CN109661198A - 凝胶片 - Google Patents
凝胶片 Download PDFInfo
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- CN109661198A CN109661198A CN201780054134.3A CN201780054134A CN109661198A CN 109661198 A CN109661198 A CN 109661198A CN 201780054134 A CN201780054134 A CN 201780054134A CN 109661198 A CN109661198 A CN 109661198A
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Abstract
本发明的目的在于,提供一种凝胶片,其在脑电波测定等中,为皮肤侧的粘合力适合于皮肤的配方(粘合力低,也能耐受端子等前端加压的凝胶),且对于与皮肤相反侧的电极单元具有充分的粘合力。一种凝胶片(1),其具有A层(10)与B层(20)的层叠结构,其特征在于,A层(10)的23℃、10Hz下的储能模量为12000~40000Pa,B层(20)的23℃、10Hz下的储能模量为2000~10000Pa。
Description
技术领域
本发明涉及凝胶片。特别是涉及需要减轻对皮肤的损伤的脑电波测定、老年人康复中使用的生物体用电极、医疗用带等中的皮肤贴附用凝胶片。
背景技术
凝胶片适合作为贴附于生物体的手术胶带、各种医疗用设备类的固定用带、贴附于生物体的生物体电极用垫、心电图用电极、建筑材料、电子材料等的工业用粘合带等使用。根据各用途而凝胶片所要求的特性不同。
例如,固定用带要求紧紧地固定于皮肤,且降低贴附时的蒸发、皮疹、剥离时的损伤,另外,对于生物体电极用垫,从长时间贴附的方面出发,需要维持对皮肤的粘合性,在此基础上,还需要维持电极单元侧的粘合力。
随着近年来的老龄化,医疗用电极(脑电波测定用、康复用肌肉刺激电极)中,要求更简单且测定精度良好者。例如脑电波测定中,以往将纤维素纤维中包含生理盐水者作为电极,但纤维素纤维的水的保持差,在经时的水分量变化、测定时的处理方面存在难点。
因此,专利文献1等中,为了获得心电图,提出了使用水凝胶的方案。然而,在原本用于粘着于皮肤的设计上,凝胶原材料具有柔软性、粘合力,因此,在头皮上安装电极时,头发有时缠绕在粘合介质上,或会追随皮肤的微小的凹凸,因此,剥离时对皮肤造成损伤为课题。另外,水凝胶是非常软的原材料,因此,脑电波测定等利用点接触的测定中,也有无法耐受电极的凸部的挤压而破损的可能性。
现有技术文献
专利文献
专利文献1:日本特表2016-501049号公报
发明内容
发明要解决的问题
因此,本发明鉴于上述以往的情况,目的在于,提供一种凝胶片,其在脑电波测定等中,为皮肤侧的粘合力适合于皮肤的配方(粘合力低、也能耐受端子等的前端加压的凝胶),且对于与皮肤相反侧的电极单元,具有充分的粘合力。
用于解决问题的方案
本发明人等进行深入研究,结果发现:使具有不同组成的凝胶层叠,使贴附于皮肤的一侧和其相反侧具有不同的流变特性,使皮肤侧比相反侧更硬,从而可以得到对柔和的皮肤的损伤小的具有粘合性和回弹性的凝胶片,完成了发明。即,本发明的主旨如以下所述。
(1)一种凝胶片,其具有A层与B层的层叠结构,前述A层的23℃、10Hz下的储能模量为12000~40000Pa,前述B层的23℃、10Hz下的储能模量为2000~10000Pa。
(2)根据前述(1)所述的凝胶片,其中,前述A层对电木板的粘合力为0.1~2.0N/20mm,前述B层对电木板的粘合力为2.5~15N/20mm。
(3)根据前述(1)或(2)所述的凝胶片,其厚度为0.2mm~2.0mm。
(4)根据前述(1)~(3)中任一项所述的凝胶片,其中,前述A层与前述B层的厚度比率为A/B=0.25~3.5。
(5)根据前述(1)~(4)中任一项所述的凝胶片,其中,前述A层和前述B层为包含高分子基质、水和多元醇的水凝胶,前述高分子基质为选自(甲基)丙烯酰胺系单体和(甲基)丙烯酸酯中的一种以上的单官能单体、与交联性单体的共聚物。
(6)根据前述(5)所述的凝胶片,其中,前述A层中进一步包含聚乙烯醇。
(7)根据前述(1)~(6)中任一项所述的凝胶片,其中,前述A层和前述B层的10Hz下的交流阻抗均为1000Ω以下。
(8)根据前述(1)~(7)中任一项所述的凝胶片,其中,其为在皮肤上贴附前述A层的表面而使用的皮肤贴附用凝胶片。
