摘要
以甲基丙烯酸烯丙酯和1,1,5,5-四甲基-3,3-二苯基三硅氧烷为原料,硅氢加成得到含苯基硅氧烷的丙烯酸酯单体。采用核磁(1H-NMR)法表征了产物的封端基团,超高效液相色谱三重串联飞行时间质谱法(UPLC-QTof-MS)对不同封端基团产物的具体结构进行分析,鉴定出甲基丙烯酸-3-(1,1,5,5-四甲基-3,3-二苯基-5-甲基丙烯酰氧基三硅氧基)丙酯、1,1,5,5-四甲基-1,5-二(γ-甲基丙烯酰氧丙基)-3,3-二苯基三硅氧烷和甲基丙烯酸-3-(1,1,5,5-四甲基-5-丙基-3,3-二苯基三硅氧基)丙酯3个主要组分。建立了有机硅改性丙烯酸酯类功能材料的定性分析方法,对其进一步开发利用及其反应机理研究方面具有重要的指导意义。
Phenyl siloxane-containing acrylate monomer was prepared through hydrosilylation of allyl methacrylate with 1, 1, 5, 5-tetramethyl-3, 3-diphenyltrisiloxane. The end-groups of product were analyzed by nuclear magnetic resonance (1H -NMR). The specific structures with different endgroups were analyzed by triple ultra performance liquid chromatography - time of flight mass speetrometry(UPLC - QTof - MS). And the results showed that there were three main components, including seperately 3-(5-methacryloyloxy-1, 1, 5, 5-tetramethyl-3, 3-diphenyhrisiloxanyl)propyl methacrylate, 1, 5-bis(γ-methacryloxypropyl)-1, 1, 5, 5-tetramethyl-3, 3-diphenyl trisiloxane and 3-(1, 1, 5, 5-tetramethyl-3, 3-diphenyl-5-propyltrisiloxanyl)propyl methacrylate. In this paper, the qualitative analysis method of acrylate modified by silicone was established, which has an important guiding significance for its further development and reaction mechanism.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第11期1428-1433,共6页
Journal of Instrumental Analysis
基金
浙江省重大科技专项重点工业项目(2013C0187)