CN114671963A - 一种导电水凝胶及其制备方法和应用 - Google Patents
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Abstract
本申请公开了一种导电水凝胶及其制备方法和应用,所述导电水凝胶由丙烯酸类物质和烯基咪唑类物质聚合而成;所述导电水凝胶包含金属配位离子。本申请采用一步法,利用丙烯酸类物质和烯基咪唑类物质与金属离子的离子配位作用,赋予水凝胶粘附性、导电性、透光性等多种性能,制备方法简便。利用的光引发剂作为诱导剂,可以缩短交联的时间以及交联的不均匀问题。所得导电水凝胶良好的拉伸性、可塑性、粘附性、导电性、和透光性,有广泛的应用前景。
Description
技术领域
本申请涉及一种导电水凝胶及其制备方法和应用,属于水凝胶技术领域。
背景技术
水凝胶即为分散介质为水的凝胶,科学地将水凝胶定义为由亲水性聚合物链,经化学交联或物理交联所形成的一种具有三维网状结构的高分子聚合物。水凝胶能够吸水溶胀而不溶解,具有良好的机械性能和生物相容性,鉴于水凝胶这种独特的结构及性能,引起研究人员的广泛关注。
金属配位水凝胶具有优异的性能,包括韧性、自愈和粘合性,在电子皮肤、生物医学传感器、软机器人等方面具有广阔的应用前景。但实现水凝胶与大多数表面之间的理想粘合仍然是一个挑战。例如,需要传感器与皮肤的保形接触,这可能在界面上形成间隙并且不舒服。目前研究人员已经做出巨大努力来制备具有保形粘附和灵敏感测的集成水凝胶。利用微纤维膜和基于银纳米颗粒薄膜组成皮肤粘合应变传感器。通过直接在皮肤表面交联粘性蘑菇形乙烯基硅氧烷将皮肤变形转化为电信号。然而,可重复使用性受到限制,即三个循环后的粘合强度降低了48%。再者有文献报道将腺嘌呤和胸腺嘧啶引入聚丙烯酰胺骨架中制备了粘合水凝胶,该凝胶对各种固体材料具有优异的粘合性能,断裂强度较低。因此,制备出具有可逆且顺应的粘附力,韧性和高灵敏度的金属水凝胶将克服机械强度对水凝胶应用的限制,广泛应用于生物医用传感等诸多领域。
发明内容
根据本申请的一个方面,提供了一种导电水凝胶及其制备方法和应用,该多功能导电离子水凝胶具有良好的拉伸性、可塑性、粘附性、导电性、和透光性,解决了常见的导电水凝胶性能单一,无法满足实际情况的问题。
所述导电水凝胶由丙烯酸类物质和烯基咪唑类物质聚合而成;
所述导电水凝胶包含金属配位离子。
可选地,所述丙烯酸类物质选自甲基丙烯酸衍生物。
可选地,所述甲基丙烯酸衍生物选自甲基丙烯酸钠、甲基丙烯酸羟乙酯、甲基丙烯酸酐中的至少一种;
烯基咪唑类物质选自1-乙烯基咪唑、1-丙烯基咪唑中的至少一种。
可选地,所述金属配位离子选自碱金属离子、碱土金属离子、过渡金属离子中至少一种;
优选地,碱金属离子包括锂离子;
优选地,碱土金属离子选自镁离子、钙离子中的至少一种;
优选地,过渡金属离子镍离子、锌离子、钴离子、锆离子中的至少一种。
优选地,所述金属配位离子选自镍离子、锌离子、钴离子中的至少一种。
根据本申请的又一个方面,提供了导电水凝胶的制备方法,所述方法至少包括以下步骤:
将含有丙烯酸类物质、烯基咪唑类物质、金属盐、交联剂、光引发剂的混合物,光引发反应,得到所述导电水凝胶。
可选地,所述丙烯酸类物质与所述咪唑类物质的摩尔比为0.5~2:0.5~2。
具体地,所述丙烯酸类物质与所述烯基咪唑类物质为合成水凝胶的单体。
具体地,所述丙烯酸类物质与所述烯基咪唑类物质的摩尔比中,丙烯酸类物质的摩尔用量可独立选自0.5、0.75、1、1.25、1.5、1.75、2,或上述两点之间的任意数值。
具体地,所述丙烯酸类物质与所述咪唑类物质的摩尔比中,咪唑类物质的摩尔用量可独立选自0.5、0.75、1、1.25、1.5、1.75、2,或上述两点之间的任意数值。
