CN104779057A - 一种高容量废弃pvc基复合电极材料及其制备方法 - Google Patents
一种高容量废弃pvc基复合电极材料及其制备方法 Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229920000915 polyvinyl chloride Polymers 0.000 title abstract 6
- 239000004800 polyvinyl chloride Substances 0.000 title abstract 6
- 239000002131 composite material Substances 0.000 title abstract 3
- 239000002699 waste material Substances 0.000 title abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 229920001353 Dextrin Polymers 0.000 claims abstract description 7
- 239000004375 Dextrin Substances 0.000 claims abstract description 7
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019425 dextrin Nutrition 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 4
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 claims abstract description 4
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- 238000002156 mixing Methods 0.000 claims description 9
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000010957 pewter Substances 0.000 claims description 8
- 229910000498 pewter Inorganic materials 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-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
- 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
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 230000004913 activation Effects 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
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
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- 229910000077 silane Inorganic materials 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
- 229910001245 Sb alloy Inorganic materials 0.000 abstract 2
- 239000002140 antimony alloy Substances 0.000 abstract 2
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 abstract 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 abstract 2
- 239000006087 Silane Coupling Agent Substances 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
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- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 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
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle 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
- 239000010959 steel Substances 0.000 description 1
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- 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
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- H—ELECTRICITY
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- 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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- 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
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- 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
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- 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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Abstract
本发明公开了一种高容量废弃PVC基复合电极材料,其特征在于,由下列重量份的原料制成:锡锑合金1-2、丁苯橡胶1-2、三乙醇胺1-2、纳米氧化锗2-4、纳米硫化钴1-3、改性废弃PVC基活性炭110-120、蒸馏水10-15、糊精1-3、硅烷偶联剂KH5701-2;本发明利用废弃的PVC材料制备的活性炭,具有比表面积大、导电效率高、制备工艺简单等优点,掺杂的纳米氧化锗提高了电极材料的导电性、电化学性能和电容量,表面包覆的锡锑合金增加了电极材料的孔隙,提高导电率和比表面积,解决炭基电极材料电容量、能量密度低的难题。
