抗菌型聚丙烯酸酯基纳米复合乳液的合成与性能研究
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摘要
聚丙烯酸酯以其优异的光稳定性、化学稳定性、成膜柔软、膜光洁透明等性能，被广泛应用于皮革涂饰剂、纺织涂层剂、木器漆、建筑涂料等领域中。但是，纯聚丙烯酸酯本身存在着“热粘冷脆”、抗菌性、卫生性能差等缺陷。近年来，随着纳米科技的快速发展，聚合物基无机纳米复合乳液迅速成为材料领域的研究热点。
本研究正是基于以上背景，通过对无机纳米材料进行筛选，优选出抗菌性能优异的无机纳米材料并将其引入聚丙烯酸酯中，研究无机纳米材料的尺寸、形貌对复合乳液及薄膜性能的影响，制备一种“软而不粘”、抗菌性优异、卫生性能良好的聚丙烯酸酯基纳米复合乳液。具体内容包括以下几个方面：
1.首先对无机纳米材料进行筛选，考察市售氧化镁(MgO)、二氧化钛(TiO_2)、氧化锌(ZnO)、三氧化二铝(Al2O3)、蒙脱土(MMT)、二氧化硅(SiO2)等不同种类的无机纳米材料对聚丙烯酸酯乳液及薄膜性能，尤其是抗菌性的影响。然后，以阴离子型聚合物(PA30)为分散剂对优选出的纳米ZnO进行表面改性，对其改性条件进行优化；最后，将PA30改性纳米ZnO引入聚丙烯酸酯中，对聚丙烯酸酯/纳米ZnO复合乳液的制备工艺进行探索和初步优化。
2.由于纳米ZnO形貌丰富、结构多样，且纳米ZnO形貌、尺寸对材料性能有较大的影响。因此，采用微波水热技术制备不同尺寸的球形ZnO以及不同形貌的纳米ZnO；通过扫描电镜(SEM)、X射线衍射(XRD)等对产物的形貌结构进行表征；考察了球形ZnO尺寸及纳米ZnO形貌对纳米ZnO性能的影响。然后，采用常规乳液聚合法在PA30改性纳米ZnO的分散液中原位引发丙烯酸酯类单体聚合，制备聚丙烯酸酯/纳米ZnO复合乳液。考察球形ZnO尺寸、纳米ZnO形貌对复合乳液及薄膜、涂饰后革样及整理后织物性能的影响。
结果表明：球形ZnO及聚丙烯酸酯/球形ZnO纳米复合薄膜的抗菌性随球形ZnO尺寸的增大而降低。与其他几种形貌ZnO相比，球形ZnO、花状ZnO均具有良好的抗菌和紫外吸收性能；聚丙烯酸酯/球形ZnO纳米复合薄膜、聚丙烯酸酯/花状ZnO纳米复合薄膜对白色念珠菌的抗菌效果良好，但对霉菌的抗菌效果不佳。
与纯聚丙烯酸酯乳液涂饰后革样相比，聚丙烯酸酯/花状ZnO纳米复合乳液涂饰后革样的透气性提高了232.65%。聚丙烯酸酯/球形ZnO纳米复合乳液整理后织物的透湿率较纯聚丙烯酸酯乳液整理后织物提高了129.21%。
聚丙烯酸酯/球形ZnO纳米复合薄膜的抗菌作用由锌离子的溶出作用和ZnO的光催化作用共同所致，聚丙烯酸酯/花状ZnO纳米复合薄膜的抗菌作用则以ZnO的光催化作用为主。
3.对抗菌性能较优的球形、花状ZnO进行掺银处理，以提高其对霉菌的抗菌效果；采用SEM、XRD、TEM等对复合粒子的形貌结构及组成进行分析；考察化学吸附还原法、微波辅助还原法和氧化还原法等三种纳米粒子制备方法以及纳米粒子形貌对粒子性能的影响。然后，采用常规乳液聚合法在PA30改性纳米ZnO/Ag复合粒子的分散液中原位引发丙烯酸酯类单体聚合，制备聚丙烯酸酯/纳米ZnO/Ag复合乳液；考察复合粒子制备方法、复合粒子形貌、用量对乳液及薄膜性能的影响。最后，将所得乳液应用到皮革、纺织涂层中考察其应用性能。
结果表明：采用化学吸附还原法所制备的花状ZnO/Ag复合粒子以及含该复合粒子的聚丙烯酸酯薄膜的抗菌性优于采用微波辅助还原法和氧化还原法所制备的复合粒子。掺银以后纳米粒子及复合薄膜对霉菌的抗菌效果显著提高。
球形ZnO/Ag复合粒子和花状ZnO/Ag复合粒子的抗菌性能相差不大。但是，聚丙烯酸酯/花状ZnO/Ag纳米复合薄膜的抗菌性能优于聚丙烯酸酯/球形ZnO/Ag纳米复合薄膜。
与纯聚丙烯酸酯乳液涂饰后革样相比，采用聚丙烯酸酯/花状ZnO/Ag纳米复合乳液涂饰后革样的透气性提高了138.46%；采用聚丙烯酸酯/花状ZnO纳米复合乳液整理后织物的透湿性最好，较纯聚丙烯酸酯乳液整理后织物提高了12.84%。
聚丙烯酸酯/花状ZnO/Ag纳米复合薄膜的抗菌作用主要以花状ZnO/Ag复合粒子的光催化抗菌为主，Ag系抗菌剂的金属粒子接触抗菌为辅；复合薄膜对白色念珠菌、霉菌抗菌效果的差异，与两种菌种的细胞壁结构和化学组成密切相关。
本研究所研制的聚丙烯酸酯基纳米复合薄膜“软而不粘”、抗菌性能优异、卫生性能良好。反应以水为介质，安全环保、无毒、无污染。目前，有关纳米材料形貌、尺寸对复合材料性能，尤其是抗菌性能影响的研究国内外还鲜见报道。
As one of the most common used film-forming materials, polyacrylate is widely used in leather finishing agent, textile adhesive, wood and construction paints due to its excellent gloss, flexibility, transparent and chemical stability. However, the drawback of neat polyacrylate, such as weak climate-resistance, poor antimicrobial activities and lower sanitation properties often restrict its application. Recently, polymer/inorganic nanocomposites have attracted a great deal of attention with the rapid development of nanotechnology.
This research is based on the above background. Inorganic nanomaterials with excellent antimicrobial activities were bought into polyacrylte firstly. Then the influences of inorganic nanomaterials with different morphologies and sizes on the properties of the nanocomposites were investigated in details. At last, polyacrylate-based nanocomposites with excellent antibacterial and sanitation properties were obtained. The main contents are listed as follows.
