高官能度水性聚氨酯丙烯酸酯的结构改性和应用研究
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摘要
本论文针对水性紫外光固化涂料发展和应用的技术瓶颈,开展了高官能度水性聚氨酯丙烯酸酯(MWPUA)的改性和应用研究。首先,设计合成出一系列线型和支化型产品,提高和优化了聚合物的官能度,有效解决了此类涂膜在硬度、强度、耐水耐溶剂性等方面的固有不足。接着,为满足特殊性能和工艺的要求,研制出MWPUA/SiO_2和MWPUA/CB两种新型纳米复合涂料,并开发出以聚合物为连续相的高固体分可水分散(HSWPUA)体系。最后,在植物高效的捕光和传能机制启示下,从仿生角度对典型的夺氢型光引发剂硫杂蒽酮-叔胺体系进行了合成和引发效率的优化,为提高有色涂层的深层光固化效率探索了新的技术途径。研究工作和主要结果如下:
在优化软硬段结构和工艺条件、解决线型产品官能度结构和性能调控等问题的基础上,以多胺化合物替代之前的二胺扩链剂,以此为中心连接多条丙烯酸酯封端的预聚体支链,采用增加“端”数目的方式实现官能基团的进一步扩增,实现了较高空间位阻和复杂因素影响下的有效和完全反应,合成制备出一系列具有更高官能度的水性聚氨酯丙烯酸酯(WPUA)新产品。通过系统研究平均官能度对聚合物性能和结构的影响规律和作用机理,优化各主要性能,从根本上解决了传统低官能度WPUA在涂膜硬度、强度和耐水耐溶剂性方面的不足。
选用含有光固化功能基团的硅烷偶联剂对纳米SiO_2进行表面改性、以及通过接枝法使纳米炭黑和聚合物形成化学键合等方法,实现了MWPUA/SiO_2和MWPUA/炭黑两种纳米复合涂料中纳米粒子的稳定均匀分散,并使MWPUA/SiO_2体系的耐磨性和附着力,以及MWPUA/炭黑的光固化性能得到显著提升,满足了木地板涂料和黑色色漆对实用性能的特殊需求。
针对WPUA水分散体对设备和工艺技术要求复杂的问题,提出了高固体分可水分散型聚氨酯丙烯酸酯(HSWPUA)的新概念,并先后研制了HSWPUA/丙酮、HSWPUA/乙醇/丙酮和HSWPUA/丙烯酸酯复合体系,样品固含量达到70%以上。这类兼备高固体分、光固化和水可分散性三种绿色涂料技术于一体的产品,适应了多种涂布方式,并获得了令人满意的黏度、附着力和水分散稳定性等综合性能。
模拟植物高效的捕光和传能机制,对同为捕光激发和传能的夺氢型硫杂蒽酮-叔胺光引发剂进行仿生改性的探讨,设计合适的桥键结构和模拟蛋白质超分子体系,将原来独立的光敏单元和光引发单元合理结合于同一大分子或聚合物中,并对照植物光系统的结构与机制,系统研究了新型光引发剂的分布形态、复合结构、能量和电子传递途径对引发效率的影响和作用机理,获得了很好的初步成绩。
A research on the modification and application of multi-functional waterborne polyurethane acrylate (WPUA) was made with the intention to break the bottlenecks of waterborne UV coatings in their development and application. A series of linear and branched WPUA products with increased functionalities of polymer molecules were synthesized, in order to overcome the shortcomings of films in rigidity, strength and the resistance to water and solvent. Subsequently, to meet the requirments for special performances and technologies, two novel nano-composite coatings, MWPUA/SiO_2 and MWPUA/CB, were developed; moreover, a high-solid-content and water-dispersible system (HSWPUA) with polymer as the continous phase was originally obtained. Finally, bio-inspired by the high-efficient light-harvesting and energy-transferring mechanisms of plants, thioxanthone/amine photoinitiator was synthesized in bionic way and the photoinitiating efficiency was optimized to explore a new technical way of improving the UV curing efficiency of deep layers in colored coating. Briefly, the major work and results we made and got are as follows:
After modifying the soft and hard segments and addressing the problems of linear product about the functional structure and performance regulation, diamine used before was replaced by polyamine compounds, which were then centered on to connect prepolymer branched chains that were terminal-capped by acrylate. Thus the functional groups got increased with the increase of terminal number, making the reaction effective and complete even under the effect of high space hindrance and the influence of complex factors, and a series of novel WPUA products with increased functionalities were obtained. Systemic research was made on the effect and influence of average functionality on the properties and structures of polymer and, based on it, the functionalities and combination properties were modified to primarily overcome the shortcomings of traditional WPUA in rigidity, strength and the resistance to water and solvent.
Surface modification was conducted to nano SiO_2 by introducing coupling agents having UV curable groups, and chemical bonds were established between nano CB and MWPUA polymer by means of grafting. In this way, nano particles in MWPUA/SiO_2 and MWPUA/CB got dispersed uniformly and stably, MWPUA/SiO_2 obtained strengthened abrasive resistance and adhesive power, and MWPUA/CB got greatly improved UV curing performance, favorable for the special demand of applied wood floor coatings and black coatings.
To meet the higher requirments of WPUA dispersion for more complicated equipments and technologies, a new concept of“high-solid-content and water-dispersable polyurethane acrylate”was proposed, and HSWPUA/acetone, HSWPUA/ethanol/acetone and HSWPUA/acrylate complexes were actually prepared. The obtained samples have solid contents over 70%. Such product, combining the technologies of high-solid-content, UV curing and water dispersion, can be accomodated to different coating methods with satisfactory combination properties like viscosity, adhesive power and water dispersion stability.
