功能材料
功能材料
공능재료
JOURNAL OF FUNCTIONAL MATERIALS
2014年
21期
21025-21030,21034
,共7页
翟倩倩%严岑琪%赵士贵%周传健%周凯运
翟倩倩%嚴岑琪%趙士貴%週傳健%週凱運
적천천%엄잠기%조사귀%주전건%주개운
溶胶-凝胶法%硅烷%钛酸丁酯%杂化硅树脂%耐高温
溶膠-凝膠法%硅烷%鈦痠丁酯%雜化硅樹脂%耐高溫
용효-응효법%규완%태산정지%잡화규수지%내고온
sol-gel process%silane%tetra-n-butyltitanate%titanium containing hybrid silicone resin%heat-resistant
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-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℃3 d实现固化.通过涂层外观分析、光学显微镜、扫描电镜、紫外-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.
以鈦痠四正丁酯、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為原料,乙酰丙酮(acac)為螯閤劑、鹽痠為催化劑、乙醇為溶劑,利用溶膠-凝膠法、控製 n (Ti)∶n (Si)=0.1~0.5,50℃水解溫度下製備瞭含鈦硅樹脂,鈦的引入使得雜化硅樹脂在不使用催化劑和室溫固化劑的情況下,140℃3 d實現固化.通過塗層外觀分析、光學顯微鏡、掃描電鏡、紫外-可見吸收光譜、傅裏葉變換紅外光譜、變溫傅裏葉變換紅外光譜、熱重進行瞭錶徵.結果錶明成功閤成瞭含 Si—O—Ti 共價鍵的雜化硅樹脂;噹n (acac)/n (Ti)=0.3時,含鈦硅樹脂預聚物的儲存穩定性較好;R/(Si+Ti)≥1.36時,能製備錶麵光滑的硅樹脂;含鈦雜化硅樹脂具有較好的耐熱性且其熱性能隨鈦含量的增大而提高.
이태산사정정지、갑기삼을양기규완、이갑기이을양기규완、갑기분기이갑양기규완위원료,을선병동(acac)위오합제、염산위최화제、을순위용제,이용용효-응효법、공제 n (Ti)∶n (Si)=0.1~0.5,50℃수해온도하제비료함태규수지,태적인입사득잡화규수지재불사용최화제화실온고화제적정황하,140℃3 d실현고화.통과도층외관분석、광학현미경、소묘전경、자외-가견흡수광보、부리협변환홍외광보、변온부리협변환홍외광보、열중진행료표정.결과표명성공합성료함 Si—O—Ti 공개건적잡화규수지;당n (acac)/n (Ti)=0.3시,함태규수지예취물적저존은정성교호;R/(Si+Ti)≥1.36시,능제비표면광활적규수지;함태잡화규수지구유교호적내열성차기열성능수태함량적증대이제고.
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.