CN106986972B - 一种多性能水凝胶及其合成方法 - Google Patents
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Abstract
本发明涉及一种多性能水凝胶，该水凝胶具有规则的内部三维网络结构，孔径在8‑20微米。同时本发明还提出以球形聚合物刷作为一种新型交联剂制备高性能水凝胶的合成方法，即利用乳液聚合合成出一种球形聚合物刷,再通过原位聚合制备高性能水凝胶,该方法易于控制，所制备的水凝胶在力学性能和缺口不敏感性能上有了大幅度提升，并能作为催化剂载体应用与催化反应，在制备多性能水凝胶的领域有着潜在的应用价值。
Description
技术领域
本发明涉及高分子材料领域，具体为制备高性能水凝胶及其制备方法。
背景技术
水凝胶是指由亲水性高分子经物理、化学交联后形成的三维网状高分子聚合物。由于水凝胶自身的亲水性、良好的渗透性和优异的生物相容性，近年来在生物组织培养和药物控释等领域受到广泛的关注。传统方法利用小分子交联剂合成的水凝胶机械性能差，受到外力作用易发生破碎，制约着水凝胶的工业应用。在水凝胶的实际应用中，除了优异的机械性能外，还需要其他特性，例如缺口不敏感性，自修复性，形状记忆功能，强吸水性等，因此制备多功能的水凝胶依然是难以解决的问题。
乳液聚合是指用水或其它液体介质的乳液中，按胶束机理或低聚物机理，生成彼此孤立的乳胶粒，在其中进行加聚，生成高聚物的一种方法。
发明内容
本发明的目的运用乳液聚合合成一种球形聚合物刷，并以此电解质刷作为一种新型的大分子交联剂用于水凝胶的合成。
本发明的具体技术方案是：
一种多性能水凝胶，该水凝胶具有规则的内部三维网络结构，孔径在8-20微米。
进一步的，所述水凝胶的断裂伸长率达到9100％。
进一步的，所述水凝胶的可承受压强为1.75MPa。
进一步的，所述吸水溶胀率超过2000。
本发明还提出了一种多性能水凝胶的合成方法，取0.1-2g PS-PAA球形聚合物刷溶于水配成0.01-1wt％的水溶液，并取该溶液0.1-1mL，丙烯酸0.2-2mL，水0.3-2mL，光引发剂0.02-0.3g，混合于玻璃模具，并超声5-40min后，放置于紫外灯下照射10-120min后得到水凝胶。
进一步的，所述的PS-PAA聚合物刷是0.5-1.5g。
进一步的，所述聚合物刷溶于水配成0.1-0.5wt％的水溶液，取该水溶液0.2-0.5mL,丙烯酸0.3-1mL，水0.3-1mL，光引发剂0.05-0.1g，混合于玻璃模具，并超声10-30min后，放置于紫外灯下照射20-80min后得到水凝胶。
进一步的，所述PS-PAA球形聚合物刷是如下合成方法合成的，
(1)乳液聚合法合成PS核:1-8g(优选2-5g)苯乙烯单体，0.01-1g(优选0.05-0.5g)十二烷基磺酸钠(SDS)，0.01-1g(优选0.02-0.1g)过硫酸钾，20-150mL(优选30-100mL)去离子水于三口烧瓶中，机械搅拌。反应温度调节至283-373K(优选303-363K)，0.5-3h(优选1-2h)后降温至273-323K(优选273-303K)，将0.05-2g(优选0.1-0.5g)光引发剂溶液加入恒压滴液漏斗中并以0.05-2mL/min(优选0.3-1mL)的速度缓慢滴加到反应体系中，滴加完毕后，继续反应0.5-3h(优选1-2h)；
(2)在上述PS核表面均匀接入聚丙烯酸链(PAA):称取0.1-2g(优选0.5-1.5g)PS核乳液，稀释到固含量为0.01-1％(优选0.05-0.5％)，再按PS核固含量的50-100％(优选60-80％)称取丙烯酸，加入到烧瓶中，打开紫外灯及冷凝水，反应1-5h(优选1.5-3h)，反应结束，得到PS-PAA球形聚合物刷。
多性能水凝胶应用于催化反应(以丙烯酸含量为70％的S0.1A0.7水凝胶为例)：
取0.01-1g(优选0.02-0.5g)水凝胶放置于500mL烧杯中，同时加入20-200mL(优选50-150mL)0.05-0.2M(优选0.1-0.15M)AgNO3水溶液，室温下搅拌35-60h(优选40-50h)，以完成银离子的吸附。用去离子水多次洗涤水凝胶后，放置于50-200mL(优选100-150mL)0.1-1M(优选0.3-0.6M)NaBH4水溶液中，氮气鼓泡出去溶液中的氧气，在氮气氛围下，保持室温缓慢搅拌5-20h(优选10-15h)，完成银离子的还原反应。之后取负载完纳米银粒子的水凝胶0.01-1g(优选0.04-0.08g)，加入20-100mL(优选30-60mL)0.1-0.5M(优选0.2-04M)NaBH4和20-100mL(优选30-60mL)0.001-0.005M(优选0.002-0004M)对硝基苯酚溶液中，每隔1-4min(优选2-3min)进行紫外测试。用于催化还原对硝基苯酚的实验数据表明，该水凝胶作为催化剂载体负载银纳米粒子以后表现出较高的催化活性，且该催化剂易于回收和利用。
附图说明
图1水凝胶合成示意图；
图2水凝胶的内部结构扫描电镜图(以丙烯酸含量为50wt％的水凝胶为例)；
图3水凝胶的内部结构扫描电镜图(以丙烯酸含量为50wt％的水凝胶为例)；
