CN106531462A - 一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料 - Google Patents
一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料 Download PDFInfo
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Abstract
本发明公开了一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,由下列重量份的原料制成:活性炭5‑6、浓度为2wt%的硝酸铜溶液30‑35、吡咯80‑85、壳聚糖10‑12、浓度为2wt%的乙酸溶液100‑110、十二烷基苯磺酸钠2‑3、氯化铁3‑4、1mol/L的盐酸适量、1mol/L的氢氧化钠适量、去离子水适量、石墨烯0.2‑0.25、硝酸铁4‑4.2、硝酸锂6‑7、磷酸二氢铵1.2‑1.4、柠檬酸1.9‑2、葡萄糖0.5‑0.6、无水乙醇适量。本发明制成的电极材料具有较快的电子与离子传输速率,电化学性能优异,制成的超级电容器放电比电容大,循环稳定性佳。
Description
技术领域
本发明涉及超级电容器技术领域,尤其涉及一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料。
背景技术
超级电容器是一种介于电池与传统电容器之间的新型储能器件,兼具两者的优点,具有功率密度高、能量密度高、充电时间短、使用寿命长和对环境无污染等优点。作为一种绿色环保、性能优异的新型储能器件,超级电容器在国防、军工、电动汽车、电脑、移动通信等众多领域有着广泛应用。导电聚合物因其成本低而备受关注,具有较大比表面积的导电聚合物被认为是超级电容器的理想电极材料,适用于此类电容器的导电聚合物有: 聚吡咯、聚苯胺、聚噻吩及其衍生物。在众多导电聚合物中,聚吡咯因其高的电导率、有趣的氧化还原性能、环境稳定性以及可通过化学或电化学方法易于制备等优点成为近年来的研究热点。
《片状聚吡咯/氧化石墨烯复合材料的制备及电化学性能》一文中通过原位聚合在低温条件下制备具有片状微结构的聚吡咯/氧化石墨烯复合材料,通过电化学分析,与纯聚吡咯及氧化石墨烯相比,复合材料显示出优越的电容特性。但是本文确是以 PTFE 为黏结剂制备片状电极材料,虽然增加了电极材料的机械强度,但是由于黏结剂的添加使电极的电阻增大,电导率降低,电极成分复杂,不利于电极材料的稳定性,这就需要对电极材料的成型方法以及如何提高了电极材料的增和性能进行进一步研究。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料。
本发明是通过以下技术方案实现的:
一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,由下列重量份的原料制成:活性炭5-6、浓度为2wt%的硝酸铜溶液30-35、吡咯80-85、壳聚糖10-12、浓度为2wt%的乙酸溶液100-110、十二烷基苯磺酸钠2-3、氯化铁3-4、1mol/L的盐酸适量、1mol/L的氢氧化钠适量、去离子水适量、石墨烯0.2-0.25、硝酸铁4-4.2、硝酸锂6-7、磷酸二氢铵1.2-1.4、柠檬酸1.9-2、葡萄糖0.5-0.6、无水乙醇适量。
根据权利要求书1所述一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,由下列具体方法制备而成:
(1)将活性炭置于浓度为2wt%的硝酸铜溶液中,磁力搅拌器搅拌24小时后过滤,烘干,然后在炭化炉中氮气保护下以10-15℃/min的升温速率升温至200℃,恒温100-120分钟后出料,粉碎后得到改性活性炭待用;
(2)将壳聚糖均匀的搅拌分散到浓度为2wt%的乙酸溶液中,加入十二烷基苯磺酸钠,搅拌反应40-60分钟后加入1mol/L的盐酸调节溶液pH为4,将氯化铁溶于50-60倍量的去离子水中,搅拌均匀后加入吡咯、步骤(1)得到的改性活性炭,室温下搅拌反应60-90分钟后静置,加入1mol/L的氢氧化钠调节溶液为中性,最后真空抽滤,将得到的滤饼用去离子水洗涤2-3次后置于真空干燥箱中干燥,得到壳聚糖聚吡咯炭复合材料;
(3)将硝酸铁、硝酸锂混合,溶于总量3-4倍量的去离子水中,然后依次加入磷酸二氢铵、柠檬酸,以300-400转/份的速度搅拌30-40分钟后加入葡萄糖,搅拌均匀后水浴加热至80-85℃,继续搅拌90-120分钟,静置40-60分钟待用;将石墨烯分散于5-7倍量的无水乙醇中形成分散液,然后与上述混合液混合,以800-1000转/份的速度搅拌20-30分钟后在120-130℃下干燥2-3小时,再将得到的固体放置在管式炉中,氮气保护下,650-700℃下烧结6-7小时,自然冷却后取出,粉碎,过200目筛;
(4)将步骤(2)步骤(3)得到的产物放入研钵中,研磨至物料混合均匀,然后倒入模具中,加热至150-160℃,将模具放置在电动压片机上,在10MPa的压力下热压20-30分钟,待磨具冷却到常温后进行脱模,最后用砂纸将得到的电极材料表面打磨光滑即可。
