螺环型硅钛树脂的合成与表征

Synthesis and characterization of spirocyclic silicon-titanium resin

以端羟基聚二甲基硅氧烷为原料、钛酸四丁酯为Ti源,合成了螺环型硅钛树脂。采用FT-IR(红外光谱)法、1H-NMR(核磁共振氢谱)法、GPC(凝胶渗透色谱)法、元素分析法和TGA(热失重分析)法等对产物的结构和性能进行了表征,并探讨了反应时间对反应进程的影响。研究结果表明:螺环型硅钛树脂的初始分解温度为300℃,800℃时的残炭率为27%左右,说明该硅钛树脂的热稳定性较好;聚合物在不同温度热解时,其热解速率在热解时间为5~20 min时相对最大,400℃之后热失重现象明显减弱且失重率较小;合成硅钛树脂的聚合速率很大,并且主要的聚合反应是环聚反应。

With hydroxyl-terminated polydimethylsiloxane as raw material, tetrabutyl titanate as Ti source, a spirocyclic silicon-titanium resin was synthesized. The structure and properties of product were characterized by FT-IR （infrared spectrum） , 1H-NMR （nuclear magnetic resonance hydrogen spectrum） , GPC （gel permeation chromatography）, element analysis and TGA （thermo-gravimetric analysis） methods, and the influences of reaction time on reaction process were discussed. The research results showed that the spirocyelic silicon-titanium resin had the better thermal stability because its initial decomposition temperature was 300 %, and its carbon residual rate at 800 ℃ was about 27%. When the polymer was pyrolyzed at different temperatures, its pyrolysis speed was relatively maximal at pyrolysis time for 5-20 min, but the hot weightlessness was significantly weakened at higher than 400 ℃, and the weightlessness rate was less. The polymerization speed of synthesizing silicon-titanium resin was very large, which main polymerization was polycyclization.