CN106571238A - Composite electrode material for super-capacitor, and preparation method for composite electrode material - Google Patents
Composite electrode material for super-capacitor, and preparation method for composite electrode material Download PDFInfo
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- CN106571238A CN106571238A CN201610946377.5A CN201610946377A CN106571238A CN 106571238 A CN106571238 A CN 106571238A CN 201610946377 A CN201610946377 A CN 201610946377A CN 106571238 A CN106571238 A CN 106571238A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 239000003990 capacitor Substances 0.000 title abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 9
- XBBXDTCPEWHXKL-UHFFFAOYSA-N rhodium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Rh+3].[Rh+3] XBBXDTCPEWHXKL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims abstract description 9
- 229910021523 barium zirconate Inorganic materials 0.000 claims abstract description 8
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 5
- 230000005855 radiation Effects 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 230000001546 nitrifying effect Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 1
- 229910052788 barium Inorganic materials 0.000 claims 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 2
- 229920001661 Chitosan Polymers 0.000 abstract 2
- 239000011149 active material Substances 0.000 abstract 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 230000004087 circulation Effects 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- -1 meanwhile Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- 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
- H01G11/24—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
-
- 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
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention belongs to the technical field of capacitors, and specifically relates to a composite electrode material for a super-capacitor, and a preparation method for the composite electrode material. The material is made of the following raw materials: barium zirconate, nitrated chitosan, diisocyanate, rhodium sesquioxide, 2,2'-dihydroxymethyl propionic acid, and industrial pure silicone oil. Compared with the prior art, the material is advantageous in that the specific surface area of an electrode is increased through adding the nitrated chitosan so as to form an ion transmission porous structure; various types of raw materials are mixed to act; the composite material is enabled to generate active materials through employing a microwave device for carrying out the radiation processing; the material is repeatedly processed under the vacuum condition after the material is made into powder; the composite material is higher in power density and energy density, prolongs the cycle life, is used for making the electrode of the super-capacitor, can improve the capacity of the super-capacitor, and can reduce the internal resistance of the super-capacitor, generates more active materials; the size of the material can be controlled; the thickness of the material is with the range from 80 microns to 120 microns; and the electrochemical AC impedance is 5 Ohms.
Description
Technical field
The invention belongs to capacitor technology field, and in particular to a kind of combination electrode material for ultracapacitor and its
Preparation method.
Background technology
Ultracapacitor is a kind of novel energy storage apparatus, with power it is high, that energy conversion efficiency is high, training performance is good is excellent
Point, therefore one of focus referred to as in mechanism of new electrochemical power sources research, ultracapacitor be between traditional capacitor and rechargeable battery it
Between a kind of environmentally friendly, novel energy-storing that can not be substituted, energy saver；Compared with traditional capacitor, ultracapacitor
Both the characteristics of there is fast charging and discharging, and the energy storage mechnism with electrochemical cell, but also with long circulation life, without dirt
Dye, wider operating temperature range, the features such as consumption is big, just because of the above, ultracapacitor is in electric automobile, logical
News, consumption and the field such as recreation electronic, signal monitoring are more and more concerned, and which the requirement for complying with era development occurs, at present, surpass
The electrode material of level capacitor mainly by absorbent charcoal material, conducting polymer and composite and transition metal oxide and its
Combination electrode material, active Carbon-based supercapacitor research history are longer, and current commercialized degree is higher, and technology is most ripe, but
Its complex manufacturing, long the production cycle, and specific capacity is relatively low, it was reported that conducting polymer ultracapacitor can show very
High power density, but their specific capacity is but much lower than carbon/carbon supercapacitor and metal-oxide ultracapacitor；
Although metal-oxide or water alloyed oxide and CNT can produce great energy density and power density, but use this
The ultracapacitor cost of a little material manufactures is more much higher than other materials, therefore, further study correlated performance have improvement or
The electrode material of raising is used for button or winding type super capacitor is extremely important.
The content of the invention
The purpose of the present invention is for existing problem, there is provided a kind of combination electrode material for ultracapacitor and
Its preparation method.
The present invention is achieved by the following technical solutions：A kind of combination electrode material for ultracapacitor, by with
The raw material of lower weight portion is made：Barium zirconate 20-25 parts, nitrification shitosan 4-7 parts, diisocyanate 12-16 parts, rhodium sesquioxide
3-5 parts, 2,2 '-dihydro methylpropanoic acid 8-12 parts, technical pure silicone oil 3-6 parts；
Wherein, the preparation method of the nitrification shitosan is：It is 68% that shitosan is added equivalent to 60 times of mass fractions of its weight
Salpeter solution in, 2,4- toluene diisocynate of the Deca equivalent to concentrated nitric acid weight 1/3rd during mechanical agitation
Ester, dripped off in 8 minutes, and after reaction 2-3 hours, terminating reaction obtains nitrifying shitosan.
