八聚(四甲基铵)硅酸盐引发D4均聚合制备八臂星型乙烯基硅油  

Preparation of Eight Arm Star Vinyl Silicone Oil Through Ring Opening Polymerization of D4 Catalyzed by Octapoly(tetramethylammonium)Silicate

作　　者：杨琳琳[1] 王晓佳 黄明 陈婕 李文清[1] 李晓晨 徐金昌 华西林[1] 杨雄发[1] 来国桥[1] YANG Linlin;WANG Xiaojia;HUANG Ming;CHEN Jie;LI Wenqing;LI Xiaochen;XU Jinchang;HUA Xilin;YANG Xiongfa;LAI Guoqiao(College of Material,Chemistry and Chemical Engineering,Key Laboratory of Organosilicon Chemistry and Material Technology,Ministry of Education,Hangzhou Normal University,Hangzhou 311121,China;Hebei Houfeng Silicone Products Co.,Ltd.,Wen'an 065800,China)

机构地区：[1]杭州师范大学材料与化学化工学院有机硅化学及材料技术教育部重点实验室,浙江杭州311121 [2]河北厚丰有机硅制品股份有限公司,河北文安065800

出　　处：《杭州师范大学学报（自然科学版）》2022年第4期342-348,共7页Journal of Hangzhou Normal University(Natural Science Edition)

摘　　要：倍半硅氧烷催化剂八聚(四甲基铵)硅酸盐催化八甲基环四硅氧烷开环聚合,以1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷为封端剂,制备了聚倍半硅氧烷为核的八臂星型乙烯基硅油,系统研究了封端剂用量、聚合时间、聚合反应温度和反应溶剂等对聚合反应的影响规律.结果表明,在无溶剂状态下100℃聚合6 h,可获得分子量5.2×10^(4)的聚倍半硅氧烷为核的八臂星型乙烯基硅油.此后,将所得聚倍半硅氧烷为核的八臂星型乙烯基硅油与乙烯基MQ树脂、二甲基含氢硅油和铂络合物混合制备了高透明的加成型硅橡胶,研究了硅橡胶的机械力学性能,还尝试着将其用作发光二极管(LED)封装材料.当乙烯基MQ树脂用量为八臂星型乙烯基硅油质量分数的30%,Karstedt's铂催化剂用量为硅橡胶总质量的0.1%,硅氢与硅乙烯基摩尔比1∶1时,硅橡胶经100℃固化2 h,其硬度约40 Shore A,在可见光范围内透光率高于90%,用该加成型硅橡胶封装的LED具有较高的光效,较窄的色温分布.Eight-arm star-shaped vinyl silicone oils with polysilsesquioxane as core were prepared through ring-opening polymerization of octamethylcyclotetrasiloxane catalyzed by octapoly(tetramethylammonium)silicate as silsesquioxane catalyst and 1,3-divinyl-1,1,3,3-tetramethyldisiloxane as end capping agent.The effects of amount of end-capped agent,polymerization time and temperature,and reaction solvents on the ring opening polymerization were studied in detail.The results showed that the molecular weight of polymer could reach 5.2×10^(4) when the ring opening polymerization was carried out at 100℃for 6 h without solvents.Then,the obtained eight-arm star-shaped vinyl silicone oils with polysilsesquioxane as core mixed with MQ silicone resin,and dimethyl hydrogen silicone oil catalyzed by Karstedt's catalyst to prepare the highly transparent additional silicone rubber.The mechanical properties of the silicone rubber were studied,and it was also tried to be used as the packaging material for light emitting diodes(LEDs).It revealed that the hardness of additional type silicone rubber was about 40 Shore A and transmittance in the visible light range was higher than 90%when the mixture of eight-arm star-shaped vinyl silicone oils with polysilsesquioxane,30 wt%vinyl MQ resin and dimethyl hydrogen silicone oil with the molar ratio of-Si-H to vinyl of 1∶1 was cured at 100℃for 2 h catalyzed by 8 ppm Karstedt's catalyst.The LED packaged with the silicone rubber exhibited higher luminous efficiency and relative narrow color temperature distribution.

关 键 词：加成型硅橡胶 聚倍半硅氧烷 八甲基环四硅氧烷 开环聚合 LED封装 

分 类 号：TQ322.4[化学工程—合成树脂塑料工业]