CN107445150A - A kind of preparation method of multifunctional graphite vinyl aeroge - Google Patents
A kind of preparation method of multifunctional graphite vinyl aeroge Download PDFInfo
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- CN107445150A CN107445150A CN201710569305.8A CN201710569305A CN107445150A CN 107445150 A CN107445150 A CN 107445150A CN 201710569305 A CN201710569305 A CN 201710569305A CN 107445150 A CN107445150 A CN 107445150A
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- preparation
- aeroge
- graphite vinyl
- multifunctional graphite
- multifunctional
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of preparation method of multifunctional graphite vinyl aeroge, prepares the graphene oxide colloidal solution less than 10mg/mL concentration first.The titania nanotube of certain mass is put into graphene oxide dispersion and is sufficiently stirred, recycles ultrasonic cell disruption instrument to carry out ultrasonic disperse and obtains mixed solution；Then mixed solution is put into reactor, composite aquogel is obtained by hydro-thermal self-assembling reaction.Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, multifunctional graphite vinyl aerogel material is produced after freeze-drying water removal.The preparation method is simple, workable, and energy consumption is low pollution-free, and material specific surface area is high, electrode material can be used as to be applied in ultracapacitor, is used to adsorb bisphenol-A at the same time as adsorbent, embodies the multifunctionality of material.
Description
Technical field
The present invention relates to a kind of aeroge and preparation method thereof, particularly a kind of preparation side of multifunctional graphite vinyl aeroge
Method, belong to nano material preparation and electrochemical technology field.
Background technology
In recent years, ultracapacitor is because with bigger than conventional capacitor energy density, higher than secondary cell power density
Advantage, and be that one kind has extended cycle life, cryogenic property is superior, stability is high and environmental pollution is small, so as to attract
Extensive concern.Ultracapacitor has a wide range of applications, such as portable instrument equipment, data accumulating storage system, electronic
Automobile power source and emergent back-up source etc., particularly on electric automobile, ultracapacitor is combined with battery, provides Gao Gong respectively
Rate and high-energy, both reduce power volume, extend the life-span of battery again.The key of ultracapacitor development is electrode material
The structure and performance of material, it is therefore necessary to a kind of high performance electrode material of R and D.Graphene is current studies the most
One of extensive carbon material, it is the cellular hexaplanar structure for having single layer of carbon atom arrangement form, therefore with excellent
Physical and chemical performance.Graphene aerogel, be a kind of aeroge using graphene as skeleton unit, be provided simultaneously with graphene and
The characteristic of aeroge, not only there is unique tridimensional network, also possess high conductivity, larger specific surface area, high hole
The advantages that rate and preferable thermal conductivity so that it has very big prospect in the application of ultracapacitor.
In order to further improve the capacitive property of graphene, research at present typically by graphene and transition metal oxide and
The Material claddings such as conducting polymer, prepare compound gas electrode material.Such as Ramadoss（Carbon, 2013,63 phases, the
434-445 pages）Et al. by hydrothermal method, prepared titanium dioxide granule/graphene combination electrode material, its capacitance energy
Enough reach 165F/g.Ruirui Liu （Electrochimica Acta, 2015,156 phases, the 274-282 pages）Et al. two
It is compound to have prepared titanium dioxide nano-rod/graphene as raw material for titan oxide particles and graphene oxide and CNT
Aeroge, as the electrode material of ultracapacitor, its capacitance can only reach 100F/g to the composite aerogel.However, these
It is general with the chemical property of titanium dioxide/graphene composite aerogel, its application is received a definite limitation.The present invention endeavours
In being introduced into super long titanium dioxide nanotube, finally synthesize the compound airsetting of titania nanotube/graphene of high-capacitance
Glue.The aeroge not only electrochemical performance, while be used as adsorbent Adsorption bisphenol-A, is also presented very efficient
Performance.
The content of the invention
The present invention proposes a kind of preparation method of multifunctional graphite vinyl aeroge, it is therefore intended that prepare high-specific surface area,
The multifunctional material of high-capacitance and long circulation life, as electrode of super capacitor and efficient absorption agent material.
A kind of 1. preparation method of multifunctional graphite vinyl aeroge, it is characterised in that the multifunctional graphite vinyl aeroge
Preparation method, comprise the following steps that：
（1）Compound concentration is less than 10mg/ml graphene oxide solution first；
（2）The titania nanotube of certain mass is put into graphene oxide dispersion and is sufficiently stirred, recycles ultrasonic wave
Cell crushing instrument carries out ultrasonic disperse and obtains mixed solution；
（3）Then mixed solution is put into reactor, composite aquogel is obtained by hydro-thermal self-assembling reaction；
（4）Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, multifunctional graphite vinyl is produced after freeze-drying water removal
Aerogel material.