可选地,所述金属盐选自金属配位离子的可溶性盐;
优选地,所述可溶性盐选自金属配位离子的氯化盐、硝酸盐、硫酸盐中的至少一种;
具体地,可溶性镍盐选自六水合氯化镍、六水合硝酸镍、六水合硫酸镍镍中的至少一种。
可溶性锌盐选自六水合氯化锌、六水合硝酸锌、六水合硫酸锌中的至少一种。
可溶性钴盐选自六水合氯化钴、六水合硝酸钴、六水合硫酸钴中的至少一种。
优选地,所述混合物中,金属离子的浓度为0.015mol/L~0.1mol/L。
进一步优选地,所述混合物中,金属离子的浓度为0.02mol/L~0.03mol/L。
具体地,所述混合物中,金属离子的浓度下限可独立选自0.015mol/L、0.02mol/L、0.025mol/L、0.03mol/L、0.035mol/L;金属离子的浓度上限可独立选自0.04mol/L、0.05mol/L、0.075mol/L、0.085mol/L、0.1mol/L
可选地,所述交联剂选自聚乙二醇二丙烯酸酯、N,N′-亚甲基双丙烯酰胺中的至少一种;
优选地,所述交联剂的用量为所述丙烯酸类物质和烯基咪唑类物质摩尔总量的0.2%~0.4%。
具体地,所述交联剂的用量可独立选自所述丙烯酸类物质和烯基咪唑类物质摩尔总量的0.2%、0.25%、0.3%、0.35%、0.4%,或上述两点之间的任意数值。
可选地,所述光引发剂选自芳香酮类化合物;
优选地,所述芳香酮类化合物选自2-羟基-2-甲基-1-苯基丙酮、2-羟基-4-(2-羟乙氧基)-2-甲基苯丙酮中的至少一种;
优选地,所述光引发剂的用量为所述丙烯酸类物质和咪唑类物质摩尔总量的0.2%~0.4%。
具体地,所述光引发剂的用量可独立选自所述丙烯酸类物质和咪唑类物质摩尔总量的0.2%、0.25%、0.3%、0.35%、0.4%,或上述两点之间的任意数值。
可选地,所述混合物中还包括溶剂;
所述溶剂包括水。
可选地,所述光引发反应的条件为:
光引发光源为紫外光,反应时间为30~45分钟;
优选地,所述紫外光波长为320~390nm。
具体地,将混合物在功率为200~300W的高压汞灯紫外固化箱中,光照反应30~45分钟。
具体地,反应时间可独立选自30分钟、35分钟、40分钟、42分钟、45分钟,,或上述两点之间的任意数值。
可选地,所述方法还包括,在光引发反应前,对所述混合物进行搅拌;
可选地,所述搅拌的条件为:
搅拌速度为500~1000r/min,搅拌时间为20~30分钟。
根据本申请的又一个方面,提供了上述任一导电水凝胶、上述任一方法制备得到的导电水凝胶在可穿戴电子设备材料中应用。
根据本申请的又一个方面,提供了上述任一导电水凝胶、上述任一方法制备得到的导电水凝胶在医用胶粘剂中应用。
根据本申请的又一个方面,提供了上述任一导电水凝胶、上述任一方法制备得到的导电水凝胶在可拉伸生物电子器件中应用。
根据本申请的又一个方面,提供了上述任一导电水凝胶、上述任一方法制备得到的导电水凝胶在电子检测仪器粘贴片中应用。
本申请能产生的有益效果包括:
1)本申请导电水凝胶具有良好的拉伸性、粘附性、自修复性、透光性等多种性能,有广泛的应用前景。
2)本申请采用一步法,利用丙烯酸类物质和咪唑类物质与金属离子的离子配位作用,赋予水凝胶粘附性、导电性、透光性等多种性能,制备方法简便。
3)本申请所提供的制备方法中,丙烯酸类物质、咪唑类物质的羧酸阴离子都可以提供配位结构位点,可以形成更加稳定的网络结构,提高水凝胶的机械强度。金属离子的引入同时赋予了水凝胶导电性能,因此可满足大部分导电水凝胶作为电子器件对力学性能和结构稳定性的要求。
4)本申请所提供的制备方法,利用的光引发剂作为诱导剂,可以缩短交联的时间以及交联的不均匀问题。
