CN107936259A - 一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法 - Google Patents
一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法。首先通过可逆加成断裂链转移自由基(RAFT)聚合制备了温敏外臂,然后在加入交联剂的同时进一步加入可以捕获和原位还原Au3+的功能单体。最后加入金纳米粒子的前驱体,在不外加还原剂的条件下,通过中心内核中功能单体和Au3+的相互作用,使得金纳米粒子精确的还原在温度响应型核交联星型聚合物的内核中。本发明利用温度响应型核交联星型聚合物作为还原剂和稳定剂制备尺寸不同的窄分布的金纳米粒子,可以用于催化、免疫分析、生物检测、临床诊断等方面。另外由于聚合物是温敏性的,因而通过改变温度还可以实现金纳米粒子的循环利用。
Description
技术领域
本发明涉及一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法,属于高分子材料和纳米材料领域。
背景技术
金纳米粒子具有尺寸和形貌依赖的性能,在光学、电学、磁学、药物的负载、催化等领域有着重要的应用。但由于较大的比表面积以及表面较高的反应活性使得金纳米粒子很容易聚集。目前主要以含硫醇的化合物充当稳定剂,在外加还原剂的条件下制备金纳米粒子。但是在某些条件下(较高的温度、光照)S-Au键是不稳定的,使得稳定剂从金纳米粒子表面剥离,导致金纳米粒子聚集。
星型聚合物是指多个线形外臂连接到同一中心核上的非线性聚合物.目前主要通过“臂优先”、“核优先”、以及“接枝”这三种途径制备星型聚合物。通过“臂优先”的途径所制备的星型聚合物由于中心内核的尺寸有别于其他的星型聚合物,因而这种方法所制备的星型聚合物又被称之为核交联星型聚合物(CCS polymer)。星型聚合物因为有着不同于线性聚合物的拓扑结构,使得其物理/化学性能也有别于线性聚合物,在药物的负载、基因转染、催化材料、抗菌和防污的生物材料等领域有着广泛的应用。
用核交联星型聚合物作为模板,通过原位还原的方法制备金纳米粒子,与目前一些制备金纳米粒子的方法相比有着一下的优点:首先相比于传统的聚合物胶束,由于内部是交联的因而核交联星型聚合物不存在临界胶束浓度,稳定性更高。其次制备核交联星型聚合物通常采用活性聚合,因而可以精确控制核交联星型聚合物的结构,从而进一步可以实现纳米粒子在核交联星型聚合物上不同位置上的精确负载,制备不同结构的纳米粒子。再次由于核交联星型聚合物的外臂是永久的连接在纳米粒子上的因而所制备的纳米粒子有着更高的稳定性。另外由于核交联星型聚合物结构可设计性,在聚合过程中可以可以引入温敏单体,制备温度响应型的核交联星型聚合物,从而可以制备分散状态可控的“智能”的纳米粒子。
发明内容
本发明的目的是提供一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法。通过“臂优先”的途径及RAFT聚合,制备出了可以负载金纳米粒子的温度响应型核交联星型聚合物。然后进一步加入氯金酸,通过原位还原就可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中。
为实现上述目的,本发明采用的技术方案为:
(1)温度响应型核交联星型聚合物的合成
将链转移剂三硫代碳酸酯(DMP)、温敏单体和油溶性引发剂偶氮二异丁腈(AIBN),按照1:(50~100):0.1摩尔比加入到乙腈中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,得到温度响应型外臂,其中温敏单体可以是NIPAM、PEGA或者是DEGA。将上述的温度响应型外臂作为大分子链转移剂、功能单体、交联剂和引发剂AIBN,按照(50~100):(10~50):(100~200):1质量比加到乙醇中,其中功能单体可以是DMAEMA、AA或者是4-VP,交联剂可以是Bis或者是DVB,在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,便得到纯净的可以负载金纳米粒子的温度响应型核交联星型聚合物。
(2)金纳米粒子的负载
取一定量的上述所制备的温度响应型核交联星型聚合物溶到pH=7的溶液中,然后再加入不同含量的氯金酸,避光搅拌便可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中,其中核交联星型聚合物和氯金酸的质量比为(10~50):1,核交联星型聚合物的浓度为5~50mg/ml。
与现有技术相比,本发明具有如下优点:
(1)核交联星型聚合物的内核中含有与Au3+有相互作用的功能单体,不需要外加还原剂,就可以将金纳米粒子还原,避免了还原剂加入反应之后所引入的小分子;
(2)核交联星型聚合物的外臂是永久连接在金纳米粒子上的,在较低温度下,亲水的外臂可以形成较强的空间位阻,阻碍了金纳米粒子的聚集,因而在此条件下金纳米粒子有着较高的催化性能;
(3)核交联星型聚合物的外臂是温敏性的,温度的升高,外臂的构像会从亲水的无规线团转变为疏水的球体,因而通过升高温度,外臂的疏水性会增强,从而使得金纳米粒子聚集沉淀,实现金纳米粒子的循环利用。
附图说明
图1是本发明的温度响应型核交联星型聚合物负载金纳米粒子的合成示意图;
图2是本发明的温度响应型核交联星型聚合物负载了金纳米粒子之后的紫外光谱;
图3是本发明的温度响应型核交联星型聚合物负载金纳米粒子的透射电子显微镜;
图4是本发明的温度响应型核交联星型聚合物负载金纳米粒子之后催化对硝基酚的紫外谱。