本说明书包含成为本申请的优先权基础的日本专利申请号2016-193461号、2017-041815号的公开内容。
发明的效果
根据本发明,以多层构成且使贴附于皮肤的一侧的储能模量更高来形成硬的层和软的层,从而根据皮肤和电极单元各被粘物发挥硬度(回弹力、耐久力)和粘合力,作为脑电波测定等中使用的电极,可以适合用于不缠绕于头发,通过凝胶片对头皮挤压电极的凸部而固定的用途等。
附图说明
图1为示意性示出本发明的凝胶片的实施方式的截面的图。
具体实施方式
以下,对本发明详细进行说明。
图1中示出本发明的凝胶片的一实施方式的截面。该实施方式的凝胶片1将A层10和B层20层叠而构成。而且,其特征在于,A层10的23℃、10Hz下的储能模量为12000~40000Pa,B层20的23℃、10Hz下的储能模量为2000~10000Pa。
该凝胶片1适合作为生物体用电极使用,使A层10贴附于皮肤,B层20的表面与电极单元接触。与B层20相比,A层10硬,B层较软,因此,对于电极单元良好地密合,在与电极单元之间不会产生气泡。
另外,优选的是,A层10对电木板的粘合力为0.1~2.0N/20mm,B层20对电木板的粘合力为2.5~15N/20mm。对于B层20,特别优选2.5~8.0N/20mm。A层的粘合力小,因此,从皮肤剥离时不会造成损伤,不会缠绕头发。采用不从电极单元拆卸B层侧的构成的情况下,期望B层的粘合力高。
需要说明的是,本发明中,对电木板的粘合力是指,依据JIS Z0237:2009,将凝胶片切成120mm×20mm,在测定对象的A层或B层一侧贴附电木板,使2kg的压接辊往复1次,制作试验片,用流变仪(Sun Scientific Co.,Ltd.制、CR-500DX),将测定条件设为角度90度、速度300mm/分钟,测定从测定开始点进行了规定的剥离的时刻(30、40、50、60、70mm)下的应力值(N/20mm),3个试验(总15点)的值的平均值。测定在温度23±5℃、湿度55%±10%的环境下进行。
A层10和B层20必须具有粘合性和缓冲性(回弹力),将凝胶片作为生物体用电极使用的情况下,优选进一步具有导电性。特别是,对于A层10和B层20,考虑对人体的用途优选由包含水的水凝胶构成。水凝胶的保水性等优异,在医疗·医药、食品、土木、生物工程、运动相关等宽范围的领域中使用。
作为前述水凝胶,例如优选使用包含高分子基质、水和多元醇的水凝胶。
作为高分子基质的一例,可以由具有1个烯属不饱和基团的单官能单体、与交联性单体的共聚物形成,但不限定于此。
作为单官能单体,优选使用(甲基)丙烯酰胺系单体、(甲基)丙烯酸酯等水溶性单体。
作为该(甲基)丙烯酰胺系单体的具体例,可以举出(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺等N,N-二烷基(甲基)丙烯酰胺、N-异丙基(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-乙基(甲基)丙烯酰胺、N-丙基(甲基)丙烯酰胺等N-烷基(甲基)丙烯酰胺;N-羟基乙基(甲基)丙烯酰胺、N-羟基甲基(甲基)丙烯酰胺等N-羟基烷基(甲基)丙烯酰胺;N-乙氧基甲基(甲基)丙烯酰胺、N-丙氧基甲基(甲基)丙烯酰胺、N-丁氧基甲基(甲基)丙烯酰胺、N-异丁氧基甲基(甲基)丙烯酰胺、N-戊氧基甲基(甲基)丙烯酰胺、N-己氧基甲基(甲基)丙烯酰胺、N-庚氧基甲基(甲基)丙烯酰胺、N-辛氧基甲基(甲基)丙烯酰胺、N-乙氧基乙基(甲基)丙烯酰胺、N-丙氧基乙基(甲基)丙烯酰胺、N-丁氧基乙基(甲基)丙烯酰胺等N-烷氧基烷基(甲基)丙烯酰胺;二甲基氨基丙基(甲基)丙烯酰胺等含氨基的阳离子性丙烯酰胺系化合物;4-丙烯酰基吗啉、叔丁基丙烯酰胺磺酸等含磺酸基的阴离子性单官能单体或其盐;和它们的衍生物等。其中,优选使用选自由(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺、N-异丙基(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-乙基(甲基)丙烯酰胺、N-丙基(甲基)丙烯酰胺、N-羟基乙基(甲基)丙烯酰胺、N-羟基甲基(甲基)丙烯酰胺、二甲基氨基丙基(甲基)丙烯酰胺、4-丙烯酰基吗啉、叔丁基丙烯酰胺磺酸和其盐组成的组中的至少1种等,但不限定于此。