A kind of preparation method of the combination electrode material for ultracapacitor, comprises the following steps：
（1）By barium zirconate, the sodium hydroxide solution immersion 20-25 minutes that rhodium sesquioxide mass concentration is 8%, use after taking-up
Deionized water rinsing, is then dried to obtain compound standby；
（2）Above-mentioned gained compound is mixed with nitrification shitosan, diisocyanate, 2,2 '-dihydro methylpropanoic acid, technical pure silicone oil
After conjunction, the stirring reaction 2.5-3 hour under conditions of 80-90 DEG C, then with the microwave device spoke that radiant power is 500-600W
Penetrate process 25-30 minutes；
（3）Above-mentioned resulting material is processed in 180-200 DEG C of granulator and obtains powder body, then taken out under conditions of 300MPa
Vacuum, pressurize 8 minutes, was repeated once every 5 minutes, was obtained for preparing the composite of electrode material after evacuating 6 times altogether.
As further improvement of these options, the step（1）Middle dry run, baking temperature are 120-140 DEG C,
Drying time is 30-40 minutes.
The present invention has advantages below compared to existing technology：Compare table by increasing nitrification shitosan increase electrode in the present invention
The loose structure that area is transmitted with ion, plurality of raw materials immixture produce composite using microwave device radiation treatment
Active substance, is processed after powder body is made under vacuum repeatedly, is that composite has higher power density and energy
Density, extends its cycle life, for electrode of super capacitor, it is possible to increase capacity of super capacitor, reduction internal resistance, produces more
Many active substances, meanwhile, electrode material size is controllable, and between 80-120 microns, electrochemical AC impedance is 5 Europe to thickness
Nurse.
Specific embodiment
Embodiment 1
A kind of combination electrode material for ultracapacitor, is made up of the raw material of following weight portion：20 parts of barium zirconate, nitrification shell
7 parts of polysaccharide, 15 parts of diisocyanate, 4 parts of rhodium sesquioxide, 10 parts of 2,2 '-dihydro methylpropanoic acid, 6 parts of technical pure silicone oil；
Wherein, the preparation method of the nitrification shitosan is：It is 68% that shitosan is added equivalent to 60 times of mass fractions of its weight
Salpeter solution in, 2,4- toluene diisocynate of the Deca equivalent to concentrated nitric acid weight 1/3rd during mechanical agitation
Ester, dripped off in 8 minutes, and after reacting 2 hours, terminating reaction obtains nitrifying shitosan.
A kind of preparation method of the combination electrode material for ultracapacitor, comprises the following steps：
（1）By barium zirconate, the sodium hydroxide solution immersion 20-25 minutes that rhodium sesquioxide mass concentration is 8%, use after taking-up
Deionized water rinsing, is then dried to obtain compound standby；
（2）Above-mentioned gained compound is mixed with nitrification shitosan, diisocyanate, 2,2 '-dihydro methylpropanoic acid, technical pure silicone oil
After conjunction, the stirring reaction 2.5-3 hour under conditions of 80-90 DEG C, then with the microwave device spoke that radiant power is 500-600W
Penetrate process 25-30 minutes；
（3）Above-mentioned resulting material is processed in 180-200 DEG C of granulator and obtains powder body, then taken out under conditions of 300MPa
Vacuum, pressurize 8 minutes, was repeated once every 5 minutes, was obtained for preparing the composite of electrode material after evacuating 6 times altogether.
Wherein, the step（1）Middle dry run, baking temperature are 120-140 DEG C, and drying time is 30-40 minutes.
In the present invention, composite is tested to which after being used to prepare ultracapacitor, and test process takes constant current to fill
Electric discharge, electric current density is 0.5A/g, it can be found that capacitor prepared by the present embodiment combination electrode material has preferably after detection
Chemical property and higher coulombic efficiency, coulombic efficiency is 99.996%, and first charge-discharge specific capacitance reaches 207F/g,
Specific capacitance of discharging after 1000 circulations is positively retained at 99.2% or so.
Embodiment 2
A kind of combination electrode material for ultracapacitor, is made up of the raw material of following weight portion：22 parts of barium zirconate, nitrification shell
6 parts of polysaccharide, 14 parts of diisocyanate, 5 parts of rhodium sesquioxide, 12 parts of 2,2 '-dihydro methylpropanoic acid, 3 parts of technical pure silicone oil；
Wherein, the preparation method of the nitrification shitosan is：It is 68% that shitosan is added equivalent to 60 times of mass fractions of its weight
Salpeter solution in, 2,4- toluene diisocynate of the Deca equivalent to concentrated nitric acid weight 1/3rd during mechanical agitation
Ester, dripped off in 8 minutes, and after reacting 2.5 hours, terminating reaction obtains nitrifying shitosan.
Its preparation method is same as Example 1.
