含钛杂化硅树脂的制备与耐热性能研究

Preparation and thermal properties of titanium-containing hybrid silicone resin

以钛酸四正丁酯、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、甲基苯基二甲氧基硅烷为原料,乙酰丙酮（acac）为螯合剂、盐酸为催化剂、乙醇为溶剂,利用溶胶G凝胶法、控制n（Ti）∶n（Si）=0.1-0.5,50 ℃水解温度下制备了含钛硅树脂,钛的引入使得杂化硅树脂在不使用催化剂和室温固化剂的情况下,140 ℃3d实现固化.通过涂层外观分析、光学显微镜、扫描电镜、紫外G可见吸收光谱、傅里叶变换红外光谱、变温傅里叶变换红外光谱、热重进行了表征.结果表明成功合成了含Si-O-Ti共价键的杂化硅树脂;当n（acac）/n（Ti）=0.3时,含钛硅树脂预聚物的储存稳定性较好;R/（Si＋Ti）≥1.36时,能制备表面光滑的硅树脂;含钛杂化硅树脂具有较好的耐热性且其热性能随钛含量的增大而提高.

In this paper,a kind of titanium-containing hydrid silicone resin was prepared by the hydrolysis-con-densation of tetra-n-butyltitanate,methyltriethoxysilane,dimethyldiethoxylsilane and methylphenyldimethox-ysilane through sol-gel method in ethanol system,using hydrochloric acid as catalyst,acetylacetone as comple-xing agent,hydrolysis temperature 50 ℃,and n (Ti)∶n (Si)=0.1-0.5.The curing condition was 140 ℃ for 3 d. The appearance and structure of titanium-containing hybrid silicone resin was characterized by optical micro-scope,scanning electron microscope (SEM),energy dispersive spectroscopy (EDS),ultraviolet and visible spectroscopy (UV-Vis),Fourier transform infrared spectroscopy (FT-IR )and thermal gravimetric analysis (TGA).The results indicate that,titanium-containing hybrid silicone resin consists of Ti-O-Si covalent bond,when n (acac)/n (Ti)=0.3,the storage stability was well,and when R/(Si+Ti)≥1.36,the resin had a smooth surface without cracks.The introduction of Ti improves its thermal property.