CN109817471A - Modification method of graphene-based lithium ion capacitor positive electrode material - Google Patents
Modification method of graphene-based lithium ion capacitor positive electrode material Download PDFInfo
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- CN109817471A CN109817471A CN201811600967.8A CN201811600967A CN109817471A CN 109817471 A CN109817471 A CN 109817471A CN 201811600967 A CN201811600967 A CN 201811600967A CN 109817471 A CN109817471 A CN 109817471A
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- graphene
- positive electrode
- ion capacitor
- based lithium
- phenylenediamine
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 44
- 239000003990 capacitor Substances 0.000 title claims abstract description 16
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000007774 positive electrode material Substances 0.000 title abstract 4
- 238000002715 modification method Methods 0.000 title abstract 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical group NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001338 self-assembly Methods 0.000 claims abstract description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 7
- OVOZYARDXPHRDL-UHFFFAOYSA-N 3,4-diaminophenol Chemical compound NC1=CC=C(O)C=C1N OVOZYARDXPHRDL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- HEMGYNNCNNODNX-UHFFFAOYSA-N 3,4-diaminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1N HEMGYNNCNNODNX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 12
- 238000000280 densification Methods 0.000 claims description 7
- 230000000802 nitrating effect Effects 0.000 claims description 6
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 238000003756 stirring Methods 0.000 abstract description 11
- CLWRFNUKIFTVHQ-UHFFFAOYSA-N [N].C1=CC=NC=C1 Chemical group [N].C1=CC=NC=C1 CLWRFNUKIFTVHQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
- 239000010405 anode material Substances 0.000 description 6
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000006258 conductive agent Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 101000878457 Macrocallista nimbosa FMRFamide Proteins 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HMVJXTUUQJUYJI-UHFFFAOYSA-N (3,4-diaminophenyl)methanol Chemical compound NC1=CC=C(CO)C=C1N HMVJXTUUQJUYJI-UHFFFAOYSA-N 0.000 description 1
- LIOBPVZSSVYQSS-UHFFFAOYSA-N 2-(3,4-diaminophenyl)acetic acid Chemical compound NC1=CC=C(CC(O)=O)C=C1N LIOBPVZSSVYQSS-UHFFFAOYSA-N 0.000 description 1
- -1 3,4- diamino cyanophenyl Chemical group 0.000 description 1
- COOOBYQQEQSCHM-UHFFFAOYSA-N C=O.NC1=C(C=CC=C1)N Chemical compound C=O.NC1=C(C=CC=C1)N COOOBYQQEQSCHM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JZSORJRHANDTGE-UHFFFAOYSA-N benzene-1,2-diamine formic acid Chemical compound C(=O)O.NC1=C(C=CC=C1)N JZSORJRHANDTGE-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Classifications
-
- 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 modification method of a graphene-based lithium ion capacitor positive electrode material, which comprises the steps of dispersing a high-density graphene-based positive electrode material formed by self-assembly of reduced graphene oxide in an ethanol solvent, adding excessive nitrogen source molecules containing an o-phenylenediamine structure, heating to 40-70 ℃, stirring, refluxing, reacting for 6-48 hours, washing and filtering by using ethanol-pure water-ethanol for 3 times in sequence, and drying to obtain a nitrogen-doped product. The nitrogen source molecule containing an o-phenylenediamine structure is o-phenylenediamine, 3, 4-diaminobenzoic acid and 3, 4-diaminophenol. According to the invention, a pyridine nitrogen functional group is introduced through selective reaction at a specific site, so that the electrochemical circulation stability of the graphene-based positive electrode material is effectively improved.
Description
Technical field
The invention belongs to changing for technical field of chemical power, especially a kind of graphene-based lithium-ion capacitor positive electrode
Property method.
Background technique
Supercapacitor, also known as electrochemical capacitor or super capacitor have power density height, good rate capability, follow
The advantages such as the ring service life grows (> 100,000 time), the temperature limit for width (- 40 DEG C~+80 DEG C) that works and maintenance cost are low, have attracted academia
With the extensive concern of industry.Energy density and power density are to evaluate two key parameters of performance of the supercapacitor.By public affairs
Formula E=1/2CV2As can be seen that energy density and the operating voltage of supercapacitor is square directly proportional.Therefore, work is widened
Voltage window can effectively improve the energy density of supercapacitor.And to realize this point, an effective method is exactly to design
Asymmetric super-capacitor.Asymmetric super-capacitor is the positive electrode (fake capacitance electrode) separately constituted by two kinds of different materials
It is constituted with negative electrode (electric double layer capacitance electrode).Similar with lithium ion battery, the technical bottleneck of supercapacitor mainly collects at present
In on positive electrode, and this kind of fake capacitance positive electrode is required to include: bigger serface, high surface, fast electric
Son transmission, the stabilization open architecture for being suitble to ion intercalation/deintercalation.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of modifications of graphene-based lithium-ion capacitor positive electrode
Method is realized using C=O original in material and is mixed based on the understanding to graphene-based material molecule structure and chemical property
The target of pyridine-N functional group introduces nitrogen-containing functional group by surface chemical reaction to realize to graphene-based material electrochemical
The regulation of matter.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that: a kind of graphene-based lithium-ion capacitor
The method of modifying of positive electrode disperses the graphene-based positive electrode of the densification formed after redox graphene self assembly
In alcohol solvent, the excessive nitrogen source molecule containing o-phenylenediamine structure is added, is heated to 40 DEG C~70 DEG C, is stirred at reflux reaction
It 6~48 hours, is then successively washed and is filtered each 3 times with the pure water-ethanol of ethyl alcohol-, nitrating product can be obtained in drying.
