CN109192541A - A kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor - Google Patents
A kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor Download PDFInfo
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- CN109192541A CN109192541A CN201811104002.XA CN201811104002A CN109192541A CN 109192541 A CN109192541 A CN 109192541A CN 201811104002 A CN201811104002 A CN 201811104002A CN 109192541 A CN109192541 A CN 109192541A
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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
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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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- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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 methods of the dedicated doping vario-property graphene oxide of supercapacitor, belong to novel energy resource material technology field.Water, n-hexane, nano graphene oxide, polyallylamine are first uniformly mixed by the present invention, and carbon dioxide is passed through in whipping process, and self-control lotion is made；After being again uniformly mixed self-control lotion, cerium salt, manganese salt, precipitating reagent is slowly added dropwise under stirring, adjusts pH, continues after being stirred to react, it is still aging, material must be aged；Ageing material is transferred to reaction kettle again, and is continually fed into inert gas into reaction kettle, under inert gas shielding state, heat temperature raising, after insulation reaction, cooling, discharging, stratification collects oily phase；It is mutually centrifugated oily, collects lower sediment thing, it is then washed, dry to get the dedicated doping vario-property graphene oxide of supercapacitor.The gained dedicated doping vario-property graphene oxide of supercapacitor of the invention has excellent chemical property.
Description
Technical field
The invention discloses a kind of preparation methods of the dedicated doping vario-property graphene oxide of supercapacitor, belong to new energy
Field of material technology.
Background technique
Energy problem is most one of serious problem that today's society faces.Therefore develop low cost, environmental-friendly novel
Energy conversion and storage device are one of the effective ways for solving energy problem.In all equipment, with traditional capacitor
And secondary cell is compared, the specific power of supercapacitor is 10 times of battery or more, and the ability for storing charge compares conventional capacitive
Device is high, and has the characteristics that charge/discharge speed is fast, no pollution to the environment, has extended cycle life, is wide using temperature limit range, becomes most
One of electrochemical energy storage device of potentiality.And have in fields such as mixed power electric car, mobile communication extensive
Application prospect.
It is well known that electrode material for super capacitor includes 3 major class substantially: carbon with electric double layer capacitance has counterfeit electricity
Metal hydroxides, oxide and the conducting polymer of appearance.Since single electrode material has some defects of itself, closely
Several years, the extensive concern of binary or even multiple elements design electrode material by everybody.Wherein, NiO/ redox graphene (rGO)
Combination electrode material is one of interested project of many researchers, and main cause is: NiO theoretical specific capacitance with higher,
RGO nanometer sheet electric conductivity with higher.The synergistic effect of the two so that composite material than pure electrode material chemical property
It is greatly improved.For example, having synthesized NiO/rGO combination electrode material by microwave-assisted effect, which goes out
Higher specific capacitance (specific capacitance reaches 799F/g when 0.3A/g)；It is obtained using the method for electrophoretic deposition and electrochemical deposition
The composite membrane of NiO and graphene, for the film in 2A/g, specific capacitance reaches 400F/g；It has been prepared by circumfluence method novel more
Hole graphene/NiO nanocomposite, electrode material specific capacitance in 200mA/g reach 429.7F/g.Traditional at present is super
Graphene oxide chemical property used in grade capacitor can not be promoted further, and when use inorganic, metal oxide doping, nothing
Machine metal-oxide powder is difficult to effectively penetrate into graphene interlayer structure, and powder is easy to happen group during the preparation process
It is poly-, anti-drop is not risen so as to cause the chemical property of graphene oxide, therefore also needs to study it.