Bio-inspired by the high-efficient light-harvesting and energy-transferring mechanisms of plants, bionic investigation was made into thioxanthone/amine, a photoinitiator having similar light-harvesting and energy transferring processes. Through designing proper bridges and imitating protein supramolecular systems, the formerly separate photosensitive cells and photoinitiating cells were integrated into the same macromolecule or polymer. Based on the comparison with the structure and mechanism of plant photosystem, systemic research was made on how the arrangement, composite structure, energy transferr and electron-transfer affect the photoinitiating efficiency, and meaningful results were got primarily.
在优化软硬段结构和工艺条件、解决线型产品官能度结构和性能调控等问题的基础上,以多胺化合物替代之前的二胺扩链剂,以此为中心连接多条丙烯酸酯封端的预聚体支链,采用增加“端”数目的方式实现官能基团的进一步扩增,实现了较高空间位阻和复杂因素影响下的有效和完全反应,合成制备出一系列具有更高官能度的水性聚氨酯丙烯酸酯(WPUA)新产品。通过系统研究平均官能度对聚合物性能和结构的影响规律和作用机理,优化各主要性能,从根本上解决了传统低官能度WPUA在涂膜硬度、强度和耐水耐溶剂性方面的不足。
选用含有光固化功能基团的硅烷偶联剂对纳米SiO_2进行表面改性、以及通过接枝法使纳米炭黑和聚合物形成化学键合等方法,实现了MWPUA/SiO_2和MWPUA/炭黑两种纳米复合涂料中纳米粒子的稳定均匀分散,并使MWPUA/SiO_2体系的耐磨性和附着力,以及MWPUA/炭黑的光固化性能得到显著提升,满足了木地板涂料和黑色色漆对实用性能的特殊需求。
针对WPUA水分散体对设备和工艺技术要求复杂的问题,提出了高固体分可水分散型聚氨酯丙烯酸酯(HSWPUA)的新概念,并先后研制了HSWPUA/丙酮、HSWPUA/乙醇/丙酮和HSWPUA/丙烯酸酯复合体系,样品固含量达到70%以上。这类兼备高固体分、光固化和水可分散性三种绿色涂料技术于一体的产品,适应了多种涂布方式,并获得了令人满意的黏度、附着力和水分散稳定性等综合性能。
模拟植物高效的捕光和传能机制,对同为捕光激发和传能的夺氢型硫杂蒽酮-叔胺光引发剂进行仿生改性的探讨,设计合适的桥键结构和模拟蛋白质超分子体系,将原来独立的光敏单元和光引发单元合理结合于同一大分子或聚合物中,并对照植物光系统的结构与机制,系统研究了新型光引发剂的分布形态、复合结构、能量和电子传递途径对引发效率的影响和作用机理,获得了很好的初步成绩。
A research on the modification and application of multi-functional waterborne polyurethane acrylate (WPUA) was made with the intention to break the bottlenecks of waterborne UV coatings in their development and application. A series of linear and branched WPUA products with increased functionalities of polymer molecules were synthesized, in order to overcome the shortcomings of films in rigidity, strength and the resistance to water and solvent. Subsequently, to meet the requirments for special performances and technologies, two novel nano-composite coatings, MWPUA/SiO_2 and MWPUA/CB, were developed; moreover, a high-solid-content and water-dispersible system (HSWPUA) with polymer as the continous phase was originally obtained. Finally, bio-inspired by the high-efficient light-harvesting and energy-transferring mechanisms of plants, thioxanthone/amine photoinitiator was synthesized in bionic way and the photoinitiating efficiency was optimized to explore a new technical way of improving the UV curing efficiency of deep layers in colored coating. Briefly, the major work and results we made and got are as follows:
After modifying the soft and hard segments and addressing the problems of linear product about the functional structure and performance regulation, diamine used before was replaced by polyamine compounds, which were then centered on to connect prepolymer branched chains that were terminal-capped by acrylate. Thus the functional groups got increased with the increase of terminal number, making the reaction effective and complete even under the effect of high space hindrance and the influence of complex factors, and a series of novel WPUA products with increased functionalities were obtained. Systemic research was made on the effect and influence of average functionality on the properties and structures of polymer and, based on it, the functionalities and combination properties were modified to primarily overcome the shortcomings of traditional WPUA in rigidity, strength and the resistance to water and solvent.
Surface modification was conducted to nano SiO_2 by introducing coupling agents having UV curable groups, and chemical bonds were established between nano CB and MWPUA polymer by means of grafting. In this way, nano particles in MWPUA/SiO_2 and MWPUA/CB got dispersed uniformly and stably, MWPUA/SiO_2 obtained strengthened abrasive resistance and adhesive power, and MWPUA/CB got greatly improved UV curing performance, favorable for the special demand of applied wood floor coatings and black coatings.
To meet the higher requirments of WPUA dispersion for more complicated equipments and technologies, a new concept of“high-solid-content and water-dispersable polyurethane acrylate”was proposed, and HSWPUA/acetone, HSWPUA/ethanol/acetone and HSWPUA/acrylate complexes were actually prepared. The obtained samples have solid contents over 70%. Such product, combining the technologies of high-solid-content, UV curing and water dispersion, can be accomodated to different coating methods with satisfactory combination properties like viscosity, adhesive power and water dispersion stability.
Bio-inspired by the high-efficient light-harvesting and energy-transferring mechanisms of plants, bionic investigation was made into thioxanthone/amine, a photoinitiator having similar light-harvesting and energy transferring processes. Through designing proper bridges and imitating protein supramolecular systems, the formerly separate photosensitive cells and photoinitiating cells were integrated into the same macromolecule or polymer. Based on the comparison with the structure and mechanism of plant photosystem, systemic research was made on how the arrangement, composite structure, energy transferr and electron-transfer affect the photoinitiating efficiency, and meaningful results were got primarily.
引文
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