1. The effects of inorganic nanoparticles including commercially MgO, TiO2, ZnO, Al2O3, MMT and SiO2on the properties of the nanocomposites were investigated in details. Then anionic polymer (PA30) was used to modify the chosen ZnO, and the optimum modification conditions were obtained. At last, the preparation method and optimum conditions of polyacrylate/ZnO nanocomposites were studied.
2. There are various ZnO nano structures with different shapes and sizes, and each of them displays some unique properties. ZnO nano structures with various morphologies and sizes were successfully obtained via microwave-assisted hydrothermal process in this study. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to investigate the morphology and crystal structure of obtained ZnO. Then polyacrylate/ZnO nanocomposite latexes were prepared by in-situ emulsion polymerization of acrylate monomers in the presence of PA30modified ZnO nanostructures. The influences of ZnO nano structures with various morphologies and sizes on the performances of the obtained ZnO, nanocompsite latexes and films, as well as the finished leather samples and treated fabrics were investigated.
The results showed that the antimicrobial activities of sphere-like ZnO and polyacrylate/sphere-like ZnO nanocompsoite film were both decreased with the increasing of the diameter of ZnO.
Sphere-like ZnO and flower-like ZnO had better antimicrobial activities and ultraviolet absorption property than those of ZnO with other morphologies. Polyacrylate-based films containing sphere-like ZnO and flower-like ZnO showed excellent antimicrobial activities on candida albicans. However, the antimicrobial activities of films containing sphere-like ZnO and flower-like ZnO on aspergillus flavus were poor.
Experimental results showed that vapor permeability of the leather finished by polyacrylate/flower-like ZnO nanocomposite latex increased by232.65%, compared to that finished by pure polyacrylate latex. The moisture permeability of fabric treated by polyacrylate/sphere-like ZnO nanocomposite latex was increased by129.21%, compared to that treated by pure polyacrylate latex.
The releasing of Zn ions and the photo catalysis activity of ZnO played an important role in the antimicrobial activities of polyacrylate/ZnO nanocomposite film containing sphere-like ZnO, and the excellent antimicrobial properties of polyacrylate-based film containing flower-like ZnO might attribute to the photo catalysis activity of ZnO.
