几种含α-官能团的二硅氧烷的合成与表征  

Preparation and Characterization of Several Bis (α-functional group)-contained Disiloxanes

作　　者：周振宇[1] 王政[1] 顾晓丹[1] 张一[1] 张墩明[1] 

机构地区：[1]南京大学化学化工学院,南京210093

出　　处：《有机硅材料》2009年第5期288-292,共5页Silicone Material

摘　　要：以氯甲基二甲基氯硅烷为原料制备了几种含官能团的二硅氧烷封端剂。将氯甲基二甲基氯硅烷在50%乙醇水溶液中水解,可得到85%收率的1,3-双氯甲基-1,1,3,3-四甲基二硅氧烷(产物Ⅰ);产物Ⅰ同醋酸和三乙胺在对二甲苯中回流18h,得到90%收率的1,3-双乙酰氧甲基-1,1,3,3-四甲基二硅氧烷(产物Ⅱ);在盐酸催化下,产物Ⅱ同过量甲醇在室温下进行酯交换反应24h,得到约80%收率的1,3-双羟甲基-1,1,3,3-四甲基二硅氧烷。用1HNMR、GC-MS、IR、元素分析等方法对产物进行了表征,以确定产物的含量、结构和主要副产物的结构,简单探讨了反应的影响因素。Three bis（α-functional group）-contained disiloxanes were prepared from chloromethyl-dimethyl-chlorosilane.Chloromethyl-dimethyl-chlorosilane was hydrolyzed in 50% alcohol aqueous solution,and 1,3-bis（chloromethyl）-1,1,3,3-tetramethyl disiloxane（Product I）was obtained with a yield of 85%.Product I was fluxed for 18 h with acetic acid and triethylamine in p-xylene to produce 1,3-bis（acetoxymethyl）-1,1,3,3-tetramethyl-disiloxane（Product II）with a yield of 90%.Catalyzed with hydrochloric acid,1,3-bis（hydroxymethyl）-1,1,3,3-tetramethyl-disiloxane was obtained with a yield of 80% by the reaction of Product II and excess methanol at room temperature for 24 h.1H-NMR,GC-MS,IR,and elemental analysis were used to determine the composition,structure of the products,and the main by-products.Factors which influencing the reactions were also briefly discussed.

关 键 词：氯甲基二甲基氯硅烷 1 3-双氯甲基-1 3 3-四甲基二硅氧烷 1 3-双乙酰氧甲基-1 1 3 3-四甲基二硅氧烷 1 3-双羟甲基-1 1 3 3-四甲基二硅氧烷 酯交换 

分 类 号：O627.41[理学—有机化学]