Summary of the invention
The present invention solves the technical problem of: for graphene oxide chemical property used in conventional Super capacitor
When can not further be promoted, and use inorganic, metal oxide doping, inorganic, metal oxide powder is difficult to effectively penetrate into
In graphene interlayer structure, and powder is easy to happen reunion during the preparation process, so as to cause the electrochemistry of graphene oxide
The drawbacks of anti-drop can not be risen, provides a kind of preparation method of dedicated doping vario-property graphene oxide of supercapacitor.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) according to parts by weight, 60~80 parts of water are successively taken, 80~120 parts of n-hexanes, 15~20 parts of nano graphene oxides, 4
~8 parts of polyallylamines, are uniformly mixed, and carbon dioxide is continually fed into whipping process, derived from lotion processed；
(2) according to parts by weight, 200~300 parts of self-control lotions, 1~3 part of cerium salt are successively taken, 10~20 parts of manganese salts are stirred
After uniformly, precipitating reagent is slowly added dropwise under stirring, adjusts pH to 8.5~9.0, continues after being stirred to react, it is still aging, it obtains
Ageing material；
(3) ageing material is transferred to reaction kettle again, and is continually fed into inert gas into reaction kettle, in inert gas shielding state
Under, it is heated to 55~60 DEG C, cooling after 30~40min of insulation reaction, discharging, stratification collects oily phase；
(4) it is mutually centrifugated oily, collects lower sediment thing, it is then washed, dry to change to get the dedicated doping of supercapacitor
Property graphene oxide.
Step (1) is described to be continually fed into carbon dioxide are as follows: is continually fed into carbon dioxide gas with 60~80mL/min rate.
Step (2) cerium salt is cerous nitrate, cerium chloride, any one in cerous sulfate.
Step (2) manganese salt is manganese chloride, manganese sulfate, any one in manganese nitrate.
Step (2) is described to be slowly added dropwise to be added dropwise with 2~4mL/min rate.
Step (2) described precipitating reagent is the ammonium hydroxide that mass fraction is 8~10% or the urea liquid that mass fraction is 8~10%
In any one.
Step (3) is described to be continually fed into inert gas are as follows: with 80~100mL/min rate be continually fed into inert gas 30~
45min。
Step (3) inert gas is any one in nitrogen or argon gas.
The beneficial effects of the present invention are:
(1) for technical solution of the present invention first using water as water phase, n-hexane is oily phase, but also oleophylic not only hydrophilic using graphene oxide
The certain emulsification of excellent surface activation plays, System forming microemulsion system is made during being stirred, and utilize
Polyallylamine and carbon dioxide cooperate the stabilization to realize microemulsion system, avoid occurring mutually to separate in subsequent preparation process,
The stabilization process is to react what the three-dimensional crosslinked network to be formed was realized by carbon dioxide and polyallylamine, three-dimensional crosslinked network
Emulsion particle can be effectively fixed in web frame hole by formation, effectively improve the stability of microemulsion；
(2) technical solution of the present invention is by introducing cerium salt and manganese salt in self-control microemulsion system, on the one hand, two kinds of metal salts exist
Ionizable in aqueous solution to generate corresponding metal ion, on the other hand, the metal ion for ionizing generation can be oxidized graphene
The carboxyl of edge generates Electrostatic Absorption, so that metal ion is fixed on oil/water interface, after precipitating reagent is added, makes to put down
Weighing apparatus is destroyed, and metal ion and hydroxide ion combine in interface and form corresponding hydroxide, and once have hydroxide
Object nucleus, which generates, to be oxidized graphene package and enters in oil droplet kernel, and further growing up and rolling into a ball for nucleus is effectively prevented
It is poly-, then by subsequent oily, water two-phase separation and separate after oil removing phase to get obtain favorable dispersibility doped with metal
The graphene oxide of oxide, so that the chemical property of graphene oxide be made effectively to be promoted on the original basis；
(3) technical solution of the present invention realizes the doping to Mn oxide by using rare earth Ce elements, makes the manganese oxygen being prepared
Anisotropic expansion occurs for the cell parameter of compound, and tunnel size also changes, effectively increases the chemical property of material, make to mix
Graphene oxide chemical property after miscellaneous is further promoted.