3. Ag particles were doped on the surface of sphere-like ZnO and flower-like ZnO to improve the antimicrobial activities of ZnO on aspergillus flavus. SEM, XRD and TEM were used to investigate the morphology, structure and chemical composition of the obtained composite particles. The influences of different methods including chemical and adsorption reduction method, microwave-assisted reduction method and oxidation-reduction method, and the morphologies of ZnO on the properties of the obtained ZnO/Ag composite particles were investigated. Then polyacrylate/ZnO/Ag nanocomposites were obtained by in-situ emulsion polymerization of acrylate monomers in the presence of PA30modified ZnO/Ag composite particles. The effects of ZnO/Ag composite particles with different preparation methods, morphologies, and the dosages of ZnO/Ag composite particles on the properties of the polyacrylate/ZnO/Ag nanocompsite latexes and films were investigated in detail. At last, the composite latex was used in leather finishing and textile treating.
The results indicated that the antimicrobial activities of ZnO/Ag composite particles and polyacrylate/flower-like ZnO/Ag composite prepared by chemical and adsorption reduction method were higher than that prepared by microwave-assisted reduction method and oxidation-reduction method. Besides, the inhibition abilities to aspergillus flavus were greatly improved with the doping of Ag on the surface of ZnO.
The antimicrobial activities of sphere-like ZnO/Ag composite particles and flower-like ZnO/Ag composite particles were almost alike. However, the antimicrobial activities of the film containing flower-like ZnO/Ag composite particles was higher than that of the film containing sphere-like ZnO/Ag composite particles.
Experimental results showed the vapor permeability of the leather finished by polyacrylate/flower-like ZnO/Ag composite latex was increased by138.46%, compared to that finished by polyacrylate/flower-like ZnO composite latex. The moisture permeability of fabrics treated by polyacrylate/flower-like ZnO composite latex was increased by12.84%, compared to that treated by pure polyacrylate latex.
The photocatalysis activites of ZnO/Ag composite particles played an important role in the antimicrobial activities of polyacrylate/flower-like ZnO/Ag nanocomposite film. The contaction of metal ions also influenced the antimicrobial activities of the nanocomposite film. However, the reason for the different antimicrobial activities on candida albicans and aspergillus flavus were probably due to the different structures and compositions of the two kinds of bacteria.
Polyacrylate-based nanocomposites prepared by the above method had excellent antimicrobial and sanitation properties. The as-prepared composite film was soft but not sticky. Besides, the reaction was carried out in water media, which was non-toxic, pollution-free, and safe. There were few reports about the influences of inorganic nanomaterials with different morphologies and sizes on the properties of the nanocomposites, especially the antimicrobial activities.
