CN107190366A - 超级电容器用氮掺杂多孔碳纤维的制备方法 - Google Patents
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Abstract
本发明公开了一种以棉花为碳源制备机械性能良好的超级电容器用氮掺杂多孔碳纤维的新方法。具体涉及一种以棉花为原料，通过碳化、氮源的引入，结合化学活化法制备机械性能良好的超级电容器用多孔碳纤维的新方法。本发明包括具体步骤如下：首先将棉花高温碳化为纤维，将碳纤维与活化试剂、氮源按一定质量比混合，再向其中加入适量蒸馏水浸渍一定时间后烘干，而后在管式炉中活化处理一定时间，固体洗涤、干燥，得到超级电容器用氮掺杂多孔碳纤维。
Description
技术领域
本发明涉及一种超级电容器用氮掺杂多孔碳纤维的制备方法，具体涉及一种首先将棉花碳化制备碳纤维，再将其与氮源、活化试剂混合，高温活化制备超级电容器用氮掺杂多孔碳纤维的新方法。
背景技术
超级电容器由于具有充放电速率快、高能力密度和功率密度、优异的循环稳定性以及高稳定性而成为科研工作者们广泛关注的储能设备。根据能源储存机理不同超级电容器可分为双电层和赝电容两种电容器，电极材料是决定超级电容器性能的关键因素之一。多孔碳由于具有大的比表面积，稳定的化学性质，大的孔体积、连通且均一的孔道、可调的孔径等诸多优点而成为具有应用前景的超级电容器电极材料。目前，应用于超级电容器的多孔碳材料有很多种，如球形碳，颗粒状碳，纤维状碳等。其中，多孔碳纤维质量轻，拉伸强度和热稳定性优异，其表面分布着丰富的孔隙结构，可增大其与电解质的接触面积，缩短了离子传输路径。提高储能效率，这些性质促进了多孔碳纤维被广泛研究。
目前，制备碳纤维的前驱体主要有沥青、聚丙烯腈、苯酚树脂等，其都是从煤和石油中提取出来的，属于不可再生资源。专利CN106521717A公开了一种高比表面积多孔碳纤维的制备方法，步骤如下：将聚丙烯腈、造孔剂(二氧化硅)和N，N一二甲基甲酞胺的纺丝液进行静电纺丝后碳化，经过热碱洗、干燥后得到高比表面多孔碳纤维。专利CN103806129A公开了一种氮掺杂多孔碳纤维材料及其制备方法与应用，其步骤如下：(1)将氮源和碳源溶解于水中，经静置沉淀、过滤得到所述氮源与所述碳源结合的前驱物；所述氮源为三聚氰胺和/或三聚氰酸；所述碳源为有机酸和/或有机胺；(2)将所述前驱物置于管式炉中进行锻烧得到多孔碳纤维，其具有高的比表面积和好的电化学性能。专利CN103225135A公开了一种多孔碳纤维及其制备方法。其步骤如下：将由造孔剂(碳酸钙)、高分子聚合物(聚丙烯睛、聚酞亚胺、沥青、聚乙烯醇、聚乙烯毗咯烷酮和酚醛树脂中的至少一种)和有机溶剂(N，N一二甲基甲酞胺、N一甲基毗咯烷酮和二甲基亚矾中的至少一种)组成的纺丝液进行纺丝后碳化酸洗，得到所述多孔碳纤维。专利CN105671692A公开了一种密胺树脂改性的富氮多孔碳纤维电极材料的制备方法。其是用三聚氰胺和甲醛合成密胺树脂；将聚丙烯睛溶解于N，N一二甲基甲酞胺中，再加入密胺树脂配制成纺丝液；通过静电纺丝制得MF/PAN复合纤维原丝；将MF/PAN复合纤维进行预氧化、碳化等热处理得到富氮碳纤维；将NCNF制成超级电容器电极，具有较好性能。
以上专利均以不可再生资源为前驱体制备多孔碳纤维，其成本较高，不利于可持续发展。因此以可再生的生物质为原料制备多孔碳纤维具有重要的研究意义。棉花是一种天然的具有纤维结构的生物质资源，碳化后仍能保持纤维结构，同时具有良好的机械性能。因此，以棉花为原料，通过碳化、活化、氮掺杂的方式制备具有高比表面积、含一定氮官能团、良好机械性能的超级电容器电极材料具有一定研究价值。
本专利是以棉花为原料，将其碳化为纤维，再通过氮源的引入，结合化学活化制备机械性能良好的超级电容器用氮掺杂多孔碳纤维。本路线原料来源广泛、合成方法简便，通过调节活化试剂和氮源的加入量控制多孔碳纤维的孔隙发达程度和氮官能团的掺杂量，最终制备机械性能良好的超级电容器用氮掺杂多孔碳纤维。
发明内容
本发明目的是提供一种以棉花为碳源制备机械性能良好的超级电容器用氮掺杂多孔碳纤维的新方法。
本发明首先将棉花高温碳化为纤维，将碳纤维与活化试剂、氮源按质量比1∶3∶2～1∶6∶5(g/g/g)混合，向其中加入适量蒸馏水混合均匀，将混合物浸渍14h后在110℃烘箱中干燥6h，将混合物在700～1000℃管式炉中活化处理0.5～2h，固体洗涤、干燥，得到的氮掺杂多孔碳纤维进行电化学性能测试。
本发明的特征在于：所述活化剂为碳酸氢钾和氢氧化钾的混合物或碳酸氢钾和氢氧化钠的混合物。
本发明的特征在于：所述氮源为尿素或三聚氰胺。
