CN109970897A - 一种无机/高分子复合材料及其制备方法 - Google Patents
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Abstract
本发明提供一种无机/高分子复合材料的制备方法，包括以下步骤，将聚合单体和无机半导体混合,密封，在紫外光源的照射下进行本体聚合，所述聚合物单体与无机半导体的质量之比为7：3～999：1。所述聚合单体为丙烯酰胺、N,N‑二甲基丙烯酰胺、N,N‑亚甲基双丙烯酰胺、甲基丙烯酰胺、N‑异丙基丙烯酰胺、丙烯酰吗啉或1，3，5‑三丙烯酰基六氢均三嗪中的一种或几种；所述无机半导体为纳米TiO2、纳米ZnO、纳米Fe3O4、纳米Fe2O3、纳米CdS中的一种或几种；所述紫外光源的光强为30～50mW/cm2。本发明还提供由该制备方法制备得到的无机/高分子复合材料，本发明所制备的无机/高分子复合材料中的无机半导体粒子分布均匀。
Description
技术领域
本发明涉及高分子复合材料制备领域，具体地，涉及一种无机/高分子复合材料的制备方法，更涉及一种无机/高分子复合材料。
背景技术
传统的无机/高分子复合材料是由半导体光催化聚合制得的，这反应需要采用溶剂，反应原料在溶剂中进行分散聚合和溶液聚合。(Scientific Reports,2016,6:20981；Nano letters,2017,17(7):4497-4501；Progress in Organic Coatings,2018,115:1-8.)1918-1922.)。
在反应过程中，受激发的无机半导体容易与溶剂形成无机半导体复合物，而该无机半导体复合物不溶于溶剂，造成反应体系形成两相溶液，因而造成制备得到的无机/高分子复合材料的无机半导体颗粒分布不均匀。再者，由于使用了溶剂，反应得到的无机/高分子复合材料需要复杂的分离、提纯操作。
发明内容
本发明为克服上述现有技术所述的至少一种缺陷，提供一种无机/高分子复合材料的制备方法。所述制备方法制备得到无机/高分子复合材料，所述无机/高分子复合材料中的无机粒子分布均匀，且该方法操作简单，不需要复杂的分离、提纯操作。
本发明的另一个目的在于提供所述制备方法制备得到的无机/高分子复合材料。所制备的无机/高分子复合材料中的无机粒子分布均匀。
本发明的一种无机/高分子复合材料的制备方法，将聚合单体和无机半导体混合,密封，在紫外光源的照射下进行本体聚合，所述聚合物单体与无机半导体的质量之比为7：3～999：1；所述聚合单体为丙烯酰胺、N,N-二甲基丙烯酰胺、N,N-亚甲基双丙烯酰胺、甲基丙烯酰胺、N-异丙基丙烯酰胺、丙烯酰吗啉或1，3，5-三丙烯酰基六氢均三嗪中的一种或几种；所述无机半导体为纳米TiO2、纳米ZnO、纳米Fe3O4、纳米Fe2O3、纳米CdS中的一种或几种，所述紫外光源的光强为30～50mW/cm2。
本发明的原理是将具有丙烯酰胺结构的聚合单体、无机半导体作为光敏剂，混合形成感光液。紫外光激发感光液，感光液中的无机半导体吸收光子产生空穴-电子对，空穴-电子对向丙烯酰胺结构的单体转移引发单体聚合，得到无机/高分子复合材料，由于感光液不会分散形成两相溶液，无机半导体不会聚集，使得制得的无机/高分子复合材料颗粒分布均匀。
进一步地，所述无机半导体的粒径为10～50nm。使用10～50nm粒径的无机半导体，反应速率快，反应时间不超过2h，而反应时间过长，会使形成的分子链在氧化环境中氧化降解，影响体系的转化率。