4)本申请所提供的导电水凝胶具有粘附性,可用于制备医用胶黏剂等产品;利用导电性及粘附性可使水凝胶与皮肤紧密接触,得以最大程度地将皮肤变形转化为电信号,可用于制作可拉伸电子器件、传感器等。
附图说明
图1为本申请实施例3中样品Z1-Z4的拉伸测试图;
图2为本申请实施例2中样品J1-J3的拉伸测试图;
图3为本申请实施例1、3、4中样品D1、样品N2、样品M1-M4的拉伸测试图;
图4为本申请实施例2中样品J1的差示扫描量热图像。
具体实施方式
下面结合实施例详述本申请,但本申请并不局限于这些实施例。
如无特别说明,本申请的实施例中的原料均通过商业途径购买,其中甲基丙烯酸钠(NaMac),AR>99%(国药控股化学试剂有限公司);六水氯化钴(CoC12·6H2O),分析纯AR(国药控股化学试剂有限公司);六水氯化锌(ZnC12·6H2O),分析纯AR(国药控股化学试剂有限公司);六水氯化镍(NiC12·6H2O)分析纯AR(国药控股化学试剂有限公司);聚乙二醇二丙烯酸酯(PEGDA),AR>99%(上海阿拉丁生化科技股份有限公司);2-羟基-2-甲基-1-苯基丙酮,R>99%(上海阿拉丁生化科技股份有限公司);以上试剂均直接使用,未进行进一步纯化。
实施例1考察不同单体比例对水凝胶成胶及性能的影响
1、单体比例为1:1
在室温状态下称取0.9411g 1-乙烯基咪唑,1.0808g甲基丙烯酸钠,210μL聚乙二醇二丙烯酸酯(约占单体摩尔总量的0.2%),5.5μL 2-羟基-2-甲基-1-苯基丙酮(约占单体摩尔总量的0.2%),0.07g六水氯化锌,置于一个洁净的50ml烧杯中,加入10ml蒸馏水后置于磁力工作台上以800r/min的搅拌速度搅拌25min。将以上混合均匀后的溶液,用5mL针管注入到两块10*10cm的玻璃夹板中,玻璃板之间的厚度0.1cm。注入溶液后,排空玻璃板中的小气泡,再将玻璃板放置在波长365nm紫外固化箱中照射35分钟,待玻璃板温度冷却至室温后,取出水凝胶,编号样品D1,放入自封袋中保存。
2、单体比例为1:2
在室温状态下称取0.9411g 1-乙烯基咪唑,1.6212g甲基丙烯酸钠,315μL聚乙二醇二丙烯酸酯(约占单体摩尔比的0.2%),8.3μL 2-羟基-2-甲基-1-苯基丙酮(约占单体摩尔比的0.2%),0.07g六水氯化锌,置于一个洁净的50ml烧杯中,加入10ml蒸馏水后置于磁力工作台上以800r/min的搅拌速度搅拌25min。将以上混合均匀后的溶液,用5mL针管注入到两块10*10cm的玻璃夹板中,玻璃板之间的厚度0.1cm。注入溶液后,排空玻璃板中的小气泡,再将玻璃板放置在波长365nm紫外固化箱中照射35分钟,待玻璃板温度冷却至室温后,取出水凝胶,编号样品D2,放入自封袋中保存。
3、单体比例为2:1
在室温状态下称取1.4117g乙烯基咪唑,1.0808g甲基丙烯酸钠,315μL聚乙二醇二丙烯酸酯(约占单体摩尔比的0.2%),8.3μL 2-羟基-2-甲基-1-苯基丙酮(约占单体摩尔比的0.2%),0.07g六水氯化锌,置于一个洁净的50ml烧杯中,加入10ml蒸馏水后置于磁力工作台上以800r/min的搅拌速度搅拌25min。将以上混合均匀后的溶液,用5mL针管注入到两块10*10cm的玻璃夹板中,玻璃板之间的厚度0.1cm。注入溶液后,排空玻璃板中的小气泡,再将玻璃板放置在波长365nm紫外固化箱中照射35分钟,待玻璃板温度冷却至室温后,取出水凝胶,编号样品D3,放入自封袋中保存。
4、单体比例为2:2
