CN111718445A - 一种pam/pvp/paa三网络水凝胶的制备方法 - Google Patents

一种pam/pvp/paa三网络水凝胶的制备方法 Download PDF

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CN111718445A
CN111718445A CN202010648913.XA CN202010648913A CN111718445A CN 111718445 A CN111718445 A CN 111718445A CN 202010648913 A CN202010648913 A CN 202010648913A CN 111718445 A CN111718445 A CN 111718445A
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汪济奎
严辉
肖俊
赵忠华
周佳
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East China University of Science and Technology
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Abstract

本发明涉及一种PAM/PVP/PAA三网络水凝胶的制备方法。所述三重网络水凝胶为由三种聚合物形成的交联聚合物互穿网络，对凝胶的力学性能有极大的增强，水凝胶的制备方法具体包括以下步骤：1）将丙烯酰胺（AM），丙烯酸（AA），六水合氯化铁，聚乙烯比咯烷酮(PVP)按比例溶于水中混合均匀，2）依次加入交联剂，引发剂，进行氩气驱氧处理后，加入引发剂促进剂，3）将得到的混合溶液经过超声处理后，在40℃下反应1小时，最后再在室温下放置24小时。本发明制备的三网络复合水凝胶具有较高的机械强度和良好的自修复性能，且具有一定的导电性能，其制备过程简单，原料绿色无毒无害，可以应用在医用器械、仿生电子皮肤、可注射水凝胶等方面。