进一步地，所述聚合单体为N,N-二甲基丙烯酰胺、N,N-亚甲基双丙烯酰胺的组合，其中所述N,N-二甲基丙烯酰胺与N,N-亚甲基双丙烯酰胺的质量之比为18.9：1。这种组合的选择，使得无机/高分子复合材料表面较粗糙。
进一步地，所述无机半导体为锐钛型TiO2。利用锐钛型TiO2制备得到的无机/高分子复合材料，其表面更为连续，表面应力分散，这种无机/高分子复合材料不容易生成裂纹。
进一步地，所述锐钛型TiO2的粒径为25nm。
进一步地，所述紫外光源的光强为30mW/cm2。
进一步地，所述聚合物单体与无机半导体的质量之比为19：1～199：1。
本发明还提供一种由所述制备方法制备得到无机/高分子复合材料。
与现有技术相比，本发明的有益效果是：
1.本发明公开的制备方法制备得到无机/高分子复合材料，所述无机/高分子复合材料中的无机半导体粒子分布均匀。该方法优化了用于高分子聚合的无机半导体材料的制备工艺条件，操作简单，不需要复杂的分离、提纯操作。
2.本发明制得的无机/高分子复合材料，表面有一定粗糙度，并且无机/高分子复合材料中的无机半导体粒子分布均匀。
附图说明
图1为紫外引发机理图；
图2是本发明对比例1制备得到的无机纳米粒子复合物的扫描电子显微镜图；
图3是本发明实例2制备得到的无机/高分子复合材料扫描电子显微镜图；
图4是本发明实例9制备得到的无机/高分子复合材料扫描电子显微镜图；
图5是本发明实例14制备得到的无机/高分子复合材料扫描电子显微镜图；
图6是本发明实例17制备得到的无机/高分子复合材料扫描电子显微镜图；
图7是N,N-二甲基丙烯酰胺单体的核磁共振氢谱图；
图8是本发明实例2制备得到的无机/高分子复合材料核磁共振氢谱图；
图9是本发明实例9制备得到的无机/高分子复合材料核磁共振氢谱图；
图10是本发明实例14制备得到的无机/高分子复合材料核磁共振氢谱图；
图11是本发明实例17制备得到的无机/高分子复合材料核磁共振氢谱图。
具体实施方式
下面结合具体实施方式对本发明作进一步的说明。
以下实施例是在紫外光源的辐射波长为250～400nm的中压汞灯点光源下制备的，在中压汞灯点光源的光照40min，反应温度为30℃。
实施例1
在25mL配有磁力搅拌器圆底烧瓶中，加入丙烯酰胺和纳米25nm锐钛型TiO2光敏剂，丙烯酰胺和纳米25nm锐钛型TiO2光敏剂的质量比为199：1，在搅拌下，通氮气20min后用石英玻璃塞密封，振荡10min，然后超声分散20min，将团聚的纳米颗粒打散。然后用光强为30mW/cm2的中压汞灯点光源，从反应器的顶端光照40min，反应温度为30℃。在紫外光照下进行本体聚合，紫外光激发感光液，感光液中的无机半导体吸收光子产生空穴-电子对，空穴-电子对向丙烯酰胺转移引发单体聚合，得到无机/高分子复合材料。引发机理如图1所示。
实施例2～19
实施例2-实施例19的制备方法基本与实施例1相同，主要区别在于如以下表1所示。
表1
对比例1
在25mL配有磁力搅拌器圆底烧瓶中，将0.01g德固赛P-25纳米颗粒溶于加入蒸馏水中，搅拌，通氮气20min后用石英玻璃塞密封，然后用光强为30mW/cm2的中压汞灯点光源，从反应器的顶端光照40min，反应温度为30℃。光照结束后，得到的无机纳米粒子复合物。所得凝胶状产物，冷冻干燥后的扫描电子显微镜照片如图2所示。表面粗糙度较小，且无机纳米粒子分布不均匀。
表征
选择部分实施例的实验结果进行扫描电子显微镜和核磁共振，得到图3-图6的扫描电子显微镜图，以及图8-图11的核磁共振氢谱图。图2是对比例1制备的无机纳米粒子复合物扫描电子显微镜图；图7是N,N-二甲基丙烯酰胺单体的核磁共振氢谱图。
