B CN 201410067615 A CN201410067615 A CN 201410067615A CN 103771415 B CN103771415 B CN 103771415B
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Abstract
The present invention relates to a kind of Graphene doping active carbon with high specific surface area material and its preparation method and application, belong to absorbent charcoal material preparation method technical field.The present invention utilizes after the graphene powder that obtains heat treatment or microwave exposure and the mixing of coconut carbon material with highly basic by weight 1: (1～50) mix; load in reactor; it is warming up to 700～900 DEG C under nitrogen protection; start activation; constant temperature 120 minutes; reaction cools to room temperature under nitrogen protection after terminating, take out product and reclaim and wash, and carries out drying manufactured goods.Simultaneously, high-temperature process further to Graphene deoxidation, thus can ensure the high conductivity of obtained absorbent charcoal material.Product safety of the present invention is reliable, improves the safety production process in production process more continuous, improves production efficiency, reduce production cost, constant product quality, be with a wide range of applications.
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 activated carbon
Material preparation method technical field.
Background technology
The active carbon with high specific surface area of preparation is prepared by highly basic activation amorphous carbon at present, and its electric conductivity is very poor, super in preparation
Need additional conductive agent during level capacitor, affect its application in the capacitor.The present invention is by a certain amount of Graphene and carbonized stock
After mixing, activated by KOH.The height ratio that the electric conductivity of activated carbon is prepared is controlled by controlling the addition of Graphene
Surface activity carbon.Graphene provides high conduction performance and high-specific surface area simultaneously, and compared with Activated Graphite alkene, cost is significantly
Reduction.It is contemplated that have fabulous application prospect on ultracapacitor.
Summary of the invention
It is an object of the invention to provide the continuous preparation method of a kind of Graphene doping active carbon with high specific surface area, use dry method
Mixing raw material and continuously carbonizing reactor 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 activated carbon is 2000～3000m2/g。
The preparation method of a kind of activated carbon as described in the present invention, it comprises the steps:
With strong basic solid according to 1 after graphene powder and carbonized stock are mixed: after the mass ratio of (1～50) is dry mixed,
The inert atmosphere of 500～1500 DEG C carries out priming reaction, obtains active carbon with high specific surface area.
As a kind of preferred version, the addition of described graphene powder is the 1～50% of carbonized stock quality.
As a kind of preferred version, prepared by the described stripped method of Graphene graphene oxide.
As a kind of preferred version, described highly basic is at least two in potassium hydroxide, sodium hydroxide, calcium hydroxide.
As a kind of preferred version, described inert atmosphere realizes by being passed through nitrogen or argon.
As a kind of preferred version, the temperature of described priming reaction is 700～1200 DEG C.
As a kind of preferred version, described stripping method one in microwave stripping, thermal reduction stripping and ball-milling method are peeled off.
As a kind of preferred version, at least one in potassium hydroxide, sodium hydroxide of described highly basic.
A kind of such as present invention states activated carbon application in hydrogen storage material, lithium ion battery, ultracapacitor or fuel cell, with
And nanometer electronic device, high-frequency circuit, photon sensor, gene electronics check order and reduce the manufacture of noise device.
The present invention has following beneficial effect compared with existing technique:
1, safe and reliable: to use dry mixed raw material, it is to avoid the process for preparation etching apparatus of KOH solution, improve life
Safety during product.
2, produce continuously: whole course of reaction is all carried out under solid state shape, it is to avoid whole process is in liquid, the most biphase solid turning
The problem that variable speed is come, makes production more continuous.
3, increase rate production efficiency, reduces production cost；Use full-automatic carbonization reactor, full-automatic from being fed to discharging
Operation, increase rate production efficiency, reduce production cost.
4, using activated carbon product steady quality prepared by the present invention, specific surface area reaches 2000～3000m2/ g, has extensively
Application prospect.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.
Embodiment 1
Graphite oxide microwave is peeled off and obtains Graphene, weigh 30g Graphene；By coconut carbon material and Graphene by weight 100:
After 1 mixing, join fast-crushing in pulverizer with KOH solid by the mass ratio of 1: 4 and mix homogeneously；Then will mixing
Raw material after Jun Yun loads in nickel reactant device, after closed reactor, is passed through nitrogen, and the air in metathesis reactor, at nitrogen
Protection is lower to heat up, programming rate 10～12 DEG C/min, to 450 DEG C, and constant temperature dehydration in 2 hours；It is further continued for programming rate 10～12 DEG C
/ min, is warmed up to 850 DEG C, starts activation, constant temperature 120min, and reaction cools to room temperature under nitrogen protection after terminating, takes
Going out product and carry out washing washing, carry out drying and make product, its BET surface area is 2540m2/g。
Embodiment 2
Utilize the method that active carbon with high specific surface area material is prepared in KOH activator activation, including following preparation process:
Graphite oxide microwave is peeled off and obtains Graphene, weigh 40g Graphene；By coconut carbon material with Graphene in mass ratio
After 2: 1 mixing, join fast-crushing in pulverizer with KOH solid by the weight ratio of 1: 1 and mix homogeneously；Then will be mixed
Raw material after closing uniformly loads in nickel reactant device, after closed reactor, is passed through nitrogen, and the air in metathesis reactor, at nitrogen
Heat up under gas shielded, programming rate 10～12 DEG C/min, to 450 DEG C, constant temperature dehydration in 2 hours；It is further continued for programming rate
10～12 DEG C/min, being warmed up to 800 DEG C, start activation, constant temperature 120min, reaction cools to room after terminating under nitrogen protection