A kind of preparation method of multifunctional graphite vinyl aeroge of the present invention also includes following preferred scheme：
In the preferable scheme of the present invention, step（1）The concentration of middle graphene oxide is 1~10mg/ml；
In the preferable scheme of the present invention, step（2）The quality of middle titania nanotube is 5~30mg；
In the preferable scheme of the present invention, step（2）Middle titania nanotube is super long titanium dioxide nanotube, and diameter exists
10-30nm, length 1-10um, specific surface area 90-110m2/g；
In the preferable scheme of the present invention, step（3）Middle hydro-thermal self-assembling reaction temperature is 90-240 DEG C, reaction time 6-
24h；
In the preferable scheme of the present invention, step（4）In the quick-frozen time be 10-60min, be put into freezing and drain system in machine
In the moisture that is frozen take away, freeze-drying time 1-2 days.
Compared with the prior art, beneficial effects of the present invention are embodied in：
（1）A kind of preparation method of multifunctional graphite vinyl aeroge provided by the invention, technique is simple, easily realizes that industrialization should
With；
（2）The accumulation of graphene sheet layer will be effectively reduced, by hydro-thermal self assembly by introducing titania nanotube
Reaction and freeze-drying, produce the graphene aerogel material of more high-specific surface area；
（3）The graphene aerogel obtained not only has excellent chemical property（High capacitance, internal resistance are small, stable circulation
Property it is good etc.）Electrode material for super capacitor can be done as stability and high efficiency, additionally it is possible to as efficient adsorbent, for adsorbing in water
Bisphenol-A.Compared with prior art, the multifunctional graphite vinyl aeroge that the present invention prepares embodies the multifunctionality of material,
Belong to environmentally friendly material.
Brief description of the drawings
Fig. 1 is the electron microscope of multifunctional graphite vinyl aeroge in the embodiment of the present invention 1；
Fig. 2 is the specific surface area curve that the embodiment of the present invention 1 provides multifunctional graphite vinyl aeroge；
Fig. 3 is that cyclic voltammetric of the multifunctional graphite vinyl aeroge of the offer of the embodiment of the present invention 2 under different scanning speed is bent
Line；
Fig. 4 is constant current charge-discharge of the multifunctional graphite vinyl aeroge of the offer of the embodiment of the present invention 2 under different current densities
Curve；
Fig. 5 is the multifunctional graphite vinyl aeroge absorption property curve that the embodiment of the present invention 3 provides.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
Prepare a kind of multifunctional graphite vinyl aeroge, including following implementation steps：（1）Compound concentration is 2mg/ml oxygen first
Graphite alkene solution；（2）5mg titania nanotube is put into graphene oxide dispersion and is sufficiently stirred, is recycled super
Sound wave cell crushing instrument carries out ultrasonic disperse and obtains mixed solution, ultrasonic power 500W, ultrasonic time 30min；（3）Then will
Mixed solution is put into reactor, obtains composite aquogel by hydro-thermal self-assembling reaction, hydrothermal temperature is 150 DEG C, instead
It is 12h between seasonable；（4）Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, cooling time 30min, freezing is done
Multifunctional graphite vinyl aerogel material is produced after being removed water after dry 24h.
Comparative example 1：
The present embodiment is one of comparative example of above-described embodiment 1.
In the present embodiment, the quality that adds titania nanotube is 10mg, specific preparation method with embodiment 1
Preparation method is essentially identical.
Comparative example 2：
The present embodiment is the two of the comparative example of above-described embodiment 1.
In the present embodiment, the quality that adds titania nanotube is 15mg, specific preparation method with embodiment 1
Preparation method is essentially identical.
Comparative example 3：
The present embodiment is the three of the comparative example of above-described embodiment 1.
In the present embodiment, the quality that adds titania nanotube is 20mg, specific preparation method with embodiment 1
Preparation method is essentially identical.
Embodiment 2
Prepare a kind of multifunctional graphite vinyl aeroge, including following implementation steps：（1）Compound concentration is 2mg/ml oxygen first
Graphite alkene solution；（2）10mg titania nanotube is put into graphene oxide dispersion and is sufficiently stirred, is recycled super
Sound wave cell crushing instrument carries out ultrasonic disperse and obtains mixed solution, ultrasonic power 500W, ultrasonic time 30min；（3）Then will
Mixed solution is put into reactor, obtains composite aquogel by hydro-thermal self-assembling reaction, hydrothermal temperature is 150 DEG C, instead
It is 6h between seasonable；（4）Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, cooling time 30min, freeze-drying
Multifunctional graphite vinyl aerogel material is produced after being removed water after 24h.
Comparative example 1：
The present embodiment is one of comparative example of above-described embodiment 2.
In the present embodiment, the hydro-thermal reaction time is used as 12h, specific preparation method and the preparation method in embodiment 2
It is essentially identical.
Comparative example 2：
The present embodiment is the two of the comparative example of above-described embodiment 2.
In the present embodiment, the hydro-thermal reaction time is used as 18h, specific preparation method and the preparation method in embodiment 2
It is essentially identical.
Comparative example 3：
The present embodiment is the three of the comparative example of above-described embodiment 2.
In the present embodiment, the hydro-thermal reaction time is used as 24h, specific preparation method and the preparation method in embodiment 2
It is essentially identical.