结合图2和图3-图6，经过冷冻干燥除去未反应的聚合单体和无机半导体，所得的凝胶状无机/高分子复合材料表面有一定粗糙度，无机半导体粒子分布均匀。
结合图7和图8-图11分析，除N,N-二甲基丙烯酰胺单体特征氢的化学位移外，聚合物化学位移1.42对应的次甲基-CH-上的氢，1.83对应于亚甲基-CH2-上的氢，7.19为溶剂峰，说明了N,N-二甲基丙烯酰胺单体聚合形成了无机/高分子复合材料。
结合图2和图5，从扫面电镜图像可以看出，用ZnO光敏剂制备得到的无机/高分子复合材料，比用溶液聚合制备得到的粒子，分布更均匀，且比用溶液聚合得到的无机纳米粒子复合物表面粗糙。结合图3和图5，从扫面电镜图像可以看出，光敏剂为锐钛型TiO2的无机/高分子复合材料的表面更为连续，而用ZnO光敏剂制得的无机/高分子复合材料，则更多的分布在表面，聚合物连续性下降，会造成表面应力集中，使材料更容易生成裂纹。
结合图3和图4，从后扫面电镜图像可以看出，N，N-二甲基丙烯酰胺制备得到的无机/高分子复合材料，其表面比丙烯酰吗啉制得的无机/高分子复合材料粗糙。
结合图3和图6，从整体上看只使用N，N-二甲基丙烯酰胺单体的表面更为平整，而N，N-二甲基丙烯酰胺和N，N-亚甲基双丙烯酰胺共混单体的表面较粗糙。
评价分散度
本申请所称的分散度，是评价无机粒子分布的分散均匀程度，通过观察扫描电镜图中粒子的分布，以1-10为评价范围。
数值越高，说明无机离子越分散；数值越低，说明无机离子越聚合。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。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的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。
Claims (8)
1.一种无机/高分子复合材料的制备方法，其特征在于，将聚合单体和无机半导体混合,密封，在紫外光源的照射下进行本体聚合，所述聚合物单体与无机半导体的质量之比为7：3～999：1；
所述聚合单体为丙烯酰胺、N,N-二甲基丙烯酰胺、N,N-亚甲基双丙烯酰胺、甲基丙烯酰胺、N-异丙基丙烯酰胺、丙烯酰吗啉或1，3，5-三丙烯酰基六氢均三嗪中的一种或几种；
所述无机半导体为纳米TiO2、纳米ZnO、纳米Fe3O4、纳米Fe2O3、纳米CdS中的一种或几种；
所述紫外光源的光强为30～50mW/cm2。
2.根据权利要求1所述无机/高分子复合材料的制备方法，其特征在于，所述无机半导体的粒径为10～50nm。
3.根据权利要求1所述无机/高分子复合材料的制备方法，其特征在于，所述聚合单体为N,N-二甲基丙烯酰胺与N,N-亚甲基双丙烯酰胺的组合，其中所述N,N-二甲基丙烯酰胺与N,N-亚甲基双丙烯酰胺的质量之比为18.9：1。
4.根据权利要求1所述无机/高分子复合材料的制备方法，其特征在于，所述无机半导体为锐钛型TiO2。
5.根据权利要求4所述无机/高分子复合材料的制备方法，其特征在于，所述无机半导体的粒径为25nm。
6.根据权利要求1所述无机/高分子复合材料的制备方法，其特征在于，所述紫外光源的光强为30mW/cm2。
7.根据权利要求1所述无机/高分子复合材料的制备方法，其特征在于，所述聚合物单体与无机半导体的质量之比为19：1～199：1。
8.权利要求1～7任一所述制备方法制备得到的无机/高分子复合材料。
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