CN104851610A - 一种高导电秸秆基活性炭复合电极材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种高导电秸秆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:氯化钾1-2、聚吡咯2-3、正硅酸乙酯1-3、氯金酸0.5-1、锌合金3-5、二茂钴1-2、乙酰丙酮钯1-3、聚苯胺复合材料3-5、秸秆1000-1200、无水氢氧化钾3-5、去离子水5-10;本发明的聚苯胺复合材料具有价格便宜、电荷密度高等的优点,添加到电极材料中能够提高导电性和储电性能;添加的聚吡咯由于具有较好的导电性、光电性、热电性可在常温或低温下使用,较易沉积在各种基片上,并且成本较低、容易制备,在一定程度上提高了电容器的导电性能。
Description
技术领域
本发明涉及化学能源材料领域,特别是一种高导电秸秆基活性炭复合电极材料及其制备方法。
背景技术
超级电容器兼有普通电容器功率密度大和二次电池能量密度高的优点,可以快速充放电而且寿命长,被认为是介于二次电池和电容器之间的一种储能器件。它的电容量大,漏电流小,电压记忆性好,充放电简单而且循环次数多。可用于微型计算机存储器的后备电源、汽车启动装置及太阳能、风能等洁净能源系统,成为近几年广为关注的研究热点。多孔炭材料以其低廉的价格、高的比表面积、可控的孔隙结构和良好的物理化学稳定性在超级电容器领域内倍受关注。由于我国是农业大国,农作物收割会产生许多的秸秆,大部分的秸秆采用焚烧的方法进行处理,不仅污染了空气,破坏了土壤的土质,并且对人们的身体健康有害。所以炭的来源广泛,需要经过特定的处理制备出具有一定比表面积和孔径分布的多孔炭,进而应用于超级电层电容器的电极材料。本发明添加的聚吡咯由于具有较好的导电性、光电性、热电性可在常温或低温下使用,可以方便地沉积在各种基片上,并且成本较低、容易制备,在一定程度上提高了电容器的导电性能。
聚苯胺具有良好的导电性和快速可逆的氧化还原特性,且原料廉价易得,近年来在能量存贮领域受到人们的广泛关注。聚苯胺本身是绝缘性,经掺杂后才具有导电性,而且它主要掺杂点是亚胺氮原子。质子携带的正电荷经分子链内部的电荷转移,沿分子链产生周期性的分布。且苯二胺和醌二亚胺必须同时存在才能保证有效的质子酸掺杂。质子掺杂是聚苯胺由绝缘态转变为金属态的关键。不同的合成方式对聚苯胺的导电性和稳定性影响很大,本发明在合成聚苯胺的同时掺杂二氧化硅和蒙脱土,增强了聚苯胺的稳定性、导电性,并且产物粒径均匀,而且都在纳米级别,从而使产物具有了纳米粒子的特性。
发明内容
本发明的目的是提供一种高导电秸秆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:
一种高导电秸秆基活性炭复合电极材料,由下列重量份的原料制成:氯化钾1-2、聚吡咯2-3、正硅酸乙酯1-3、氯金酸0.5-1、锌合金3-5、二茂钴1-2、乙酰丙酮钯1-3、聚苯胺复合材料3-5、秸秆1000-1200、无水氢氧化钾3-5、去离子水5-10;
所述聚苯胺复合材料是由下列重量份的原料制成:对甲苯磺酸4-6、盐酸6-8、纳米二氧化硅3-5、蒙脱土2-4、苯胺8-12、过硫酸铵0.4-0.7、去离子水30-50;制备方法是将对甲苯磺酸加到4-6mol/l的盐酸溶液中,搅拌均匀形成混合溶液,再将纳米二氧化硅、蒙脱土加到混合溶液中超声分散30-50分钟,再加入对甲苯磺酸质量0.5-2倍的苯胺单体,冰水浴下搅拌1-2小时形成均匀乳液,再将过硫酸铵缓慢滴加到乳液中,继续搅拌反应3-4小时,减压抽滤,固体沉淀依次用去离子水和对甲苯磺酸洗涤成中性,80-90°C下真空干燥8-12小时,即可得到聚苯胺复合材料。
本发明所述一种高导电秸秆基活性炭复合电极材料,由以下具体的步骤制成:
(1)将秸秆清洗干净后烘干,水分控制在20-25%左右,隔绝空气经过6-8小时常温物理炭化堆积得到生物质炭,再将该生物质炭粉碎成颗粒,加到沸腾炉中,通入预先预热至300-400°C的水蒸气和二氧化碳混合气体,在800-1000°C下进行氧化反应1-2小时,取出后加到熔融的无水氢氧化钾中,得到高比表面积活性炭备用;
(2)将正硅酸乙酯加到乙醇的水溶液中,搅拌溶解后加入步骤(1)的产物和除锌合金外的其他剩余成分,在80-100°C下加热搅拌,干燥后通入纯氨气,于500-600°C下保温50-100分钟,然后迅速冷却至室温粉碎至200-400目粉末备用;
