CN109233275A - 一种高电导率聚吡咯凝胶及其制备方法 - Google Patents

一种高电导率聚吡咯凝胶及其制备方法 Download PDF

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CN109233275A
CN109233275A CN201811158484.7A CN201811158484A CN109233275A CN 109233275 A CN109233275 A CN 109233275A CN 201811158484 A CN201811158484 A CN 201811158484A CN 109233275 A CN109233275 A CN 109233275A
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夏友谊
吴玉真
王蒋超
刘宁
胡建
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Abstract

本发明提供了一种高电导率聚吡咯凝胶及其制备方法，属于导电高分子材料技术领域。本发明制备的高电导率聚吡咯凝胶，是由聚吡咯纳米粒子经线性组装、连接而成的多孔结构材料。其具体制备过程是：室温下，将紫红色铝试剂水溶液和吡咯单体按一定体积比混合、超声，得到A溶液。而后，将含三价铁离子水溶液一次性加至A溶液，室温下反应，经大量蒸馏水浸泡，得到聚吡咯凝胶。将此凝胶于‑20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。本发明所获得的聚吡咯凝胶导电性能优良，电导率高达8.7～11S/cm,有望作为新材料在超级电容器、电磁屏蔽、电催化等领域实际应用。此外，本发明制备过程方便、工艺简单、适合于规模化生产。