本研究正是基于以上背景，通过对无机纳米材料进行筛选，优选出抗菌性能优异的无机纳米材料并将其引入聚丙烯酸酯中，研究无机纳米材料的尺寸、形貌对复合乳液及薄膜性能的影响，制备一种“软而不粘”、抗菌性优异、卫生性能良好的聚丙烯酸酯基纳米复合乳液。具体内容包括以下几个方面：
1.首先对无机纳米材料进行筛选，考察市售氧化镁(MgO)、二氧化钛(TiO_2)、氧化锌(ZnO)、三氧化二铝(Al2O3)、蒙脱土(MMT)、二氧化硅(SiO2)等不同种类的无机纳米材料对聚丙烯酸酯乳液及薄膜性能，尤其是抗菌性的影响。然后，以阴离子型聚合物(PA30)为分散剂对优选出的纳米ZnO进行表面改性，对其改性条件进行优化；最后，将PA30改性纳米ZnO引入聚丙烯酸酯中，对聚丙烯酸酯/纳米ZnO复合乳液的制备工艺进行探索和初步优化。
2.由于纳米ZnO形貌丰富、结构多样，且纳米ZnO形貌、尺寸对材料性能有较大的影响。因此，采用微波水热技术制备不同尺寸的球形ZnO以及不同形貌的纳米ZnO；通过扫描电镜(SEM)、X射线衍射(XRD)等对产物的形貌结构进行表征；考察了球形ZnO尺寸及纳米ZnO形貌对纳米ZnO性能的影响。然后，采用常规乳液聚合法在PA30改性纳米ZnO的分散液中原位引发丙烯酸酯类单体聚合，制备聚丙烯酸酯/纳米ZnO复合乳液。考察球形ZnO尺寸、纳米ZnO形貌对复合乳液及薄膜、涂饰后革样及整理后织物性能的影响。
结果表明：球形ZnO及聚丙烯酸酯/球形ZnO纳米复合薄膜的抗菌性随球形ZnO尺寸的增大而降低。与其他几种形貌ZnO相比，球形ZnO、花状ZnO均具有良好的抗菌和紫外吸收性能；聚丙烯酸酯/球形ZnO纳米复合薄膜、聚丙烯酸酯/花状ZnO纳米复合薄膜对白色念珠菌的抗菌效果良好，但对霉菌的抗菌效果不佳。
与纯聚丙烯酸酯乳液涂饰后革样相比，聚丙烯酸酯/花状ZnO纳米复合乳液涂饰后革样的透气性提高了232.65%。聚丙烯酸酯/球形ZnO纳米复合乳液整理后织物的透湿率较纯聚丙烯酸酯乳液整理后织物提高了129.21%。
聚丙烯酸酯/球形ZnO纳米复合薄膜的抗菌作用由锌离子的溶出作用和ZnO的光催化作用共同所致，聚丙烯酸酯/花状ZnO纳米复合薄膜的抗菌作用则以ZnO的光催化作用为主。
3.对抗菌性能较优的球形、花状ZnO进行掺银处理，以提高其对霉菌的抗菌效果；采用SEM、XRD、TEM等对复合粒子的形貌结构及组成进行分析；考察化学吸附还原法、微波辅助还原法和氧化还原法等三种纳米粒子制备方法以及纳米粒子形貌对粒子性能的影响。然后，采用常规乳液聚合法在PA30改性纳米ZnO/Ag复合粒子的分散液中原位引发丙烯酸酯类单体聚合，制备聚丙烯酸酯/纳米ZnO/Ag复合乳液；考察复合粒子制备方法、复合粒子形貌、用量对乳液及薄膜性能的影响。最后，将所得乳液应用到皮革、纺织涂层中考察其应用性能。
结果表明：采用化学吸附还原法所制备的花状ZnO/Ag复合粒子以及含该复合粒子的聚丙烯酸酯薄膜的抗菌性优于采用微波辅助还原法和氧化还原法所制备的复合粒子。掺银以后纳米粒子及复合薄膜对霉菌的抗菌效果显著提高。
球形ZnO/Ag复合粒子和花状ZnO/Ag复合粒子的抗菌性能相差不大。但是，聚丙烯酸酯/花状ZnO/Ag纳米复合薄膜的抗菌性能优于聚丙烯酸酯/球形ZnO/Ag纳米复合薄膜。
与纯聚丙烯酸酯乳液涂饰后革样相比，采用聚丙烯酸酯/花状ZnO/Ag纳米复合乳液涂饰后革样的透气性提高了138.46%；采用聚丙烯酸酯/花状ZnO纳米复合乳液整理后织物的透湿性最好，较纯聚丙烯酸酯乳液整理后织物提高了12.84%。
聚丙烯酸酯/花状ZnO/Ag纳米复合薄膜的抗菌作用主要以花状ZnO/Ag复合粒子的光催化抗菌为主，Ag系抗菌剂的金属粒子接触抗菌为辅；复合薄膜对白色念珠菌、霉菌抗菌效果的差异，与两种菌种的细胞壁结构和化学组成密切相关。
本研究所研制的聚丙烯酸酯基纳米复合薄膜“软而不粘”、抗菌性能优异、卫生性能良好。反应以水为介质，安全环保、无毒、无污染。目前，有关纳米材料形貌、尺寸对复合材料性能，尤其是抗菌性能影响的研究国内外还鲜见报道。
As one of the most common used film-forming materials, polyacrylate is widely used in leather finishing agent, textile adhesive, wood and construction paints due to its excellent gloss, flexibility, transparent and chemical stability. However, the drawback of neat polyacrylate, such as weak climate-resistance, poor antimicrobial activities and lower sanitation properties often restrict its application. Recently, polymer/inorganic nanocomposites have attracted a great deal of attention with the rapid development of nanotechnology.
This research is based on the above background. Inorganic nanomaterials with excellent antimicrobial activities were bought into polyacrylte firstly. Then the influences of inorganic nanomaterials with different morphologies and sizes on the properties of the nanocomposites were investigated in details. At last, polyacrylate-based nanocomposites with excellent antibacterial and sanitation properties were obtained. The main contents are listed as follows.
1. The effects of inorganic nanoparticles including commercially MgO, TiO2, ZnO, Al2O3, MMT and SiO2on the properties of the nanocomposites were investigated in details. Then anionic polymer (PA30) was used to modify the chosen ZnO, and the optimum modification conditions were obtained. At last, the preparation method and optimum conditions of polyacrylate/ZnO nanocomposites were studied.
