【作者】 洪利维；

【导师】 马家举；

【作者基本信息】 安徽理工大学 ， 应用化学， 2009， 硕士

【摘要】 耐高温涂料是一种特殊涂料,它既具有一般涂料的特性,而且还具有耐高温的优点。随着现代高新技术的发展,特别是高速飞行器(如火箭、导弹)的发展,对涂料的耐热性能提出越来越高的要求。UV(ultraviolet,紫外光)固化是一种新型“绿色”辐射固化技术,其应用范围日益扩大。因此研制UV固化耐高温涂料具有一定的现实意义。在综合分析国内外研究动态的基础上,对所要合成的含氟聚酰胺酸酯进行分子结构及合成工艺路线的设计。以4,4’-六氟亚异丙基-邻苯二甲酸酐(6FDA),均苯四酸二酐(PMDA),4,4,-二氨基二苯醚(ODA),丙烯酸羟乙酯(HEA)为单体,以N-甲基吡咯烷酮(NMP)为溶剂,氮气保护下用直接、混酐、TDI等三种方法分别合成了含氟光敏聚酰胺酸酯(FPAE)。对含氟聚酰胺酸(FPAA)进行粘度测试,实验结果表明:以PMDA,6FDA与ODA为原料合成的含氟聚酰胺酸(FPAA)的最佳工艺条件为:反应温度控制在室温,二酐与二胺摩尔比为1.05~1.15:1,反应时间为3~3.5h。利用FTIR,UV,TGA等测试手段对合成产物FPAE进行了表征,结果显示:(1)直接法、混酐法、TDI法所合成的含氟光敏聚酰胺酸酯(FPAE)其紫外吸收区分别是:250~340nm,270~370nm,250~340nm;紫外可见光谱的最大吸收波长分别为为267nm、305nm、282nm;(2)在强极性溶剂(NMP、DMF、DMSO)中均具有较好的溶解性;(3)TGA图显示在100~300℃间FPAE均有较大的热失重,这点表明FPAE在100℃时开始酰亚胺化并转化为FPSPI, FPSPI在320~500℃基本保持稳定,500℃开始分解并迅速失重。选择光引发剂、单体与所合成的FPAE进行复配涂膜,并对固化涂膜进行TGA分析,结果显示:(1)UV固化后的FPAE涂膜在300℃下仍具有耐热性。(2)光热双重固化后的FPAE涂膜在350℃下仍具有耐热性。更多还原

【Abstract】 High-temperature resistant coating is a kind of special coating. It not only has the characteristics of ordinary coatings, but also has the merit of high-temperature resisting. Along with the development of high-tech, especially the development of high-speed aircraft (such as rocket and missile), more demand has been put forward for high-temp- -erature resisting capability of coatings.UV curing is a new“green”radiation curing technology and its application range expands increasingly. Therefore, developing UV curing high-temperature resistant coating has practical significance.Based on synthetic analysis of research developments at home and abroad, the molecular structure and synthesis technology route of fluoride polyamide acid ester had been designed. In this paper, synthesis of fluorine poly (amic ester) (FPAE) by using 4,4’-(hexafluoroisopropylidene) diphthalic anhydride (6FDA), pyromellitic dianhydride (PMDA), 4,4’-oxydianiline (ODA) and hydroxyl ethyl acrylate (HEA) as monomers, and N-methyl-pyrrollidone (NMP) as solvent, was conducted in nitrogen atmosphere. Meanwhile, the synthesis of FPAE by three methods(direct method, mixed anhydride method, TDI method) was carried out and the products’viscosity had been tested. The experiment results shows that the optimum reaction conditions of fluorine polyamide acid (FPAA) synthesis in room temperature are as following: n(6FDA+PMDA):nODA=1.05~1.15, reaction time 3~3.5h.FPAE was characterized by Fourier-trasform infrared spectroscopy (FTIR), ultraviolet spectroscopy (UV), thermal gravimetric analysis (TGA).The results are as following:(1)The wavelength absorption range of UV spectrum of the three products ,which was respectively prepared by direct method, mixed anhydride method and TDI method, are 250~340nm,270~370nm,250~340nm;the maximal wavelength absorption of UV spectrum are respectively 267nm,305nm,282nm; (2) They have good solubility in strong polar solvent(NMP,DMF,DMSO); (3)TGA curves show that FPAE lose weight obviously in the temperature range of 100~300℃, which reflects that FPAE starts imidization and transforms to FPSPI at 100℃. FPSPI does not change significantly in the temperature range of 320-500℃and starts decomposition at 500℃leading to losing weight rapidly.Choosing photoinitiators, monomer and FPAE to make compound coating film, then TGA was use to analyze the solidified coating film. The results are as following: (1) FPAE coating film prepared by UV curing still has heat-resistant property at 300℃;(2) FPAE coating film prepared by UV-heat dual curing still has heat-resistant property at 350℃.更多还原