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作 者:吕维华[1] 杨兴锴[1] 唐蓉萍[1] 夏德强[1] 杨智[1] 伍家卫[1]
出 处:《精细化工》2015年第2期205-210,共6页Fine Chemicals
基 金:兰财建(2010)122号(2010-1-219);甘教技(2011)44号(1115-01)~~
摘 要:在无乳化剂条件下,以四甲基四乙烯基环四硅氧烷和乙烯基三甲氧基硅烷为有机硅单体,用甲基丙烯酸甲酯、甲基丙烯酸(钠)和烯丙基羟乙基醚共聚物替代乳化剂制备超支化无皂纳米核壳硅丙乳液;通过L9(3)4正交实验优化配方为m(MAA)∶m(AOE)∶m(YDH)∶m(V4)∶m(MMA)=8∶9∶4∶20∶59;讨论了体系p H和引发剂用量对乳液凝胶率和粒径的影响,得出引发剂为m(K2S2O8)∶m(Na HSO3)=2∶1,用量为单体总量0.5%,p H=5±0.5时,凝胶率0.12%。用TEM和粒径分析确定该乳液为核壳结构,并且平均粒径70 nm;通过红外光谱分析得知环硅烷已开环聚合,且与其他单体共聚;热重分析进一步确定了乳液为核壳结构,核段失重峰426.6℃,壳段失重峰504.5℃,SEM表明乳液成膜性好。The emulsifier-free core-shell nano-silicone-acrylic emulsion was prepared from tetravinyltetramethylcyclotetrasiloxane, vinyhrimethoxysilane, methyl methacrylate, methacrylate and 2- allyloxyethanol. The optimum formulation m(MAA) :m(AOE) :m(YDH) :m(V4) :m(MMA) = 8:9:4: 20:59 was determined by the orthogonal test L9 (3)4. The effects of pH value and the amount of initiator on gel fraction and particle size were discussed. The conclusion was that the gel fraction was 0. 12% when pH was 5± 0.5, m ( K2 S2O8 ) : m ( NaHSO3 ) = 2:1 and the amount of initiator was 0. 5 % of the total monomers. TEM and size distribution report showed that the latex particles were core-shell structure and the average particle size was 70 nm. FTIR showed that silicon-oxygen tings were opened and all monomers had participated in the copolymerization. TG further identified that the emulsion was core-shell structure. The “core” weight loss peak was 426. 6 ℃ and the “shell” weight loss peak was 504.5℃, respectively. SEM showed that the film-forming property of the emulsion was excellent.
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