Specific embodiment
According to parts by weight, 60~80 parts of water are successively taken, 80~120 parts of n-hexanes, 15~20 parts of nano graphene oxides,
4~8 parts of polyallylamines pour into No. 1 beaker, are stirred 30~60min with blender with 400~600r/min revolving speed, and
Carbon dioxide gas is continually fed into No. 1 beaker material by conduit in whipping process, regulation of carbon dioxide gas is passed through
Rate is 60~80mL/min, and mixing to be mixed terminates, and stopping is passed through carbon dioxide gas, derived from lotion processed；In parts by weight
Meter, successively takes 200~300 parts of self-control lotions, 1~3 part of cerium salt, and 10~20 parts of manganese salts are added in the four-hole boiling flask of belt stirrer,
Under the conditions of speed of agitator is 600~800r/min, pass through dropping funel while stirring into four-hole boiling flask with 2~4mL/min
Precipitating reagent is added dropwise in rate, adjusts material pH to 8.5~9.0 in four-hole boiling flask, after adjusting to pH, continues with 400~500r/
Min revolving speed is stirred to react 2~3h, to the end of reacting, stops stirring, still aging 2~3h, discharging must be aged material；Again by gained
Ageing material is transferred in reaction kettle, and is continually fed into 30~45min of inert gas into reaction kettle with 80~100mL/min rate,
It is then that reaction kettle is closed, under inert gas shielding state, it is heated to 55~60 DEG C, after 30~40min of insulation reaction,
Reaction kettle is opened, to material in reactor cooled to room temperature, discharging, stratification removes water phase, collects oily phase, and will
Oil is mutually transferred in centrifuge, under the conditions of revolving speed is 8000~12000r/min, is centrifugated 10~20min, is removed supernatant,
Collect lower sediment thing, and with dehydrated alcohol wash obtained by after lower sediment thing 3~5 times, be transferred in vacuum oven, in temperature
It is 95~105 DEG C, under the conditions of pressure is 80~120Pa, is dried under vacuum to constant weight, discharges to get the dedicated doping of supercapacitor
Modified graphene oxide.The cerium salt is cerous nitrate, cerium chloride, any one in cerous sulfate.The manganese salt is manganese chloride, sulphur
Any one in sour manganese, manganese nitrate.The precipitating reagent is the ammonium hydroxide that mass fraction is 8~10% or mass fraction is 8~10%
Urea liquid in any one.The inert gas is any one in nitrogen or argon gas.
According to parts by weight, 80 parts of water are successively taken, 120 parts of n-hexanes, 20 parts of nano graphene oxides, 8 parts of polyallylamines,
It pours into No. 1 beaker, 60min is stirred with 600r/min revolving speed with blender, and pass through conduit to No. 1 in whipping process
Carbon dioxide gas is continually fed into beaker material, it is 80mL/min, mixing to be mixed that regulation of carbon dioxide gas, which is passed through rate,
Terminate, stopping is passed through carbon dioxide gas, derived from lotion processed；According to parts by weight, 300 parts of self-control lotions, 3 parts of ceriums are successively taken
Salt, 20 parts of manganese salts, is added in the four-hole boiling flask of belt stirrer, under the conditions of speed of agitator is 800r/min, passes through while stirring
Precipitating reagent is added dropwise into four-hole boiling flask with 4mL/min rate in dropping funel, material pH to 9.0 in four-hole boiling flask is adjusted, to pH tune
After section end, continue to be stirred to react 3h with 500r/min revolving speed, to the end of reacting, stops stirring, still aging 3h, discharging obtains
Ageing material；Gained ageing material is transferred in reaction kettle again, and inert gas is continually fed into 100mL/min rate into reaction kettle
45min, it is then that reaction kettle is closed, it under inert gas shielding state, is heated to 60 DEG C, after insulation reaction 40min, opens
Reaction kettle is opened, to material in reactor cooled to room temperature, discharging, stratification removes water phase, collects oily phase, and will be oily
It is mutually transferred in centrifuge, under the conditions of revolving speed is 12000r/min, is centrifugated 20min, removes supernatant, collect lower sediment
Object, and after washing gained lower sediment thing 5 times with dehydrated alcohol, it is transferred in vacuum oven, is 105 DEG C in temperature, pressure is