Description

一种高电导率聚吡咯凝胶及其制备方法
技术领域
本发明属于导电高分子材料技术领域，具体涉及一种高电导率聚吡咯凝胶及其制备方法。
背景技术
聚吡咯作为导电聚合物家族成员之一，具合成方便、稳定性佳的优势，并具有高电化学活性。由于上述优势，因此聚吡咯在化学、化工、新材料等领域有着良好的应用前景。典型的如，可作为超级电容器电极材料、防静电材料、电磁屏蔽材料、电催化材料等(李梅等，一种二硫化钼/聚吡咯超级电容器电极材料的制备方法和应用，申请号：CN201610417561.0)。因此，自聚吡咯被成功合成以来，有关聚吡咯的研究一直方兴未艾。
利用合适的化学氧化聚合方法，将聚吡咯形成凝胶状态的多孔结构，丰富了其比表面积，有助于提升其性能，如可获得高容量的超级电容特性(Yaqun Wang et al,Dopant-Enabled Supramolecular Approach for Controlled Synthesis of NanostructuredConductive Polymer Hydrogels,Nano Lett.2015,15,7736-7741)。近年来，聚吡咯凝胶的研究、开发非常活跃。然而，由于凝胶的天然多孔结构和属性，致使其密度较小，故目前聚吡咯凝胶材料普遍存在电导率较低的缺陷，因而较大程度限制了聚吡咯凝胶材料在多个方面，尤其是超级电容器用电活性电极材料领域的应用(樊新等，聚吡咯/氢氧化镍超级电容器复合电极材料的制备方法，申请号CN201711413852.3)。为此，开发高电导率聚吡咯凝胶材料成为亟待的一个重要问题。
发明内容
针对现有技术存在的以上问题，本发明提供了一种高电导率聚吡咯凝胶及其制备方法。
本发明提供的一种高电导率聚吡咯凝胶，是由聚吡咯纳米粒子(100～200nm)经线性组装、连接而成的多孔结构材料，电导率为8.7～11S/cm。
本发明同时提供了上述聚吡咯凝胶的制备方法，其具体步骤为：
a)室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比1～10:1混合，超声5min,得到粉红色A溶液。所述铝试剂的分子式是C22H23N3O9，化学结构式如下：
b)按一定体积比，将含三价铁离子水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述三价铁离子水溶液为三氯化铁、硫酸铁或硝酸铁中的一种或它们的混合物，所述三价铁离子水溶液中三价铁离子的摩尔浓度为0.1～1M，所述三价铁离子水溶液和A溶液的体积比为1～10:1。
与现有技术相比，本发明具有以下技术效果：
1、本发明的聚吡咯凝胶合成过程中，引入了铝试剂这类多羧基共轭小分子，通过该特殊小分子的掺杂，桥连了聚吡咯大分子链，有助于电子在不同聚吡咯链上的迁移，因此所获得的聚吡咯凝胶导电性能优良，电导率高达8.7～11S/cm。故该凝胶材料作为超级电容器电极材料使用时电容性能良好，质量比电容可达420～506F/g(三电极测试体系，电流密度0.25A/g)；
2、本发明的聚吡咯凝胶制备过程方便、工艺简单、适合于规模化生产，可作为新材料在超级电容器、电磁屏蔽、电催化等领域实际应用。
附图说明
图1为按照实施例1的操作步骤，分别选择圆盘状、长条状反应器皿所制备的圆盘状和长条状的聚吡咯凝胶数码照片；
如图1表明，聚吡咯凝胶可呈不同的形状，因此可根据具体的要求，选择不同形状的反应器皿，调控聚吡咯凝胶的形状。
图2为按照实施例1制备的聚吡咯凝胶的扫描电子显微电镜图片；
如图2表明，本发明的聚吡咯凝胶由聚吡咯纳米粒子(100～200nm)经线性组装、连接而成的多孔结构。
具体实施方式
以下结合具体实施例详述本发明，但本发明不局限于下述实施例。
实施例1
室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比1:1混合，超声5min,得到粉红色A溶液。按一定体积比，将三氯化铁水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述三氯化铁水溶液中三价铁离子的摩尔浓度为0.1M，所述三氯化铁水溶液和A溶液的体积比为1:1。
所得聚吡咯凝胶导电性能优良，电导率高达8.7S/cm，作为超级电容器性能优良，质量比电容可达420F/g(三电极测试体系，电流密度0.25A/g)。
实施例2
室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比10:1混合，超声5min,得到粉红色A溶液。按一定体积比，将硫酸铁水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述硫酸铁水溶液中三价铁离子的摩尔浓度为1M，所述硫酸铁水溶液和A溶液的体积比为10:1。
所得聚吡咯凝胶导电性能优良，电导率高达11S/cm，作为超级电容器性能优良，质量比电容可达506F/g(三电极测试体系，电流密度0.25A/g)。
实施例3
室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比3:1混合，超声5min,得到粉红色A溶液。按一定体积比，将硝酸铁水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述硝酸铁水溶液中三价铁离子的摩尔浓度为0.3M，所述硝酸铁水溶液和A溶液的体积比为3:1。
所得聚吡咯凝胶导电性能优良，电导率高达9.2S/cm，作为超级电容器性能优良，质量比电容可达440F/g(三电极测试体系，电流密度0.25A/g)。
实施例4
室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比5:1混合，超声5min,得到粉红色A溶液。按一定体积比，将含三价铁离子水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述三价铁离子水溶液中三价铁离子的摩尔浓度为0.5M，所述三价铁离子水溶液和A溶液的体积比为6:1。
所述三价铁离子水溶液为三氯化铁、硫酸铁和硝酸铁的混合水溶液，且该混合水溶液中三氯化铁、硫酸铁和硝酸铁三者物质的量比为1:1:1。
所得聚吡咯凝胶导电性能优良，电导率高达10.1S/cm，作为超级电容器性能优良，质量比电容可达460F/g(三电极测试体系，电流密度0.25A/g)。
实施例5
室温下，将紫红色铝试剂水溶液(摩尔浓度为10mM)和吡咯单体按体积比9:1混合，超声5min,得到粉红色A溶液。按一定体积比，将含三价铁离子水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯水凝胶。将此水凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶。所述三价铁离子水溶液中三价铁离子的摩尔浓度为8M，所述三价铁离子水溶液和A溶液的体积比为9:1。
所述三价铁离子水溶液为三氯化铁和硝酸铁的混合水溶液，且该混合水溶液中三氯化铁和硝酸铁二者物质的量比为1:2。
所得聚吡咯凝胶导电性能优良，电导率高达10.8S/cm，作为超级电容器性能优良，质量比电容可达490F/g(三电极测试体系，电流密度0.25A/g)。

Claims (2)

1.一种高电导率聚吡咯凝胶，其特征在于，该聚吡咯凝胶是由100～200nm聚吡咯纳米粒子经线性组装、连接而成的多孔结构材料，该聚吡咯凝胶的电导率为8.7～11S/cm。
2.如权利要求1所述高电导率聚吡咯凝胶的制备方法，其特征在于包括如下步骤：
(1)室温下，将摩尔浓度为10mM的铝试剂水溶液和吡咯单体按体积比1～10:1混合，超声5min,得到A溶液；所述铝试剂的分子式是C22H23N3O9，化学结构式如下：
(2)将含三价铁离子水溶液一次性加至A溶液，室温下反应30min后，经大量蒸馏水浸泡12h，得到聚吡咯凝胶；将此凝胶于-20℃冷冻干燥2h后即可得高电导率聚吡咯凝胶；
所述三价铁离子水溶液为三氯化铁、硫酸铁或硝酸铁中的一种或多种，所述三价铁离子水溶液中三价铁离子的摩尔浓度为0.1～1M，所述三价铁离子水溶液和A溶液的体积比为1～10:1。
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