作为前述(甲基)丙烯酸酯的具体例,可以举出烷基的碳数为1~18的(甲基)丙烯酸烷基酯、例如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸正己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正壬酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸正癸酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸正月桂酯、(甲基)丙烯酸十三烷酯、(甲基)丙烯酸正硬脂酯等(甲基)丙烯酸烷基酯;(甲基)丙烯酸环己酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸1-金刚烷酯等脂环式(甲基)丙烯酸酯;(甲基)丙烯酸2-甲氧基乙酯、(甲基)丙烯酸乙氧基乙氧基乙酯、甲氧基三乙二醇(甲基)丙烯酸酯等甲氧基聚乙二醇(甲基)丙烯酸酯等含烷氧基的(甲基)丙烯酸酯;(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸2-羟基丙酯、(甲基)丙烯酸2-羟基-3-苯氧基丙酯、(甲基)丙烯酸2-羟基丁酯等(芳基任选借助醚键键合于羟基烷基)(甲基)丙烯酸羟基烷酯;单(甲基)丙烯酸甘油酯;单(甲基)丙烯酸聚乙二醇酯和聚乙二醇-聚丙二醇共聚物等单(甲基)丙烯酸聚亚烷基二醇酯;(甲基)丙烯酸苄酯等具有芳香环的(甲基)丙烯酸酯;(甲基)丙烯酸四氢糠酯等具有杂环的(甲基)丙烯酸酯等。
上述单官能单体在上述(甲基)丙烯酰胺系单体的基础上,根据需要,可以使用:(甲基)丙烯酸或其盐、(甲基)丙烯酸酯、乙烯基吡咯烷酮、乙烯基乙酰胺、乙烯基甲酰胺等乙烯基酰胺系单官能单体;烯丙醇等非离子性单官能单体、苯乙烯系单体等。这些单官能单体可以分别单独使用,或组合2种以上而使用。需要说明的是,本说明书中,(甲基)丙烯酸是指,丙烯酸或甲基丙烯酸,(甲基)丙烯酸酯是指,丙烯酸酯或甲基丙烯酸酯。
A层和B层中的源自上述单官能单体的结构单元的含量没有特别限定,相对于水凝胶总量,优选10~30重量%的范围内,更优选15~25重量%。源自上述单官能单体的结构单元的含量如果过少,则水凝胶的保形性变得不充分,有变得过软、或容易撕裂的担心。另外,源自上述单官能单体的结构单元的含量如果过多,则从对水的溶解度的观点出发,变得不溶解,因此,考虑它们的均衡性而适宜设定。根据需要,可以以提高A层中的单官能单体的含量、或A层的储能模量成为12000~40000Pa的方式,使凝胶变硬。
作为前述交联性单体,优选使用分子内具备2个以上的具有聚合性的双键的单体。具体而言,可以举出N,N’-亚甲基双(甲基)丙烯酰胺、N,N’-亚乙基双(甲基)丙烯酰胺、(聚)乙二醇二(甲基)丙烯酸酯、(聚)丙二醇二(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、甘油三(甲基)丙烯酸酯等多官能(甲基)丙烯酰胺或(甲基)丙烯酸酯、四烯丙氧基乙烷、二烯丙基氯化铵等,它们可以使用1种或组合2种以上使用。需要说明的是,作为上述分子内具备2个以上的具有聚合性的双键的交联性单体,也可以使用:日本专利第2803886号公报中记载的、具有2个以上的(甲基)丙烯酰基或乙烯基、且分子量为400以上的多官能化合物即聚甘油衍生物。
交联性单体的添加量相对于水凝胶总量,优选0.01重量%~0.1重量%的范围内。添加量过少的情况下,交联密度变低,变得缺乏形状稳定性的同时,聚集力降低,凝胶材本身的保持力降低,凝胶的操作变困难。另外,剥离时,被粘物中残留凝胶材的一部分等凝胶片的操作性恶化。另外,交联性单体的添加量如果过多,则粘合力变弱,且有成为硬且脆的凝胶的可能性。
另外,水凝胶中的水的含量没有特别限定,相对于水凝胶总量,优选10~60重量%、更优选15~30重量%。水的含量如果过少,则水凝胶的相对于平衡水分量的含水量变少,水凝胶的吸湿性变强,水凝胶有时经时变质(例如溶胀)。另外,水的含量如果过多,则水凝胶的相对于平衡水分量的含水量变多,有时产生干燥所导致的水凝胶的收缩、物性变化。
作为多元醇,没有特别限定,例如可以举出乙二醇、三乙二醇、1,6-己二醇、1,9-壬二醇、丙二醇、丁二醇等二醇;甘油、季戊四醇、山梨糖醇等三元以上的多元醇类;聚乙二醇、聚丙二醇、聚甘油等多元醇缩合体;聚氧亚乙基甘油等多元醇改性体等。
多元醇中,优选使用水凝胶的使用温度区域(例如在室内使用时为20℃左右)中为液态的多元醇,具体而言,适合的是,乙二醇、三乙二醇、丙二醇、聚丙二醇、聚乙二醇、聚甘油和甘油等。
