CN106554509B - 一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法 - Google Patents

一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法 Download PDF

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CN106554509B
CN106554509B CN201611094454.5A CN201611094454A CN106554509B CN 106554509 B CN106554509 B CN 106554509B CN 201611094454 A CN201611094454 A CN 201611094454A CN 106554509 B CN106554509 B CN 106554509B
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ionic copolymer
preparation
quaternary
quaternary ionic
unit component
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CN106554509A (zh
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杨波
唐建国
王瑶
刘继宪
黄林军
王彦欣
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Qingdao University
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Abstract

本发明公开了一种四元离子共聚物‑无机复合仿生电驱动活性材料的制备方法，包括四元离子共聚物纳米乳液制备、四元离子共聚物乳胶膜制备、四元离子共聚物与无机导电填料复合电极层制备三个工艺步骤；四元离子共聚物纳米乳液制备是采用半连续乳液聚合工艺，首先对反应单体采取减压蒸馏处理去除阻聚剂并低温储存备用，然后实施聚合反应工艺制得四元离子共聚物纳米乳液；四元离子共聚物乳胶膜制备是在平底凹槽玻璃模具内常温常压环境下缓慢浇注聚合物纳米乳液得到四元离子共聚物乳胶膜；其制备原料常见易得、制备工艺简单环保，所制产品具有柔性韧性兼顾、仿生电驱动性能良好、生物相容性良好、制备成本低、应用前景广等特点。