Temperature, takes out product and carries out washing washing, carry out drying and make product, and its BET surface area is 2540m2/g。。
Embodiment 3
Utilize the method that active carbon with high specific surface area material is prepared in KOH activator activation, including following preparation process:
Graphite oxide microwave is peeled off and obtains Graphene, weigh 40g Graphene；By coconut carbon material with Graphene in mass ratio
After 4: 1 mixing, join fast-crushing in pulverizer with KOH solid by the mass ratio of 1: 50 and mix homogeneously；Then will
Raw material after mix homogeneously loads in nickel reactant device, after closed reactor, is passed through nitrogen, the air in metathesis reactor,
Nitrogen protection is lower to heat up, programming rate 10～12 DEG C/min, to 450 DEG C, and constant temperature dehydration in 2 hours；It is further continued for programming rate
10～12 DEG C/min, being warmed up to 800 DEG C, start activation, constant temperature 120min, reaction cools to room after terminating under nitrogen protection
Temperature, takes out product and carries out washing washing, carry out drying and make product, and its BET surface area is 2540m2/g。
Embodiment 4
Utilize the method that active carbon with high specific surface area material is prepared in KOH, NaOH hybrid activator activation, including following preparation step
Rapid:
Graphite oxide thermal reduction is peeled off and obtains Graphene, weigh 20g Graphene；By KOH and NaOH in molar ratio 5:
1 is mixed into mixed base, after coconut carbon material being mixed with Graphene in mass ratio 10: 3, with the quality that mixed base presses 1: 25
Ratio joins fast-crushing mix homogeneously in pulverizer；Then the raw material after mix homogeneously is loaded in nickel reactant device, close anti-
After answering device, it is passed through nitrogen, the air in metathesis reactor, heat up under nitrogen protection, programming rate 10～12 DEG C/min, arrives
450 DEG C, constant temperature dehydration in 2 hours；It is further continued for, with programming rate 10～12 DEG C/min, being warmed up to 800 DEG C, starts activation, permanent
Temperature 120min, reaction cools to room temperature under nitrogen protection after terminating, take out product and carry out washing washing, carry out drying and make
Product, its BET surface area is 2390m2/g。
The active carbon with high specific surface area material that the embodiment of the present invention 1～4 prepares, specific surface area is 2000～3000m2/ g, with
Prior art is compared, safe and reliable, produce continuously, increase rate production efficiency, reduce production cost；Use Full automatic carbon
Change reactor, from being fed to discharging full automatic working, increase rate production efficiency, reduce production cost.The embodiment of the present invention
The active carbon with high specific surface area material that 1～4 prepare, while ensureing high-specific surface area, maintains the high electricity of grapheme material
Lead.
Finally it is necessary described herein: above example is served only for saying technical scheme in further detail
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes according to the foregoing of the present invention
Some nonessential improvement and adjustment belong to protection scope of the present invention.
Claims (5)
1. the preparation method of a Graphene doping active carbon with high specific surface area, it is characterised in that comprise the steps:
With strong basic solid according to 1 after graphene powder and carbonized stock are mixed: after the mass ratio of (1～50) is dry mixed, then
Raw material after mix homogeneously is loaded in nickel reactant device, after closed reactor, is passed through nitrogen, the air in metathesis reactor,
Heating up under nitrogen protection, programming rate 10～12 DEG C/min, to 450 DEG C, constant temperature dehydration in 2 hours, then at 800～850 DEG C
Inert atmosphere in carry out priming reaction, obtain Graphene doping active carbon with high specific surface area, the interpolation of described graphene powder
Amount is the 1～50% of carbonized stock quality, prepared by the described stripped method of Graphene graphene oxide；Described activated carbon
Specific surface area is 2000～3000m2/g。
2. preparation method as claimed in claim 1, it is characterised in that described highly basic is potassium hydroxide, sodium hydroxide, hydrogen
At least two in calcium oxide.
3. preparation method as claimed in claim 1, it is characterised in that described inert atmosphere is by being passed through nitrogen or argon
Realize.
4. preparation method as claimed in claim 1, it is characterised in that described stripping method is peeled off selected from microwave, thermal reduction stripping
From and ball-milling method peel off in one.
5. preparation method as claimed in claim 1, it is characterised in that described highly basic is in potassium hydroxide, sodium hydroxide
At least one.
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| 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 |
| 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 |
| 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 |
| CN106587049B (en) * | 2016-12-06 | 2019-06-07 | 南京九致信息科技有限公司 | The method for preparing active carbon as carbon source microwave heating using almond |
| CN107500292B (en) * | 2017-09-25 | 2019-06-25 | 江苏苏利精细化工股份有限公司 | A kind of method of the modified cocoanut active charcoal of graphene oxide |
| 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 |
| CN109354018B (en) * | 2018-12-04 | 2022-05-27 | 中国人民解放军军事科学院防化研究院 | Preparation method of activated carbon microspheres with high specific surface area |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515145A (en) * | 2011-12-27 | 2012-06-27 | 常州第六元素材料科技股份有限公司 | Preparation process for high specific surface porous carbon material |
| CN102897751A (en) * | 2012-08-28 | 2013-01-30 | 常州第六元素材料科技股份有限公司 | Method for preparing graphene with high specific surface activity |
| CN103253658A (en) * | 2013-05-13 | 2013-08-21 | 常州第六元素材料科技股份有限公司 | Graphene with high volumetric specific capacitance and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515145A (en) * | 2011-12-27 | 2012-06-27 | 常州第六元素材料科技股份有限公司 | Preparation process for high specific surface porous carbon material |
| CN102897751A (en) * | 2012-08-28 | 2013-01-30 | 常州第六元素材料科技股份有限公司 | Method for preparing graphene with high specific surface activity |
| CN103253658A (en) * | 2013-05-13 | 2013-08-21 | 常州第六元素材料科技股份有限公司 | Graphene with high volumetric specific capacitance and preparation method thereof |
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