The nitrogen source molecule containing o-phenylenediamine structure is o-phenylenediamine, 3,4- diaminobenzoic acid, 3,4- diamino
Phenol.
The molar ratio range of the graphene-based positive electrode and nitrogen source molecule is from 10:1 to 1:10.
The drying temperature is 70 DEG C~100 DEG C.
It is described to be heated to 60 DEG C, it is stirred at reflux reaction 12 hours, is dried in 70 DEG C.
The beneficial effects of the present invention are: by introducing pyridine nitrogen functional group in specific site selective reaction, thus effectively
Improve the electrochemical cycle stability of graphene-based positive electrode in ground.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of nitrogen-doped graphene base anode material obtained in the embodiment of the present invention；
Fig. 2 is the cycle performance curve graph of nitrogen-doped graphene base anode material obtained in the embodiment of the present invention.
Specific embodiment
The present invention is explained in further detail below with reference to specific embodiment, the embodiment provided is only for elaboration
The present invention, the range being not intended to be limiting of the invention.
The method of modifying of graphene-based lithium-ion capacitor positive electrode of the invention, by redox graphene self assembly
The graphene-based positive electrode of the densification formed afterwards is scattered in alcohol solvent, and the excessive nitrogen containing o-phenylenediamine structure is added
Source molecule is heated to 40 DEG C~70 DEG C, is stirred at reflux reaction 6~48 hours, is then successively washed with the pure water-ethanol of ethyl alcohol-
It filters each 3 times, is dried in 70 DEG C~100 DEG C, nitrating product can be obtained.
The nitrogen source molecule containing o-phenylenediamine structure is o-phenylenediamine, 3,4- diaminophenol, 3,4- diaminobenzene
Formic acid, 3,4- diamino-phenylacetic acid, 3,4- diamino cyanophenyl, 3,4- diaminobenzene formaldehyde, 3,4- diaminobenzene methanol.
The molar ratio range of the graphene-based positive electrode and nitrogen source molecule is from 10:1 to 1:10.
It is preferred that described be heated to 60 DEG C, it is stirred at reflux reaction 12 hours, is dried in 70 DEG C.
The graphene-based positive electrode selected in this system is the densification formed after redox graphene self assembly
Material (13.5mg cm-2), capacity (120mAh/g) with higher, cycle performance is also better (to maintain 80% after 200 circles
Capacity), however, all there are also biggish rooms for promotion for its capacity and cycle performance.The present invention is based on to graphene-based material molecule
Structure and chemically Quality Research and understanding find that original C=O can be used as the active site of chemical reaction in material, can
It is reacted with nitrogenous precursor, realizes the target of incorporation pyridine-N functional group, the electrification of graphene-based material is regulated and controled with this
Property is learned, and then promotes its capacity and cyclical stability, is such graphene-based positive electrode in the future in supercapacitor
Practical application is laid a good foundation.
Embodiment 1
Material preparation: taking the graphene-based positive electrode 1.5g of the densification formed after redox graphene self assembly,
150mL dehydrated alcohol is added, stirs 30 minutes, 0.88g o-phenylenediamine is added, stirs 30 minutes, is put into 60 DEG C of oil bath pans, stirs
It mixes back flow reaction 12 hours, is then successively washed and filtered each 3 times with the pure water-ethanol of ethyl alcohol-, by obtained solid 70 in baking oven
DEG C drying, nitrating product can be obtained.
Battery preparation and test: by 0.4g nitrogen-doped graphene base anode material and conductive agent Super P and mass fraction
60% PTFE aqueous solution 8:1:1 in mass ratio mixing, is added 20mL dehydrated alcohol, and stir makes its mixing equal for 4 hours at room temperature
Even, roll-in forms a film (100 microns of thickness), and 120 DEG C are dried in vacuo 12 hours.The positive diaphragm punching press that will be prepared through the above steps
At the disk of Φ 12mm, liquid button battery then is assembled into diaphragm, lithium an- ode and electrolyte (EC:DMC=1:1)
CR2430, tests cycle performance of battery, and voltage range is 1.5~4.2V vs Li/Li+, current density 100mA/g, test
Temperature is 25 DEG C.
