活性硅氧烷单体水解共聚

(西安科技大学 材料科学与工程学院,陕西 西安 710054)

氨丙基三乙氧基硅烷; γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷; 水解共缩聚物; 耐热性能

Hydrolysis copolymerization of activesiloxane monomers
ZAN Li-na

(College of Materials Science and Engineering,Xi'an University of Science and Technology,Xi'an 710054,China)

minopropyltriethoxysilane; γ-(2,3-epoxy propoxy)propyltrimethoxy-silane; hydrolysis of copolycondensation; heat resistance

DOI: 10.13800/j.cnki.xakjdxxb.2019.0321

备注

以氨丙基三乙氧基硅烷(KH550)、γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷(KH560)为原料,无水乙醇、丙酮、甲苯、四氢呋喃为溶剂,合成有机硅氧烷的缩聚物。采用核磁共振、红外光谱对其结构进行表征,并以热重分析对其耐热性能进行评价。通过正交实验,探讨了单体摩尔配比、反应温度、酸浓度、水量和溶剂对缩聚物产率和特性粘度的影响,得到最优工艺:当单体摩尔比为1:9,反应温度为75 ℃,酸浓度为1.5 mol/L,水用量为1 mol,有机溶剂为丙酮时,合成的有机硅氧烷缩聚物达到最佳的产率和特性粘度,水解得到的硅醇发生了交联,形成网状结构,耐热等级为147.结果表明,合成有机硅氧烷缩聚物时,溶剂种类及其极性的影响可忽略; 水量对产率影响显著,合理的水量可有效提高聚硅氧烷缩聚物产量; 单体配比是控制特性粘度的关键因素。

The cohydrolysis and condensation reactions of ami-nopropyltriethoxysilane(KH550)with γ-(2,3-epoxy propoxy)propyltrimethoxy silane(KH560),ethanol,acetone,toluene,tetrahydrofuran(THF)respectively as solvent,were studied.The structure was characterized by NMR and FT-IR,in addition to evaluate its heat resistance by TGA.Obtained by orthogonal experiment,the effects of the monomer molar ratio,reaction temperature,acid concentration,water consumption and solvent on the yield and intrinsic viscosity of condensation polymer were investigated.Optimal process conditions were obtained,when the ratio of optimum molar is 1:9,reaction temperature is 75 ℃,concentration of acid is 1.5 mol/L,content of water is 1 mol,organic solvent is acetone,synthetic organosiloxane polycondensation to achieve the best yield and intrinsic viscosity,hydrolyzed silanol cross-linked to form a network structure,heat resistance grade of 147.The results show that the influence of solvent type and polarity on the synthesis of organosiloxane polycondensation is negligible.The yield of polysiloxane can be increased by the reasonable amount of water.The monomer ratio is the key factor to control the characteristic viscosity.