本发明的优点是:本发明首先利用硝酸铜对活性炭进行浸渍改性,提高了活性炭的中孔率,表面负载少量的氧化铜,在电容器充放电过程中产生赝电容效应,增强了电容器的比电容,同时可以提高电解液的浸润性;然后通过一定的工艺将改性后活性炭与壳聚糖、吡咯等聚合成复合材料,最后通过热压成型制成复合电极材料,制成的电极材料不添加粘结剂,阻抗小,电极溶胀性以及亲水性佳,比表面积大,电化学性能优异。
本发明还通过一系列的反应制成磷酸铁锂与石墨烯的复合材料,相容性好,形成了具有三维空间结构的立体导电网络,有利于提高电导率,从而提高了电化学性能;本发明制成的电极材料具有较快的电子与离子传输速率,电化学性能优异,制成的超级电容器放电比电容大,循环稳定性佳。
具体实施方式
一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,由下列重量份(公斤)的原料制成:活性炭5、浓度为2wt%的硝酸铜溶液30、吡咯80、壳聚糖10、浓度为2wt%的乙酸溶液100、十二烷基苯磺酸钠2、氯化铁3、1mol/L的盐酸适量、1mol/L的氢氧化钠适量、去离子水适量、石墨烯0.2、硝酸铁4、硝酸锂6、磷酸二氢铵1.2、柠檬酸1.9、葡萄糖0.5、无水乙醇适量。
根据权利要求书1所述一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,由下列具体方法制备而成:
(1)将活性炭置于浓度为2wt%的硝酸铜溶液中,磁力搅拌器搅拌24小时后过滤,烘干,然后在炭化炉中氮气保护下以10℃/min的升温速率升温至200℃,恒温100分钟后出料,粉碎后得到改性活性炭待用;
(2)将壳聚糖均匀的搅拌分散到浓度为2wt%的乙酸溶液中,加入十二烷基苯磺酸钠,搅拌反应40分钟后加入1mol/L的盐酸调节溶液pH为4,将氯化铁溶于50倍量的去离子水中,搅拌均匀后加入吡咯、步骤(1)得到的改性活性炭,室温下搅拌反应60分钟后静置,加入1mol/L的氢氧化钠调节溶液为中性,最后真空抽滤,将得到的滤饼用去离子水洗涤2次后置于真空干燥箱中干燥,得到壳聚糖聚吡咯炭复合材料;
(3)将硝酸铁、硝酸锂混合,溶于总量3倍量的去离子水中,然后依次加入磷酸二氢铵、柠檬酸,以300转/份的速度搅拌30分钟后加入葡萄糖,搅拌均匀后水浴加热至80℃,继续搅拌90分钟,静置40分钟待用;将石墨烯分散于5倍量的无水乙醇中形成分散液,然后与上述混合液混合,以800转/份的速度搅拌20分钟后在120℃下干燥2小时,再将得到的固体放置在管式炉中,氮气保护下,650℃下烧结6小时,自然冷却后取出,粉碎,过200目筛;
(4)将步骤(2)步骤(3)得到的产物放入研钵中,研磨至物料混合均匀,然后倒入模具中,加热至150℃,将模具放置在电动压片机上,在10MPa的压力下热压20分钟,待磨具冷却到常温后进行脱模,最后用砂纸将得到的电极材料表面打磨光滑即可。
对本实施例电极材料制成的超级电容器进行循环伏安曲线测试,结果显示放电比电容为372F/g,在400次循环充放电测试后比电容仍能保持大于90%。
Claims (2)
1.一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,其特征在于,由下列重量份的原料制成:活性炭5-6、浓度为2wt%的硝酸铜溶液30-35、吡咯80-85、壳聚糖10-12、浓度为2wt%的乙酸溶液100-110、十二烷基苯磺酸钠2-3、氯化铁3-4、1mol/L的盐酸适量、1mol/L的氢氧化钠适量、去离子水适量、石墨烯0.2-0.25、硝酸铁4-4.2、硝酸锂6-7、磷酸二氢铵1.2-1.4、柠檬酸1.9-2、葡萄糖0.5-0.6、无水乙醇适量。
2.根据权利要求书1所述一种添加磷酸铁锂石墨烯复合材料的聚吡咯炭电极材料,其特征在于,由下列具体方法制备而成:
(1)将活性炭置于浓度为2wt%的硝酸铜溶液中,磁力搅拌器搅拌24小时后过滤,烘干,然后在炭化炉中氮气保护下以10-15℃/min的升温速率升温至200℃,恒温100-120分钟后出料,粉碎后得到改性活性炭待用;
(2)将壳聚糖均匀的搅拌分散到浓度为2wt%的乙酸溶液中,加入十二烷基苯磺酸钠,搅拌反应40-60分钟后加入1mol/L的盐酸调节溶液pH为4,将氯化铁溶于50-60倍量的去离子水中,搅拌均匀后加入吡咯、步骤(1)得到的改性活性炭,室温下搅拌反应60-90分钟后静置,加入1mol/L的氢氧化钠调节溶液为中性,最后真空抽滤,将得到的滤饼用去离子水洗涤2-3次后置于真空干燥箱中干燥,得到壳聚糖聚吡咯炭复合材料;
(3)将硝酸铁、硝酸锂混合,溶于总量3-4倍量的去离子水中,然后依次加入磷酸二氢铵、柠檬酸,以300-400转/份的速度搅拌30-40分钟后加入葡萄糖,搅拌均匀后水浴加热至80-85℃,继续搅拌90-120分钟,静置40-60分钟待用;将石墨烯分散于5-7倍量的无水乙醇中形成分散液,然后与上述混合液混合,以800-1000转/份的速度搅拌20-30分钟后在120-130℃下干燥2-3小时,再将得到的固体放置在管式炉中,氮气保护下,650-700℃下烧结6-7小时,自然冷却后取出,粉碎,过200目筛;
(4)将步骤(2)步骤(3)得到的产物放入研钵中,研磨至物料混合均匀,然后倒入模具中,加热至150-160℃,将模具放置在电动压片机上,在10MPa的压力下热压20-30分钟,待磨具冷却到常温后进行脱模,最后用砂纸将得到的电极材料表面打磨光滑即可。
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