CN113150356A - 一种磁性微球的表面修饰方法 - Google Patents
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Abstract
本发明涉及一种磁性微球的表面修饰方法，包括以下步骤：将表面聚乙烯亚胺分子修饰的磁性微球分散，加入环氧单体、双环氧化物和交联剂；然后加入引发剂，得到表面环氧化物修饰的磁性微球。本发明通过自由基聚合对10‑30μm的微球进行修饰，形成的聚合物微球表面均一度高，磁不易泄漏，并为微球后续多样化应用提供了基础。
Description
技术领域
本发明涉及高分子材料技术领域，尤其涉及一种磁性微球的表面修饰方法。
背景技术
磁性微球是通过适当方法将磁性无机粒子与有机高分子结合形成的具有一定磁性及特殊结构的复合微球。磁性复合微球不仅具有普通高分子微球的众多特性还具有磁响应性，所以不仅能够通过共聚及表面改性等方法赋予其表面功能基(如－OH、－COOH、－CHO、－NH2,等)，还能在外加磁场作用下具有导向功能。
磁性复合微球已广泛用于生物医学、细胞学和分离工程等诸多领域。磁性微球的表面特性对于应用非常重要，以聚合物进行的表面修饰，因官能团种类丰富、基团密度、亲疏水性可控而具有明显优势。当前，磁性微球的制备方法主要有高分子包埋法，单体聚合法，界面沉积法，原位法及无机磁性载体的制备等，在这些方法中单体聚合法应用最多，包括乳液聚合法、分散聚合法、悬浮聚合法、种子聚合法等，单体聚合法中，需要解决的关键问题是无机磁性纳米颗粒和有机烯类单体之间的相容性问题。
以聚合物进行表面修饰的方式和难易程度因磁性微球尺寸不同而差别明显：微米级以下的磁性微球可以直接通过自由基聚合在表面形成明显的聚合物壳层来完成表面修饰，而对于微米级以上特别是十几至几十微米大小的磁性微球，因微球尺寸大，磁珠存在下的自由基聚合很容易在磁珠以外成核得到聚合物微球，而不是在其表面形成聚合物层，因此很难在其表面通过自由基聚合的方式形成均一可控的表面。
发明内容
为解决上述技术问题，本发明提供了一种磁性微球的表面修饰方法，通过自由基聚合在微米级磁性微球表面进行聚合物修饰，磁颗粒不易泄漏且微球表面均一可控。
本发明的一种磁性微球的表面修饰方法，包括以下步骤：
(1)将表面聚乙烯亚胺分子修饰的磁性微球分散，加入环氧单体、双环氧化物和交联剂；
(2)向步骤(1)得到的混合物中加入引发剂，得到表面环氧化物修饰的磁性微球。
本发明磁性微球表面的聚乙烯亚胺中有大量的胺基，胺基可以与环氧基团(环氧单体、双环氧单体)进行开环反应，将环氧单体结合于磁珠的表面，之后再引发聚合，在磁珠表面形成聚合物修饰。
大尺寸磁性微球多是磁颗粒在聚合物微球上层层组装得到，磁颗粒暴露于微球外部或仅是高分子包裹，后续使用中因外部酸碱环境改变，可能会导致磁颗粒发生解离或是脱落。本发明中，表面环氧化物的修饰不仅仅有环氧基团，在交联剂存在下，通过自由基聚合在微球表面形成了交联的网络结构，对磁性微球起到良好的封闭作用，防止大尺寸磁性微球里的磁颗粒在反复的表面修饰过程中发生解离或是脱落。
进一步地，在步骤(1)中，环氧单体、双环氧化物和交联剂的质量比为1:1-2:1。
进一步地，在步骤(1)中，磁性微球选自聚苯乙烯微球、聚甲基丙烯酸甲酯微球和聚甲基丙烯酸缩水甘油酯微球中的一种或多种。
进一步地，在步骤(1)中，聚乙烯亚胺修饰的磁性微球的尺寸为10-30微米。
进一步地，在步骤(1)中，环氧单体为同时含一个碳碳双键和环氧基的单体，优选烯丙基缩水甘油醚、甲基丙烯酸缩水甘油酯。
进一步地，在步骤(1)中，双环氧化物选自1，4-丁二醇二缩水甘油醚、乙二醇二缩水甘油醚和丙三醇二缩水甘油醚中的一种或多种。双环氧化物一个环氧基与磁性微球表面的胺基开环反应，另一个环氧基团暴露于表面。
进一步地，在步骤(1)中，交联剂为含至少两个碳碳双键的单体，优选二乙烯基苯、乙二醇二甲基丙烯酸酯。
进一步地，在步骤(1)中，引发剂为水溶性过硫化物引发剂，优选过硫酸钾、过硫酸钠和过硫酸铵。
进一步地，在步骤(1)和步骤(2)中，反应温度为60-80℃。
进一步地，在步骤(1)和步骤(2)中，反应时间为10-15℃。
进一步地，在步骤(2)中，反应完成后，还包括清洗步骤。
本发明还要求保护上述制备方法制备的磁性微球。
借由上述方案，本发明至少具有以下优点：
(1)本发明的磁性微球通过自由基聚合完成修饰，形成的聚合物表层对磁性微球起到封闭作用，大尺寸聚合物微球表面均一度高，磁不易泄漏。
(2)本发明可对磁珠表面环氧基团进行改性，从而得到表面羟基、羧基、氨基等多种功能基团的不同表面特性的磁性微球，为多样化应用提供了基础。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合详细附图说明如后。
附图说明
为了使本发明的内容更容易被清楚的理解，下面根据本发明的具体实施例并结合附图，对本发明作进一步详细的说明，其中
图1为实施例1制备的磁性微球的扫描电镜图。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
