低表面能及仿生表面微结构防污技术
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摘要
本文针对海洋防污涂料在环保、高效、广谱等方面存在的问题,由自然界生物的防污方式出发,提出了一种低表面能与表面微结构相结合的仿生防污新方法,据此开展了新型仿生防污涂料的研究工作。根据有机硅树脂与有机氟化合物各自的特点,将二者有机结合,研制了新型低表面能聚合物;并通过有机/无机杂化方式,克服了该类材料附着力及浸水稳定差的难题;在此基础上,采用纳米粒子填充法在低表面能聚合物表面构建了微米一纳米二级结构,有效地将低表面能与表面微结构结合起来。本文还提出了一种简便、快速的实验室内评价防污涂料防污效果的新方法,与接触角测试、实海挂板实验共同评估自研防污涂料的防污效果,并将三种方法得到的结果对比分析,结果表明接触角作为初步衡量防污效果的参数是不够准确的。
在低表面能树脂方面,本文先后合成出分别含氟和含硅的两种新型聚合物:含羟基官能团的含氟丙烯酸酯聚合物FPA,以及异氰酸根封端的有机硅改性聚氨酯预聚体SPU,以此研制出一种新型低表面能聚合物FPA—SPU,该聚合物同时结合了有机硅和有机氟的优点,具有较好的柔韧性和超低表面能,接触角达到103°,大大优于单纯的含氟丙烯酸酯聚合物和有机硅改性聚氨酯。在此基础上,创造性地采用酸催化溶胶—凝胶法向FPA—SPU聚合物中引入无机Si—O网络,研制出了FPA—SPU/SiO_2纳米杂化材料,通过互穿网络结构显著提高了聚合物体系的交联密度,解决了低表面能聚合物附着力及浸水稳定性差的难题,并使接触角进一步提高至109°。
随后,仿照自清洁生物的表皮微观结构,首次采用纳米粒子填充法在FPA—SPU低表面能聚合物表面构建微米一纳米二级结构,使表面接触角由109°突升到150°以上,极大增强了其疏水性能;且该方法将低表面能聚合物与表面微结构有机结合,制备方法简便易行,无需复杂仪器设备,特别适合于舰船表面的大面积施工和低成本涂布。
为了检验本文研制的新型仿生防污涂料的防污性能,提出了一种简便、快速的评估其防污效果的实验室评价方法,并通过在青岛、三亚两海域进行的实海挂板测试,探讨了防污性能的各影响因素;将材料本身的接触角测试、实验室快速评价方法和实海挂板实验的结果进行了对比,分析了接触角作为初步衡量防污效果参数的可行性,并验证了实验室评价方法的准确性和可靠性。
A novel antifouling method and the corresponding coatings were developed in this thesis to overcome the problems in marine antifouling coatings. The antifouling method, inspired by lives in nature with antifouling capability, combined the contributions of both the low surface energy property and surface microstructures. Based on that, in this thesis we mainly focused on the preparation and characterization of new kinds of antifouling coatings of environmental friendly, high efficient, and nontoxic. Novel polymers with low surface energy were firstly synthesized by integration of the characteristics of silicone and fluoropolymer; then its properties of adhesion force and water resistance are improved greatly by an organic-inorganic hybrid preparation process; finally, a micro-nano binary structures were constructed on the surfaces of the coatings by doping siclia nanoparticles in the polymers, which combines the merits of low surface energy and microstrcutres. Moreover, we proposed a facile and fast characterization method, together with contact angle and seawater exposure tests, to evaluate the antibiofouling effects of our resulted coatings. We also discussed the feasibility that the contact angle be used as a preliminary evaluating parameter.
New kinds of polymers with low surface energy were synthesized for the first time: fluoro-acrylate polymer (FPA) with -OH, and polysiloxane modifying polyurethane prepolymer with -NCO (SPU). Then FPA - SPU was synthesized by linking reaction between FPA and SPU. This unique polymer is much better than FPA or SPU with unique properties of flexility and ultralow surface energy of a contact angle of about 103°, which originated form the combination of strongpoint of silicone and fluoropolymer in its molecular structures. Further, Si-O networks were introduced into the resulted FPA-SPU polymer by acid catalyzed sol-gel method and achieved FPA - SPU/SiO_2 organic-inorganic hybrid materials. Their high crosslinking density originated from interpenetrating polymer network enabled them improved adhesion force and water resistance and higher contact angle of 109°.
Inspired by the special structures on the epidermis of some lives with antifouling capability, we constructed a micro-nano binary structures on the surfaces of FPA-SPU polymer by doping them with nanoparticles. Its contact angle was increased to above 150°and in sharp contrast to the contact angle of 109 for undoped polymer. This simple and facile method integrated the polymer of low surface energy with surface microstructures, hence it involved no complicated equipments or instructions and is suitable for coating ships cost-effectively in large areas.