水凝胶中的上述多元醇的含量没有特别限定,相对于水凝胶总量,优选20~70重量%的范围内、更优选25~65重量%的范围内。上述多元醇的含量如果过少,则所得水凝胶的保湿力、增塑性缺乏,水分的蒸散变明显,水凝胶的经时稳定性缺乏,且柔软性也缺乏,因此,有时无法得到充分的粘合性。另外,上述多元醇的含量如果过多,则会超过高分子基质能保持的多元醇的量,产生多元醇从水凝胶的表面渗出所导致的物性变动,有时无法得到充分的粘合性,因此,考虑它们的均衡性而适宜设定。
特别是,对于A层10,为了维持凝胶的柔软性、且具有缓冲作用,聚合时混合聚乙烯醇等水溶性合成聚合物,从而可以对骨架赋予S-IPN(半互穿聚合物网络(Semi-Interpenetrating Polymer Network))结构。通过含有聚乙烯醇等水溶性合成聚合物,从而A层的储能模量变高,可以使凝胶变硬。
A层中含有聚乙烯醇的情况下,聚乙烯醇的聚合度如果过小,则无法得到机械强度提高的效果,相反地聚合度如果过大,则使聚乙烯醇溶解于制作凝胶时制备的单体配混液中时,粘度上升明显,无法制备均匀的配混液,因此,考虑它们的均衡性而适宜设定。优选在粘均聚合度下为500~3000。
另外,本实施方式中使用的聚乙烯醇的皂化度如果过小,则制备配混液时的溶解性提高,但所得水凝胶的稳定性降低,故不优选。相反地皂化度如果过大,则聚乙烯醇的溶解性极端降低,配混液的制备变困难,因此,优选设为80~98%的范围内,特别优选88~98%,但不限定于此。
A层中含有聚乙烯醇的情况下,聚乙烯醇相对于构成A层的水凝胶总量的含量只要能使A层的储能模量为12000~40000Pa的范围内就没有特别限定。含量如果过少,则无法预见A层的机械强度的改善,相反地含量如果过多,则聚乙烯醇无法完全溶解于凝胶中,产生析出、溶解残留,无法得到均匀的凝胶体,因此,考虑它们的均衡性而适宜设定。具体而言,相对于水凝胶总量,优选设为0.15~5重量%。
另外,A层10和B层20中,可以根据需要含有电解质,由此,可以对构成A层10和B层20的凝胶材赋予导电性。将凝胶片1作为生物体用电极使用的情况下,优选A层10和B层20的10Hz下的交流阻抗均为1000Ω以下。
对凝胶材赋予导电性的情况下,凝胶材中的上述电解质的含量相对于A层或B层的总量,优选0.05~10重量%、更优选2~6重量%。电解质的含量如果过少,则阻抗变高,不能说导电性是良好的。另外,随着电解质的含量增加阻抗降低,但电解质的含量如果过多,则溶解所需的水的量变多,不优选。
作为上述电解质,没有特别限定,例如可以举出卤化钠(例如氯化钠)、卤化锂、卤化钾等卤化碱金属;卤化镁、卤化钙等卤化碱土金属;其他金属卤化物等。另外,作为上述电解质,还可以适合使用:各种金属的、次氯酸盐、亚氯酸盐、氯酸盐、高氯酸盐、硫酸盐、碳酸盐、硝酸盐、磷酸盐。另外,作为上述电解质,铵盐、各种络盐等无机盐类;乙酸、苯甲酸、乳酸等一元有机羧酸的盐;酒石酸等多元有机羧酸的盐;邻苯二甲酸、琥珀酸、己二酸、柠檬酸等多元羧酸的一元或二元以上的盐;磺酸、氨基酸等有机酸的金属盐;有机铵盐等也是适合的。
另外,A层10和B层20中,出于调整pH的目的,可以适宜添加氢氧化钠等碱。
另外,为了使B层20追随电极单元,可以使B层20更牢固地粘着。具体而言,可以含有作为增粘剂的亲水性的高分子、具有粘合性的水不溶性高分子。例如,作为亲水性的高分子,可以使用聚丙烯酸或其盐。作为聚丙烯酸或其盐的添加量,没有特别限定,相对于B层的总量,优选0.25~2重量%的范围。添加量如果少,则无粘合赋予的效果,添加量即使多,也不会与添加量成比例地变大,因此,期望考虑整体的均衡性的添加。
另外,作为具有粘合性的水不溶性高分子,可以添加(甲基)丙烯酸酯、乙酸乙烯酯、马来酸酯等疏水性单体、松香系的树脂等。
特别是作为具有粘合性的水不溶性高分子,可以举出:使(甲基)丙烯酸酯、乙酸乙烯酯、马来酸酯等疏水性单体中的任意者单独聚合或多种聚合而成者。具体而言,可以举出(甲基)丙烯酸异辛酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸丁酯、乙酸乙烯酯、马来酸二辛酯等疏水性单体中任意均聚物或多种的共聚物。除上述单体以外,可以使乙烯、丙烯、丁烯、(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯等疏水性单体中的任一者、或多种进一步共聚。也可以进一步含有有机硅粘合剂、天然橡胶系、合成橡胶系的粘合剂。这些之中,丙烯酸酯共聚物的各特性优异,为高粘合性,因此,适合使用。
为了使具有粘合性的水不溶性高分子分散于B层中,优选使用乳化分散有前述高分子的乳液。通常,前述乳液的固体成分为30~60重量%,剩余的大部分为水。
