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表面疏水性多孔材料的制备与应用研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/9/6 7:49:20  

摘要:有序多孔结构材料拥有独特的优点,在化学、生物及生命科学等领域展现出了可观的应用前景,譬如可用于光电器件、组织工程、微图像技术及高端分离技术等诸多方面,本课题采用自由基聚合,分别制备了两亲性嵌段共聚物、星形聚合物以及β-环糊精共聚物;再采用静态呼吸图案法制备多孔材料,灌注硅油后获得疏水功能性的两亲性嵌段共聚物多孔膜、星形聚合物多孔膜以及β-环糊精共聚物多孔膜。 

利用β-环糊精与顺丁烯二酸酐通过酯化反应制备β-环糊精衍生物,然后通过β-环糊精衍生物与苯乙烯(St)发生自由基共聚反应制备环糊精共聚物。将一定量的环糊精共聚物与N,N-二甲基甲酰胺混合均匀。随后将混合均匀的液体滴在玻璃片上,经干燥后成膜。将成膜后的多孔膜浸泡在硅油中,除去表面多余液体得到填充有硅油的膜表面。利用傅立叶红外光谱仪和核磁共振波谱仪对共聚物的结构与组成进行表征,利用偏光显微镜和扫描电子显微镜对多孔膜表面形貌进行观察,利用接触角测量仪研究多孔膜表面的润湿性。结果表明,由环糊精共聚物与N,N-二甲基甲酰胺混合溶液制备的多孔膜表面具有疏水性,水接触角可达128°。利用微生物粘附实验研究多孔膜表面对微生物粘附的情况,结果表明在浓度为25 mg/mL时可以有效降低90%以上大肠杆菌的粘附量。

通过原子转移自由基聚合(ATRP)合成嵌段共聚物PS-b-PMMA。在酸性条件下水解嵌段共聚物制备两亲性共聚物PS-b-PMAA。利用傅里叶变换红外光谱,核磁共振光谱和凝胶渗透色谱对产物进行了表征。结果表明成功的制备了两亲性共聚物PS-b-PMAA。采用呼吸图法制备多孔膜并观察它们的表面形态。结果表明,两亲性共聚物膜表面存在规则均匀的多孔形貌。当聚合物溶液的浓度为25 mg/mL时,PS-b-PMAA共聚物膜的孔径约为1 μm。将聚合物膜浸入硅油中一段时间后,水接触角达到108.7°。利用微生物粘附实验研究多孔膜表面对微生物粘附的情况,大肠杆菌的吸附量由70.0 x105cfu/cm2降至10.0 x105cfu/cm2,有效降低86%以上大肠杆菌的粘附量,表明灌注硅油后能有效提高聚合物多孔膜表面的抗细菌粘附性能。

以(3-氯丙基)三甲氧基硅烷作为反应单体,无水甲醇为溶剂,合成出多官能团引发剂(OCP-POSS)。以苯乙烯、甲基丙烯酸三氟乙酯为单体,OCP-POSS为引发剂,采用原子转移自由基聚合法(ATRP)制备POSS-(PTFEMA -b-PS)星型聚合物。将星形聚合物溶解于三氯甲烷中,利用静态呼吸图案法制备多孔膜。将多孔膜浸泡在硅油中获得具有疏水性能的膜表面。通过傅立叶变换红外光谱,核磁共振氢谱,凝胶渗透色谱等对星形聚合物的结构,组成及分子量进行分析和表征;利用偏光显微镜和扫描电子显微镜对多孔膜表面形貌进行观察;利用接触角测量仪对多孔膜的疏水性能进行表征。结果表明:通过静态呼吸图案法成功制得星型聚合物POSS-(PTFEMA-b-PS)多孔膜,将多孔膜浸泡在硅油里一段时间后疏水性能得到一定程度的提高,最高可达到116°。利用微生物粘附实验研究多孔膜表面对微生物粘附的情况,结果表明在浓度为40 mg/mL时可以有效降低92%以上大肠杆菌的粘附量。

Ordered porous structural materials have unique advantages and have shown good application prospects in the fields of chemistry, biology and life sciences, such as optoelectronic devices, tissue engineering, micro-image technology and high-end separation technology. The amphiphilic block copolymer, star polymer and β-cyclodextrin polymer were prepared by free radical polymerization. The porous materials were prepared by static breathing pattern method. Then, the amphiphilic block copolymer porous film, star polymer porous film and β-cyclodextrin polymer porous film were preapared after impregnating the silicone oil.

The β-cyclodextrin derivative was prepared by esterification reaction between β-cyclodextrin and maleic anhydride, and then the cycloester was prepared by radical copolymerization of β-cyclodextrin derivative with styrene (St). A certain amount of the cyclodextrin copolymer was uniformly mixed with N,N-dimethylformamide. The uniformly mixed liquid was then dropped on a glass slide and dried to form a film. The film-formed porous film was immersed in the silicone oil, and the surface excess liquid was taken out to obtain a surface of the film filled with the silicone oil. The structure and composition of the copolymer were characterized by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy. The surface morphology of the porous membrane was observed by polarized light microscope and scanning electron microscope. The wettability of the porous membrane surface was studied by contact angle measuring instrument. The results showed that the surface of the porous membrane prepared by the mixture of cyclodextrin copolymer and N,N-dimethylformamide had hydrophobicity and the water contact angle can reach 128°. Microbial adhesion experiments were used to study the adhesion of microporous membranes to microbes. The results showed that the concentration of E. coli could be effectively reduced by more than 90% at a concentration of 25 mg/mL.

The block copolymer PS-b-PMMA was prepared by atom transfer radical polymerization (ATRP).Amphiphilic copolymer could be formed by hydrolysis of the block copolymer at acidic conditions. The products were characterized by fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy and GPC.The results illustrated the preparation of amphiphilic copolymer was successful.The porous membranes were prepared by the breath figure method and characterized their surface morphology. The results showed that there was a regular and uniform porous morphology on the surface of the amphiphilic copolymer film. When the concentration of the polymer solution was 25 mg/mL, the pore size of the PS-b-PMAA copolymer membrane was about 1nm. After immersing the polymer film in silicone oil for a period of time, the water contact angle reached 108.7°. The microbial adhesion test was used to study the adhesion of microporous membrane surface to microorganisms. The adsorption capacity of E. coli decreased from 70.0 x 105 cfu/cm2 to 10.0 x 105 cfu/cm2, effectively reducing the adhesion of E. coli by more than 86%. The results showed that the surface of the oil film could effectively improve the antibacterial property of the polymer surface.

Polyfunctional initiator (OCP-POSS) was synthesized by using (3-chloropropyl)trimethoxysilane as the reactive monomer and anhydrous methanol as the solvent. POSS-(PTFEMA-b-PS) star polymer was prepared by atom transfer radical polymerization (ATRP) using styrene, trifluoroethyl methacrylate as monomers and OCP-POSS as initiator. The star polymer was dissolved in chloroform, and a porous film was prepared by the static breathing pattern method. The porous membrane was immersed in the silicone oil to obtained a membrane surface having hydrophobic properties. The structure, composition and molecular weight of the star polymer were characterized by Fourier transform infrared spectroscopy, nuclear magnetic resonance spectrosco.

关键词:原子转移自由基聚合(ATRP);静态呼吸图案法;疏水性能;多孔膜

atom transfer radical polymerization (ATRP); static breathing pattern method; hydrophobic properties; porous membrane

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