CN104882293A - Nitrogen-doped waste PVC-based electrode material of high volumetric capacitance and method of preparation - Google Patents
Nitrogen-doped waste PVC-based electrode material of high volumetric capacitance and method of preparation Download PDFInfo
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- CN104882293A CN104882293A CN201510155412.7A CN201510155412A CN104882293A CN 104882293 A CN104882293 A CN 104882293A CN 201510155412 A CN201510155412 A CN 201510155412A CN 104882293 A CN104882293 A CN 104882293A
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- activated carbon
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- 239000007772 electrode material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 5
- 239000002699 waste material Substances 0.000 title abstract 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 17
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229940049676 bismuth hydroxide Drugs 0.000 claims abstract description 4
- TZSXPYWRDWEXHG-UHFFFAOYSA-K bismuth;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Bi+3] TZSXPYWRDWEXHG-UHFFFAOYSA-K 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 239000011651 chromium Substances 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- OTTGETCGDDGTDM-UHFFFAOYSA-N iron trifluoroborane Chemical compound [Fe].B(F)(F)F OTTGETCGDDGTDM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims description 3
- 239000004971 Cross linker Substances 0.000 abstract 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 abstract 1
- 229920003048 styrene butadiene rubber Polymers 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 101000831616 Homo sapiens Protachykinin-1 Proteins 0.000 description 1
- 102100024304 Protachykinin-1 Human genes 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010959 steel Substances 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
-
- 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)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a nitrogen-doped waste PVC-based electrode material of high volumetric capacitance. The nitrogen-doped waste PVC-based electrode material is characterized by being prepared by the following raw materials in parts by weight: 2-3 parts of graphene oxide, 1-2 parts of lithium iron phosphate, 1-2 parts of ferric nitrate, 1-2 parts of bismuth hydroxide, 2-3 parts of chromium boride, 100-200 parts of modified waste PVC-based activated carbon, 8-16 parts of distilled water, 1-2 parts of crosslinkers TAC and 1-2 parts of styrene-butadiene rubber. According to the invention, the activated carbon prepared by the waste PVC material has the advantages of large specific surface area, high conductivity efficiency, simple preparation process and the like, and a supercapacitor prepared by doping with graphene oxide with a good specific surface area and conductivity has excellent charge and discharge stability, a high specific capacitance value, high specific power and a high specific energy value.
Description
Technical field
The present invention relates to chemical energy source Material Field, particularly a kind of N doping with high volumetric capacitance discards PVC base electrode material and preparation method thereof.
Background technology
Ultracapacitor a kind ofly novel has high-energy-density, long circulation life and charging interval short green energy-storing device, all has purposes extremely widely at numerous areas such as electric automobile, uninterrupted power supply, Aero-Space, military affairs.Active carbon because specific area is high, chemical stability is good, the advantage such as cheap and preparation method is simple, become a kind of conventional electrode material for super capacitor.But due to active carbon exist aperture little, less, irregular, electrolyte ion is difficult to enter in the duct of microporous carbon, and ion transfer is obstructed, and the specific area utilance of material with carbon element is not high, thus causes the charge-discharge performance of electrode to be restricted.Except aperture, the surface functional group of electrode material is also one of key factor affecting its chemical property.Usually, nitrogen functional carbon material not only can increase polar active point hydrophilic in material by the introducing of nitrogen-atoms, improves electrolyte to the wettability of material, can also improve the storage charge capability of material.In addition, can also can bring accurate Faraday effect by nitrogenous functional group, thus significantly improve the ratio capacitance of Carbon-based supercapacitor.Along with the extensive use of PVC plastic, how to recycle ever-increasing discarded PVC and become problem in the urgent need to address, along with the development of science and technology, the new technology of the recycling of discarded PVC is in continuous development, at present in the various electrode materials of ultracapacitor, with discarded PVC resource for the material with carbon element with higher specific area prepared by raw material by chemical activation method, being a kind of ideal electrode material for super capacitor, is also one of effective means solving " white pollution ".
Summary of the invention
The object of this invention is to provide a kind of N doping with high volumetric capacitance and discard PVC base electrode material and preparation method thereof.
