CN110289182A - The preparation method of additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT electrode material - Google Patents
The preparation method of additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT electrode material Download PDFInfo
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- CN110289182A CN110289182A CN201910325050.XA CN201910325050A CN110289182A CN 110289182 A CN110289182 A CN 110289182A CN 201910325050 A CN201910325050 A CN 201910325050A CN 110289182 A CN110289182 A CN 110289182A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 33
- 239000000654 additive Substances 0.000 title claims abstract description 31
- 230000000996 additive effect Effects 0.000 title claims abstract description 31
- 239000007772 electrode material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 title claims abstract 6
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 39
- 239000011572 manganese Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 33
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 32
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000000499 gel Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000007654 immersion Methods 0.000 claims abstract description 6
- LWLURCPMVVCCCR-UHFFFAOYSA-N iron;4-methylbenzenesulfonic acid Chemical compound [Fe].CC1=CC=C(S(O)(=O)=O)C=C1 LWLURCPMVVCCCR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 6
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- 238000002604 ultrasonography Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 229940113088 dimethylacetamide Drugs 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 2
- WRLRISOTNFYPMU-UHFFFAOYSA-N [S].CC1=CC=CC=C1 Chemical compound [S].CC1=CC=CC=C1 WRLRISOTNFYPMU-UHFFFAOYSA-N 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000005253 cladding Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- XYIFTULRAWWQDU-UHFFFAOYSA-N benzenesulfonic acid;iron Chemical compound [Fe].OS(=O)(=O)C1=CC=CC=C1 XYIFTULRAWWQDU-UHFFFAOYSA-N 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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Abstract
The invention discloses a kind of additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT electrode material preparation methods, melamine is dissolved in graphene oxide solution by the present invention, VC and ammonium hydroxide is added, ultrasonic dissolution, organogel is formed with immersion method, organogel is fired to obtain NGA；NGA is added in butyl acetate, adds the mixed liquor that p-methyl benzenesulfonic acid iron is dissolved in ethyl alcohol and water, polymerization is stored at room temperature after ultrasonic mixing, can obtain NGA PEDOT material；By resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is catalyst, obtains additive Mn carbon gels electrode material；Repetition instills the mixed liquor n times of PANI on the additive Mn carbon gels material in (1) dropwise, this method has many advantages, such as to be simple and efficient, favorable reproducibility, can prepare with scale.The features such as material specific capacitance with higher of this method preparation, wider operating voltage window, fast charging and discharging.
Description
Technical field
The invention belongs to super capacitor new material energy storage field more particularly to a kind of asymmetric capacitors that can be used for
The preparation method of the electrode material of additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT.
Background technique
In order to improve the energy density of supercapacitor, preparing Asymmetric Supercapacitor is that raising energy density is most safe
One of effective approach.Asymmetric Supercapacitor is to improve work electricity by the different electrode of two potential windows of assembling
Pressure.Prepare the electrode material that Asymmetric Supercapacitor needs two kinds of voltage windows different, the usually work current potential with respect to calibration
For positive electrode, the relatively negative conduct negative electrode material of current potential.
Additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT is that a pair can be used for preparing asymmetric all solid state super electricity
The electrode material of container.Additive Mn carbon gels@(PANI/GO) n material is as anode, and NGA@PEDOT material is as cathode.Its
In, NGA@PEDOT be it is a kind of with poly- 3,4-rthylene dioxythiophene (PEDOT) cladding nitrogen-doped graphene gel (NGA) it is novel
Material, additive Mn carbon gels@(PANI/GO) n are polyaniline and graphene oxide n-layer self assembly cladding additive Mn carbon gels material
Material.Additive Mn carbon gels@(PANI/GO) n gel rubber material has good electric conductivity, and higher specific capacitance, preparation process is simple,
And NGA PEDOT has capacity height, stable feature is a kind of negative electrode material of good asymmetric super capacitor.
