摘要
采用三重串联四级杆液质联用仪(HPLC-MS/MS)对二苯基硅二醇缩合得到的低聚物进行分析,优化了色谱条件,组分分离效果良好.对质谱碎片离子进行解析,产物为二苯基硅二醇、1,1,3,3-四苯基-1,3-二硅氧烷二醇(二聚体)、1,1,3,3,5,5-六苯基-1,5-三硅氧烷二醇(三聚体)、1,1,3,3,5,5,7,7-八苯基-1,7-四硅氧烷二醇(四聚体)的混合物.2种催化条件下得到的产物组分相同,但主成分不同,盐酸催化下主要得到二聚体,钛酸正丁酯催化下主要得到三聚体和四聚体.
Diphenylsilanediol oligomers are synthesized by the condensation of diphenylsilanediol under catalytic con- ditions and these linear Oligomers are important raw materials to the synthesis of crosslinking agent. Through the optimization of chromatographic conditions, the products are seperated on a reversed phase using a gradient elution program of acetonitrile solution（A） and 0.1 ~/00 formic acid aqueous solution（B）. High Performance Liquid Chroma- tography-Mass Spectrometry（HPLC-MS/MS） with electrospray ionization（ESI） in positive mode is used to deter mine the compounds. On the basis of analysis of the MS and MS2 fragmentation information, the products are the mixture of raw material,linear dimeric, trimeric and tetrameric species. Seperately diphenylsilanedioI, 1,1,3,3-Tet- raphenyl-1,3-disiloxanediol, 1,1,3,3,5,5 Hexaphenyl-1,5-trisiloxanediol, 1,1,3,3, 5,5,7,7-Octaphenyl-1,7- tetrasiloxanediol. Two kinds of catalysts conditions obtain the same product components, but the main component is different. HCL mainly gets dimeric, while Ti（OBu）4 mainly gets trimeric and tetrameric species. The method has the advantage of simplicity, accuracy and sensitivity.
出处
《浙江大学学报（理学版）》
CAS
CSCD
2014年第2期175-180,共6页
Journal of Zhejiang University（Science Edition）
基金
浙江省重大科技专项(优先主题)工业资助项目(2008C11114)