(3)将锌合金加热至熔融状态与步骤(2)的产物混合均匀即可。
本发明的优点是:本发明的聚苯胺复合材料具有价格便宜、电荷密度高等的优点,添加到电极材料中能够提高导电性和储电性能;添加的聚吡咯由于具有较好的导电性、光电性、热电性可在常温或低温下使用,较易沉积在各种基片上,并且成本较低、容易制备,在一定程度上提高了电容器的导电性能。
具体实施方案
下面通过具体实例对本发明进行详细说明。
一种高导电秸秆基活性炭复合电极材料,由下列重量份(公斤)的原料制成:氯化钾1、聚吡咯2、正硅酸乙酯2、氯金酸0.7、锌合金5、二茂钴1、乙酰丙酮钯2、聚苯胺复合材料4、秸秆1200、无水氢氧化钾4、去离子水10;
所述聚苯胺复合材料是由下列重量份(公斤)的原料制成:对甲苯磺酸5、盐酸7、纳米二氧化硅5、蒙脱土3、苯胺10、过硫酸铵0.4、去离子水35;制备方法是将对甲苯磺酸加到4-6mol/l的盐酸溶液中,搅拌均匀形成混合溶液,再将纳米二氧化硅、蒙脱土加到混合溶液中超声分散30-50分钟,再加入对甲苯磺酸质量0.5-2倍的苯胺单体,冰水浴下搅拌1-2小时形成均匀乳液,再将过硫酸铵缓慢滴加到乳液中,继续搅拌反应3-4小时,减压抽滤,固体沉淀依次用去离子水和对甲苯磺酸洗涤成中性,80-90°C下真空干燥8-12小时,即可得到聚苯胺复合材料。
本发明所述一种高导电秸秆基活性炭复合电极材料,由以下具体的步骤制成:
(1)将秸秆清洗干净后烘干,水分控制在20-25%左右,隔绝空气经过6-8小时常温物理炭化堆积得到生物质炭,再将该生物质炭粉碎成颗粒,加到沸腾炉中,通入预先预热至300-400°C的水蒸气和二氧化碳混合气体,在800-1000°C下进行氧化反应1-2小时,取出后加到熔融的无水氢氧化钾中,得到高比表面积活性炭备用;
(2)将正硅酸乙酯加到乙醇的水溶液中,搅拌溶解后加入步骤(1)的产物和除锌合金外的其他剩余成分,在80-100°C下加热搅拌,干燥后通入纯氨气,于500-600°C下保温50-100分钟,然后迅速冷却至室温粉碎至200-400目粉末备用;
(3)将锌合金加热至熔融状态与步骤(2)的产物混合均匀即可。
将电极材料和导电剂、粘结剂按照比例混合均匀,通过压辊机制成薄片,干燥后压在不锈钢网集流体上,制成超级电容器,其参比电极为Ag/AgCl电极,电解液为1mol/l的硫酸溶液,在-0.2V至0.8V的电压范围内进行恒流充放电测试,电流为0.2A/g时,比电容为273F/g,电流为10A/g时,比电容为171F/g。
Claims (2)
1.一种高导电秸秆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:氯化钾1-2、聚吡咯2-3、正硅酸乙酯1-3、氯金酸0.5-1、锌合金3-5、二茂钴1-2、乙酰丙酮钯1-3、聚苯胺复合材料3-5、秸秆1000-1200、无水氢氧化钾3-5、去离子水5-10;
所述聚苯胺复合材料是由下列重量份的原料制成:对甲苯磺酸4-6、盐酸6-8、纳米二氧化硅3-5、蒙脱土2-4、苯胺8-12、过硫酸铵0.4-0.7、去离子水30-50;制备方法是将对甲苯磺酸加到4-6mol/l的盐酸溶液中,搅拌均匀形成混合溶液,再将纳米二氧化硅、蒙脱土加到混合溶液中超声分散30-50分钟,再加入对甲苯磺酸质量0.5-2倍的苯胺单体,冰水浴下搅拌1-2小时形成均匀乳液,再将过硫酸铵缓慢滴加到乳液中,继续搅拌反应3-4小时,减压抽滤,固体沉淀依次用去离子水和对甲苯磺酸洗涤成中性,80-90°C下真空干燥8-12小时,即可得到聚苯胺复合材料。
2.根据权利要求1所述一种高导电秸秆基活性炭复合电极材料,其特征在于,由以下具体的步骤制成:
(1)将秸秆清洗干净后烘干,水分控制在20-25%左右,隔绝空气经过6-8小时常温物理炭化堆积得到生物质炭,再将该生物质炭粉碎成颗粒,加到沸腾炉中,通入预先预热至300-400°C的水蒸气和二氧化碳混合气体,在800-1000°C下进行氧化反应1-2小时,取出后加到熔融的无水氢氧化钾中,得到高比表面积活性炭备用;
(2)将正硅酸乙酯加到乙醇的水溶液中,搅拌溶解后加入步骤(1)的产物和除锌合金外的其他剩余成分,在80-100°C下加热搅拌,干燥后通入纯氨气,于500-600°C下保温50-100分钟,然后迅速冷却至室温粉碎至200-400目粉末备用;
(3)将锌合金加热至熔融状态与步骤(2)的产物混合均匀即可。
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