摘要
以环戊二烯二聚体(DCPD)为原料,采用与水共沸法进料,进行气相裂解得环戊二烯单体(CPD),再在二乙胺存在下将其与TiCl4反应合成了目标产物二氯二茂钛(TDC).优化了合成工艺条件:TiCl4和环戊二烯摩尔比为1∶4,二乙胺和TiCl4摩尔比为3∶1,以1,4-二氧六环为溶剂,常压下回流反应4 h,采用DMF多次溶解提纯.结果表明:合成效果好,TDC产率可达75.4%,且减少了环境的污染.
The raw material (dicyclopentadiene) is decomposed by vapor-phase thermal cracking method and using azeotrope feeding with water, and then the monomer(cyelopentadiene) is obtained. Whereafter the target product (titanocene dichloride) is synthesized via the reaction of cyelopentadiene and TICl4 in the presence of diethylamine. The resulting optimum conditions are as follows:the molar ratio of TICl4 and cyclopentadiene is 1 : 4; the molar ratio of diethylamine and TICl4 is 3 : 1; the solvent is dioxane; atmospheric refluxing 4h, multiple dissolving and purifying by DMF. The results show that the yield of titanocene dichloride can reach 75.4 % and environmental pollution is reduced.
出处
《湖南工程学院学报(自然科学版)》
2009年第1期62-65,共4页
Journal of Hunan Institute of Engineering(Natural Science Edition)
关键词
二氯二茂钛
环戊二烯
合成
titanoeene dichloride
cyclopentadiene
synthesis.