例如,作为丙烯酸酯系共聚树脂的乳液,可以适合使用昭和电工株式会社制的商品名“Polysol PSA SE-1730”、日信化学工业株式会社制的商品名“Vinyblan ADH-1048”等。
B层20中的、具有粘合性的水不溶性高分子的含量可以根据最终制品所期待的性能而调节,为了得到对电极单元的良好的粘合力,相对于B层的总量,需要添加3重量%以上。优选5重量%以上、更优选8重量%以上、特别优选10重量%以上。另外,这些水不溶性高分子单独也具有作为粘合剂的功能,因此,含量多也没有问题,但含量过多,粘合力也不会提高恒定值以上,另外,作为医疗用电极的水凝胶使用的情况下,凝胶的导电性也降低,因此,考虑它们的均衡性,相对于B层总量,优选设为20重量%以下。更优选15重量%以下,特别优选13重量%以下。
进而,B层20中,根据需要,可以添加聚乙烯醇作为分散稳定剂。由此,可以进一步提高B层的粘合力。B层中添加的聚乙烯醇确保分散稳定性,因此,皂化度优选50~75%的范围内。
B层20中的聚乙烯醇的含量从确保分散稳定性的观点出发适宜设定。优选0.05~5重量%。
进而,A层10和B层20中,根据需要,也可以含有其他添加剂。作为其他添加剂,例如可以举出防锈剂、防霉剂、抗氧化剂、消泡剂、稳定剂、表面活性剂、着色剂等。
A层10和B层20可以如下得到:将上述各材料、以及聚合引发剂、溶剂等溶解或均匀分散,进行加热或紫外线照射等而进行聚合交联,由此可以得到。聚合引发剂可以为热聚合引发剂也可以为光聚合引发剂。对于聚合引发剂的添加量,为了使聚合反应充分进行、且降低残留单体,在凝胶化前配混液100重量%中,优选0.01重量%以上,为了防止聚合引发剂的反应残留所导致的变色(黄变)、臭气,优选1.0重量%以下。更优选0.05~0.5重量%。进而,通过照射紫外线进行聚合的情况下,紫外线的累积照射量根据聚合引发剂的含量等也不同,例如优选1000mJ/cm2~10000mJ/cm2的范围内、更优选2000mJ/cm2~10000mJ/cm2的范围内。
作为上述光聚合引发剂,适合的是,在紫外线、可见光线下裂解而产生自由基者,可以举出α-羟基酮、α-氨基酮、联苯酰缩二甲醇、双酰基氧化膦、茂金属等。更具体而言,可以举出2-羟基-2-甲基-1-苯基-丙烷-1-酮(制品名:DAROCURE 1173、Ciba SpecialtyChemicals Co.,Ltd.制)、1-羟基-环己基-苯基-酮(制品名:IRGACURE 184,CibaSpecialty Chemicals Co.,Ltd.制)、1-[4-(2-羟基乙氧基)-苯基]-2-羟基-2-甲基-丙烷-1-酮(制品名:IRGACURE 2959、Ciba Specialty Chemicals Co.,Ltd.制)、2-甲基-1-[(甲基硫代)苯基]-2-吗啉基丙烷-1-酮(制品名:IRGACURE 907、Ciba Specialty ChemicalsCo.,Ltd.制)、2-苄基-2-二甲基氨基-1-(4-吗啉基苯基)-丁烷-1-酮(制品名:IRGACURE369、Ciba Specialty Chemicals Co.,Ltd.制)、2-羟基-1-{4-[4-(2-羟基-2-甲基-丙酰基)-苄基]苯基}-2-甲基-丙烷-1-酮(制品名:IRGACURE 127、CibaSpecialtyChemicals Co.,Ltd.制)等。它们可以单独使用或组合多种而使用。
凝胶片1的厚度如果过薄,则操作性上有困难,因此,考虑它们而选择适当的厚度。优选0.2mm~2.0mm的范围内。特别优选0.3mm~1.2mm、更优选0.5mm~1.0mm。
关于凝胶片1中的A层10与B层20的厚度比率,A层的比率如果过大,则有妨碍B层对电极单元的密合的可能性,相反地B层的比率如果变大,则有凝胶从横向溢出的担心,因此,考虑它们的均衡性而适宜设定。具体而言,A层10与B层20的厚度比率A/B优选0.25~3.5。
另外,凝胶片1中,为了加强凝胶片、改善裁切时的保形性等,根据需要,可以沿着面内方向埋入中间基材。该中间基材可以以夹持于A层10与B层20之间的方式埋入。或者,不埋入层间而埋入A层10内、或B层20内中的任意者。
对于埋入至凝胶片1中的中间基材,作为具体的方式,可以由无纺布或织布构成。无纺布和织布的材质可以使用纤维素、绢、麻等天然纤维、聚酯、尼龙、人造丝、聚乙烯、聚丙烯、聚氨酯等合成纤维、或它们的混纺,根据需要,可以使用粘结剂,进而,根据需要可以进行着色。
