无溶剂法合成3-(2-二甲氨基)-氧乙基-1,1,1,3,5,5,5-七甲基三硅氧烷(Me_3SiO)_2Si(Me)(OC_2H_4)NMe_2  

Solvent Free Synthesis of 3-(2-Dimethylamino)-ethyoxyl-1,1,1,3,5,5,5-heptamethyltrisiloxane(Me_3SiO)_2 Si(Me)(OC_2H_4)NMe_2

作　　者：毛桃嫣[1] 郑成[2] 林璟[2] 陈晓玲[2] 

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]广州大学精细化工研究所,广东广州510006

出　　处：《精细化工》2013年第12期1370-1373,1393,共5页Fine Chemicals

基　　金：广东省产学研项目(2012B091100492);国家大学生创新训练计划(201211078006)~~

摘　　要：利用无溶剂加热方法,以N,N-二甲基乙醇胺(DMEA)和1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)为原料,合成了(Me3SiO)2Si(Me)(OC2H4)NMe2。考察了反应时间、反应温度、反应物摩尔比、催化剂浓度等因素对反应收率的影响。通过正交实验分析法得出最佳合成条件为:MDHM和DMEA的摩尔比为1.5∶1,反应时间为25min,反应温度为100℃,催化剂用量(占反应体系总质量的百分数,下同)为0.000 8%,在该条件下,最高收率为75.6%。利用减压蒸馏分离提纯和气相色谱技术确定提纯后产物纯度,并且经过质谱分析和核磁共振波谱鉴定产物的结构。（Me3SiO）2Si （Me）（ OC2H4 ）NMe2 was synthesized by solvent-free heating method with dimethylethanolamine （DMEA） and heptamethyltrisiloxane （ MD^H M） as raw materials. The influence of reaction time, reaction temperature, reactant molar ratio, and catalyst concentration on the reaction conversion rate was discussed. Through orthogonal experiment, the solvent-free synthesis technique of （Me3 SiO）2 Si （Me） （OC2 H4 ）NMe2 was optimized. The results show that the most suitable conditions for the reaction were as follows：the molar ratio of MDHM to DMEA was 1.5：1 ,the reaction time was 25 rain,the reaction temperature was 100 ℃ ,the catalyst mass fraction was 0. 000 8% ,the product yield reached up to 75.6%. The target product was separated and purified by reduced pressure distillation and the purity of the purified product was measured by gas phase chromatography. The structure of the product was characterized by means of mass spectrum and ^1 HNMR.

关 键 词：DMEA MDHM 无溶剂合成 合成工艺优化 表面活性剂 

分 类 号：TQ423.12[化学工程]