Summary of the invention
The present invention prepares aiming at the problem that energy density of all-solid-state flexible super capacitor improves with wider window
Additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT electrode material of current potential, it is super to can be used for asymmetrical all-solid-state flexible
The preparation of capacitor
A kind of additive Mn carbon gels@(PANI/GO) n//NGA@PEDOT electrode material preparation method, this method includes following
Step:
The preparation of NGA@PEDOT
(1), melamine is dissolved in graphene oxide solution, sequentially adds VC and ammonium hydroxide, 1-4 DEG C of ultrasound makes it completely
Dissolution, then makes mixed liquor form organogel in 80 DEG C of water temperatures with immersion method, by organogel 600- under an inert atmosphere
1200 DEG C of firing 2h obtain NGA, and wherein graphene oxide solution concentration is 0.5-20mg/ml, graphene oxide and VC mass ratio
For 1:1, the mass ratio of graphene oxide and ammonium hydroxide is 4:1；The mass ratio of melamine and graphene oxide is 1:200-5:
100；NGA is nitrogen-doped graphene gel；VC is vitamin C；
(2), NGA being added in butyl acetate, the content of NGA is 15wt.%, and EDOT is added in the ratio of 50 μ l/ml,
Ultrasonic 1h；EDOT is 3,4- ethene dioxythiophene；
(3), p-methyl benzenesulfonic acid iron is dissolved in the mixed liquor of ethyl alcohol and water, wherein the volume ratio of ethyl alcohol and water is 3:1, to first
The content of benzene sulfonic acid iron is that 0.6wt.% is stored at room temperature poly- by solution drips on step (2) resulting material after ultrasonic mixing
It closes, NGA@PEDOT material can be obtained.
The preparation of additive Mn carbon gels@(PANI/GO) n
(1), the carbon gels material of additive Mn is prepared
By resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is catalyst, wherein resorcinol and formaldehyde
Molar ratio is 1:2, and the molar ratio of resorcinol and sodium carbonate is 250:1-800:1, manganese content 0.5-3wt.%.It will be above-mentioned molten
Liquid is fitted into 30 DEG C aging 2 days in closed cylindrical body glass tube, 80 DEG C aging 5 days, be put into extract 2 days in acetone and be mixed to get manganese
Miscellaneous carbon gels electrode material；
(2), the PANI and DMAc for being 1:47 by mass ratio stirs 12h, then HCl is added in said mixture and to mix
Closing liquid pH value is 2.5, and the concentration of PANI is made to be 0.5mg/ml, then the ultrasound 3h at 1-4 DEG C；PANI is polyaniline；
DMAc is dimethyl acetamide；
(3), the mixed liquor of PANI in step (2) is instilled dropwise on the additive Mn carbon gels material in (1), is stood
After 15min, vacuum filtration removes the mixed liquor of extra PANI, then graphene oxide solution is instilled to additive Mn charcoal dropwise and coagulated
On glue, after standing 15min, vacuum filtration removes extra graphene oxide solution；Wherein the concentration of graphene oxide solution is
0.5-20mg/ml；
(4) step (3) n times are repeated, additive Mn carbon gels@(PANI/GO) n material can be obtained.
Have many advantages, such as to be simple and efficient the beneficial effects of the present invention are: this method, favorable reproducibility, can prepare with scale.
The features such as material specific capacitance with higher of this method preparation, wider operating voltage window, fast charging and discharging.
Specific embodiment
In order to better understand the present invention, the present invention is further explained in the light of specific embodiments.
Specific embodiment 1: melamine is dissolved in graphene oxide solution, ultrasound keeps it completely molten at 4 DEG C
Solution, sequentially adds VC and ammonium hydroxide, and sealer low temperature ultrasonic handles 2h, is then formed with mixed liquor in 80 DEG C of water temperatures with immersion method
Machine gel, by organogel, 600 DEG C of firing 2h obtain NGA under an inert atmosphere；Wherein graphene oxide solution concentration is 0.5
Mg/ml, graphene oxide and VC mass ratio are 1:1, and the mass ratio with ammonium hydroxide is 4:1, the matter of melamine and graphene oxide
Amount is than being 1:200；1mg NGA is put into butyl acetate, the content of NGA is 15wt.%, and is added according to the ratio of 50 μ l/ml
Enter EDOT, ultrasonic 1h obtains mixed liquor；The p-methyl benzenesulfonic acid iron of 0.25g is dissolved into the mixed liquor of 3ml ethyl alcohol and 1ml water, then
It drips in above-mentioned mixed liquor, is stored at room temperature after ultrasonic mixing polymerizable after 6h.After ethyl alcohol cleans drying at room temperature 1h, it can obtain
NGA@PEDOT material.
By resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is catalyst, wherein resorcinol and formaldehyde
Molar ratio is 1:2, and the molar ratio of resorcinol and sodium carbonate is 250:1, manganese content 1wt.%.Above-mentioned solution is packed into outer diameter
For 30 DEG C aging 2 days in the closed cylindrical body glass tube of 1cm, 80 DEG C aging 5 days, be put into extract 2 days in acetone and be mixed to get manganese
Miscellaneous carbon gels electrode material.The PANI of 1g and 50mlDMAc is mixed, stirs 12h, then HCl is added in said mixture and is made
Mixed liquor pH value is 2.5, and the concentration of PANI is made to be 0.5mg/ml, and then ultrasound 3h obtains the mixing of PANI at 4 DEG C
Liquid.The mixed liquor of PANI is instilled dropwise on the carbon gels material of additive Mn, after standing 15min, vacuum filter removes extra
Then PANI instills 0.5mg/ml graphene oxide solution on material dropwise, after standing 15min, vacuum filter removal is more
Remaining graphene oxide solution.Operation 4 times is repeated, additive Mn carbon gels@(PANI/GO) can be obtained5Material.
Specific embodiment 2: melamine is dissolved in graphene oxide solution, ultrasound keeps it completely molten at 4 DEG C
VC and ammonium hydroxide is added in solution, and sealer low temperature ultrasonic handles 2h, then forms mixed liquor in 80 DEG C of water temperatures with immersion method organic solidifying
Glue, by organogel, 900 DEG C of firing 2h obtain NGA under an inert atmosphere；Wherein graphene oxide solution concentration is 10mg/ml,
Graphene oxide and VC mass ratio are 1:1, and the mass ratio with ammonium hydroxide is 4:1, and the mass ratio of melamine and graphene oxide is
1:50；1mg NGA is put into butyl acetate, the content of NGA is 15wt.%, and EDOT is added according to the ratio of 50 μ l/ml,
Ultrasonic 1h obtains mixed liquor；The p-methyl benzenesulfonic acid iron of 0.25g is dissolved into the mixed liquor of 3ml ethyl alcohol and 1ml water, then drip in
It is stored at room temperature in above-mentioned mixed liquor, after ultrasonic mixing polymerizable after 6h.After ethyl alcohol cleans drying at room temperature 1h, NGA can be obtained
PEDOT material.
By resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is catalyst, wherein resorcinol and formaldehyde
Molar ratio is 1:2, and the molar ratio of resorcinol and sodium carbonate is 500:1, manganese content 2wt.%.Above-mentioned solution is packed into outer diameter
For 30 DEG C aging 2 days in the closed cylindrical body glass tube of 1cm, 80 DEG C aging 5 days, be put into extract 2 days in acetone and be mixed to get manganese
Miscellaneous carbon gels electrode material.PANI the and 50ml DMAc of 1g is mixed, stirs 12h, then will make in HCl addition said mixture
Obtaining mixed liquor pH value is 2.5, and the concentration of PANI is made to be 0.5mg/ml, and then ultrasound 3h obtains the mixing of PANI at 4 DEG C
Liquid.The mixed liquor of PANI is instilled dropwise on the carbon gels material of additive Mn, after standing 15min, vacuum filter removes extra
Then PANI instills 10mg/ml graphene oxide solution on material dropwise, after standing 15min, vacuum filter removal is more
Remaining graphene oxide solution.Operation 19 times is repeated, additive Mn carbon gels@(PANI/GO) can be obtained20Material.
Specific embodiment 3: melamine is dissolved in graphene oxide solution, ultrasound is made it completely dissolved at 4 DEG C,
VC and ammonium hydroxide is added, sealer low temperature ultrasonic handles 2h, then forms mixed liquor in 80 DEG C of water temperatures with immersion method organic solidifying
Glue, by organogel, 1000 DEG C of firing 2h obtain NGA under an inert atmosphere；Wherein graphene oxide solution concentration is 20mg/ml,
Graphene oxide and VC mass ratio are 1:1, and the mass ratio with ammonium hydroxide is 4:1, and the mass ratio of melamine and graphene oxide is
3:100；1mg NGA is put into butyl acetate, the content of NGA is 15wt.%, and EDOT is added according to the ratio of 50 μ l/ml,
Ultrasonic 1h obtains mixed liquor；The p-methyl benzenesulfonic acid iron of 0.25g is dissolved into the mixed liquor of 3ml ethyl alcohol and 1ml water, then drip in
It drips in above-mentioned mixed liquor, is stored at room temperature after ultrasonic mixing polymerizable after 6h again.After ethyl alcohol cleans drying at room temperature 1h
Obtain NGA@PEDOT material.
By resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is catalyst, wherein resorcinol and formaldehyde
Molar ratio is 1:2, and the molar ratio of resorcinol and sodium carbonate is 800:1, manganese content 3wt.%.Above-mentioned solution is packed into outer diameter
For 30 DEG C aging 2 days in the closed cylindrical body glass tube of 1cm, 80 DEG C aging 5 days, be put into extract 2 days in acetone and be mixed to get manganese
Miscellaneous carbon gels electrode material.PANI the and 50ml DMAc of 1g is mixed, stirs 12h, then will make in HCl addition said mixture
Obtaining mixed liquor pH value is 2.5, and the concentration of PANI is made to be 0.5mg/ml, and then ultrasound 3h obtains the mixing of PANI at 4 DEG C
Liquid.The mixed liquor of PANI is instilled dropwise on the carbon gels material of additive Mn, after standing 15min, vacuum filter removes extra
Then PANI instills 20mg/ml graphene oxide solution on material dropwise, after standing 15min, vacuum filter removal is more
Remaining graphene oxide solution.Operation 29 times is repeated, additive Mn carbon gels@(PANI/GO) can be obtained30Material.
Claims (1)
- The preparation method of additive Mn carbon gels 1.@(PANI/GO) n//NGA@PEDOT electrode material, comprising the following steps:The preparation of NGA@PEDOT(1), melamine is dissolved in graphene oxide solution, sequentially adds VC and ammonium hydroxide, 1-4 DEG C of ultrasound keeps it completely molten Solution, then makes mixed liquor form organogel in 80 DEG C of water temperatures with immersion method, by organogel 600- under an inert atmosphere 1200 DEG C of firing 2h obtain NGA, and wherein graphene oxide solution concentration is 0.5-20mg/ml, graphene oxide and VC mass ratio For 1:1, the mass ratio of graphene oxide and ammonium hydroxide is 4:1；The mass ratio of melamine and graphene oxide is 1:200-5: 100；NGA is nitrogen-doped graphene gel；VC is vitamin C；(2), NGA is added in butyl acetate, the content of NGA is 15wt.%, and EDOT, ultrasound is added in the ratio of 50 μ l/ml 1h；EDOT is 3,4- ethene dioxythiophene；(3), p-methyl benzenesulfonic acid iron is dissolved in the mixed liquor of ethyl alcohol and water, wherein the volume ratio of ethyl alcohol and water is 3:1, to toluene sulphur The content of sour iron is stored at room temperature polymerization by solution drips on step (2) resulting material for 0.6wt.% after ultrasonic mixing, NGA@PEDOT material can be obtained；The preparation of additive Mn carbon gels@(PANI/GO) n(1), the carbon gels material of additive Mn is preparedBy resorcinol, formaldehyde, manganese acetate as presoma, sodium carbonate is mole of catalyst, wherein resorcinol and formaldehyde Than for 1:2, the molar ratio of resorcinol and sodium carbonate is 250:1-800:1, manganese content 0.5-3wt.%；Above-mentioned solution is filled Enter 30 DEG C aging 2 days in closed cylindrical body glass tube, 80 DEG C aging 5 days, be put into acetone and extract 2 days to get additive Mn charcoal Gel electrode material；(2), the PANI and DMAc for being 1:47 by mass ratio stirs 12h, then HCl is added in said mixture and makes mixed liquor PH value is 2.5, and the concentration of PANI is made to be 0.5mg/ml, then the ultrasound 3h at 1-4 DEG C；PANI is polyaniline；DMAc is Dimethyl acetamide；(3), the mixed liquor of PANI in step (2) is instilled dropwise on the additive Mn carbon gels material in (1), after standing 15min, Vacuum filtration removes the mixed liquor of extra PANI, then instills graphene oxide solution on additive Mn carbon gels dropwise, quiet After setting 15min, vacuum filtration removes extra graphene oxide solution；Wherein the concentration of graphene oxide solution is 0.5- 20mg/ml；(4) step (3) n times are repeated, additive Mn carbon gels@(PANI/GO) n material can be obtained.
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| CN104558597A (en) * | 2014-09-30 | 2015-04-29 | 南京新月材料科技有限公司 | Preparation method of porous graphene/polyaniline composite |
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