图4水凝胶的内部结构扫描电镜图(以丙烯酸含量为50wt％的水凝胶为例)；
图5实施例1～5的五种不同丙烯酸含量水凝胶的拉伸性能测试曲线图；
图6实施例1～5的五种不同丙烯酸含量水凝胶的压缩性能测试曲线图；
图7实施例1～5的五种不同丙烯酸含量水凝胶的缺口不敏感性测试图；
图8实施例1～5的五种不同丙烯酸含量水凝胶吸水性能测试曲线图；
图9水凝胶作为催化剂载体负载银纳米粒子后催化性能曲线图。
具体实施方式
球形聚合物刷(PS-PAA)的合成
(1)乳液聚合法合成PS核:2g苯乙烯单体，0.1g十二烷基磺酸钠(SDS)，0.03g过硫酸钾，50mL去离子水于三口烧瓶中，机械搅拌。反应温度调节至333K，1h后降温至298K，将0.2g光引发剂溶液加入恒压滴液漏斗中并以0.5mL/min的速度缓慢滴加到反应体系中，滴加完毕后，继续反应1h。
(2)在上述PS核表面均匀接入聚丙烯酸链(PAA):称取1g PS核乳液，稀释到固含量为0.1％，再按PS核固含量的100％称取丙烯酸，加入到烧瓶中，打开紫外灯及冷凝水，反应1.5h，反应结束。
多性能水凝胶的制备(如图1所示)：
取1g上述合成的聚合物刷(PS-PAA)溶于水配成(0.1wt％)的水溶液，并取一定含量的该聚合物溶液，丙烯酸，水，光引发剂(具体含量配比见下表)混合于玻璃模具，并超声20min后，放置于紫外灯下照射30min后得到水凝胶。
下表是实施例1～5的五种不同丙烯酸含量的水凝胶组分含量
多性能水凝胶应用于催化反应(以丙烯酸含量为70％的S0.1A0.7水凝胶为例)
取0.044g水凝胶放置于500mL烧杯中，同时加入100mL 0.1M AgNO3水溶液，室温下搅拌48h，以完成银离子的吸附。用去离子水多次洗涤水凝胶后，放置于100mL 0.5M NaBH4水溶液中，氮气鼓泡出去溶液中的氧气，在氮气氛围下，保持室温缓慢搅拌12h，完成银离子的还原反应。之后取负载完纳米银粒子的水凝胶0.048g，加入50mL 0.216M NaBH4和50mL0.00216M对硝基苯酚溶液中，每隔3min进行紫外测试。
本发明多性能水凝胶结构表征和性能测试
图2-图4对该水凝胶(以丙烯酸含量为50％的水凝胶S0.1A0.5为例)的内部微观结构的扫描电镜图表明，该水凝胶具有规则的内部三维网络结构，孔径大约在8-20微米。
图5拉伸性能测试数据表明，该水凝胶具有良好的拉伸性能，最高的断裂伸长率可以达到9100％(丙烯酸含量为30％的S0.1A0.3水凝胶)。
图6压缩性能测试数据表明，该水凝胶也具备良好的抗压缩性能，最高可承受的压强可到1.75MPa(丙烯酸含量为30％的S0.1A0.3水凝胶)。
图7缺口不敏感性测试数据表明，这五种水凝胶都具有缺口不敏感性的性能。
图8吸水性能测试数据表明，该水凝胶具备极好的吸水性能，最大的吸水溶胀率可以超过2000(丙烯酸含量为30％的S0.1A0.3水凝胶)。
图9将该水凝胶作为催化剂载体负载银纳米粒子，用于催化还原对硝基苯酚的实验数据表明，该水凝胶作为催化剂载体负载银纳米粒子以后表现出较高的催化活性，且该催化剂易于回收和利用。
Claims (4)
1.一种多性能水凝胶，其特征在于，取0.1-2g PS-PAA球形聚合物刷溶于水配成0.01-1wt％的水溶液，并取该溶液0.1-1mL，丙烯酸0.2-2mL，水0.3-2mL，光引发剂0.02-0.3g，混合于玻璃模具，并超声5-40min后，放置于紫外灯下照射10-120min后得到水凝胶；
该水凝胶具有规则的内部三维网络结构，孔径在8-20微米；所述水凝胶的断裂伸长率达到9100％；所述水凝胶的可承受压强为1.75MPa；所述吸水溶胀率超过2000。
2.一种多性能水凝胶的合成方法，取0.1-2g PS-PAA球形聚合物刷溶于水配成0.01-1wt％的水溶液，并取该溶液0.1-1mL，丙烯酸0.2-2mL，水0.3-2mL，光引发剂0.02-0.3g，混合于玻璃模具，并超声5-40min后，放置于紫外灯下照射10-120min后得到水凝胶。
3.根据权利要求2所述的一种多性能水凝胶的合成方法，所述的PS-PAA聚合物刷是0.5-1.5g。
4.根据权利要求2所述的一种多性能水凝胶的合成方法，所述聚合物刷溶于水配成0.1-0.5wt％的水溶液，取该水溶液0.2-0.5mL,丙烯酸0.3-1mL，水0.3-1mL，光引发剂0.05-0.1g，混合于玻璃模具，并超声10-30min后，放置于紫外灯下照射20-80min后得到水凝胶。
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| CN106519152A (zh) * | 2016-10-24 | 2017-03-22 | 中国科学技术大学 | 一种聚合物纳米粒子、复合水凝胶及其制备方法 |
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| CN106519152A (zh) * | 2016-10-24 | 2017-03-22 | 中国科学技术大学 | 一种聚合物纳米粒子、复合水凝胶及其制备方法 |
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