In the present invention, composite is tested to which after being used to prepare ultracapacitor, and test process takes constant current to fill
Electric discharge, electric current density is 0.5A/g, it can be found that capacitor prepared by the present embodiment combination electrode material has preferably after detection
Chemical property and higher coulombic efficiency, coulombic efficiency is 99.994%, and first charge-discharge specific capacitance reaches 209F/g,
Specific capacitance of discharging after 1000 circulations is positively retained at 99.3% or so.
Embodiment 3
A kind of combination electrode material for ultracapacitor, is made up of the raw material of following weight portion：25 parts of barium zirconate, nitrification shell
7 parts of polysaccharide, 16 parts of diisocyanate, 3 parts of rhodium sesquioxide, 10 parts of 2,2 '-dihydro methylpropanoic acid, 5 parts of technical pure silicone oil；
Wherein, the preparation method of the nitrification shitosan is：It is 68% that shitosan is added equivalent to 60 times of mass fractions of its weight
Salpeter solution in, 2,4- toluene diisocynate of the Deca equivalent to concentrated nitric acid weight 1/3rd during mechanical agitation
Ester, dripped off in 8 minutes, and after reacting 3 hours, terminating reaction obtains nitrifying shitosan.
Its preparation method is same as Example 1.
In the present invention, composite is tested to which after being used to prepare ultracapacitor, and test process takes constant current to fill
Electric discharge, electric current density is 0.5A/g, it can be found that capacitor prepared by the present embodiment combination electrode material has preferably after detection
Chemical property and higher coulombic efficiency, coulombic efficiency is 99.997%, and first charge-discharge specific capacitance reaches 202F/g,
Specific capacitance of discharging after 1000 circulations is positively retained at 99.4% or so.
Claims (3)
1. a kind of combination electrode material for ultracapacitor, it is characterised in that be made up of the raw material of following weight portion：Zirconic acid
Barium 20-25 parts, nitrification shitosan 4-7 parts, diisocyanate 12-16 parts, rhodium sesquioxide 3-5 parts, 2,2 '-dihydro methylpropanoic acid
8-12 parts, technical pure silicone oil 3-6 parts；
Wherein, the preparation method of the nitrification shitosan is：It is 68% that shitosan is added equivalent to 60 times of mass fractions of its weight
Salpeter solution in, 2,4- toluene diisocynate of the Deca equivalent to concentrated nitric acid weight 1/3rd during mechanical agitation
Ester, dripped off in 8 minutes, and after reaction 2-3 hours, terminating reaction obtains nitrifying shitosan.
2. a kind of preparation method of the combination electrode material for being used for as claimed in claim 1 ultracapacitor, it is characterised in that bag
Include following steps：
By barium zirconate, sodium hydroxide solution that rhodium sesquioxide mass concentration is 8% immersion 20-25 minutes, spend after taking-up from
Sub- water is rinsed, and is then dried to obtain compound standby；
Above-mentioned gained compound is mixed with nitrification shitosan, diisocyanate, 2,2 '-dihydro methylpropanoic acid, technical pure silicone oil
Afterwards, the stirring reaction 2.5-3 hour under conditions of 80-90 DEG C, then with the microwave device radiation that radiant power is 500-600W
Process 25-30 minutes；
Above-mentioned resulting material is processed in 180-200 DEG C of granulator and obtains powder body, then take out true under conditions of 300MPa
Sky, pressurize 8 minutes, was repeated once every 5 minutes, was obtained for preparing the composite of electrode material after evacuating 6 times altogether.
3. a kind of as claimed in claim 2 preparation method of the combination electrode material for ultracapacitor, it is characterised in that institute
State step（1）Middle dry run, baking temperature are 120-140 DEG C, and drying time is 30-40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610946377.5A CN106571238A (en) | 2016-10-26 | 2016-10-26 | Composite electrode material for super-capacitor, and preparation method for composite electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610946377.5A CN106571238A (en) | 2016-10-26 | 2016-10-26 | Composite electrode material for super-capacitor, and preparation method for composite electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106571238A true CN106571238A (en) | 2017-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610946377.5A Pending CN106571238A (en) | 2016-10-26 | 2016-10-26 | Composite electrode material for super-capacitor, and preparation method for composite electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109449002A (en) * | 2018-11-28 | 2019-03-08 | 北京大学 | A kind of modified Ti3C2TxMaterial and its preparation and application |
-
2016
- 2016-10-26 CN CN201610946377.5A patent/CN106571238A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109449002A (en) * | 2018-11-28 | 2019-03-08 | 北京大学 | A kind of modified Ti3C2TxMaterial and its preparation and application |
| CN109449002B (en) * | 2018-11-28 | 2020-05-05 | 北京大学 | Modified Ti3C2TxMaterial, its preparation and use |
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Application publication date: 20170419 |