CN108546333A - 一种高机械性能双网络复合水凝胶的制备 - Google Patents
一种高机械性能双网络复合水凝胶的制备 Download PDFInfo
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Abstract
本发明公开了一种高机械性能双网络复合水凝胶的制备,该复合水凝胶的制备包括以下步骤:将琼脂溶解于水中,加热至琼脂粉完全溶解,然后向上述琼脂溶液中加入水溶性聚合物单体、水溶性纤维素醚,少许光引发剂,少许交联剂,混合均匀,所得溶液放置在室温中一段时间至溶液固化,后放置在紫外灯下照射引发聚合即成。所述水凝胶利用琼脂的溶胶‑凝胶转变的特性,形成凝胶的第一层网络结构,水溶性聚合物单体形成第二层网络结构,并利用水溶性纤维素醚与水凝胶网络的非共价氢键相互作用的特性,改善水凝胶机械性能。这是一种增韧增强水凝胶的有效方法,可用于药物载体,人体组织工程。
Description
技术领域
本发明属于水凝胶制备技术领域,具体涉及一种高机械性能双网络复合水凝胶的制备。
技术背景
水凝胶是指能够吸收并保持大量水分而又不溶于水且具有一定的三维结构的一类聚合材料,。它具有网状结构的水溶性高分子中有一些疏水基团和亲水基团,亲水基团与水分子结合,将水分子连接在网状内部,而疏水基团遇水膨胀形成网络结构的骨架将水分子锁住,使其保持一定的含水量。因水凝胶特殊的三维网络体系的存在,使其性质柔软,能保持一定的形状,且含水量较高。因此被广泛应用于药物载体,组织工程等领域。但是由于大多数合成水凝胶具有较差的机械强度及韧性,所以开发用于承载软组织(如软骨,肌腱,肌肉和血管)的具有良好生物相容性的仿生水凝胶仍是一项非常具有挑战的任务。其次,其有限的扩展性与可恢复性也限制了其广泛的应用。所以合成新型高机械性能且恢复性好的水凝胶一直是科研人员探索的方向。如双网络水凝胶,纳米复合水凝胶,三嵌段聚合物水凝胶等水凝胶越来越受到大家的关注。
目前的研究中,双网络水凝胶的热度最高。已证明由具有强不对称结构的两个交联网络组成的双网络水凝胶可以通过使用各种各样的聚合物调节两个网络之间和分子间相互作用和结构来改善机械强度。双网络水凝胶通常通过多步连续的自由基聚合方法合成。首先,通常使用强的聚电解质(如聚丙烯酸,聚丙烯酰胺)来形成高度共价交联的第一层网络。由于聚电解质的强烈膨胀,当将聚电解质水凝胶浸入含有第二次聚合的中性第二单体,引发剂和交联剂的溶液中时,这些反应物将扩散到第一层网络中,并与第一层网络松散的交联形成第二网络。多步聚合方法已经证明了其产生不同的高强度水凝胶的可行性。但此聚合方法聚合周期到1~2天,耗时长,且由于润胀需要大量的中性第二单体,对中性第二单体的消耗比较大。
所述的高机械性能双网络复合水凝胶利用琼脂的溶胶-凝胶特性制作双网络水凝胶,可省去润胀过程,节约大量时间,且琼脂有成本低廉、生物可降解性、生物相容性等优点。纤维素及其衍生物是自然界最为丰富的天然多糖,具有成本低廉、生物可降解性、生物相容性好等优点。水溶性纤维素醚作为纤维素的代表衍生物之一,具备优良的水溶性和生物相容性,此外水溶性纤维素醚长链上还存在丰富的-OH基团,相比于天然纤维素,其更容易被改性并应用。纤维素醚的这些优异的特性使其能被广泛地应用于生物医药领域。利用水溶性纤维素醚与水凝胶网络的非共价氢键相互作用的特性,可改善水凝胶机械性能。
发明内容
解决的技术问题:
为了解决传统单组分水凝胶机械性能较差、生物不相容等缺点,本发明提供了高机械性能双网络复合水凝胶的制备方法
技术方案
将一定量的琼脂溶于一定量的水中,搅拌均匀,将溶液加热至琼脂粉与水完全混溶,然后向上述琼脂溶液中加入水溶性聚合物单体(丙烯酸、丙烯酰胺、乙烯醇、乙烯基吡咯烷酮等可形成聚合网络的强电解质)、水溶性纤维素醚(羟乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素、二乙氨基乙基纤维素、羧甲基纤维素、甲基纤维素、乙基纤维素、丙基纤维素等),少许光引发剂,少许交联剂(N,N′-亚甲基双丙烯酰胺、乙烯基吡啶、甲基丙烯酸羟烷基酯等),混合均匀,所得溶液放置在室温中一段时间至溶液固化,后放置在紫外灯下照射引发聚合即成。
所述的高机械性能双网络水凝胶的组分主要为聚合物单体(丙烯酸、丙烯酰胺、乙烯醇、乙烯基吡咯烷酮等可形成聚合网络的强电解质)、水溶性纤维素醚(羟乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素、二乙氨基乙基纤维素、羧甲基纤维素、甲基纤维素、乙基纤维素、丙基纤维素等)、去离子水。
所述的水溶性纤维素醚分子量没有限制,粘度分布在5000~8000mPa·s。
所述的溶液加热至琼脂与水完全混溶。。
所述的复合水凝胶的制备反应条件是紫外灯下聚合一段时间。
所述的复合水凝胶的含水量控制在75%~87%之间。
所述的复合水凝胶中的水溶性纤维素醚占固含量的比例控制在5%~25%之间。
所述的复合水凝胶中琼脂含量占固含量的比例控制在5%~15%之间。
所述的复合水凝胶中聚合物含量占固含量的比例控制在60%~90%之间。
所述的复合水凝胶是利用琼脂的溶胶-凝胶转变的特性,形成凝胶的第一层网络结构,水溶性聚合物单体形成第二层网络结构,并利用水溶性纤维素醚与水凝胶网络的非共价氢键相互作用的特性,改善水凝胶机械性能。
本发明具有以下优点:
(1)本发明所述水凝胶的原料为来源广泛的水溶性纤维素醚、水溶性聚合物单体、琼脂和去离子水,成本低廉。
(2)本发明所述的用于增强水凝胶的水溶性纤维素醚和琼脂具有良好生物相容性,环境友好等优点。