Under the conditions of 120Pa, it is dried under vacuum to constant weight, is discharged to get the dedicated doping vario-property graphene oxide of supercapacitor.The cerium salt
For cerous nitrate.The manganese salt is manganese chloride.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
According to parts by weight, 80 parts of water, 120 parts of n-hexanes are successively taken, 20 parts of nano graphene oxides pour into No. 1 beaker
In, 60min is stirred with 600r/min revolving speed with blender, and pass through conduit into No. 1 beaker material in whipping process
It is continually fed into carbon dioxide gas, it is 80mL/min that regulation of carbon dioxide gas, which is passed through rate, and mixing to be mixed terminates, and is stopped logical
Enter carbon dioxide gas, derived from lotion processed；According to parts by weight, 300 parts of self-control lotions are successively taken, 3 parts of cerium salts, 20 parts of manganese salts,
It is added in the four-hole boiling flask of belt stirrer, under the conditions of speed of agitator is 800r/min, passes through dropping funel while stirring to four
Precipitating reagent is added dropwise with 4mL/min rate in mouth flask, adjusts material pH to 9.0 in four-hole boiling flask, after being adjusted to pH, is continued
It is stirred to react 3h with 500r/min revolving speed, to the end of reacting, stops stirring, still aging 3h, discharging must be aged material；Again by institute
Material must be aged to be transferred in reaction kettle, and inert gas 45min is continually fed into 100mL/min rate into reaction kettle, then will
Reaction kettle is closed, under inert gas shielding state, is heated to 60 DEG C, after insulation reaction 40min, opens reaction kettle, to
Material in reactor cooled to room temperature, discharging, stratification remove water phase, collect oily phase, and oil is mutually transferred to centrifuge
In, under the conditions of revolving speed is 12000r/min, it is centrifugated 20min, removes supernatant, collects lower sediment thing, and with anhydrous
Obtained by ethanol washing after lower sediment thing 5 times, be transferred in vacuum oven, in temperature be 105 DEG C, under the conditions of pressure is 120Pa,
It is dried under vacuum to constant weight, is discharged to get the dedicated doping vario-property graphene oxide of supercapacitor.The cerium salt is cerous nitrate.Institute
Stating manganese salt is manganese chloride.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
According to parts by weight, 80 parts of water are successively taken, 120 parts of n-hexanes, 20 parts of nano graphene oxides, 8 parts of polyallylamines,
It pours into No. 1 beaker, 60min is stirred with 600r/min revolving speed with blender, and pass through conduit to No. 1 in whipping process
Carbon dioxide gas is continually fed into beaker material, it is 80mL/min, mixing to be mixed that regulation of carbon dioxide gas, which is passed through rate,
Terminate, stopping is passed through carbon dioxide gas, derived from lotion processed；According to parts by weight, 300 parts of self-control lotions, 20 parts of manganese are successively taken
Salt is added in the four-hole boiling flask of belt stirrer, in speed of agitator be 800r/min under the conditions of, while stirring by dropping funel to
Precipitating reagent is added dropwise with 4mL/min rate in four-hole boiling flask, adjusts material pH to 9.0 in four-hole boiling flask, after being adjusted to pH, after
It is continuous that 3h is stirred to react with 500r/min revolving speed, to the end of reacting, stop stirring, still aging 3h, discharging must be aged material；Again will
Gained ageing material is transferred in reaction kettle, and is continually fed into inert gas 45min into reaction kettle with 100mL/min rate, then
Reaction kettle is closed, it under inert gas shielding state, is heated to 60 DEG C, after insulation reaction 40min, opens reaction kettle,
To material in reactor cooled to room temperature, discharging, stratification removes water phase, collects oily phase, and oil is mutually transferred to centrifugation
In machine, under the conditions of revolving speed is 12000r/min, it is centrifugated 20min, removes supernatant, collects lower sediment thing, and use nothing
It after water-ethanol washing gained lower sediment thing 5 times, is transferred in vacuum oven, is 105 DEG C in temperature, pressure is 120Pa condition
Under, it is dried under vacuum to constant weight, is discharged to get the dedicated doping vario-property graphene oxide of supercapacitor.The manganese salt is manganese chloride.
