稀土(镧)硫醇盐的合成与表征  

Synthesis and Characterization of Rare Earth(Lanthanum) Thiolate

作　　者：祝纶宇[1,2] 许凯[1] 王洪[1,2] 刘鹏[1,2] 陈德宏[1,2] 艾好[1,2] 陈鸣才[1] 

机构地区：[1]中国科学院广州化学研究所,广东省电子有机聚合物重点实验室,广州510650 [2]中国科学院研究生院,北京100049

出　　处：《高等学校化学学报》2008年第9期1786-1790,共5页Chemical Journal of Chinese Universities

基　　金：广州市科技攻关项目(批准号:200523-D0351)资助

摘　　要：以三氧化二镧为原料,经过醇化,制备了三(月桂硫醇)镧及三(巯基乙酸异辛酯)镧,并对合成方法进行了优化.采用热失重分析、FTIR光谱、感应耦合等离子色谱、元素分析和1H NMR对目标产物进行了表征.确定合成稀土异丙醇盐最佳反应条件为:反应温度80℃,反应时间2 h;合成三(月桂硫醇)镧的反应条件为反应温度110℃,反应时间2 h,月桂硫醇的摩尔分数过量24%;合成三(巯基乙酸异辛酯)镧的反应条件为反应温度60℃,反应时间2 h,月桂硫醇过量32%.Rare earth thiolates, lanthanum tri（isooctyl thioglycolate） and lanthanum tri（dodecyl thiolate）, were prepared from lanthanum oxide by utilizing exchange reaction of rare earth alkoxide. The products were characterized via TGA, FFIR, ^1H NMR, ICP and element analysis. The optimization of synthesis condition was made. The optimal synthesis condition of lanthanum isopropoxide is at the temperature of 80 ℃ for 2 h; the optimal synthesis condition of lanthanum tri（ dodecyl thiolate） is at the temperature of 110 ℃ for 2 h and the dodecyl thiol overdoses by 24% ; and The optimal synthesis condition of lanthanum tri（ isooctyl thioglycolate） is at the temperature of 60 ℃ for 2 h and the isooctyl thioglycolate overdoses by 32%.

关 键 词：硫醇盐 镧 巯基乙酸异辛酯 月桂硫醇 

分 类 号：O623[理学—有机化学] O614.331[理学—化学]