疏水性聚倍半硅氧烷纳米杂化材料的合成及性能  

Synthesis and Properties of Hydrophobic Polysilsesquioxane Nano Hybrid Materials

作　　者：郝丽芬[1] 杨锐妮 王学川[1] 许伟[1,2] 裴萌萌 HAO Li-fen1, YANG Rui-ni1, WANG Xue-chuan1, XU Wei1,2, PEI Meng-meng1(1.Shaanxi Key Laboratory of Chemical Additives for Industry, Shaanxi University of Science and Technology, Xi＇an 710021, Shaanxi, China;2. Zhejiang Wenzhou Research Institute o fLight Industry, Wenzhou 325003,Zhejiang, China)

机构地区：[1]陕西科技大学陕西省轻化工助剂重点实验室,陕西西安710021 [2]浙江温州轻工研究院,浙江温州325003

出　　处：《精细化工》2018年第5期728-732,739,共6页Fine Chemicals

基　　金：陕西省科技厅自然科学基础研究项目(2016JQ2031);陕西省教育厅专项(17JK0108);温州市公益性技术资助项目(G20170017)~~

摘　　要：以甲基三乙氧基硅烷（MTES）和十二烷基三甲氧基硅烷（DTMS）为前驱体,以Na OH为催化剂,在乙醇-水体系中进行水解-缩合反应,制得了一种疏水性聚十二烷基/甲基倍半硅氧烷纳米杂化材料（PDMSQ NPs）。通过FTIR和XPS对PDMSQ NPs的化学结构进行了表征;用DLS、FE-SEM及TGA对PDMSQ NPs的平均粒径、微观形貌和热稳定性进行了考察,对其合成工艺条件进行了优化。结果表明,PDMSQ NPs表面C元素质量分数高达41.73%,电子结合能103.04 eV处归属为聚倍半硅氧烷中Si 2p的特征峰,PDMSQ NPs为表面含十二烷基和甲基,且以Si—O为骨架的纳米球结构。PDMSQ NPs失重5%时的温度为351℃,表明PDMSQ NPs热稳定性优良。FE-SEM分析可知,当反应温度为60℃,n（MTES）∶n（DTMS）=10.0∶1.0-10.0∶1.4时,制得的PDMSQ NPs表面光滑、呈单分散性规整球形,水静态接触角最高达168°。提出了PDMSQ NPs的形成机理。Hydrophobic poly （dodecyl/methylsilsesquioxane） hybrid nanoparticles （PDMSQ NPs） were prepared by hydrolysis and condensation reactions of methyltriethoxysilane （MTES） and dodecyltrime- thoxysilane （DTMS） using sodium hydroxyl as catalyst in ethanol/water mixed solutions. FTIR and XPS were utilized to characterize the structure of PDMSQ NPs. DLS, FE-SEM and TGA were applied to investigate the average particles size, micro-morphology and thermal stability of the samples. The results indicated that carbon content at the surface of PDMSQ NPs was as high as 41.73%, and the signal at binding energy of 103.04 eV was characteristic of Si 2p in polysilsesquioxane （PSQ）. Hence, PDMSQ NPs had nanosphere structures with Si-O bonds as skeletons and lots of dodecyl and methyl groups on its surface. The 5% weight loss temperature of PDMSQ NPs was 351℃, which demonstrated that the PDMSQ NPs had excellent thermal stability. When the molar ratio of MTES to DTMS was from 10 ： 1.0 to 10 ： 1.4 and the reaction temperature was 60℃, the surface of obtained monodisperse PDMSQ NPs was smooth with regularly spherical structures by the FE-SEM observation. Static water contact angle was up to 168°. Finally, the formation mechanism ofPDMSQ NPs was proposed.

关 键 词：聚倍半硅氧烷 水解-缩合 纳米杂化材料 功能材料 

分 类 号：TQ317[化学工程—高聚物工业]