上述无纺布的制造方法没有特别限定,可以举出干式法、湿式法、纺粘法、熔喷法、气流成网法、化学粘合法、热粘合法、针刺法、水刺法。根据单位面积重量、材质采用制法,无单位面积重量不均时,控制中间基材的位置,故更优选。对于织布,也没有特别限定,可以适宜选择平纹织物、特里科经编织物、拉舍尔经编针织物等。
另外,上述织布或无纺布的单位面积重量只要为能得到作为中间基材的规定的物性的单位面积重量就没有特别限定,例如优选10~40g/m2、更优选10~28g/m2。上述织布或无纺布的单位面积重量如果过小,则无法实现凝胶片的加强等,或单位面积重量不均变大从而凝胶片制造时的液体的渗透性根据位置而改变,由此,有中间基材的位置变动的可能性。另外,单位面积重量如果过大,则中间基材变硬,有凝胶片1对皮肤的追随性等受损的担心、对导通性造成不良影响的可能性,因此,考虑它们的均衡性而适宜设定。
另外,作为中间基材的材质,可以使用半透膜。该半透膜由玻璃纸、乙酸纤维素等构成,与织布或无纺布相比,难以通过水、保湿剂,因此,可以历经更长时间地保持A层和B层的各制造时的组成。
中间基材的厚度如果过厚,则液体的渗透性变差,有时对导通性造成不良影响,相反地如果过薄,则与单位面积重量过小的情况同样地无法实现凝胶片的加强等,或有中间基材的位置变动的可能性,因此,考虑这些而适宜设定。中间基材的厚度优选0.02mm~2.0mm范围内。另外,更优选0.02mm~0.5mm、特别优选0.03~0.3mm。
作为凝胶片1的制造方法,根据A层10和B层20的组成、中间基材的材质、厚度等而细节的条件不同,没有特别限定。例如,可以适宜采用如下方法:埋入中间基材的情况下,在对中间基材施加了恒定以上的张力的状态下,将中间基材保持在空中,向该中间基材的上侧和下侧注入单体配混液,通过光照射等进行聚合形成片状的方法;分别制作表面平滑的片状的A层和B层的凝胶材后,将在施加了恒定以上的张力的状态下保持的中间基材用这些凝胶材夹持并复合化的方法;或者,制作表面平滑的片状的A层,在该A层上根据需要在施加了恒定以上的张力的状态下载置中间基材,在该中间基材上注入B层的单体配混液,通过光照射等进一步聚合的方法;等。另外,也可以以卷状供给凝胶片,连续地进行前述制造工艺。
根据需要,可以在凝胶片1的单面设置基膜,另外,可以在设有基膜的一面的相反侧设置顶膜。
作为上述基膜,例如可以使用:由聚酯、聚烯烃、聚苯乙烯、聚氨酯等树脂形成的树脂薄膜、纸、层压有前述树脂薄膜的纸等。
这些基膜的与凝胶片1接触的面优选经脱模处理。作为脱模处理的方法,可以举出有机硅涂覆等,特别优选在热或紫外线下交联、固化反应的烧结型的有机硅涂覆。作为实施了脱模处理的薄膜,特别优选经双轴拉伸的PET(聚对苯二甲酸乙二醇酯)薄膜、OPP(拉伸聚丙烯)薄膜等。
作为上述顶膜,也可以使用基本上与基膜相同材质的膜,在设有顶膜的状态下,从其上进行紫外线照射等使其聚合的情况下,为了不妨碍光聚合,优选选择不屏蔽光的材质的薄膜。
以上的凝胶片作为脑电波测定等中的生物体用电极,可以在皮肤上贴附A层10的表面而使用。上述情况下,使去除顶膜在树脂薄膜上印刷涂覆包含Ag、Ag/AgCl等金属、碳等的导电性墨而形成导电层者、或在树脂薄膜上层压金属箔(铝、不锈钢、Ag等)、或层压混炼了碳等的导电性薄膜形成导电层者密合在B层20侧上,形成电极单元。B层20的储能模量为2000~10000Pa,与A层10相比软,因此,对电极单元的追随性良好,在与电极单元之间不会产生气泡。
实施例
以下,基于实施例和比较例,对本发明进一步详细进行说明,但本发明不限定于这些实施例。
(实施例1)
·A层的组成
相对于A层总量,计量作为单官能单体的丙烯酰胺24重量%、作为交联性单体的N,N’-亚甲基双丙烯酰胺0.036重量%、氯化钠5重量%、甘油40.9重量%,在该混合液中,加入聚乙烯醇(皂化度88%)3重量%、作为光聚合引发剂的2-羟基-2-甲基-1-苯基-丙烷-1-酮(商品名:IRGACURE IR1173)0.1重量%、和进一步作为pH缓冲剂的柠檬酸3Na、柠檬酸各1重量%,最后加入离子交换水,使整体为100重量%,得到A层的单体配混液。
·B层的组成
相对于B层总量,计量作为单官能单体的丙烯酰胺20重量%、作为交联性单体的N,N’-亚甲基双丙烯酰胺0.032重量%、氯化钠5重量%、甘油44.9重量%,在该混合液中,加入作为光聚合引发剂的2-羟基-2-甲基-1-苯基-丙烷-1-酮(商品名:IRGACURE IR1173)0.1重量%、和进一步作为pH缓冲剂的柠檬酸3Na、柠檬酸各1重量%,最后加入离子交换水,使整体为100重量%,得到B层的单体配混液。