The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
According to parts by weight, 80 parts of water, 120 parts of dehydrated alcohols, 20 parts of nano graphene oxides, 8 parts of polyenes third are successively taken
Amine pours into No. 1 beaker, is stirred 60min with blender with 600r/min revolving speed, and in whipping process by conduit to
Carbon dioxide gas is continually fed into No. 1 beaker material, it is 80mL/min that regulation of carbon dioxide gas, which is passed through rate, to be mixed mixed
Conjunction terminates, and stopping is passed through carbon dioxide gas, derived from lotion processed；According to parts by weight, 300 parts of self-control lotions, 3 parts of ceriums are successively taken
Salt, 20 parts of manganese salts, is added in the four-hole boiling flask of belt stirrer, under the conditions of speed of agitator is 800r/min, passes through while stirring
Precipitating reagent is added dropwise into four-hole boiling flask with 4mL/min rate in dropping funel, material pH to 9.0 in four-hole boiling flask is adjusted, to pH tune
After section end, continue to be stirred to react 3h with 500r/min revolving speed, to the end of reacting, stops stirring, still aging 3h, discharging obtains
Ageing material；Gained ageing material is transferred in reaction kettle again, and inert gas is continually fed into 100mL/min rate into reaction kettle
45min, it is then that reaction kettle is closed, it under inert gas shielding state, is heated to 60 DEG C, after insulation reaction 40min, opens
Reaction kettle is opened, to material in reactor cooled to room temperature, discharging, stratification removes water phase, collects oily phase, and will be oily
It is mutually transferred in centrifuge, under the conditions of revolving speed is 12000r/min, is centrifugated 20min, removes supernatant, collect lower sediment
Object, and after washing gained lower sediment thing 5 times with dehydrated alcohol, it is transferred in vacuum oven, is 105 DEG C in temperature, pressure is
Under the conditions of 120Pa, it is dried under vacuum to constant weight, is discharged to get the dedicated doping vario-property graphene oxide of supercapacitor.The cerium salt
For cerous nitrate.The manganese salt is manganese chloride.The precipitating reagent is the ammonium hydroxide that mass fraction is 10%.The inert gas is nitrogen.
Comparative example: the modified graphene oxide of Changzhou material Science and Technology Ltd. production.
1 to 4 gained modified graphene oxide of example and comparative example product are subjected to performance detection, specific detection method is such as
Under:
Constant current charge-discharge test is carried out to above-mentioned modified graphene oxide material.
The calculation formula of specific capacity are as follows:
Cm=IΔt/mΔV
In formula: Cm is specific capacitance, F/g；I is discharge current, A；Δ t is discharge time, s；M is active material in electrode material
Quality, g；Δ V is discharge voltage range, V.
Specific testing result is as shown in table 1:
Table 1: performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Specific capacitance F/g | 770 | 732 | 659 | 696 | 527 |
By 1 testing result of table it is found that the present invention gained dedicated doping vario-property graphene oxide of supercapacitor has excellent electricity
Chemical property.
Claims (8)
1. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor, it is characterised in that specific preparation step
Are as follows:
(1) according to parts by weight, 60~80 parts of water are successively taken, 80~120 parts of n-hexanes, 15~20 parts of nano graphene oxides, 4
~8 parts of polyallylamines, are uniformly mixed, and carbon dioxide is continually fed into whipping process, derived from lotion processed；
(2) according to parts by weight, 200~300 parts of self-control lotions, 1~3 part of cerium salt are successively taken, 10~20 parts of manganese salts are stirred
After uniformly, precipitating reagent is slowly added dropwise under stirring, adjusts pH to 8.5~9.0, continues after being stirred to react, it is still aging, it obtains
Ageing material；
(3) ageing material is transferred to reaction kettle again, and is continually fed into inert gas into reaction kettle, in inert gas shielding state
Under, it is heated to 55~60 DEG C, cooling after 30~40min of insulation reaction, discharging, stratification collects oily phase；
(4) it is mutually centrifugated oily, collects lower sediment thing, it is then washed, dry to change to get the dedicated doping of supercapacitor
Property graphene oxide.
2. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is that step (1) is described and is continually fed into carbon dioxide are as follows: is continually fed into carbon dioxide gas with 60~80mL/min rate.
3. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is step (2) cerium salt for any one in cerous nitrate, cerium chloride, cerous sulfate.
4. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is step (2) manganese salt for any one in manganese chloride, manganese sulfate, manganese nitrate.
5. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is that step (2) is described and is slowly added dropwise to be added dropwise with 2~4mL/min rate.
6. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is that step (2) described precipitating reagent is in the ammonium hydroxide that mass fraction is 8~10% or the urea liquid that mass fraction is 8~10%
Any one.
7. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is that step (3) is described and is continually fed into inert gas are as follows: with 80~100mL/min rate be continually fed into inert gas 30~
45min。
8. a kind of preparation method of the dedicated doping vario-property graphene oxide of supercapacitor according to claim 1, special
Sign is step (3) inert gas for any one in nitrogen or argon gas.
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