CN105977044A - Polyacrylonitrile enhanced composite electrode material with small self-discharge voltage attenuation and preparation method thereof - Google Patents
Polyacrylonitrile enhanced composite electrode material with small self-discharge voltage attenuation and preparation method thereof Download PDFInfo
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- CN105977044A CN105977044A CN201610213887.1A CN201610213887A CN105977044A CN 105977044 A CN105977044 A CN 105977044A CN 201610213887 A CN201610213887 A CN 201610213887A CN 105977044 A CN105977044 A CN 105977044A
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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
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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 polyacrylonitrile enhanced composite electrode material with small self-discharge voltage attenuation, which is prepared from the following raw materials in parts by weight: 60-63 parts of loofah, 37-40 parts of scaphium scaphigerum, an appropriate amount of distilled water, 39.5-40 parts of zinc chloride, 8-8.5 parts of lithium chloride, 15-17 parts of conductive graphite, 3-4 parts of urea, 6-7 parts of potassium perchlorate, 8-9 parts of polyacrylonitrile powder, 2-3 parts of guar gum, 8-9 parts of polytetrafluoroethylene emulsion and 0.4-0.5 part of hexadecyl trimethyl ammonium bromide. The polyacrylonitrile powder is prepared into carbonized powder through a series of processes and added into preparation of the electrode material, so that the specific surface area and the mesoporous rate are increased. Meanwhile, the surface wettability of the electrode material is improved by nitrogen-containing functional groups at the surface, so that the diffusion impedance is extremely small, leakage current and the self-discharge voltage attenuation rate are very small, and manufactured products have extremely high use values.
Description
Technical field
The present invention relates to electrode material technical field, particularly relate to little polyacrylonitrile enhancement mode combination electrode material of a kind of self discharge voltage attenuation and preparation method thereof.
Background technology
The transition of fossil energy is relied on and consumes and causes serious environmental problem and energy crisis by the mankind, and for realizing the development and utilization of the energy of sustainable development, new forms of energy and the research of novel energy device cause extensive concern.Ultracapacitor is class novel energy-storing device between traditional capacitor and battery, and compared with tradition energy storage device, it has higher energy density and power density, longer service life cycle, advantages of environment protection simultaneously.Along with the development of science and technology in recent years, ultracapacitor is gradually increased in the application trend of the aspects such as crane, fork truck, new-energy automobile, common electronic facility and factory's stand-by power supply.But, the electric conductivity of super capacitor material is poor, be related to ultracapacitor key property as the uneven problem common with electrolyte contacts face unstable properties etc. of Topical Dispersion.Electrode is to determine ultracapacitor performance most critical factor, therefore the research of electrode material always this field academia and the focus of industrial quarters.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that polyacrylonitrile enhancement mode combination electrode material that a kind of self discharge voltage attenuation is little and preparation method thereof.
The present invention is achieved by the following technical solutions:
The polyacrylonitrile enhancement mode combination electrode material that a kind of self discharge voltage attenuation is little, is prepared by the raw materials in: Retinervus Luffae Fructus 60-63, Semen Sterculiae Lychnophorae 37-40, distilled water are appropriate, zinc chloride 39.5-40, lithium chloride 8-8.5, electrically conductive graphite 15-17, carbamide 3-4, potassium perchlorate 6-7, polyacrylonitrile powder 8-9, guar gum 2-3, ptfe emulsion 8-9, cetyl trimethylammonium bromide 0.4-0.5.
