CN105885076A - 一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法 - Google Patents

一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法 Download PDF

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CN105885076A
CN105885076A CN201610144363.1A CN201610144363A CN105885076A CN 105885076 A CN105885076 A CN 105885076A CN 201610144363 A CN201610144363 A CN 201610144363A CN 105885076 A CN105885076 A CN 105885076A
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叶先龙
高力群
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Shenzhen Zhi-Shun Technology Co., Ltd.
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Abstract

本发明涉及一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法，属于导电复合材料技术领域。针对目前聚吡咯材料溶解性差，力学性能较低，无法满足现有生产的需求的问题，通过将微晶纤维素进行改性负载石墨烯材料，随后将纤维素复合石墨烯材料与聚吡咯热压复合，制备一种加工难度较小，力学性能较好的柔性导电材料，本发明通过将柔性材料与导电材料进行复合，大大改善其加工性能，同时其复合材料电导率可达0.35～0.45s/cm，通过微晶纤维素和吡咯进行复合制备，绿色安全，对环境无污染。

Description

一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法
技术领域
本发明涉及一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法，属于导电复合材料技术领域。
背景技术
导电高分子是目前广受关注的研究课题之一，纳米导电高分子具有电导率高，环境稳定性好，生物相容性好的特点，并且广泛的应用于电子工业、光学仪器、化学和电化学传感器、电致色变元件、致动器、场发射器件等领域。在所有导电高分子中，聚吡咯是研究最广泛的导电高分子，其合成简便，抗氧化性能良好，与其它导电高分子相比电导率较高、易成膜、柔软等优点而日益受到人们的关注。聚吡咯已被用于制作生物感应器、功能分子膜、二次电池和非线性光学装置等。 从纯聚合物、掺杂薄膜到双层膜复合材料和现在的纳米复合材料, 聚吡咯的热稳定性、机械延展性等均有了很大提高。
但是与大多数共辆导电高分子一样，聚吡咯难熔难溶，难溶于普通溶剂，导致其加工操作困难较大，无法完全对其保证进行有效的加工和处理，所以需要一种较为柔性的导电材料，在不损害其电化学性能的同时，使其加工操作的难度大大降低。
发明内容
本发明所要解决的技术问题：针对目前聚吡咯材料溶解性差，力学性能较低，无法满足现有生产的需求的问题，提供了一种通过将微晶纤维素进行改性负载石墨烯材料，随后将纤维素复合石墨烯材料与聚吡咯热压复合，制备一种加工难度较小，力学性能较好的柔性导电材料，导电性能较好，且加工制作十分方便。
为解决上述技术问题，本发明采用如下所述的技术方案是：
（1）按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在200～300W下超声分散10～15min，制备得石墨烯分散液备用；
（2）称取55～60g微晶纤维素，将其置于100～200mL去离子水中，随后搅拌混合并超声分散20～30min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于50～60℃下干燥3～4h，待干燥完成后，将其置于30MPa下额的均质机中均质处理50～60min；
（3）待均质处理完成后，量取8～10mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置10～15min后，将步骤（1）制备的石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在80～85℃下热压20～24h，制备得微晶纤维素柔性薄膜；
（4）将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加200～250mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加20～25mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；
（5）待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理25～30min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在200～300W超声振荡清洗5～10min，并置于40～50℃下真空干燥6～8h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
本发明的应用方法：按重量份数计，分别称取75～85份将上述制备的高柔性导电复合材料、10～15份炭黑粉末和5～10份聚偏氟乙烯，搅拌混合制备得混合电极材料，随后按固液质量比50:1，将二甲基甲酰胺滴加至混合电极材料中，并将其置于玛瑙研钵中碾磨混合10～15min，随后均匀涂覆置1cm2的镍片表面，在1～2MPa下压制1～2min后，将其置于65～70℃下干燥6～8h，即可制备得电池电极。
本发明与其他方法相比，有益技术效果是：
（1）本发明通过将柔性材料与导电材料进行复合，大大改善其加工性能，同时其复合材料电导率可达0.35～0.45s/cm；
（2）通过微晶纤维素和吡咯进行复合制备，绿色安全，对环境无污染。
具体实施方式
首先按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在200～300W下超声分散10～15min，制备得石墨烯分散液备用；称取55～60g微晶纤维素，将其置于100～200mL去离子水中，随后搅拌混合并超声分散20～30min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于50～60℃下干燥3～4h，待干燥完成后，将其置于30MPa下额的均质机中均质处理50～60min；待均质处理完成后，量取8～10mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置10～15min后，将步骤（1）制备的石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在80～85℃下热压20～24h，制备得微晶纤维素柔性薄膜；将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加200～250mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加20～25mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理25～30min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在200～300W超声振荡清洗5～10min，并置于40～50℃下真空干燥6～8h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
实例1
首先按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在200W下超声分散10min，制备得石墨烯分散液备用；称取55g微晶纤维素，将其置于100mL去离子水中，随后搅拌混合并超声分散20min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于50℃下干燥3h，待干燥完成后，将其置于30MPa下额的均质机中均质处理50min；待均质处理完成后，量取8mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置10min后，将石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在80℃下热压20h，制备得微晶纤维素柔性薄膜；将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加200mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加20mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理25min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在200W超声振荡清洗5min，并置于40℃下真空干燥6h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
按重量份数计，分别称取75份将上述制备的高柔性导电复合材料、15份炭黑粉末和10份聚偏氟乙烯，搅拌混合制备得混合电极材料，随后按固液质量比50:1，将二甲基甲酰胺滴加至混合电极材料中，并将其置于玛瑙研钵中碾磨混合10min，随后均匀涂覆置1cm2的镍片表面，在1MPa下压制1min后，将其置于65℃下干燥6h，即可制备得电池电极。
实例2
首先按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在250W下超声分散12min，制备得石墨烯分散液备用；称取57g微晶纤维素，将其置于150mL去离子水中，随后搅拌混合并超声分散25min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于55℃下干燥4h，待干燥完成后，将其置于30MPa下额的均质机中均质处理55min；待均质处理完成后，量取9mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置12min后，将石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在82℃下热压22h，制备得微晶纤维素柔性薄膜；将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加225mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加22mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理27min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在250W超声振荡清洗8min，并置于45℃下真空干燥7h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
按重量份数计，分别称取80份将上述制备的高柔性导电复合材料、15份炭黑粉末和5份聚偏氟乙烯，搅拌混合制备得混合电极材料，随后按固液质量比50:1，将二甲基甲酰胺滴加至混合电极材料中，并将其置于玛瑙研钵中碾磨混合12min，随后均匀涂覆置1cm2的镍片表面，在2MPa下压制1min后，将其置于67℃下干燥7h，即可制备得电池电极。
实例3
首首先按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在300W下超声分散15min，制备得石墨烯分散液备用；称取60g微晶纤维素，将其置于200mL去离子水中，随后搅拌混合并超声分散30min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于60℃下干燥4h，待干燥完成后，将其置于30MPa下额的均质机中均质处理60min；待均质处理完成后，量取10mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置15min后，将石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在85℃下热压24h，制备得微晶纤维素柔性薄膜；将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加250mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加25mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理30min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在300W超声振荡清洗10min，并置于50℃下真空干燥8h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
按重量份数计，分别称取85份将上述制备的高柔性导电复合材料、10份炭黑粉末和5份聚偏氟乙烯，搅拌混合制备得混合电极材料，随后按固液质量比50:1，将二甲基甲酰胺滴加至混合电极材料中，并将其置于玛瑙研钵中碾磨混合15min，随后均匀涂覆置1cm2的镍片表面，在2MPa下压制2min后，将其置于70℃下干燥8h，即可制备得电池电极。