In order to realize object of the present invention, the present invention is by following scheme implementation:
The N doping with high volumetric capacitance discards a PVC base electrode material, is made up of the raw material of following weight portion: graphene oxide 2-3, LiFePO4 1-2, ferric nitrate 1-2, bismuth hydroxide 1-2, boronation two chromium 2-3, modified abandoned PVC matrix activated carbon 100-120, distilled water 8-16, crosslinking agent TAC1-2, butadiene-styrene rubber 1-2;
Described modified abandoned PVC matrix activated carbon is made up of the raw material of following weight portion: sodium metasilicate 1-2, precipitated silica 2-3, methyl triethoxysilane 2-3, zirconium fluoride 1-2, zinc stearate 1-2, titanium tetrachloride 2-3, borontrifluoride iron 1-2, discarded PVC material 400-500, potassium bichromate 20-30, ammoniacal liquor 40-60, preparation method is that discarded PVC powder is broken into and is evengranularly laid on ceramic evaporation ware by (1), in the environment of oxygen, heat up with the speed of 5 ° of C/min, 2-3 hour is maintained at 300-350 ° of C, again discarded PVC and potassium bichromate are mixed after end and put into calciner, heat up with the speed of 10 ~ 30 ° of C per minute, be heated to the active carbon that 600-700 ° of C obtains activation, naturally cool to room temperature, by active carbon, methyl triethoxysilane, sodium metasilicate and the mixing of all the other surplus materials, stirring reaction 20-40 minute when being heated to 80-90 ° of C, be added to again in ammoniacal liquor, control pressure and under 100-120 ° of C, maintain 2-3 hour in 2-3MPa temperature, take out oven dry ball milling and become 200-400 order powder, .
A kind of N doping with high volumetric capacitance of the present invention discards PVC base electrode material, is specifically made up of following steps:
(1) by distilled water, butadiene-styrene rubber and modified abandoned PVC matrix activated carbon mixing and stirring, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;
(2) by the product of step (1) and crosslinking agent TAC and remaining surplus materials mixed grinding thereof, grinding is placed in tube furnace, passes into pure ammonia, annealing in process 2-4 hour at 400-600 ° of C temperature, obtains the discarded PVC based combined electrode material that nitrogen is coated.
Advantage of the present invention is: the active carbon that the present invention utilizes discarded PVC material to prepare, there is the advantages such as specific area is large, electrical efficiency is high, preparation technology is simple, doping has the graphene oxide of good specific area and conductivity, and the ultracapacitor prepared has good stable charge/discharge, high ratio capacitance value, high specific power and high energy values.
specific embodiments
Below by instantiation, the present invention is described in detail.
The N doping with high volumetric capacitance discards a PVC base electrode material, is made up of the raw material of following weight portion (kilogram): graphene oxide 3, LiFePO4 1, ferric nitrate 1, bismuth hydroxide 2, boronation two chromium 3, modified abandoned PVC matrix activated carbon 110, distilled water 13, crosslinking agent TAC2, butadiene-styrene rubber 1;
Described modified abandoned PVC matrix activated carbon is made up of the raw material of following weight portion (kilogram): sodium metasilicate 1, precipitated silica 2, methyl triethoxysilane 2, zirconium fluoride 2, zinc stearate 1, titanium tetrachloride 2, borontrifluoride iron 2, discarded PVC material 400, potassium bichromate 26, ammoniacal liquor 56, preparation method is that discarded PVC powder is broken into and is evengranularly laid on ceramic evaporation ware by (1), in the environment of oxygen, heat up with the speed of 5 ° of C/min, 2-3 hour is maintained at 300-350 ° of C, again discarded PVC and potassium bichromate are mixed after end and put into calciner, heat up with the speed of 10 ~ 30 ° of C per minute, be heated to the active carbon that 600-700 ° of C obtains activation, naturally cool to room temperature, by active carbon, methyl triethoxysilane, sodium metasilicate and the mixing of all the other surplus materials, stirring reaction 20-40 minute when being heated to 80-90 ° of C, be added to again in ammoniacal liquor, control pressure and under 100-120 ° of C, maintain 2-3 hour in 2-3MPa temperature, take out oven dry ball milling and become 200-400 order powder, .
A kind of N doping with high volumetric capacitance of the present invention discards PVC base electrode material, is specifically made up of following steps:
(1) by distilled water, butadiene-styrene rubber and modified abandoned PVC matrix activated carbon mixing and stirring, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;
(2) by the product of step (1) and crosslinking agent TAC and remaining surplus materials mixed grinding thereof, grinding is placed in tube furnace, passes into pure ammonia, annealing in process 2-4 hour at 400-600 ° of C temperature, obtains the discarded PVC based combined electrode material that nitrogen is coated.
Proportionally mix with the electrode material in embodiment and conductive agent, binding agent, add a small amount of absolute ethyl alcohol to mix, uniform application vacuumize on stainless (steel) wire collector, take saturated calomel electrode as reference electrode, polytetrafluoroethylene is barrier film, with the KOH electrolyte aqueous solution of 6mol/l for electrolyte, in the scope of 1.2-2.5V, under constant current (5mA), carry out loop test, capacity: 1.71F, internal resistance: 1.6 Ω m, circulation volume conservation rate (%): 98.6.