According to ultracapacitor novel plant Quito pore carbon electrode material a kind of described in claims 1, following concrete grammar it is prepared from:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by；Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder；
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material；
(3) polyacrylonitrile powder is put in air dry oven, after being warming up to 300 DEG C of oxidations 4 hours with the heating rate of 2 DEG C/min, then be warming up to 800 DEG C with the heating rate of 5 DEG C/min, carbonization 30 minutes, obtain polyacrylonitrile carbon powder stand-by；Potassium perchlorate is dissolved in same amount of distilled water, add carbamide, stir and mix with the guar gum being dissolved in 2 times amount distilled water after being completely dissolved, above-mentioned polyacrylonitrile carbon powder, electrically conductive graphite is added after stirring 30 minutes with the speed of 300 revs/min, put in mortar, grind 60 minutes, obtain mixed material；
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, the plant base porous carbon material that step (2) obtains, mixed material that step (3) obtains and remaining residual components, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110-120 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
The invention have the advantage that the present invention uses the plant component such as Retinervus Luffae Fructus, Semen Sterculiae Lychnophorae as carbon source, resource natural reproducible, reduce the dependence to fossil energy, and utilize zinc chloride and lithium chloride salt-mixture as activator, not only solve and utilize the shortcoming of perishable reaction vessel in activation of potassium hydroxide technique, and the plant base porous carbon material prepared has the distribution of optimized pore structure and hole dimension, has good chemical property, technique is simple simultaneously, and feasibility is high.
Polyacrylonitrile powder is made carbonization powder by a series of technique by the present invention, add in the preparation of electrode material of the present invention, enhance specific surface area and mesoporous, simultaneously and owing to surface nitrogen-containing functional group improves the surface wettability of electrode material, diffusion impedance is the least, leakage current, self discharge voltage degradation rate are the least, and the product made has high use value.
Detailed description of the invention
The polyacrylonitrile enhancement mode combination electrode material that a kind of self discharge voltage attenuation is little, is made up of the raw material of following weight portion (kilogram): Retinervus Luffae Fructus 60, Semen Sterculiae Lychnophorae 37, distilled water are appropriate, zinc chloride 39.5, lithium chloride 8, electrically conductive graphite 15, carbamide 3, potassium perchlorate 6, polyacrylonitrile powder 8, guar gum 2, ptfe emulsion 8, cetyl trimethylammonium bromide 0.4.
According to ultracapacitor novel plant Quito pore carbon electrode material a kind of described in claims 1, following concrete grammar it is prepared from:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by；Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder；
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material；
(3) polyacrylonitrile powder is put in air dry oven, after being warming up to 300 DEG C of oxidations 4 hours with the heating rate of 2 DEG C/min, then be warming up to 800 DEG C with the heating rate of 5 DEG C/min, carbonization 30 minutes, obtain polyacrylonitrile carbon powder stand-by；Potassium perchlorate is dissolved in same amount of distilled water, add carbamide, stir and mix with the guar gum being dissolved in 2 times amount distilled water after being completely dissolved, above-mentioned polyacrylonitrile carbon powder, electrically conductive graphite is added after stirring 30 minutes with the speed of 300 revs/min, put in mortar, grind 60 minutes, obtain mixed material；
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, the plant base porous carbon material that step (2) obtains, mixed material that step (3) obtains and remaining residual components, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
In described embodiment, the electrode of preparation is as working electrode, metallic nickel is colelctor electrode, politef is barrier film, with 2mol/L potassium hydroxide as electrolyte, in the range of 1.2-2.5V, under constant current (5mA), it is circulated test, at room temperature determines that its capacity is 1.73F by charging and discharging curve, internal resistance is 1.62m Ω, and circulation volume conservation rate is 97.8%.
Claims (2)
1. the polyacrylonitrile enhancement mode combination electrode material that a self discharge voltage attenuation is little, it is characterized in that, be prepared by the raw materials in: Retinervus Luffae Fructus 60-63, Semen Sterculiae Lychnophorae 37-40, distilled water are appropriate, zinc chloride 39.5-40, lithium chloride 8-8.5, electrically conductive graphite 15-17, carbamide 3-4, potassium perchlorate 6-7, polyacrylonitrile powder 8-9, guar gum 2-3, ptfe emulsion 8-9, cetyl trimethylammonium bromide 0.4-0.5.