实施例1
称取聚乙烯亚胺修饰的磁性微球1g(15um)分散于200g去离子水中，向其中加入甲基丙烯酸缩水甘油酯1g、1,4-丁二醇二缩水甘油醚2g、乙二醇二甲基丙烯酸酯1g，于80℃下反应10h，滴加过硫酸钠水溶液(1％)40g，滴加完毕，继续反应12h。依次用无水乙醇和去离子水清洗，得到表面环氧基团修饰的磁性微球。
实施例2
称取聚乙烯亚胺修饰的磁性微球1g(25um)分散于200g去离子水中，向其中加入烯丙基缩水甘油醚1g、乙二醇二缩水甘油醚1.5g、乙二醇二甲基丙烯酸酯1g，于70℃下反应12h，滴加过硫酸钠水溶液(1％)40g，滴加完毕，继续反应10h。依次用无水乙醇和去离子水清洗，得到表面环氧基团修饰的磁性微球。
实施例3
称取实施例2制备得到的表面环氧基团修饰的磁性微球1g分散于200g0.1M NaOH水溶液中，于75℃下搅拌4h，去离子水清洗至上清中性后，烘干得磁性微球粉末。取以上磁性微球粉末0.5g超声分散于100g N,N-二甲基甲酰胺，加入吡啶0.1g、琥珀酸酐1g，于室温下搅拌6h，依次用无水乙醇、0.1M NaOH、去离子水清洗至上清中性，得到表面羧基的磁性微球。
由图1可见，实施例1制备的磁性微球表面均一，无磁性颗粒聚集情况。
显然，上述实施例仅仅是为清楚地说明所作的举例，并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (10)
1.一种磁性微球的表面修饰方法，其特征在于，包括以下步骤：
(1)将表面聚乙烯亚胺分子修饰的磁性微球分散，加入环氧单体、双环氧化物和交联剂；
(2)向步骤(1)得到的混合物中加入引发剂，得到表面环氧化物修饰的磁性微球。
2.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述环氧单体、双环氧化物和交联剂的质量比为1:1-2:1。
3.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述磁性微球选自聚苯乙烯微球、聚甲基丙烯酸甲酯微球和聚甲基丙烯酸缩水甘油酯微球中的一种或多种。
4.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述环氧单体为同时含一个碳碳双键和环氧基的单体。
5.根据权利要求4所述的表面修饰方法，其特征在于：在步骤(1)中，所述同时含一个碳碳双键和环氧基的单体选自烯丙基缩水甘油醚和/或甲基丙烯酸缩水甘油酯。
6.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述双环氧化物选自1，4-丁二醇二缩水甘油醚、乙二醇二缩水甘油醚和丙三醇二缩水甘油醚中的一种或多种。
7.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述交联剂为含至少两个碳碳双键的单体。
8.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(1)中，所述交联剂选自二乙烯基苯和/或乙二醇二甲基丙烯酸酯。
9.根据权利要求1所述的表面修饰方法，其特征在于：在步骤(2)中，所述引发剂为水溶性过硫化物引发剂。
10.一种权利要求1-9任一项所述的制备方法制备的磁性微球。
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| CN108192081A (zh) * | 2017-12-28 | 2018-06-22 | 苏州英芮诚生化科技有限公司 | 一种环氧树脂包覆的磁珠的制备方法 |
| CN108620048A (zh) * | 2018-05-25 | 2018-10-09 | 天津大学 | 聚乙烯亚胺修饰的磁性微球制备方法及应用 |
| CN108745220A (zh) * | 2018-05-14 | 2018-11-06 | 苏州知益微球科技有限公司 | 一种均粒环氧基磁性微球的制备方法 |
| CN110713565A (zh) * | 2019-09-26 | 2020-01-21 | 浙江海洋大学 | 一种超支化pei修饰的磁性二氧化硅分子印迹聚合物的制备方法 |
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| CN108192081A (zh) * | 2017-12-28 | 2018-06-22 | 苏州英芮诚生化科技有限公司 | 一种环氧树脂包覆的磁珠的制备方法 |
| CN108745220A (zh) * | 2018-05-14 | 2018-11-06 | 苏州知益微球科技有限公司 | 一种均粒环氧基磁性微球的制备方法 |
| CN108620048A (zh) * | 2018-05-25 | 2018-10-09 | 天津大学 | 聚乙烯亚胺修饰的磁性微球制备方法及应用 |
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