·凝胶片的制造
在经有机硅涂覆的PET薄膜上滴加所得B层的单体配混液,通过恒定的间隙,从而将液体均匀地推开,以厚度成为0.6mm的方式固定。其中使用金属卤化物灯以能量500mJ/cm2进行紫外线照射,从而得到厚度0.6mm的B层。在所得B层上滴加A层的单体配混液,从其上同样地覆盖经有机硅涂覆的PET薄膜,将液体均匀地推开,以厚度成为0.3mm的方式固定。其中使用金属卤化物灯,进行能量3000mJ/cm2(相对于B层,合计为3500mJ/cm2)的红外线照射,得到总厚度0.9mm的凝胶片。需要说明的是,凝胶片的厚度如下测定:将贴附于两面的PET薄膜剥离,用测微器测定。
(实施例2)
使A层和B层的厚度分别为0.6mm、0.3mm,除此之外,与上述实施例1同样地制作凝胶片。
(实施例3)
使A层中的聚乙烯醇的含量为2重量%、甘油的含量为41.9重量%,除此之外,与上述实施例2同样地制作凝胶片。
(实施例4)
上述实施例1中,如下述变更B层的单体配混液。
即,相对于B层总量,计量作为单官能单体的丙烯酰胺18重量%、作为交联性单体的N,N’-亚甲基双丙烯酰胺0.030重量%、氯化钠2重量%、甘油39.9重量%,在该混合液中,加入作为光聚合引发剂的2-羟基-2-甲基-1-苯基-丙烷-1-酮(商品名:IRGACURE IR1173)0.1重量%、和进一步作为pH缓冲剂的柠檬酸3Na、柠檬酸各1重量%,最后添加作为水不溶性高分子的丙烯酸酯系共聚物的乳液(固体成分50重量%、商品名“Polysol PSA SE-1730”、昭和高分子株式会社制)21.8重量%(固体成分10.9重量%、水10.9重量%)、作为分散稳定剂的两亲性高分子即皂化度为65%的聚乙烯醇0.2重量%,搅拌几分钟直至成为均匀,得到乳白色的配混液。加入离子交换水16重量%,使整体为100重量%,得到B层的单体配混液。
作为该B层,使用上述单体配混液,除此之外,与实施例1同样地制作凝胶片。
(实施例5)
使A层和B层的厚度分别为0.6mm、0.3mm,除此之外,与上述实施例4同样地制作凝胶片。
(实施例6)
凝胶片的制造工序中,在A层与B层之间埋入成为中间基材的尼龙网,除此之外,与上述实施例5同样地制作凝胶片。
(实施例7)
凝胶片的制造工序中,在A层与B层之间埋入成为中间基材的尼龙网,除此之外,与上述实施例2同样地制作凝胶片。
(实施例8)
上述实施例7的B层的单体配混液中,追加作为增粘剂的聚丙烯酸Na(固体成分20重量%水溶液、商品名“JURYMER AC-20H”、东亚合成株式会社制)5重量%并溶解,使作为单官能单体的丙烯酰胺的含量为19重量%,使水的含量为24重量%,除此之外,与上述实施例7同样地制作凝胶片。
(实施例9)
如表2所示那样变更上述实施例8的A层和B层的单体配混液的组成,不埋入中间基材,除此之外,与上述实施例8同样地制作凝胶片。
(实施例10)
如表2所示那样变更A层和B层的单体配混液的组成,除此之外,与上述实施例8同样地制作凝胶片。
(比较例1)
不形成层叠结构,由实施例1中的不含聚乙烯醇的B层单体(厚度0.9mm)构成凝胶片。
(比较例2)
A层中,不含有聚乙烯醇,将作为单官能单体的丙烯酰胺的含量减少至20重量%,将作为交联性单体的N,N’-亚甲基双丙烯酰胺的含量增加至0.5重量%,使水的含量为28重量%、甘油的含量为44.4重量%,除此之外,与上述实施例2同样地制作凝胶片。
(比较例3)
作为A层,采用厚度2mm的导电性橡胶(Exseal公司制、半导电凝胶(Asker-C硬度15)、聚氨酯树脂制),除此之外,与上述实施例2同样地制作凝胶片。
(比较例4)
不形成层叠结构,由实施例1中的A层单体(厚度0.9mm)构成凝胶片。
将实施例1~10和比较例1~4中得到的凝胶片的组成归纳示于表1和表2。
[表1]
[表2]
(凝胶片的评价)
对于实施例1~10和比较例1~4中得到的凝胶片,进行各种试验。
·凝胶片的粘合力测定
依据JIS Z0237:2009,将凝胶片切成120mm×20mm,在剥离PET薄膜呈现的凝胶面(A层或B层)上贴附电木板,使2kg的压接辊往复1次进行压接,作为试验片。测定使用流变仪(Sun Scientific Co.,Ltd.制、CR-500DX),测定条件在角度90度、速度300mm/分钟下进行。测定从测定开始点起进行规定的剥离的时刻(30、40、50、60、70mm)中的应力值(N/20mm),将3个试验(共计15点)的值的平均值作为粘合力。作为测定环境,在温度23±5℃、湿度55%±10%的环境下实施。将测定结果示于表3和表4。