Claims (1)

1. 一种聚吡咯/微晶纤维素高柔性导电复合材料的制备方法，其特征在于具体制备步骤为：
（1）按体积比1:1，将1.2mL浓度为0.1mg/mL的石墨烯添加至浓度为0.02mol/L的十六烷基三甲基溴化铵中，在200～300W下超声分散10～15min，制备得石墨烯分散液备用；
（2）称取55～60g微晶纤维素，将其置于100～200mL去离子水中，随后搅拌混合并超声分散20～30min，待分散完成后，对其过滤并收集滤渣，用去离子水洗涤至pH至7.0后，将其置于50～60℃下干燥3～4h，待干燥完成后，将其置于30MPa下额的均质机中均质处理50～60min；
（3）待均质处理完成后，量取8～10mL均质悬浊液，将其置于索氏抽提器中抽滤成膜，带静置10～15min后，将步骤（1）制备的石墨烯分散液置于索氏抽提器中再次抽滤，随后收集复合薄膜，在80～85℃下热压20～24h，制备得微晶纤维素柔性薄膜；
（4）将上述制备的微晶纤维素柔性薄膜平铺至500mL烧杯中，随后添加200～250mL的吡咯单体，使其将纤维素膜完全淹没，同时滴加20～25mL质量浓度为10%的三氯化铁溶液，随后将烧杯置于紫外辐照箱中，调节紫外灯与烧杯间距为10cm；
（5）待调整灯距后，对辐照箱中通入氮气排除空气，随后打开紫外灯，对其辐照接枝改性处理25～30min，待接枝完成后，收集接枝完成的纤维素膜，将其置于质量分数为30%乙醇溶液中，在200～300W超声振荡清洗5～10min，并置于40～50℃下真空干燥6～8h，即可制备得一种聚吡咯/微晶纤维素高柔性导电复合材料。
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