CN105885076B - 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 PDFInfo
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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
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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