摘要
紫外光固化是一种环保技术，具有环境友好、效率高、经济和节约能源等优点，在日益苛刻的环保要求下，该项技术获得了前所未有的发展，已被广泛用于电子材料封装、塑料制件表面保护、木地板上光、汽车小面积修补等行业中。另一方面，通过纳米无机相来提高有机涂层的耐刮伤性、耐磨性等性能已成为学术界共识。若将纳米无机相引入至紫外光固化涂料中，则可完美结合纳米复合与紫外光固化技术的优点，大大推动紫外光涂料的发展与应用。目前，文献中虽然对紫外光固化纳米复合涂层也有一些研究报道，但仍然存在研究体系有限、制备方法少、不同纳米复合体系的紫外光固化动力学行为缺乏系统研究等问题。本研究以SiO_2和TiO_2为纳米无机相，设计制备了三种不同的紫外光固化纳米复合涂层体系，系统研究了这些纳米复合涂层的紫外光固化动力学、表面性能、热学性能和光学性能，以期为紫外光固化纳米复合涂层的应用提供理论基础。具体研究内容及结果如下：
紫外光固化纳米SiO_2颗粒涂层
按Stober方法制备了纳米二氧化硅醇溶胶粒子，在同一介质中直接采用甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)改性，再通过乙醇脱除获得浓缩的改性二氧化硅粒子在游离MPS中的分散液，在浓缩液中加入光引发剂，涂膜光固化后得到了高无机相含量的纳米SiO_2颗粒涂层。考察了纳米SiO_2粒径对浓缩液粘度、光固化动力学以及涂层表面特性、热学和光学性能的影响规律。研究表明，该方法制备的涂层表面光滑且透明，随着纳米SiO_2粒径的增加，纳米复合涂层的光固化速度，最终双键转化率和表干时间增加，但表面粗糙度、玻璃化转变温度和紫外光吸收性能有所下降。
紫外光固化环氧丙烯酸酯／二氧化硅纳米复合涂层
将按前述类似方法制备的改性SiO_2粒子(40nm)与环氧丙烯酸酯(EA)和三羟甲基丙烷三丙烯酸酯(TMPTA)等组分超声共混制备了紫外光固化环氧丙烯酸酯／SiO_2纳米复合涂层。考察了纳米SiO_2含量对涂层形态、紫外光固化行为、热稳定性和光学性能的影响规律，用红外光谱系统地研究了纳米复合涂层的紫外光固化动力学的影响因素，包括引发剂类型、用量、光强、膜厚、固化气氛、杂质(MPS、乙醇和水)等，并与这些因素对纯环氧丙烯酸酯的紫外光固化动力学的影响规律进行了比较。同时，采用四乙氧基硅烷(TEOS)在EA存在下水解，除乙醇，然后与TMPTA、引发剂等组分混合(即原位法)制备了紫外光固化环氧丙烯酸酯／SiO_2纳米复合涂层，比较了该方法与上述方法(即共混法)制备的纳米复合涂层的固化行为、微结构和性能。
研究表明，采用SiO_2浓缩液超声共混法制得的纳米复合涂层中，纳米SiO_2含量即使高达22.5％时仍具有良好的分散性，突出的涂层透明性。随着纳米SiO_2含量的增加，涂层的紫外屏蔽性增加，热稳定性提高，但纳米SiO_2对EA涂层的阻燃性几乎没有影响。
动力学研究表明，纳米SiO_2的引入不可思议地提高了EA体系的紫外光固化速度，但是由于纳米二氧化硅胶体粒子上的多孔性，纳米复合涂层与EA体系相比具有更强的氧敏感性，从而导致涂层的表干时间随着纳米SiO_2用量的增加而变长。与EA体系相比，纳米复合涂层具有更高的固化速度和最终转化率。MPS和乙醇的存在提高了纳米复合涂层的紫外光固化速度，然而水的存在却减慢涂层的光固化速度。
与共混法相比，原位法得到的纳米复合涂层中TEOS只是部分水解，生成的是一种与有机相缠结的无机相结构。原位法制备的纳米复合涂层比共混法制备的纳米复合涂层具有更高的UV固化速度，但是，共混法制备的纳米复合材料由于良好的纳米二氧化硅的分散而具有高的玻璃化转变温度和强的紫外吸收性能。紫外光固化环氧丙烯酸酯／TiO_2纳米复合涂层
以TMPTA和醋酸丁酯为分散介质，通过纳米TiO_2粉体的球磨分别制备了TST和TSB两种分散良好的纳米TiO_2浆料。将上述浆料与EA、TMPTA、1，6-己二醇二丙烯酸酯(HDDA)等组分混合制备了两个系列的紫外光固化环氧丙烯酸酯／TiO_2纳米复合涂层。考察了纳米TiO_2的引入和醋酸丁酯的存在对纳米复合涂层紫外光固化行为和性能的影响规律。研究发现，引入纳米TiO_2可以提高涂层的热稳定性和紫外屏蔽性能。与采用TST浆料制备的纳米复合涂层相比，利用TSB浆料制备的纳米复合涂层具有较高的最终双键转化率、良好的透明性，但是表面粗糙度稍大、紫外屏蔽性能、热学性能和玻璃化转变温度均较低。动力学研究表明，由于纳米TiO_2强的UV吸收性能，它的引入会严重地降低引发剂的引发效率，进而降低紫外光固化体系的固化速率，且随着TiO_2含量的增加，这种降低作用越明显，但是醋酸丁酯的存在有助于减弱纳米TiO_2对紫外光固化速度的降低作用。此外，低效引发剂的使用、固化气氛中氧气浓度的增加、膜厚的降低以及辐射光强的减弱都会加强氧气对含TiO_2纳米复合涂层的阻聚作用。
UV curing technology is one technology with advantages such as environmental-friend, efficiency, economy and energy saving. Due to even strict environmental protection policy, this new technology has gained a very rapidly development in the past few years and therefore being widely used in electronic packaging, surface protection of plastic device, flooring and small pitch car refinish. On the other hand, in recent years, nanocomposites become the hot topic for research and development in order to improve the property and comprehensive performance of traditional organic coating. The UV curable nanocomposite coatings combine the advantages of nanomaterials and UV curing technology together and propel the development and application of UV curable coatings greatly. Up to now, some UV curable nanocomposite coatings were reported. However, the types of the coatings are still limited and only a few reports about its preparation and photopolymerization kinetics were available. In this study, three series of nancomposite coatings with SiO_2 and TiO_2 as inorganic phase were prepared. Their UV curing behavior, surface property, thermal property and optical property were investigated as well. All these results are expected to provide some concrete evidence for the development and application of UV curable nanocomposites. The detailed research contents and results are summarized as follows:
UV-curable SiO_2 particle nanocomposite coatings
Nanosilica sols with various particle size were firstly synthesized by Stober method, and then modified by 3-trimethoxysilylpropyl methacrylate (MPS). After that, the ethanol was evaporated and resulted in condensed nanoslica sol with residual free MPS as the dispersing media. The particle size, viscosity and surface modification situation for the condensed nanosilica sol were characterized as well. The obtained paste-like slurries were then cured under UV irradiation directly after adding the photoinitiator, Irgacure 651. With increasing nanosilica particle size, the photopolymerization rate, final double bond conversion, and tack-free time of nanocomposites increased, while the surface roughness, glass-transition temperature, and UV absorbance of nanocomposites decreased.