具体实施方式
实施例1：首先将棉花在管式炉中800℃下碳化1h，将得到的碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、尿素按质量比1∶4∶2(g/g/g)混合，向其中加入适量蒸馏水混合均匀，将混合物浸渍14h后在110℃烘箱中干燥6h，将混合物在800℃管式炉中活化处理1h，固体洗涤、干燥，得到的氮掺杂多孔碳纤维进行电化学性能测试，以6mol/L的氢氧化钾为电解液，测得比容量为306F/g，循环5000次容量保持率为96％左右。
实施例2：改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、尿素的质量比1∶5∶2(g/g/g)，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为334F/g，循环5000次容量保持率为97％左右。
实施例3：改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶2)、尿素的质量比1∶6∶3(g/g/g)，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为313F/g，循环5000次容量保持率为97％左右。
实施例4：改变碳纤维与活化试剂(KHCO3∶NaOH的质量比为1∶3)、尿素的质量比1∶5∶2(g/g/g)，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为320F/g，循环5000次容量保持率为97％左右。
实施例5：改变碳纤维与活化试剂(KHCO3∶NaOH的质量比为1∶3)、尿素的质量比1∶6∶2(g/g/g)，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为302F/g，循环5000次容量保持率为96％左右。
实施例6：改变碳纤维与活化试剂(KHCO3∶NaOH的质量比为1∶3)、三聚氰胺的质量比1∶5∶2(g/g/g)，将混合物在900℃管式炉中活化处理1h，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为298F/g，循环5000次容量保持率为97％左右。
实施例7：改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶3)、三聚氰胺的质量比1∶5∶2(g/g/g)，将混合物在800℃管式炉中活化处理2h，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为315F/g，循环5000次容量保持率为97％左右。
实施例8：改变碳纤维与活化试剂(KHCO3∶KOH的质量比为1∶3)、尿素的质量比1∶5∶3(g/g/g)，将混合物在800℃管式炉中活化处理1.5h，其他条件同实施例1，得到的氮掺杂多孔碳纤维的比电容为332F/g，循环5000次容量保持率为97％左右。
Claims (3)
1.一种超级电容器用氮掺杂多孔碳纤维的制备方法，其具体步骤如下：首先将棉花高温碳化为纤维，将碳纤维与活化试剂、氮源按质量比1∶3∶2～1∶6∶5(g/g/g)混合，向其中加入适量蒸馏水混合均匀，将混合物浸渍14h后在110℃烘箱中干燥6h，将混合物在700～1000℃管式炉中活化处理0.5～2h，固体洗涤、干燥，得到的氮掺杂多孔碳纤维进行电化学性能测试。
2.一种如权利要求1所述的氮掺杂多孔碳纤维的制备方法，其特征在于：所述活化剂为碳酸氢钾和氢氧化钾的混合物或碳酸氢钾和氢氧化钠的混合物。
3.一种如权利要求1所述的氮掺杂多孔碳纤维的制备方法，其特征在于：所述氮源为尿素或三聚氰胺。
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| CN111517306A (zh) * | 2020-04-29 | 2020-08-11 | 内蒙古民族大学 | 一种类石墨烯/生物质碳纤维气凝胶及其制备方法和应用 |
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| CN115467159A (zh) * | 2022-09-06 | 2022-12-13 | 昆明云大新能源有限公司 | 一种原位刻蚀氮掺杂改性碳布及其制备方法与应用 |
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