在室温状态下称取1.8822g乙烯基咪唑,2.1616g甲基丙烯酸钠,420μL聚乙二醇二丙烯酸酯(约占单体摩尔比的0.2%),11μL 2-羟基-2-甲基-1-苯基丙酮(约占单体摩尔比的0.2%),0.07g六水氯化锌,置于一个洁净的50ml烧杯中,加入10ml蒸馏水后置于磁力工作台上以800r/min的搅拌速度搅拌25min。将以上混合均匀后的溶液,用5mL针管注入到两块10*10cm的玻璃夹板中,玻璃板之间的厚度0.1cm。注入溶液后,排空玻璃板中的小气泡,再将玻璃板放置在波长365nm紫外固化箱中照射35分钟,待玻璃板温度冷却至室温后,取出水凝胶,编号样品D4,放入自封袋中保存。
实施例2考察不同金属离子对水凝胶成胶及性能的影响
具体实验过程与样品D4的制备方法基本相同,不同之处在于:变换不同种类同一浓度的金属离子,具体条件见表1,所得对应金属配位的导电水凝胶记为样品J1-J3。
实施例3考察不同浓度金属离子对水凝胶成胶及性能的影响
具体实验过程与样品D1的制备方法基本相同,不同之处在于:变换不同种类不同浓度的金属离子,具体条件见表1,所得对应金属配位的导电水凝胶记为样品N1-N4(镍离子),Z1-Z4(锌离子)。
实施例4考察其他金属离子对水凝胶性能的影响
具体实验过程与样品D1的制备方法基本相同,不同之处在于:所采用金属离子分别为锂离子、镁离子、钙离子和锆离子,所得对应金属配位的导电水凝胶记为样品M1-M4。
实施例5对所得导电水凝胶样品进行单向拉伸测试
测试方法如下:
1.取导电水凝胶样品,用手指捏住两端进行直线拉伸。
2.取导电水凝胶为,长3cm,宽0.1cm的哑铃型样品,两端夹具各夹0.9cm,留取中间1.2cm做实验区域,取样品在万能拉伸试验机上进行单向拉伸,拉伸速度设置为100mm/min。
拉伸应变的计算方法如下:
式中,L为样品的拉伸长度,mm;L0为样品的初始长度,mm。
断裂应力的计算方法如下:
式中,F为载荷N;A0为样品的横截面积,mm2。
水凝胶的韧性是通过应力应变曲线的积分面积计算得到的,弹性模量是通过应力-应变曲线(应变在0%-20%的范围内)的初始斜率计算得到的。
拉伸实验结果显示:添加0.025mol/L锌离子的水凝胶在的机械强度较高;具体地,图1为同一单体比例下(即甲基丙烯酸钠与1-乙烯基咪唑为1:1),在不同浓度锌离子溶液下交联后形成的水凝胶的拉伸测试图,可以看出金属离子浓度的改变对水凝胶的机械性能有较大影响,随着锌离子浓度的不断增大应变呈现一个先增大后减小的趋势;图2为同一单体比例下同一离子浓度(即甲基丙烯酸钠与1-乙烯基咪唑为2:2,且离子浓度均为0.025mol/L时)在不同离子种类下交联后形成的水凝胶的拉伸测试图,可以看出离子种类不同,水凝胶的机械强度也会不同,图2可看出钴离子添加后,获得应变为660%;图3为同一单体比例同一金属离子浓度(即甲基丙烯酸钠与1-乙烯基咪唑为1:1,且金属离子浓度均为0.025mol/L时)在不同离子种类下交联后形成的水凝胶的拉伸测试图,通过图2、图3可以看出,缩小单体比例会使水凝胶机械强度减弱,而钴离子浓度为0.025mol/L,单体比例为2:2时,水凝胶的拉伸性能最优;相比于采用锂离子、镁离子、钙离子和锆离子得到的水凝胶,采用锌离子及镍离子得到的水凝胶拉伸性能较高。
实施例6对所得导电水凝胶样品进行循环拉伸测试
测试方法如下:
采用使用相同的万能拉伸机在室温下对水凝胶进行了拉伸循环测试,并将所有水凝胶样品切成长、宽、厚分别为10mm、5mm和1mm的哑铃型样条。测试过程中,拉伸循环的最大应变设置为200%,拉伸速度设置为100mm/min,循环次数为10次。
此外,水凝胶的耗散能是通过拉伸循环曲线的积分面积计算得到的,弹性模量是通过拉伸循环曲线(应变在0%-20%的范围内)的初始斜率计算得到的。
测试结果表明:实验结束后的水凝胶样品的长、宽、厚均并未发生改变,说明该水凝胶具有一定抗疲劳性。
实施例7对所得导电水凝胶样品进行抗冻性能测试
