CN104788849A - 一种多孔废弃pvc基活性炭复合电极材料及其制备方法 - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000007772 electrode material Substances 0.000 title claims abstract description 22
- 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 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000004793 Polystyrene Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 7
- 229920002223 polystyrene Polymers 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Inorganic materials [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 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
- 235000011114 ammonium hydroxide Nutrition 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
- 238000003756 stirring Methods 0.000 claims description 6
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 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
- 238000001354 calcination Methods 0.000 claims description 3
- 229910052923 celestite Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 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
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen 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
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims description 3
- YTXFOSVCYYHADT-UHFFFAOYSA-N 2,1,3-benzoxadiazol-5-ol Chemical compound C1=C(O)C=CC2=NON=C21 YTXFOSVCYYHADT-UHFFFAOYSA-N 0.000 abstract 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 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
- 239000003610 charcoal Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 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
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- 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
- 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
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- 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
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- H—ELECTRICITY
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- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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Abstract
本发明公开了一种多孔废弃PVC基活性炭复合电极材料,其特征在于,由下列重量份的原料制成:碳纳米管2-3、层状锰酸锂2-3、硝酸锰1-2、氢氧化镁1-2、天青石粉1-2、改性废弃PVC基活性炭110-130、聚苯乙烯1-2、蒸馏水9-15、甲基三乙氧基硅烷2-3;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,添加的氢氧化镁增加了活性炭的孔隙,增大比表面积,提高导电率,添加的层状锰酸锂具有资源丰富、成本低、无污染、安全性好、倍率性能好等优点,进一步提高了活性炭基电极材料的性能。
Description
技术领域
本发明涉及化学能源材料领域,特别是一种多孔废弃PVC基活性炭复合电极材料及其制备方法。
背景技术
活性炭作为电极材料具有微孔丰富的特征,但是单位比表面积利用率低,原因可能是因为过小的微孔不利于电解液的浸润,导致电子无法迁移,影响电容器能量密度和功率密度。因此,在制备高比表面积活性炭材料的同时对其孔径结构进行合理控制,是提高超级电容器的能量密度和功率密度的一种有效的手段。随着PVC塑料的广泛应用,如何回收利用不断增加的废弃PVC成为迫切需要解决的问题,伴随着科技的发展,废弃PVC的资源化利用的新技术在不断的发展,目前在超级电容器的各种电极材料中,以废弃PVC资源为原料通过化学活化方法制备具有较高的比表面积的碳材料,是一种较为理想的超级电容器电极材料,也是解决“白色污染”的有效手段之一,本发明在制备电极材料中添加的氢氧化镁在高温下能够分解,产生的气体能够增加活性炭的孔隙,增大比表面积,提高导电率,并且添加导电效果的碳纳米管和具有资源丰富、成本低、无污染、安全性好、倍率性能好等优点的层状锰酸锂,进一步提高活性炭作为电极材料的性能。
发明内容
本发明的目的是提供一种多孔废弃PVC基活性炭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:
一种多孔废弃PVC基活性炭复合电极材料,由下列重量份的原料制成:碳纳米管2-3、层状锰酸锂2-3、硝酸锰1-2、氢氧化镁1-2、天青石粉1-2、改性废弃PVC基活性炭110-130、聚苯乙烯1-2、蒸馏水9-15、甲基三乙氧基硅烷2-3;
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。
本发明所述一种多孔废弃PVC基活性炭复合电极材料,由以下步骤具体制成:
(1)将蒸馏水、聚苯乙烯、碳纳米管和改性废弃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)将步骤(1)的产物和甲基三乙氧基硅烷及其余剩余物质混合研磨,研磨后置于管式炉中,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,添加的氢氧化镁增加了活性炭的孔隙,增大比表面积,提高导电率,添加的层状锰酸锂具有资源丰富、成本低、无污染、安全性好、倍率性能好等优点,进一步提高了活性炭基电极材料的性能。
具体实施方案
下面通过具体实例对本发明进行详细说明。
一种多孔废弃PVC基活性炭复合电极材料,由下列重量份(公斤)的原料制成:碳纳米管3、层状锰酸锂3、硝酸锰1、氢氧化镁1、天青石粉1、改性废弃PVC基活性炭120、聚苯乙烯1、蒸馏水13、甲基三乙氧基硅烷2;
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。
本发明所述一种多孔废弃PVC基活性炭复合电极材料,由以下步骤具体制成:
(1)将蒸馏水、聚苯乙烯、碳纳米管和改性废弃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)将步骤(1)的产物和甲基三乙氧基硅烷及其余剩余物质混合研磨,研磨后置于管式炉中,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:1.72F,内阻:1.8Ω·m,循环容量保持率(%):98.2。
Claims (2)
1.一种多孔废弃PVC基活性炭复合电极材料,其特征在于,由下列重量份的原料制成:碳纳米管2-3、层状锰酸锂2-3、硝酸锰1-2、氢氧化镁1-2、天青石粉1-2、改性废弃PVC基活性炭110-130、聚苯乙烯1-2、蒸馏水9-15、甲基三乙氧基硅烷2-3;
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所述一种多孔废弃PVC基活性炭复合电极材料,其特征在于,由以下步骤具体制成:
(1)将蒸馏水、聚苯乙烯、碳纳米管和改性废弃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)将步骤(1)的产物和甲基三乙氧基硅烷及其余剩余物质混合研磨,研磨后置于管式炉中,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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