To test the antifouling performances of the resulted coatings, a simple and efficient lab-used evaluation method based on contact angles was proposed and used to analyze the possibilities affecting the antifouling performances measured in sea areas of Qingtao and Sanya. By comparison the contact angles with the lab-used evaluation method as well as the antifouling experiments, our technique was proved to be a qualified method for evaluating the antifouling properties. Also, its accuracy and reliability are further examined.
在低表面能树脂方面,本文先后合成出分别含氟和含硅的两种新型聚合物:含羟基官能团的含氟丙烯酸酯聚合物FPA,以及异氰酸根封端的有机硅改性聚氨酯预聚体SPU,以此研制出一种新型低表面能聚合物FPA—SPU,该聚合物同时结合了有机硅和有机氟的优点,具有较好的柔韧性和超低表面能,接触角达到103°,大大优于单纯的含氟丙烯酸酯聚合物和有机硅改性聚氨酯。在此基础上,创造性地采用酸催化溶胶—凝胶法向FPA—SPU聚合物中引入无机Si—O网络,研制出了FPA—SPU/SiO_2纳米杂化材料,通过互穿网络结构显著提高了聚合物体系的交联密度,解决了低表面能聚合物附着力及浸水稳定性差的难题,并使接触角进一步提高至109°。
随后,仿照自清洁生物的表皮微观结构,首次采用纳米粒子填充法在FPA—SPU低表面能聚合物表面构建微米一纳米二级结构,使表面接触角由109°突升到150°以上,极大增强了其疏水性能;且该方法将低表面能聚合物与表面微结构有机结合,制备方法简便易行,无需复杂仪器设备,特别适合于舰船表面的大面积施工和低成本涂布。
为了检验本文研制的新型仿生防污涂料的防污性能,提出了一种简便、快速的评估其防污效果的实验室评价方法,并通过在青岛、三亚两海域进行的实海挂板测试,探讨了防污性能的各影响因素;将材料本身的接触角测试、实验室快速评价方法和实海挂板实验的结果进行了对比,分析了接触角作为初步衡量防污效果参数的可行性,并验证了实验室评价方法的准确性和可靠性。
A novel antifouling method and the corresponding coatings were developed in this thesis to overcome the problems in marine antifouling coatings. The antifouling method, inspired by lives in nature with antifouling capability, combined the contributions of both the low surface energy property and surface microstructures. Based on that, in this thesis we mainly focused on the preparation and characterization of new kinds of antifouling coatings of environmental friendly, high efficient, and nontoxic. Novel polymers with low surface energy were firstly synthesized by integration of the characteristics of silicone and fluoropolymer; then its properties of adhesion force and water resistance are improved greatly by an organic-inorganic hybrid preparation process; finally, a micro-nano binary structures were constructed on the surfaces of the coatings by doping siclia nanoparticles in the polymers, which combines the merits of low surface energy and microstrcutres. Moreover, we proposed a facile and fast characterization method, together with contact angle and seawater exposure tests, to evaluate the antibiofouling effects of our resulted coatings. We also discussed the feasibility that the contact angle be used as a preliminary evaluating parameter.
New kinds of polymers with low surface energy were synthesized for the first time: fluoro-acrylate polymer (FPA) with -OH, and polysiloxane modifying polyurethane prepolymer with -NCO (SPU). Then FPA - SPU was synthesized by linking reaction between FPA and SPU. This unique polymer is much better than FPA or SPU with unique properties of flexility and ultralow surface energy of a contact angle of about 103°, which originated form the combination of strongpoint of silicone and fluoropolymer in its molecular structures. Further, Si-O networks were introduced into the resulted FPA-SPU polymer by acid catalyzed sol-gel method and achieved FPA - SPU/SiO_2 organic-inorganic hybrid materials. Their high crosslinking density originated from interpenetrating polymer network enabled them improved adhesion force and water resistance and higher contact angle of 109°.
Inspired by the special structures on the epidermis of some lives with antifouling capability, we constructed a micro-nano binary structures on the surfaces of FPA-SPU polymer by doping them with nanoparticles. Its contact angle was increased to above 150°and in sharp contrast to the contact angle of 109 for undoped polymer. This simple and facile method integrated the polymer of low surface energy with surface microstructures, hence it involved no complicated equipments or instructions and is suitable for coating ships cost-effectively in large areas.
To test the antifouling performances of the resulted coatings, a simple and efficient lab-used evaluation method based on contact angles was proposed and used to analyze the possibilities affecting the antifouling performances measured in sea areas of Qingtao and Sanya. By comparison the contact angles with the lab-used evaluation method as well as the antifouling experiments, our technique was proved to be a qualified method for evaluating the antifouling properties. Also, its accuracy and reliability are further examined.
引文
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