Claims (2)
1. a N doping with high volumetric capacitance discards PVC base electrode material, it is characterized in that, be made up of the raw material of following weight portion: graphene oxide 2-3, LiFePO4 1-2, ferric nitrate 1-2, bismuth hydroxide 1-2, boronation two chromium 2-3, modified abandoned PVC matrix activated carbon 100-120, distilled water 8-16, crosslinking agent TAC1-2, butadiene-styrene rubber 1-2;
Described modified abandoned PVC matrix activated carbon is made up of the raw material of following weight portion: sodium metasilicate 1-2, precipitated silica 2-3, methyl triethoxysilane 2-3, zirconium fluoride 1-2, zinc stearate 1-2, titanium tetrachloride 2-3, borontrifluoride iron 1-2, discarded PVC material 400-500, potassium bichromate 20-30, ammoniacal liquor 40-60, preparation method is that discarded PVC powder is broken into and is evengranularly laid on ceramic evaporation ware by (1), in the environment of oxygen, heat up with the speed of 5 ° of C/min, 2-3 hour is maintained at 300-350 ° of C, again discarded PVC and potassium bichromate are mixed after end and put into calciner, heat up with the speed of 10 ~ 30 ° of C per minute, be heated to the active carbon that 600-700 ° of C obtains activation, naturally cool to room temperature, by active carbon, methyl triethoxysilane, sodium metasilicate and the mixing of all the other surplus materials, stirring reaction 20-40 minute when being heated to 80-90 ° of C, be added to again in ammoniacal liquor, control pressure and under 100-120 ° of C, maintain 2-3 hour in 2-3MPa temperature, take out oven dry ball milling and become 200-400 order powder, .
2. a kind of N doping with high volumetric capacitance discards PVC base electrode material according to claim 1, it is characterized in that, is specifically made up of following steps:
(1) by distilled water, butadiene-styrene rubber and modified abandoned PVC matrix activated carbon mixing and stirring, be heated to 50-60 ° of C, form slurry, for subsequent use after spraying dry;
(2) by the product of step (1) and crosslinking agent TAC and remaining surplus materials mixed grinding thereof, grinding is placed in tube furnace, passes into pure ammonia, annealing in process 2-4 hour at 400-600 ° of C temperature, obtains the discarded PVC based combined electrode material that nitrogen is coated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510155412.7A CN104882293A (en) | 2015-04-02 | 2015-04-02 | Nitrogen-doped waste PVC-based electrode material of high volumetric capacitance and method of preparation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510155412.7A CN104882293A (en) | 2015-04-02 | 2015-04-02 | Nitrogen-doped waste PVC-based electrode material of high volumetric capacitance and method of preparation |
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| Publication Number | Publication Date |
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| CN104882293A true CN104882293A (en) | 2015-09-02 |
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| CN201510155412.7A Pending CN104882293A (en) | 2015-04-02 | 2015-04-02 | Nitrogen-doped waste PVC-based electrode material of high volumetric capacitance and method of preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115216789A (en) * | 2022-08-10 | 2022-10-21 | 电子科技大学 | Titanium mesh in-situ growing iron modified TiO for nitrate electroreduction 2 Nano belt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887079A (en) * | 2014-03-05 | 2014-06-25 | 南京理工大学 | Nanocomposite material of nitrogen doped with graphene/manganese ferrite and preparation method thereof |
| CN104362314A (en) * | 2014-10-22 | 2015-02-18 | 重庆工商大学 | Composite oxide electrode material and preparation method thereof |
| US20150125743A1 (en) * | 2012-05-04 | 2015-05-07 | Nano-Nouvelle Pty Ltd | Battery electrode materials |
-
2015
- 2015-04-02 CN CN201510155412.7A patent/CN104882293A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150125743A1 (en) * | 2012-05-04 | 2015-05-07 | Nano-Nouvelle Pty Ltd | Battery electrode materials |
| CN103887079A (en) * | 2014-03-05 | 2014-06-25 | 南京理工大学 | Nanocomposite material of nitrogen doped with graphene/manganese ferrite and preparation method thereof |
| CN104362314A (en) * | 2014-10-22 | 2015-02-18 | 重庆工商大学 | Composite oxide electrode material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张倩: "《聚氯乙烯制备及生产工艺学》", 31 December 2014 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115216789A (en) * | 2022-08-10 | 2022-10-21 | 电子科技大学 | Titanium mesh in-situ growing iron modified TiO for nitrate electroreduction 2 Nano belt |
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Application publication date: 20150902 |