(3)本发明所述的高机械性能水凝胶相比于普通的传统水凝胶具有更高的机械性能。
(4)本发明所述的复合水凝胶含制备步骤简单,制备周期短。
附图说明
图1为普通丙烯酸(PAA)水凝胶与所述高机械性能双网络水凝胶的拉伸测试对比图,如图所示,相比于普通水凝胶较低的断裂伸长率,所述的高机械性能双网络水凝胶表现出了更高的断裂伸长率。图2为普通丙烯酸(PAA)水凝胶与所述高机械性能双网络水凝胶的压缩测试对比图,如图所示,相比于普通水凝胶较低的压缩性能,所述的高机械性能双网络水凝胶表现出了更好的压缩性能,综上表明该复合水凝胶具有更高的机械性能。
具体实施方式
为了更好的理解本发明,下面结合具体实例来进一步说明。若未特别指明,实施例中所用的技术手段为本领域技术人员所熟知的常规手段。
实施例1:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酸、0.1~1.5g羟乙基纤维素,少许光引发剂,少许N,N-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例2:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酰胺、0.1~1.5g羟乙基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例3:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g乙烯醇、0.1~1.5g羟乙基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例4:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酸、0.1~1.5g羟丙基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例5:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酸、0.1~1.5g甲基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例6:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酸、0.1~1.5g乙基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例7:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酸、0.1~1.5g羟丙基甲基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例8:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酰胺、0.1~1.5g羟甲基纤维素,少许光引发剂,少许N,N′-亚甲基双丙烯酰胺做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
实施例9:
将0.1~1g的琼脂溶于25ml的水中,搅拌均匀,将溶液加热至至琼脂粉与水完全混溶,然后向上述溶液中加入3~10g丙烯酰胺、0.1~1.5g羟乙基纤维素,少许光引发剂,少许乙烯基吡啶做交联剂混合均匀。放置在室温中一段时间至溶液固化,后放置在紫外灯下聚合50~60min。
Claims (7)
1.一种高机械性能双网络复合水凝胶的制备,其特性是通过以下步骤得到的:
(1)将一定量的琼脂粉溶于去离子水,加热至琼脂完全溶解。
(2)将一定量的水溶性聚合物单体,水溶性纤维素醚加入上述热溶液,并向其中加入少许光引发剂,少许交联剂,然后充分搅拌。室温静置上述反应物变成固体,将固体放到紫外灯下聚合一段时间。
2.根据权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶的第一网络由琼脂分子构建,琼脂的含量占固含量的5%~15%之间。
3.根据权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶制备过程中添加的水溶性聚合物单体可为丙烯酸、丙烯酰胺、乙烯醇、乙烯基吡咯烷酮等可形成聚合网络的强电解质。
4.根据权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶的第二网络由水溶性聚合物单体聚合构建,聚合物的含量占固含量的60%~90%之间。
5.根据权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶制备过程中添加的水溶性纤维素醚可为甲基纤维素、乙基纤维素、丙基纤维素、羟乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素、二乙氨基乙基纤维素、羧甲基纤维素等。
6.权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶制备过程中通过添加水溶性纤维素醚再次增强水凝胶的机械性能,纤维素醚占固含量的5%~25%之间。
7.根据权利要求1所述的高机械性能双网络复合水凝胶,其特征在于:水凝胶制备过程中添加的交联剂为N,N′-亚甲基双丙烯酰胺或乙烯基吡啶或甲基丙烯酸羟烷基酯。
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