Description
技术领域
本发明涉及化学能源材料领域,特别是一种高容量废弃PVC基复合电极材料及其制备方法。
背景技术
随着信息化社会的不断扩大和环境及能源危机的出现,能源储存与转换问题成为当今的研究热点。在各种能源转换系统中,超级电容器由于具有充放电速度快、循环寿命长,相对安全、使用温度宽、环境友好和免维护等优良特性而被广泛应用于各领域。根据储能机理的不同,超级电容器可分为双电层电容器和赝电容器。双电层电容器主要依靠电极和电解液界面的双电层来存储电荷,利用电极材料巨大的比表面积通过物理过程储存电能,其电极材料主要为高比表面积的碳材料。活性炭具有很大的比表面积和丰富的内孔结构,可为双电层的形成提供巨大的表面积,因此是最早应用于超级电容器的一种电极材料,但唯一不足的是活性炭能量密度较低。纳米氧化锗具有良好的导电性,它以纳米粒子的存在形式附着在炭极材料表面,提高了电极材料的电化学性能,并且能够在电化学反应中起到催化的作用,提高电极材料的电容量,锡锑合金包覆活性炭,提高活性炭的孔隙,提高导电率和比表面积,解决炭基电极材料电容量、能量密度低的难题。
发明内容
本发明的目的是提供一种高容量废弃PVC基复合电极材料及其制备方法。
为了实现本发明的目的,本发明通过以下方案实施:
一种高容量废弃PVC基复合电极材料,由下列重量份的原料制成:锡锑合金1-2、丁苯橡胶1-2、三乙醇胺1-2、纳米氧化锗2-4、纳米硫化钴1-3、改性废弃PVC基活性炭110-120、蒸馏水10-15、糊精1-3、硅烷偶联剂KH5701-2;
所述改性废弃PVC基活性炭是由下列重量份的原料制成:偏硅酸钠1-2、沉淀法白炭黑2-3、甲基三乙氧基硅烷2-3、氟化锆1-2、硬脂酸锌1-2、四氯化钛2-3、三氟化铁1-2、废弃PVC材料400-500、重铬酸钾20-30、氨水40-60;制备方法是(1)将废弃的PVC粉碎成颗粒均匀的平铺在陶瓷蒸发皿上,在氧气的环境中,以5°C/min的速度升温,在300-350°C维持2-3小时,结束后再将废弃的PVC和重铬酸钾混合均匀放入煅烧炉中,以每分钟10~30°C的速度升温,加热至600-700°C获得活化的活性炭,自然冷却至室温,将活性炭、甲基三乙氧基硅烷、偏硅酸钠和其余剩余物质混合,加热至80-90°C时搅拌反应20-40分钟,再加到氨水中,控制压强在2-3MPa温度在100-120°C下维持2-3小时,取出烘干球磨成200-400目粉末,即可。
本发明所述一种高容量废弃PVC基复合电极材料,由以下步骤具体制成:
(1)将蒸馏水、丁苯橡胶、糊精和改性废弃PVC基活性炭混合搅拌均匀,加热至50-60°C,形成浆料,喷雾干燥后备用;
(2)将锡锑合金加热至熔融和步骤(1)的产物及其余剩余物质混合搅拌均匀,置于管式炉中,通入纯氨气,在400-600°C温度下退火处理2-4小时,得到氮包覆的废弃PVC基复合电极材料。
本发明的优点是:本发明利用废弃的PVC材料制备的活性炭,具有比表面积大、导电效率高、制备工艺简单等优点,掺杂的纳米氧化锗提高了电极材料的导电性、电化学性能和电容量,表面包覆的锡锑合金增加了电极材料的孔隙,提高导电率和比表面积,解决炭基电极材料电容量、能量密度低的难题。
具体实施方案
下面通过具体实例对本发明进行详细说明。
一种高容量废弃PVC基复合电极材料,由下列重量份(公斤)的原料制成:锡锑合金2、丁苯橡胶1、三乙醇胺2、纳米氧化锗4、纳米硫化钴2、改性废弃PVC基活性炭110、蒸馏水14、糊精2、硅烷偶联剂KH5702;
所述改性废弃PVC基活性炭是由下列重量份(公斤)的原料制成:偏硅酸钠1、沉淀法白炭黑2、甲基三乙氧基硅烷2、氟化锆2、硬脂酸锌1、四氯化钛2、三氟化铁2、废弃PVC材料400、重铬酸钾26、氨水56;制备方法是(1)将废弃的PVC粉碎成颗粒均匀的平铺在陶瓷蒸发皿上,在氧气的环境中,以5°C/min的速度升温,在300-350°C维持2-3小时,结束后再将废弃的PVC和重铬酸钾混合均匀放入煅烧炉中,以每分钟10~30°C的速度升温,加热至600-700°C获得活化的活性炭,自然冷却至室温,将活性炭、甲基三乙氧基硅烷、偏硅酸钠和其余剩余物质混合,加热至80-90°C时搅拌反应20-40分钟,再加到氨水中,控制压强在2-3MPa温度在100-120°C下维持2-3小时,取出烘干球磨成200-400目粉末,即可。
本发明所述一种高容量废弃PVC基复合电极材料,由以下步骤具体制成:
(1)将蒸馏水、丁苯橡胶、糊精和改性废弃PVC基活性炭混合搅拌均匀,加热至50-60°C,形成浆料,喷雾干燥后备用;
(2)将锡锑合金加热至熔融和步骤(1)的产物及其余剩余物质混合搅拌均匀,置于管式炉中,通入纯氨气,在400-600°C温度下退火处理2-4小时,得到氮包覆的废弃PVC基复合电极材料。
以实施例中的电极材料和导电剂、粘结剂按照比例混合,加入少量的无水乙醇混合均匀,均匀涂抹在不锈钢网集流体上真空干燥,以饱和甘汞电极为参比电极,聚四氟乙烯为隔膜,以6mol/l的KOH电解质水溶液为电解液,在1.2-2.5V的范围内,在恒流(5mA)下进行循环测试,容量:1.67F,内阻:1.4Ω·m,循环容量保持率(%):98.7。
Claims (2)
1.一种高容量废弃PVC基复合电极材料,其特征在于,由下列重量份的原料制成:锡锑合金1-2、丁苯橡胶1-2、三乙醇胺1-2、纳米氧化锗2-4、纳米硫化钴1-3、改性废弃PVC基活性炭110-120、蒸馏水10-15、糊精1-3、硅烷偶联剂KH5701-2;
所述改性废弃PVC基活性炭是由下列重量份的原料制成:偏硅酸钠1-2、沉淀法白炭黑2-3、甲基三乙氧基硅烷2-3、氟化锆1-2、硬脂酸锌1-2、四氯化钛2-3、三氟化铁1-2、废弃PVC材料400-500、重铬酸钾20-30、氨水40-60;制备方法是(1)将废弃的PVC粉碎成颗粒均匀的平铺在陶瓷蒸发皿上,在氧气的环境中,以5°C/min的速度升温,在300-350°C维持2-3小时,结束后再将废弃的PVC和重铬酸钾混合均匀放入煅烧炉中,以每分钟10~30°C的速度升温,加热至600-700°C获得活化的活性炭,自然冷却至室温,将活性炭、甲基三乙氧基硅烷、偏硅酸钠和其余剩余物质混合,加热至80-90°C时搅拌反应20-40分钟,再加到氨水中,控制压强在2-3MPa温度在100-120°C下维持2-3小时,取出烘干球磨成200-400目粉末,即可。
2.根据权利要求1所述一种高容量废弃PVC基复合电极材料,其特征在于,由以下步骤具体制成:
(1)将蒸馏水、丁苯橡胶、糊精和改性废弃PVC基活性炭混合搅拌均匀,加热至50-60°C,形成浆料,喷雾干燥后备用;
(2)将锡锑合金加热至熔融和步骤(1)的产物及其余剩余物质混合搅拌均匀,置于管式炉中,通入纯氨气,在400-600°C温度下退火处理2-4小时,得到氮包覆的废弃PVC基复合电极材料。
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