Description

一种PAM/PVP/PAA三网络水凝胶的制备方法
技术领域
本发明属于水凝胶制备领域，具体涉及一种PAM/PVP/PAA三网络水凝胶的制备方法。
背景技术
水凝胶是一种通过化学键或者物理相互作用而交联形成的具有三维网络结构的功能高分子材料，高分子网络中含有大量的水并且触感柔软、能保持一定的形状。由于其物理化学特性，水凝胶在软骨替代品、医用器械和柔性电子器件等领域有着广泛应用，但现今水凝胶的进一步应用仍然受限于其较差的力学性能。传统的水凝胶在受到机械载荷作用时不可避免的会出现局部应力集中，局部应力的积累会使网丝断裂，通过裂纹的扩展产生网络缺陷，最终导致整个机体的突然断裂。并且传统的水凝胶没有自修复性能，这样减少了水凝胶的使用次数和寿命。为了提高水凝胶的机械强度和自修复性能。
目前，通过构建双网络结构、添加纳米复合材料等手段，已经获得了提高水凝胶力学性能的方法。双网络(DN)水凝胶可以通过构建柔性和刚性互联网络有效地耗散能量，从而保证水凝胶优异的力学性能。但由于不可逆共价键的存在，当化学交联形成的网状结构断裂时，会造成水凝胶的永久性损伤和较差的抗疲劳性能。结果表明，引入物理交联形成物理化学交联和全物理交联可以有效地解决水凝胶的疲劳性能差问题。Okay等人以聚丙烯酰胺(PAM)和PDMA为原料，通过化学-物理交联制备了具有高机械强度的三网水凝胶。
发明内容
本发明的目的是针对现有技术中存在的上述不足，提供一种具有良好机械性能且自修复效果很好的水凝胶的制备方法，其通过一步法制备而成，制备工艺简单易操作。
为解决上述技术问题，本发明提供的技术方案是：
一种PAM/PVP/PAA三网络水凝胶的制备方法，其特征包括如下步骤：
（1）将丙烯酰胺（AM），丙烯酸（AA），六水合氯化铁，聚乙烯比咯烷酮(PVP)按一定的质量比溶于水中，得到均匀的混合溶液A；
（2）依次加入交联剂，引发剂，进行氩气驱氧处理后，加入引发剂促进剂得到混合溶液B，其中交联剂、引发剂、引发剂促进剂与丙烯酰胺的质量比为（0.001-0.004）∶（0.02-0.04）∶0.0015∶1;
（3）将溶液B低温超声处理后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放置24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶;
[按上述方案，步骤（1）中所述混合溶液A中丙烯酰胺（AM），丙烯酸（AA），六水合氯化铁，聚乙烯比咯烷酮(PVP)的总浓度为40-50wt%；其中丙烯酸和PVP的质量比为2∶1；
按上述方案，步骤（2）中所述交联剂为N,N’-亚甲基双丙烯酰胺；引发剂为过硫酸铵；引发剂促进剂为N,N,N’,N’-四甲基乙二胺；充氩气鼓泡10min;
按上述方案，步骤（3）中所述低温超声20min。
本发明采用一步法合成水凝胶，制备方法简单易操作，反应条件温和，且制备出的三网络复合水凝胶力学性能优异，自修复效果良好。PAM/PVP/PAA三网络复合水凝胶中引入了化学交联网络，离子键配位的物理交联网络和PVP与PAA之间形成的氢键，可以保证在各种环境和负载条件下具有较高的、稳定的机械性能和设备性能。
本发明以聚乙烯比咯烷酮（PVP）、丙烯酸和丙烯酰胺为原料，原料具有良好的生物相容性和生物降解性，且通过万能拉力机试验机测得拉伸强度为0.6～1.2MPa，拉断伸长率为可达500%，压缩强度为1.5～13.6MPa(压缩形变为70％左右)。在软骨替代品、医用器械和柔性电子器件等领域有着广泛应用前景。
具体实施方式
通过下列实施例描述本发明，在不违反本发明的宗旨下，本发明应不限于以下实施例具体明示的内容。
在以下实施例中，如无特殊说明，其中所采用的原料均为本领域常用的原料，实施例中采用的方法均为本领域常规的方法。
实施例1
准确称量6.39g丙烯酰胺（AM）、1.278g丙烯酸（AA）、0.17496g六水合氯化铁、0.639g聚乙烯比咯烷酮(PVP)在室温下溶于20mL去离子水中，溶解形成均匀溶液后，再依次加入30.6mg的N,N’-亚甲基双丙烯酰胺、0.1278g的过硫酸铵、50uL的N,N,N’,N’-四甲基乙二胺，然后再充氩气鼓泡10min，低温下超声处理20min后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶。将样品制成标准样条后再在室温下通过万能试验机进行性能测试，测得样条拉伸强度为1.146MPa，断裂伸长率为524.17%，压缩强度为12.230MPa（压缩形变为76.58%）。
实施例2
准确称量6.39g丙烯酰胺（AM）、1.278g丙烯酸（AA）、0.1050g六水合氯化铁、0.639g聚乙烯比咯烷酮(PVP)在室温下溶于20mL去离子水中，溶解形成均匀溶液后，再依次加入30.6mg的N,N’-亚甲基双丙烯酰胺、0.1278g的过硫酸铵、50uL的N,N,N’,N’-四甲基乙二胺，然后再充氩气鼓泡10min，低温下超声处理20min后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶。将样品制成标准样条后再在室温下通过万能试验机进行性能测试，测得样条拉伸强度为0.924MPa，断裂伸长率为643.58%，压缩强度为10.48MPa（压缩形变为68.38%）。
实施例3
准确称量6.39g丙烯酰胺（AM）、1.62g丙烯酸（AA）、0.17496g六水合氯化铁、0.81g聚乙烯比咯烷酮(PVP)在室温下溶于20mL去离子水中，溶解形成均匀溶液后，再依次加入30.6mg的N,N’-亚甲基双丙烯酰胺、0.1278g的过硫酸铵、50uL的N,N,N’,N’-四甲基乙二胺，然后再充氩气鼓泡10min，低温下超声处理20min后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶。将样品制成标准样条后再在室温下通过万能试验机进行性能测试，测得样条拉伸强度为1.042MPa，断裂伸长率为472.33%，压缩强度为8.93MPa（压缩形变为72.48%）。
实施例4
准确称量3.195g丙烯酰胺（AM）、5.112g丙烯酸（AA）、0.17496g六水合氯化铁、2.556g聚乙烯比咯烷酮(PVP)在室温下溶于20mL去离子水中，溶解形成均匀溶液后，再依次加入30.6mg的N,N’-亚甲基双丙烯酰胺、0.2556 g的过硫酸铵、50uL的N,N,N’,N’-四甲基乙二胺，然后再充氩气鼓泡10min，低温下超声处理20min后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶。将样品制成标准样条后再在室温下通过万能试验机进行性能测试，测得样条拉伸强度为0.678MPa，断裂伸长率为782.43%，压缩强度为7.32MPa（压缩形变为72.45%）。
实施例5
准确称量6.39g丙烯酰胺（AM）、2.556g丙烯酸（AA）、0.17496g六水合氯化铁、1.278g聚乙烯比咯烷酮(PVP)在室温下溶于20mL去离子水中，溶解形成均匀溶液后，再依次加入30.6mg的N,N’-亚甲基双丙烯酰胺、0.1278g的过硫酸铵、50uL的N,N,N’,N’-四甲基乙二胺，然后再充氩气鼓泡10min，低温下超声处理20min后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放24h，即得到成模具形状的PAM/PVP/PAA三网络复合水凝胶。将样品制成标准样条后再在室温下通过万能试验机进行性能测试，测得样条拉伸强度为1.024MPa，断裂伸长率为462.82%，压缩强度为7.34MPa（压缩形变为78.29%）。

Claims (2)

1.一种PAM/PVP/PAA三网络水凝胶的制备方法，其特征在于，包括如下步骤：
（1）将丙烯酰胺（AM），丙烯酸（AA），六水合氯化铁，聚乙烯比咯烷酮(PVP)按一定的质量比溶于水中，得到均匀的混合溶液A；
（2）依次加入交联剂，引发剂，进行氩气驱氧处理后，加入引发剂促进剂得到混合溶液B，其中交联剂、引发剂、引发剂促进剂与丙烯酰胺的质量比为（0.001-0.004）∶（0.02-0.04）∶0.0015∶1;
（3）将溶液B低温超声处理后密封至聚四氟乙烯模具中，加热至40℃，保温反应1h，再在室温下放置24h，即得到成模具形状的PAM/PVP/PAA三网络水凝胶。
2.如权力要求1所述的一种PAM/PVP/PAA三网络水凝胶的制备方法，其特征在于，所述混合溶液A中丙烯酰胺（AM），丙烯酸（AA），六水合氯化铁，聚乙烯比咯烷酮(PVP)的总浓度为40-50wt%；其中丙烯酸和PVP的质量比为2∶1；交联剂为N,N’-亚甲基双丙烯酰胺；引发剂为过硫酸铵；引发剂促进剂为N,N,N’,N’-四甲基乙二胺；充氩气鼓泡10min;低温超声20min。
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