Description

一种四元离子共聚物-无机复合仿生电驱动活性材料的制备 方法
技术领域
本发明涉及高分子无机复合材料制备技术领域，尤其涉及的是一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法。
背景技术
仿生电驱动活性材料(Bionic electric driving active materials,简称BEDAM)是根据仿生学原理模拟生物体组织细胞在生命活动过程中通过电位、极性的变化传递电信号实现基体组织神经传导、肌肉收缩等生命活动的智能材料，其能够在低压直流电场作用下实现类似生物体组织收缩、膨胀、弯曲等复杂形态变化，并广泛应用于人工器官、医疗器械、智能衣物、触摸传感器、仿生机器人等诸多领域。目前，BEDAM的基体材料主要选用离子型电致动聚合物(简称IEAP)，然后通过表面电极制备实现BEDAM组装。
IEAP是一类含有定量水分子和阴阳离子的高分子材料，具有质轻、柔性、工作电压低、形变性能好、生物相容性好、安全性高等诸多优势，其所含离子存在状态为金属阳离子能够以水合离子形式在高分子缝隙间自由移动，非金属阴离子刚性连接在高分子链上不可移动；当在IEAP上下表面覆盖电极层并施加直流电压后，IEAP基体内的水合阳离子在直流电场作用下定向移动到负极侧，与高分子链刚性连接的非金属阴离子尽管同样受到直流电场作用却难以向正极侧移动，这一差异使离子迁移过程产生失衡，大量水合阳离子集中在IEAP负极侧使其快速膨胀，IEAP正极侧因失去水合阳离子不断收缩，IEAP整体向正极侧弯曲形变；当改变直流电压方向，水合阳离子反方向移动，IEAP整体向反方向弯曲形变。
自科研工作者初次发现IEAP的低电压驱动形变特性以来，能够满足其电致形变特性的基体材料屈指可数，主要集中于以美国Nafion系列产品为代表的全氟代磺酸基阳离子交换膜。近年来，广大科研工作者针对全氟代磺酸基阳离子交换膜及其衍生产品的仿制研究开展了大量工作并取得了一定成果，但并未从根本上解决全氟代磺酸基阳离子交换膜生产工艺复杂、工艺污染物处理成本高等核心问题；产品价格的居高不下严重限制了IEAP和BEDAM的应用发展。
发明内容
本发明所要解决的技术问题是针对现有技术的不足提供一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法。
为实现上述目标，本发明的技术方案为：
一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法，包括四元离子共聚物纳米乳液制备、四元离子共聚物乳胶膜制备、四元离子共聚物与无机导电填料复合电极层制备三个工艺步骤；四元离子共聚物由四种组分组成，分别为：刚性结构单元组分、柔性结构单元组分、离子交换功能单元组分和缓冲增强功能单元组分；四元离子共聚物纳米乳液制备方法为：采用半连续乳液聚合工艺，首先对反应单体采取减压蒸馏处理去除阻聚剂并低温储存备用；提前配制质量分数为1-4％的过硫酸钾水溶液；按照工艺配方依次将磁子、乳化剂十二烷基硫酸钠、离子交换功能单元组分、缓冲增强功能单元组分、去离子水加入圆底烧瓶内，将刚性结构单元组分、柔性结构单元组分混合于恒压滴液漏斗中备用，向圆底烧瓶内充氮气15-60min确保无氧环境，同步打开恒温磁力搅拌器，温度设定45-70℃，转速设定300r/min；转速稳定后，将二分之一混合组分向圆底烧瓶中滴加，滴加速度1-3d/s，并开始计时，乳化0.5-1.5小时后，迅速升温至65-95℃；达到预设温度后，向圆底烧瓶中加入30-60％的引发剂水溶液，待无混合组分回流时，向圆底烧瓶中滴加剩余混合组分，滴加速度0.2-2d/s，并分1-3次加入剩余引发剂水溶液；混合组分滴加完毕后，保温反应0.5-3小时，室温冷却至45-55℃时过滤反应产物得到白色聚合物纳米乳液，最终降至室温密封保存；四元离子共聚物乳胶膜制备方法为：在常温常压环境下，向平底凹槽玻璃模具内缓慢浇注定量聚合物纳米乳液，可通过增减乳液体积将成膜厚度准确调控至0.1-4.0mm，并放置24-120小时，待乳液干透即可得四元离子共聚物乳胶膜；四元离子共聚物与无机导电填料复合电极层制备方法为：采用平面旋涂工艺涂抹含有无机导电填料的预制导电乳液在常温常压下干燥而成，以30-70％聚合物纳米乳液为胶黏剂，与40-80％无机导电填料混合，超声震荡15-30min得到预制导电乳液，平面旋涂于四元离子共聚物乳胶膜表面，室温干燥12-48小时可得一侧复合电极层，电极层厚度范围0.05-0.2μm；重复上述步骤完成另一侧复合电极层制备，可最终得到一种四元离子共聚物-无机复合仿生电驱动活性材料。
所述的制备方法，无机导电填料通常可选用碳纤维、碳纳米管、石墨烯、纳米金线、纳米银线、纳米钯线等，也可混合使用。
所述的制备方法，刚性结构单元组分选用甲基丙烯酸甲酯、苯乙烯及其衍生物和丙烯腈等单体，约占总单体的20-60mol％；柔性结构单元组分选用长链乙烯醚、丙烯酸酯类和对苯烷基乙烯基醚等单体，约占总单体的20-70mol％；离子交换功能单元组分通常含有碱金属阳离子、非金属阴离子以及不饱和双键等结构，属于同时包含有机、无机两相的表面活性物质，可选用烯烃基磺酸盐或苯乙烯磺酸盐等高电离度的有机磺酸盐，约占总单体量的5-40mol％；缓冲增强功能单元组分主要发挥有机、无机两相增容作用和吸水锁水能力分别提升材料力学性能和离子交换性能，通常选用结构与离子交换功能单元组分类似，低电离度的有机羧酸盐，该组分一方面自身存在电离水解平衡，能够最大限度锁住水分子提高离子传导能力，同时自身也具有离子传导能力，另一方面就整体而言其有机相比重更大，在离子聚合物体系内能够对有机磺酸盐结构起到过渡缓冲作用，缓冲增强功能单元组分可选用单体有丙烯酸及其衍生酸类、丙烯酸盐类及其衍生物羧酸盐类单体，约占总单体量的10-40mol％；同一工艺配方中，以上各单体用量之和为100％。