·凝胶片的粘合力测定(使用感的评价)
将凝胶片切成40mm见方,将A层的表面推到头皮上1分钟,之后,将凝胶片用手剥离,评价头发的黏住情况。将未感到疼痛时记作○,将无疼痛但凝胶附着于头发的情况、或头发被拉伸的情况记作△,将头发脱落的情况记作×。作为测定环境,在温度23±5℃、湿度55%±10%的环境下实施。将测定结果示于表3和表4。
·凝胶片的粘弹性特性
测定凝胶片的A层和B层的各储能模量、损耗模量和损耗角正切(tanθ)。具体而言,使用粘弹性测定装置(Anton Paar公司制、MR-102),进行23℃、10Hz的频率下的应变量1%的粘弹性测定。用夹具使25φ的凝胶片粘贴在25φ的SUS制平行板上,推到直至成为1N的载荷点后,在10Hz下测定储能模量和损耗模量,由该值算出损耗角正切(tanθ)。将测定结果示于表3和表4。储能模量越高,越体现弹性,因此,成为硬度的指标。
·凝胶片的硬度测定
利用Tensilon万能试验机(Orientec Company Limited,制、RTE-1210),在温度23±5℃、湿度55±10%、试验速度0.1mm/分钟的条件下,推到SUS制的12φ的圆柱,测定凝胶片的杨氏模量。测定在前述条件下直至成为2.98N的S-S曲线。凝胶片的试验片设为25mm×40mm,确保对于圆柱12φ充分的面积。
杨氏模量由2.0N左右~2.5N左右的应力的S-S曲线通过下述的数学式算出。
杨氏模量=2点间的应力值的差/截面积×(凝胶片厚度-2.0N时的时间×单位时间的位移量)/应变量(2.0N~2.5N的变形量)
·凝胶片的肖氏硬度测定
依据JIS K 7312,测定凝胶片的A层和B层的表面的Asker-C强度。将测定结果示于表3和表4。如表3和表4所示那样,A层的表面的Asker-C硬度为9~42,由于测定时推到的凸部而表面凹陷,但恢复。另外,B层的表面的Asker-C硬度为0,由于推到的凸部而在表面产生擦伤。
·凝胶片的应力缓和力的测定
利用Tensilon万能试验机(Orientec Company Limited,制、RTE-1210),在温度23±5℃、湿度55±10%、试验速度0.1mm/分钟的条件下,推到SUS制的12φ的圆柱,施加直至40N的位移后,在成为40N的时刻固定位移,保持40秒。测定此时的应力缓和值。将所得值除以40N,以比例表示相对于所施加的应力减少了多少应力值。
·凝胶片的电性能评价
首先,将凝胶片分离为A层和B层。接着,将A层和B层各切成20mm见方,使所得A层彼此或者B层彼此重叠,形成试验片。将这些试验片用SUS板夹持,根据存储示波器(输入电压10V、10Hz、电阻1MΩ)的条件,测定A层和B层各自的交流阻抗(Ω)。将测定结果示于表3和表4。
[表3]
[表4]
如表3和表4所示那样,通过本发明,可以得到各层中体现不同的行为的凝胶片,体现分别适于皮肤侧和电极单元侧的物性。
使实施例、比较例中得到的凝胶片层叠在电极单元上,所述电极单元是在树脂薄膜上层压混炼有碳的导电性薄膜而得到的,结果,对于比较例4中得到的凝胶片,过硬,且粘合力低,无对电极单元的追随性,密合性差。
附图标记说明
1 凝胶片
10 A层
20 B层
本说明书中引用的全部发行物、专利和专利申请通过直接引用引入至本说明书中。
Claims (8)
1.一种凝胶片,其具有A层与B层的层叠结构,所述A层的23℃、10Hz下的储能模量为12000~40000Pa,所述B层的23℃、10Hz下的储能模量为2000~10000Pa。
2.根据权利要求1所述的凝胶片,其中,所述A层对电木板的粘合力为0.1~2.0N/20mm,所述B层对电木板的粘合力为2.5~15N/20mm。
3.根据权利要求1或2所述的凝胶片,其厚度为0.2mm~2.0mm。
4.根据权利要求1~3中任一项所述的凝胶片,其中,所述A层与所述B层的厚度比率为A/B=0.25~3.5。
5.根据权利要求1~4中任一项所述的凝胶片,其中,所述A层和所述B层为包含高分子基质、水和多元醇的水凝胶,所述高分子基质为选自(甲基)丙烯酰胺系单体和(甲基)丙烯酸酯中的一种以上的单官能单体、与交联性单体的共聚物。
6.根据权利要求5所述的凝胶片,其中,所述A层中进一步包含聚乙烯醇。
7.根据权利要求1~6中任一项所述的凝胶片,其中,所述A层和所述B层的10Hz下的交流阻抗均为1000Ω以下。
8.根据权利要求1~7中任一项所述的凝胶片,其为在皮肤上贴附所述A层的表面而使用的皮肤贴附用凝胶片。
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