2. There are various ZnO nano structures with different shapes and sizes, and each of them displays some unique properties. ZnO nano structures with various morphologies and sizes were successfully obtained via microwave-assisted hydrothermal process in this study. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to investigate the morphology and crystal structure of obtained ZnO. Then polyacrylate/ZnO nanocomposite latexes were prepared by in-situ emulsion polymerization of acrylate monomers in the presence of PA30modified ZnO nanostructures. The influences of ZnO nano structures with various morphologies and sizes on the performances of the obtained ZnO, nanocompsite latexes and films, as well as the finished leather samples and treated fabrics were investigated.
The results showed that the antimicrobial activities of sphere-like ZnO and polyacrylate/sphere-like ZnO nanocompsoite film were both decreased with the increasing of the diameter of ZnO.
Sphere-like ZnO and flower-like ZnO had better antimicrobial activities and ultraviolet absorption property than those of ZnO with other morphologies. Polyacrylate-based films containing sphere-like ZnO and flower-like ZnO showed excellent antimicrobial activities on candida albicans. However, the antimicrobial activities of films containing sphere-like ZnO and flower-like ZnO on aspergillus flavus were poor.
Experimental results showed that vapor permeability of the leather finished by polyacrylate/flower-like ZnO nanocomposite latex increased by232.65%, compared to that finished by pure polyacrylate latex. The moisture permeability of fabric treated by polyacrylate/sphere-like ZnO nanocomposite latex was increased by129.21%, compared to that treated by pure polyacrylate latex.
The releasing of Zn ions and the photo catalysis activity of ZnO played an important role in the antimicrobial activities of polyacrylate/ZnO nanocomposite film containing sphere-like ZnO, and the excellent antimicrobial properties of polyacrylate-based film containing flower-like ZnO might attribute to the photo catalysis activity of ZnO.
3. Ag particles were doped on the surface of sphere-like ZnO and flower-like ZnO to improve the antimicrobial activities of ZnO on aspergillus flavus. SEM, XRD and TEM were used to investigate the morphology, structure and chemical composition of the obtained composite particles. The influences of different methods including chemical and adsorption reduction method, microwave-assisted reduction method and oxidation-reduction method, and the morphologies of ZnO on the properties of the obtained ZnO/Ag composite particles were investigated. Then polyacrylate/ZnO/Ag nanocomposites were obtained by in-situ emulsion polymerization of acrylate monomers in the presence of PA30modified ZnO/Ag composite particles. The effects of ZnO/Ag composite particles with different preparation methods, morphologies, and the dosages of ZnO/Ag composite particles on the properties of the polyacrylate/ZnO/Ag nanocompsite latexes and films were investigated in detail. At last, the composite latex was used in leather finishing and textile treating.
The results indicated that the antimicrobial activities of ZnO/Ag composite particles and polyacrylate/flower-like ZnO/Ag composite prepared by chemical and adsorption reduction method were higher than that prepared by microwave-assisted reduction method and oxidation-reduction method. Besides, the inhibition abilities to aspergillus flavus were greatly improved with the doping of Ag on the surface of ZnO.
The antimicrobial activities of sphere-like ZnO/Ag composite particles and flower-like ZnO/Ag composite particles were almost alike. However, the antimicrobial activities of the film containing flower-like ZnO/Ag composite particles was higher than that of the film containing sphere-like ZnO/Ag composite particles.
Experimental results showed the vapor permeability of the leather finished by polyacrylate/flower-like ZnO/Ag composite latex was increased by138.46%, compared to that finished by polyacrylate/flower-like ZnO composite latex. The moisture permeability of fabrics treated by polyacrylate/flower-like ZnO composite latex was increased by12.84%, compared to that treated by pure polyacrylate latex.
The photocatalysis activites of ZnO/Ag composite particles played an important role in the antimicrobial activities of polyacrylate/flower-like ZnO/Ag nanocomposite film. The contaction of metal ions also influenced the antimicrobial activities of the nanocomposite film. However, the reason for the different antimicrobial activities on candida albicans and aspergillus flavus were probably due to the different structures and compositions of the two kinds of bacteria.
Polyacrylate-based nanocomposites prepared by the above method had excellent antimicrobial and sanitation properties. The as-prepared composite film was soft but not sticky. Besides, the reaction was carried out in water media, which was non-toxic, pollution-free, and safe. There were few reports about the influences of inorganic nanomaterials with different morphologies and sizes on the properties of the nanocomposites, especially the antimicrobial activities.
引文
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