本发明制备的BEDAM，裁剪成1cm×5cm条形置于去离子水中浸泡活化2-12小时，经检测，在材料上下表面仅施加1-2v直流电压，条形材料能够像生物体组织一样产生弯曲形变，弯曲速度16-24°/s，最大弯曲角度40-120°；改变电压方向，条形材料产生反方向弯曲形变，抗疲劳强度(最高形变次数)11-20次。
本发明中缓冲增强功能单元组分的使用使材料抗疲劳强度(最高形变次数)显著提升，离子含量明显提高(Na+质量百分数范围增长至10％-20％)，含水率提高(以厚度1.5mm样品为例，含水率提升至18％)，响应形变速度大幅提高，驱动电压显著降低。
具体实施方式
以下结合具体实施例，对本发明进行详细说明。
实施例1
(1)实验准备工作：将刚性结构单元组分甲基丙烯酸甲酯、柔性结构单元组分丙烯酸正丁酯进行减压蒸馏提纯，分别量取20ml甲基丙烯酸甲酯和20ml丙烯酸正丁酯于恒压滴液漏斗内混合备用；室温配制质量分数为1％的过硫酸钾水溶液(引发剂)备用；
(2)甲基丙烯酸甲酯－丙烯酸正丁酯-丙烯酸钠－丙烯磺酸钠四元离子共聚物纳米乳液聚合：安装实验反应装置，分别取1.2g十二烷基苯磺酸钠、12ml丙烯酸钠、4g丙烯磺酸钠、50ml去离子水依次加入到圆底烧瓶内(250ml)，打开恒温磁力搅拌器，温度设定48℃，转速设为300r/min，同步向圆底烧瓶内充入氮气30min确保无氧环境；待转速稳定后，缓慢滴加二分之一事先装入恒压滴液漏斗内的混合单体，滴加速度2d/s，预乳化20min，快速升温至72℃，加入40％事先备好的引发剂水溶液；待圆底烧瓶内壁无单体回流时继续滴加剩余混合单体，滴加速度1d/s，并分3次加入剩余引发剂水溶液；待混合单体全部加入后，保温反应1.5小时，自然降温至45℃过滤即得到四元离子共聚物纳米乳液，室温密封保存；
(3)四元离子共聚物乳胶膜制备：量取10ml共聚物纳米乳液向水平桌面上的平底凹槽玻璃模具内缓慢浇注，常温常压下自然放置72小时，揭下即得共聚物乳胶膜；
(4)BEDAM组装：分别取4g纳米银线、3g碳纤维、5g共聚物乳液，三者均匀混合，超声15min可得导电乳液；使用旋转涂胶机将导电乳液均匀旋涂在共聚物乳胶膜表面形成复合电极层，并于常温常压下自然放置24小时；重复上述步骤在共聚物乳胶膜另一表面旋涂复合电极层可完成BEDAM组装；
(5)BEDAM直流电驱动形变实验：使用直流稳压电源向BEDAM上下表面提供2V直流电压，BEDAM产生弯曲形变，弯曲速度24°/s，5秒弯曲角度约120°；切换电源正负极，BEDAM产生反向弯曲形变；BEDAM最高变形次数11次。
实施例2
(1)实验准备工作：将苯乙烯、丙烯酸正丁酯进行减压蒸馏提纯，分别量取20ml苯乙烯和20ml丙烯酸正丁酯于恒压滴液漏斗内混合备用；室温配制质量分数为2％的过硫酸钾水溶液(引发剂)备用；
(2)苯乙烯－丙烯酸正丁酯-丙烯酸钠－丙烯磺酸钠四元离子共聚物纳米乳液聚合：同实施例1第(2)步；
(3)四元离子共聚物乳胶膜制备：同实施例1第(3)步；；
(4)BEDAM组装：分别取5g纳米银线、5g共聚物乳液，二者均匀混合，超声15min可得导电乳液；使用旋转涂胶机将导电乳液均匀旋涂在共聚物乳胶膜表面形成复合电极层，并于常温常压下自然放置36小时；重复上述步骤在共聚物乳胶膜另一表面旋涂复合电极层可完成BEDAM组装；
(5)BEDAM直流电驱动形变实验：使用直流稳压电源向BEDAM上下表面提供2V直流电压，BEDAM产生弯曲形变，弯曲速度20°/s，5秒弯曲角度约100°；切换电源正负极，BEDAM产生反向弯曲形变；BEDAM最高变形次数14次。
实施例3
(1)实验准备工作：同实施例1第(1)步；
(2)甲基丙烯酸甲酯－丙烯酸正丁酯—丙烯酸钠－丙烯磺酸钠四元离子共聚物纳米乳液聚合：同实施例1第(2)步；
(3)四元离子共聚物乳胶膜制备：同实施例1第(3)步；；
(4)BEDAM组装：分别取3g纳米金线、3g碳纳米管、5g共聚物乳液，三者均匀混合，超声20min可得导电乳液；使用旋转涂胶机将导电乳液均匀旋涂在共聚物乳胶膜表面形成复合电极层，并于常温常压下自然放置24小时；重复上述步骤在共聚物乳胶膜另一表面旋涂复合电极层可完成BEDAM组装；
(5)BEDAM直流电驱动形变实验：使用直流稳压电源向BEDAM上下表面提供2V直流电压，BEDAM产生弯曲形变，弯曲速度16°/s，5秒弯曲角度约80°；切换电源正负极，BEDAM产生反向弯曲形变；BEDAM最高变形次数20次。
实施例4
(1)实验准备工作：同实施例2第(1)步；
(2)苯乙烯－丙烯酸正丁酯-丙烯酸钠－丙烯磺酸钠四元离子共聚物纳米乳液聚合：同实施例2第(2)步；
(3)四元离子共聚物乳胶膜制备：同实施例1第(3)步；；
(4)BEDAM组装：分别取3g纳米金线、3g石墨烯、5g共聚物乳液，三者均匀混合，超声20min可得导电乳液；使用旋转涂胶机将导电乳液均匀旋涂在共聚物乳胶膜表面形成复合电极层，并于常温常压下自然放置36小时；重复上述步骤在共聚物乳胶膜另一表面旋涂复合电极层可完成BEDAM组装；
(5)BEDAM直流电驱动形变实验：使用直流稳压电源向BEDAM上下表面提供2V直流电压，BEDAM产生弯曲形变，弯曲速度18°/s，5秒弯曲角度约90°；切换电源正负极，BEDAM产生反向弯曲形变；BEDAM最高变形次数18次。
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。