UV-curable epoxy acrylate/SiO_2 nanocomposite coatings
The condensed nanosilica (40nm) was also incorporated into epoxy acrylate prepolymer and trimethylolpropane triacrylate (TMPTA) reactive dilute to prepare
UV-curable epoxy acrylate/SiO_2 nanocomposite coatings. Effect of the silica content on the UV-cured coatings was investigated. The influence of photoinitiator types, photoinitiator content, UV irradiation intensity, coating thickness, curing with or without oxygen and the impurities such as ethanl, MPS, water, etc. on the UV-curing behavior were also investigated. Finally, the influence of preparing method, namely blending method described above and in situ method in which tetraethyl orthosilicate (TEOS) was directly hydrolyzed and condensed in EA, on the structure and property of nanocomoposites were compared.
Improved inorganic particles dispersion state, thermal and optical properties were observed as well. It was also found that embedment of condensed functional nanosilica prepared by sol-gel method can surprisingly accelerate the UV curing process of epoxy acrylate matrix. It's found that the existence of MPS and ethanol can accelerate the curing speed while the presence of water decelerate the curing speed. Finally, the UV curable nanocomposites are more sensitive to the oxygen compared with the pure organic system. During the blending method, TEOS completely hydrolyzed to form nanosilica particles, which were evenly dispersed in the polymer matrix. However, for the in situ method, TEOS only partially hydrolyzed to form inorganic phases intertwisted with organic molecules. The nanocomposites prepared by the in situ method had much higher curing rates than those from the blending method, but the latter had greater glass transition temperatures and UV shielding property than the former because the blending method caused uniformly dispersed nanosilica particles whereas the in situ method did not.
UV-curable epoxy acrylate/TiO_2 nanocomposite coatings
Nano-TiO_2 slurries with TMPTA or n-butyl acetate as dispersing media were prepared by ball milling methods. Then, these slurries were incorporated into epoxy acrylate matrix to prepare two series of the nanocomposite formulations. In order to further improve the dispersion of titanium dioxide in the formulation, the ultrasonication was used to treat the formulation.The influence of nano-TiO_2 content and volatile organic compound on UV-curing behaviour, surface property, thermal property, optical property and titanium dioxide dispersing state of nanocomposites were investigated.
TEM pictures show that the titanium dioxide has a good dispersion both in trimethylolpropane triacrylate and n-butyl acetate after the ball milling. The viscosity
measurement showed that the type of the slurry has a great effect on the viscosity of nanocomposite formulation. In brief, titanium dioxide with TMPTA as dispersion media enhanced the viscosity of formulation, while the titanium dioxide with n-butyl acetate as dispersion media decreased the viscosity.
It was found that nano-TiO_2 slurry with different medium had various impacts on the photopolymerization kinetics, tack free time, thermal and optical properties of nanocomposites. The nano-TiO_2 slurry in TMPTA decreased the UV cured rate of the nanocomposites, while the nano-TiO_2 slurry in butyl acetate increased the UV cured rate of the nanocomposites. With the increasing nano-TiO_2 content, this tendency is more obvious. However, the former could more efficiently improve tack free time, thermal stability and UV shielding properties of their nanocomposite coats than the latter.
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