Embodiment 3
Prepare a kind of multifunctional graphite vinyl aeroge, including following implementation steps：（1）Compound concentration is 2mg/ml oxygen first
Graphite alkene solution；（2）10mg titania nanotube is put into graphene oxide dispersion and is sufficiently stirred, is recycled super
Sound wave cell crushing instrument carries out ultrasonic disperse and obtains mixed solution, ultrasonic power 500W, ultrasonic time 30min；（3）Then will
Mixed solution is put into reactor, obtains composite aquogel by hydro-thermal self-assembling reaction, hydrothermal temperature is 90 DEG C, reaction
Time is 12h；（4）Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, cooling time 30min, freeze-drying
Multifunctional graphite vinyl aerogel material is produced after being removed water after 24h.
Comparative example 1：
The present embodiment is one of comparative example of above-described embodiment 3.
In the present embodiment, hydrothermal temperature is used as 120 DEG C, specific preparation method and the preparation side in embodiment 3
Method is essentially identical.
Comparative example 2：
The present embodiment is the two of the comparative example of above-described embodiment 2.
In the present embodiment, hydrothermal temperature is used as 150 DEG C, specific preparation method and the preparation side in embodiment 3
Method is essentially identical.
Comparative example 3：
The present embodiment is the three of the comparative example of above-described embodiment 2.
In the present embodiment, hydrothermal temperature is used as 180 DEG C, specific preparation method and the preparation side in embodiment 3
Method is essentially identical.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (9)
- A kind of 1. preparation method of multifunctional graphite vinyl aeroge, it is characterised in that the system of the multifunctional graphite vinyl aeroge Preparation Method, comprise the following steps that：（1）Compound concentration is less than 10mg/ml graphene oxide solution first；（2）The titania nanotube of certain mass is put into graphene oxide dispersion and is sufficiently stirred, recycles ultrasonic wave Cell crushing instrument carries out ultrasonic disperse and obtains mixed solution；（3）Then mixed solution is put into reactor, composite aquogel is obtained by hydro-thermal self-assembling reaction；（4）Finally columnar water gel is put into liquid nitrogen and carries out quick-frozen sizing, multifunctional graphite vinyl is produced after freeze-drying water removal Aerogel material.
- 2. the preparation method of multifunctional graphite vinyl aeroge according to claim 1, it is characterised in that step（1）It is described Graphene oxide solution graphene oxide according to 1-10mg/mL by mechanical agitation and be ultrasonically treated 10-60min in water or Disperse to obtain the solution of stable uniform in person's ethanol.
- 3. the preparation method of multifunctional graphite vinyl aeroge according to claim 1, it is characterised in that step（2）It is described Titania nanotube be super long titanium dioxide nanotube, diameter is in 10-30nm, length 1-10um, specific surface area 90- 110m2/g。
- 4. the preparation method of multifunctional graphite vinyl aeroge according to claim 1, it is characterised in that step（2）It is described Certain mass titania nanotube be 5-30mg.
- 5. the preparation method of functional graphene aeroge according to claim 1, it is characterised in that step（2）Described Power using ultrasonic cell disruption instrument is 300-500W, ultrasonic time 30-60min.
- 6. the preparation method of multifunctional graphite vinyl aeroge according to claim 1, it is characterised in that step（3）It is described Hydro-thermal self-assembling reaction temperature be 90-180 DEG C, reaction time 6-24h.
- 7. the preparation method of multifunctional graphite vinyl aeroge according to claim 1, it is characterised in that step（4）It is described The quick-frozen time be 10-60min, be put into freezing and drain in machine and take the moisture being frozen in system away, freeze-drying time 24-48h, Remaining is prepared aeroge.
- 8. multifunctional graphite vinyl aeroge prepared by the preparation method described in claim 1, it is characterised in that as electrode material Applied to preparing ultracapacitor.
- 9. multifunctional graphite vinyl aeroge prepared by the preparation method described in claim 1, it is characterised in that should as adsorbent For adsorbing bisphenol-A.
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| CN201710569305.8A CN107445150A (en) | 2017-07-13 | 2017-07-13 | A kind of preparation method of multifunctional graphite vinyl aeroge |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368807A (en) * | 2019-07-05 | 2019-10-25 | 南京中微纳米功能材料研究院有限公司 | A kind of preparation method of graphene-tin indium oxide nanofiber complex three-dimensional body block |
| CN111560162A (en) * | 2020-07-06 | 2020-08-21 | 华北电力大学 | Preparation method of enhanced PC/ABS alloy flame-retardant plate |
| CN113278400A (en) * | 2021-07-13 | 2021-08-20 | 信维通信（江苏）有限公司 | Graphene foam composite wave-absorbing material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110368807A (en) * | 2019-07-05 | 2019-10-25 | 南京中微纳米功能材料研究院有限公司 | A kind of preparation method of graphene-tin indium oxide nanofiber complex three-dimensional body block |
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| CN113278400A (en) * | 2021-07-13 | 2021-08-20 | 信维通信（江苏）有限公司 | Graphene foam composite wave-absorbing material and preparation method thereof |
| CN113278400B (en) * | 2021-07-13 | 2021-09-24 | 信维通信（江苏）有限公司 | Graphene foam composite wave-absorbing material and preparation method thereof |
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Application publication date: 20171208 |