Claims (2)

1.一种四元离子共聚物-无机复合仿生电驱动活性材料的制备方法，其特征在于，包括四元离子共聚物纳米乳液制备、四元离子共聚物乳胶膜制备、四元离子共聚物与无机导电填料复合电极层制备三个工艺步骤；四元离子共聚物由四种组分组成，分别为：刚性结构单元组分、柔性结构单元组分、离子交换功能单元组分和缓冲增强功能单元组分；四元离子共聚物纳米乳液制备方法为：采用半连续乳液聚合工艺，首先对反应单体采取减压蒸馏处理去除阻聚剂并低温储存备用；提前配制质量分数为1-4％的过硫酸钾水溶液；按照工艺配方依次将磁子、乳化剂十二烷基硫酸钠、离子交换功能单元组分、缓冲增强功能单元组分、去离子水加入圆底烧瓶内，将刚性结构单元组分、柔性结构单元组分混合于恒压滴液漏斗中备用，向圆底烧瓶内充氮气15-60min确保无氧环境，同步打开恒温磁力搅拌器，温度设定45-70℃，转速设定300r/min；转速稳定后，将二分之一混合组分向圆底烧瓶中滴加，滴加速度1-3d/s，并开始计时，乳化0.5-1.5小时后，迅速升温至65-95℃；达到预设温度后，向圆底烧瓶中加入30-60％的引发剂水溶液，待无混合组分回流时，向圆底烧瓶中滴加剩余混合组分，滴加速度0.2-2d/s，并分1-3次加入剩余引发剂水溶液；混合组分滴加完毕后，保温反应0.5-3小时，室温冷却至45-55℃时过滤反应产物得到白色聚合物纳米乳液，最终降至室温密封保存；四元离子共聚物乳胶膜制备方法为：在常温常压环境下，向平底凹槽玻璃模具内缓慢浇注定量聚合物纳米乳液，可通过增减乳液体积将成膜厚度准确调控至0.1-4.0mm，并放置24-120小时，待乳液干透即可得四元离子共聚物乳胶膜；四元离子共聚物与无机导电填料复合电极层制备方法为：采用平面旋涂工艺涂抹含有无机导电填料的预制导电乳液在常温常压下干燥而成，以30-70％聚合物纳米乳液为胶黏剂，与40-80％无机导电填料混合，超声震荡15-30min得到预制导电乳液，平面旋涂于四元离子共聚物乳胶膜表面，室温干燥12-48小时可得一侧复合电极层，电极层厚度范围0.05-0.2μm；重复上述步骤完成另一侧复合电极层制备，可最终得到一种四元离子共聚物-无机复合仿生电驱动活性材料；刚性结构单元组分选用甲基丙烯酸甲酯或苯乙烯，占总单体的20-60mol％；柔性结构单元组分选用丙烯酸正丁酯，占总单体的20-70mol％；离子交换功能单元组分含有碱金属阳离子、非金属阴离子以及不饱和双键结构，属于同时包含有机、无机两相的表面活性物质，选用烯烃基磺酸盐或苯乙烯磺酸盐，占总单体量的5-40mol％；缓冲增强功能单元组分发挥有机、无机两相增容作用和吸水锁水能力分别提升材料力学性能和离子交换性能，选用结构与离子交换功能单元组分类似，低电离度的有机羧酸盐，该组分一方面自身存在电离水解平衡，能够最大限度锁住水分子提高离子传导能力，同时自身也具有离子传导能力，另一方面就整体而言其有机相比重更大，在离子聚合物体系内能够对有机磺酸盐结构起到过渡缓冲作用，缓冲增强功能单元组分选用单体有丙烯酸及其衍生酸类、丙烯酸盐类及其衍生物羧酸盐类单体中的一种，占总单体量的10-40mol％；同一工艺配方中，以上各单体用量之和为100％。
2.根据权利要求1所述的制备方法，其特征在于，无机导电填料选用碳纤维、碳纳米管、石墨烯、纳米金线、纳米银线、纳米钯线之一或者混合使用。
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