测试方法如下:
使用差示量热扫描仪(Mettler Toledo DSC-1,America)对水凝胶样品进行表征。将样品包封在密封的坩埚中进行测试,并将空盘用作惰性参比。差示量热扫描仪在40μL/min的氮气流速下开始运行,并以1Hz的速率记录实验数据。测量范围是-140℃到0℃,所以水凝胶样品首先在0℃下平衡,然后以10℃/min的速率冷却到-140℃。
图4为样品J1的差示扫描量热图像,从图中可以看出在-22度左右有一个大概-2.8毫瓦的放热峰,表明材料有一定的抗冻性能。
以上所述,仅是本申请的几个实施例,并非对本申请做任何形式的限制,虽然本申请以较佳实施例揭示如上,然而并非用以限制本申请,任何熟悉本专业的技术人员,在不脱离本申请技术方案的范围内,利用上述揭示的技术内容做出些许的变动或修饰均等同于等效实施案例,均属于技术方案范围内。
Claims (10)
1.一种导电水凝胶,其特征在于,所述导电水凝胶由丙烯酸类物质和烯基咪唑类物质聚合而成;
所述导电水凝胶包含金属配位离子。
2.根据权利要求1所述的导电水凝胶,其特征在于,所述丙烯酸类物质选自甲基丙烯酸衍生物;
优选地,所述甲基丙烯酸衍生物选自甲基丙烯酸钠、甲基丙烯酸羟乙酯、甲基丙烯酸酐中的至少一种;
优选地,烯基咪唑类物质选自1-乙烯基咪唑、1-丙烯基咪唑中的至少一种。
3.根据权利要求1所述的导电水凝胶,其特征在于,所述金属配位离子选自碱金属离子、碱土金属离子、过渡金属离子中至少一种;
优选地,所述碱金属离子包括锂离子;
所述碱土金属离子选自镁离子、钙离子中的至少一种;
所述过渡金属离子镍离子、锌离子、钴离子、锆离子中的至少一种。
4.权利要求1-3任一项所述的导电水凝胶的制备方法,其特征在于,所述方法至少包括以下步骤:
将含有丙烯酸类物质、烯基咪唑类物质、金属盐、交联剂、光引发剂的混合物,光引发反应,得到所述导电水凝胶。
5.根据权利要求4所述的制备方法,其特征在于,所述丙烯酸类物质与所述烯基咪唑类物质的摩尔比为0.5~2:0.5~2;
优选地,所述金属盐选自金属配位离子的可溶性盐;
进一步优选地,所述可溶性盐选自金属配位离子的氯化盐、硝酸盐、硫酸盐中的至少一种;
所述混合物中,金属配位离子的浓度为0.015mol/L~0.1mol/L;
优选地,所述交联剂选自聚乙二醇二丙烯酸酯、N,N′-亚甲基双丙烯酰胺中的至少一种;
优选地,所述交联剂的用量为所述丙烯酸类物质和烯基咪唑类物质摩尔总量的0.2%~0.4%;
优选地,所述光引发剂选自芳香酮类化合物;
进一步优选地,所述芳香酮类化合物选自2-羟基-2-甲基-1-苯基丙酮、2-羟基-4-(2-羟乙氧基)-2-甲基苯丙酮中的至少一种;
优选地,所述光引发剂的用量为所述丙烯酸类物质和烯基咪唑类物质摩尔总量的0.2%~0.4%;
优选地,所述混合物中还包括溶剂;
所述溶剂包括水。
6.根据权利要求4所述的制备方法,其特征在于,所述光引发反应的条件为:
光引发光源为紫外光,反应时间为30~45分钟;
优选地,所述紫外光波长为320~390nm。
7.权利要求1-3任一项所述导电水凝胶、权利要求4-6任一项所述方法制备得到的导电水凝胶在可穿戴电子设备材料中应用。
8.权利要求1-3任一项所述导电水凝胶、权利要求4-6任一项所述方法制备得到的导电水凝胶在医用胶粘剂中的应用。
9.权利要求1-3任一项所述导电水凝胶、权利要求4-6任一项所述方法制备得到的导电水凝胶在可拉伸生物电子器件中的应用。
10.权利要求1-3任一项所述导电水凝胶、权利要求4-6任一项所述方法制备得到的导电水凝胶在电子检测仪器粘贴片中的应用。
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