Embodiment 2
Material preparation: taking the graphene-based positive electrode 1.5g of the densification formed after redox graphene self assembly,
150mL dehydrated alcohol is added, stirs 30 minutes, 1.01g 3 is added, 4- diaminophenol stirs 30 minutes, is put into 60 DEG C of oil baths
Pot in, be stirred at reflux reaction 12 hours, then with the pure water-ethanol of ethyl alcohol-successively wash suction filtration it is each 3 times, by obtained solid in
70 DEG C of drying, can be obtained nitrating product in baking oven.
Battery preparation and test: by 0.4g nitrogen-doped graphene base anode material and conductive agent Super P and mass fraction
60% PTFE aqueous solution 8:1:1 in mass ratio mixing, is added 20mL dehydrated alcohol, and stir makes its mixing equal for 4 hours at room temperature
Even, roll-in forms a film (100 microns of thickness), and 120 DEG C are dried in vacuo 12 hours.The positive diaphragm punching press that will be prepared through the above steps
At the disk of Φ 12mm, liquid button battery then is assembled into diaphragm, lithium an- ode and electrolyte (EC:DMC=1:1)
CR2430, tests cycle performance of battery, and voltage range is 1.5~4.2V vs Li/Li+, current density 100mA/g, test
Temperature is 25 DEG C.
Embodiment 3
Material preparation: taking the graphene-based positive electrode 1.5g of the densification formed after redox graphene self assembly,
150mL dehydrated alcohol is added, stirs 30 minutes, 1.14g 3 is added, 4- diaminobenzoic acid stirs 30 minutes, is put into 60 DEG C of oil
In bath, it is stirred at reflux reaction 12 hours, is then successively washed and is filtered each 3 times with the pure water-ethanol of ethyl alcohol-, by obtained solid
70 DEG C of drying, can be obtained nitrating product in baking oven.
Battery preparation and test: by 0.4g nitrogen-doped graphene base anode material and conductive agent Super P and mass fraction
60% PTFE aqueous solution 8:1:1 in mass ratio mixing, is added 20mL dehydrated alcohol, and stir makes its mixing equal for 4 hours at room temperature
Even, roll-in forms a film (100 microns of thickness), and 120 DEG C are dried in vacuo 12 hours.The positive diaphragm punching press that will be prepared through the above steps
At the disk of Φ 12mm, liquid button battery then is assembled into diaphragm, lithium an- ode and electrolyte (EC:DMC=1:1)
CR2430, tests cycle performance of battery, and voltage range is 1.5~4.2V vs Li/Li+, current density 100mA/g, test
Temperature is 25 DEG C.
As shown in Figure 1,1720cm-1The peak C=O at place substantially weakens, corresponding 1600cm-1The peak C=N at place is bright
Aobvious enhancing illustrates that reaction is occurred by design scheme:
Therefore, pyridine nitrogen functional group successfully is introduced in specified site.
As shown in Fig. 2, the discharge capacity of nitrogen-doped graphene base anode material reaches 110mAh/g, and cyclical stability is obvious
It is promoted, after 500 charge and discharge cycles, can still maintain 80% of initial capacity or so.
Embodiment described above is merely to illustrate technical idea and feature of the invention, in the art its object is to make
Technical staff it will be appreciated that the contents of the present invention and implement accordingly, patent model of the invention only cannot be limited with the present embodiment
It encloses, i.e., same changes or modifications made by all disclosed spirit are still fallen in the scope of the patents of the invention.
Claims (5)
1. a kind of method of modifying of graphene-based lithium-ion capacitor positive electrode, which is characterized in that by redox graphene
The graphene-based positive electrode of the densification formed after self assembly is scattered in alcohol solvent, is added and is excessively contained o-phenylenediamine knot
The nitrogen source molecule of structure is heated to 40 DEG C~70 DEG C, is stirred at reflux reaction 6~48 hours, then with the pure water-ethanol of ethyl alcohol-according to
Secondary washing filters each 3 times, and nitrating product can be obtained in drying.
2. the method for modifying of graphene-based lithium-ion capacitor positive electrode according to claim 1, which is characterized in that described
Nitrogen source molecule containing o-phenylenediamine structure is o-phenylenediamine, 3,4- diaminobenzoic acid, 3,4- diaminophenol.
3. the method for modifying of graphene-based lithium-ion capacitor positive electrode according to claim 1, which is characterized in that described
The molar ratio range of graphene-based positive electrode and nitrogen source molecule is from 10:1 to 1:10.
4. the method for modifying of graphene-based lithium-ion capacitor positive electrode according to claim 1, which is characterized in that described
Drying temperature is 70 DEG C~100 DEG C.
5. the method for modifying of any one of -4 graphene-based lithium-ion capacitor positive electrodes according to claim 1, feature
It is, it is described to be heated to 60 DEG C, it is stirred at reflux reaction 12 hours, is dried in 70 DEG C.
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| CN201811600967.8A CN109817471A (en) | 2018-12-26 | 2018-12-26 | Modification method of graphene-based lithium ion capacitor positive electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113659143A (en) * | 2021-08-06 | 2021-11-16 | 东莞市创明电池技术有限公司 | Preparation method of negative electrode material of sodium ion battery, negative electrode material and sodium ion battery |
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