具体实施方式:
实施例1
(1)温度响应型核交联星型聚合物的合成
将链转移剂三硫代碳酸酯(DMP)、温敏单体(PEGA)和油溶性引发剂偶氮二异丁腈(AIBN),按照1:50:0.1摩尔比加入到乙腈中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,得到温度响应型外臂。将上述的温度响应型外臂作为大分子链转移剂、功能单体(DMAEMA)、交联剂(二乙烯苯(DVB))和引发剂(AIBN),按照50:10:100:1摩尔比加到乙醇中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,便得到纯净的可以负载金纳米粒子的温度响应型核交联星型聚合物。
(2)温度响应型核交联星型聚合物用于金纳米粒子的负载
取30mg上述所制备的温度响应型核交联星型聚合物溶到3mL的pH=7的溶液中,加入2mg氯金酸,避光搅拌便可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中。
实施例2
(1)温度响应型核交联星型聚合物的合成
将链转移剂三硫代碳酸酯(DMP)、温敏单体(DEGA)和油溶性引发剂偶氮二异丁腈(AIBN),按照1:50:0.1摩尔比加入到乙腈中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,得到温度响应型外臂。将上述的温度响应型外臂作为大分子链转移剂、功能单体(DMAEMA)、交联剂(二乙烯苯(DVB))和引发剂AIBN,按照50:10:100:1质量比加到乙醇中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,便得到纯净的可以负载金纳米粒子的温度响应型核交联星型聚合物。
(2)温度响应型核交联星型聚合物用于金纳米粒子的负载
取30mg上述所制备的温度响应型核交联星型聚合物溶到3mL的pH=7的溶液中,加入2mg氯金酸,避光搅拌便可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中。
实施例3
(1)温度响应型核交联星型聚合物的合成
将链转移剂三硫代碳酸酯(DMP)、温敏单体(PEGA)和油溶性引发剂偶氮二异丁腈(AIBN),按照1:50:0.1摩尔比加入到乙腈中。在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,得到温度响应型外臂。将上述的温度响应型外臂作为大分子链转移剂、功能单体(AA)、交联剂(二乙烯苯(DVB))和引发剂(AIBN),按照50:10:100:1质量比加到乙醇中,在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,便得到纯净的可以负载金纳米粒子的温度响应型核交联星型聚合物。
(2)温度响应型核交联星型聚合物用于金纳米粒子的负载
取30mg上述所制备的温度响应型核交联星型聚合物溶到3mL的pH=7的溶液中,加入2mg氯金酸,避光搅拌便可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中。
Claims (4)
1.一种可以负载金纳米粒子的温度响应型核交联星型聚合物及其制备方法,其特征在于制备过程如下所示:
A.将链转移剂三硫代碳酸酯(DMP)、温敏单体和油溶性引发剂偶氮二异丁腈(AIBN),按照1:(50~100):0.1摩尔比加入到乙腈中,在惰性气氛下,60~80℃反应12~24h,聚合结束后,对聚合物提纯,得到温度响应型外臂,其中温敏单体可以是N-异丙基丙烯酰胺(NIPAM)、聚乙二醇单甲醚(PEGA)或者是丙烯酸乙氧基乙氧基乙酯(DEGA);
B.将上述的温度响应型外臂作为大分子链转移剂,再依次加入功能单体、交联剂和引发剂AIBN,按照(50~100):(10~50)(100~200):1质量比加到乙醇中,在惰性气氛下,60~80℃反应12~24h,聚合结束后,通过沉淀,便得到纯净的可以负载金纳米粒子的温度响应型核交联星型聚合物,其中功能单体是甲基丙烯酸二甲氨基乙酯(DMAEMA)、丙烯酸(AA)、4-乙烯基吡啶(4-VP)这几种单体的一种,交联剂可以是N,N-亚甲基双丙烯酰胺(Bis)或者是二乙烯苯(DVB);
C.取一定量的上述所制备的温度响应型核交联星型聚合物溶到去离子水中,其中溶液的pH=3~8,然后再加入不同含量的氯金酸,避光搅拌便可以将金纳米粒子负载到温度响应型核交联星型聚合物的内核中,其中核交联星型聚合物和氯金酸的质量比为(10~50):1,核交联星型聚合物的浓度为5~30mg/ml。
2.根据权利要求1所述的可以负载金纳米粒子的温度响应型核交联星型聚合物,其特征在于外臂是由具有温敏性的单体NIPAM、PEGA或者DEGA聚合形成的,随着温度的升高,外臂会从亲水形式转变为疏水形式,从而可以改变金纳米粒子在溶液中的溶解性,进一步影响金纳米粒子的催化性能。
3.根据权利要求1所述的可以负载金纳米粒子的温度响应型核交联星型聚合物,其特征在于内核含有可以捕获和原位还原Au3+的DMAEMA、AA或者4-VP作为功能单体,加入金纳米粒子的前驱体之后,利用聚合物自身的作用就可以将金纳米粒子负载到内核中,避免了还原剂的加入。
4.根据权利要求1所述的可以负载金纳米粒子的温度响应型核交联星型聚合物,其特征在于所制备的温敏外臂的分子量为0.5×104~5×104;核交联星型聚合物的分子量为10×104~100×104。
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