2. according to ultracapacitor novel plant Quito pore carbon electrode material a kind of described in claims 1, it is characterised in that be prepared from by following concrete grammar:
(1) by Retinervus Luffae Fructus under being passed through nitrogen protection, being warming up to 800 DEG C with the heating rate of 5 DEG C/min, insulation carbonization naturally cooled to room temperature after 1 hour, pulverized, and crossed 200 mesh sieves stand-by；Remove shell after Semen Sterculiae Lychnophorae is soaked in the distilled water of 5 times amount expansion and obtain Semen Sterculiae Lychnophorae suspension with crust, above-mentioned 200 mesh powder are added thereto, after stirring, add zinc chloride, lithium chloride, be spray-dried after ultrasonic 2 hours, obtain mixed-powder；
(2) mixed-powder is put in horizontal pipe furnace; under the protection being passed through nitrogen; it is incubated 2 hours at a temperature of 1000 DEG C; after being cooled to room temperature, product is put in the distilled water of 2 times amount and filter after ultrasonic 1.5 hours; the filter cake obtained is put in vacuum drying oven and dry, obtain plant base porous carbon material；
(3) polyacrylonitrile powder is put in air dry oven, after being warming up to 300 DEG C of oxidations 4 hours with the heating rate of 2 DEG C/min, then be warming up to 800 DEG C with the heating rate of 5 DEG C/min, carbonization 30 minutes, obtain polyacrylonitrile carbon powder stand-by；Potassium perchlorate is dissolved in same amount of distilled water, add carbamide, stir and mix with the guar gum being dissolved in 2 times amount distilled water after being completely dissolved, above-mentioned polyacrylonitrile carbon powder, electrically conductive graphite is added after stirring 30 minutes with the speed of 300 revs/min, put in mortar, grind 60 minutes, obtain mixed material；
(4) ptfe emulsion will add the distilled water of 5 times amount, stir and add, after being completely dispersed uniformly, the plant base porous carbon material that step (2) obtains, mixed material that step (3) obtains and remaining residual components, after stirring 1.5 hours with the speed of 1000 revs/min, material is transferred in rubber mill, the slurry obtaining 400 mesh is ground with the speed of 200 revs/min, then slurry is coated with on a current collector uniformly, it is vacuum dried 6 hours under conditions of temperature 110-120 DEG C, on desktop electric tablet machine, under the pressure of 10MPa, tabletting is carried out after taking-up, dry to constant weight at a temperature of 80 DEG C and get final product in being placed again into vacuum drying oven after cutting.
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| CN201610213887.1A CN105977044A (en) | 2016-04-07 | 2016-04-07 | Polyacrylonitrile enhanced composite electrode material with small self-discharge voltage attenuation and preparation method thereof |
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| CN201610213887.1A CN105977044A (en) | 2016-04-07 | 2016-04-07 | Polyacrylonitrile enhanced composite electrode material with small self-discharge voltage attenuation and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102804303A (en) * | 2010-01-09 | 2012-11-28 | 戴斯分析公司 | Energy storage devices including a solid multilayer electrolyte |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN104247111A (en) * | 2012-04-09 | 2014-12-24 | 昭和电工株式会社 | Method for producing collector for electrochemical elements, method for producing electrode for electrochemical elements, collector for electrochemical elements, electrochemical element, and coating liquid for forming collector for electrochemical elements |
| CN104821234A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | High-aluminum powder/modified straw composite electrode material and preparation method thereof |
-
2016
- 2016-04-07 CN CN201610213887.1A patent/CN105977044A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102804303A (en) * | 2010-01-09 | 2012-11-28 | 戴斯分析公司 | Energy storage devices including a solid multilayer electrolyte |
| CN104247111A (en) * | 2012-04-09 | 2014-12-24 | 昭和电工株式会社 | Method for producing collector for electrochemical elements, method for producing electrode for electrochemical elements, collector for electrochemical elements, electrochemical element, and coating liquid for forming collector for electrochemical elements |
| CN104098083A (en) * | 2014-07-15 | 2014-10-15 | 黑龙江大学 | Method for preparing porous nano carbon materials with biomass serving as carbon source |
| CN104821234A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | High-aluminum powder/modified straw composite electrode material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 呼小洲等: "混合盐活化胖大海基多孔碳的制备及超级电容器电极材料性能", 《应用化学》 * |
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