摘要
以A lC l3微量水的催化体系研究了桥式四氢双环戊二烯通过两步法反应合成金刚烷。在常压反应器中考察了反应中每步的催化剂用量、反应温度、时间、溶剂用量及微量水的用量对反应结果的影响。实验结果表明endoTCD异构化为exoTCD的适宜工艺条件为:反应温度30℃、反应时间0.5 h、A lC l3与endoTCD的摩尔比为0.24、溶剂与endoTCD的摩尔比为0.3;exoTCD异构化为ADH的适宜工艺条件为:反应温度80℃、反应时间5 h、A lC l3与endoTCD的摩尔比为0.56、加水量与催化剂A lC l3的质量比为0.01。在上述工艺条件下,金刚烷的收率达86.4%。
Using tendo-tetrahydrodicyclopentadiene as raw material and AlCl3-trace water system as catalyst, adamantane was synthesized by two steps. The effect of different factors on the isomerization reaction , such as amount of AlCl3 used, reaction temperature, reaction time, concentration of solvent and amount of water was investigated at normal atmosphere. When endo-TCD was isomerized to exo-TCD ,the best reaction conditions were ：temperature,30 ℃ ; reation time,0. 5 h ; n （cat）/n （reactant） = 0. 24 ; n （ solvent ）/n （ endo-TCD ） = 0. 3. when exo-TCD was isomerized to ADH, the best reaction conditions were ： temperature, 80 ℃ ; reation time, 5 h ; n （cat）/n （reactant） = 0. 56 ; m（ water）/m（cat） =0. 01. Under optimum reaction condition, the yield of adamantane is up to 86. 4%. K
出处
《南京工业大学学报（自然科学版）》
CAS
2006年第3期86-89,共4页
Journal of Nanjing Tech University(Natural Science Edition)
关键词
金刚烷
两步法
微量水
合成
adamantine
two steps
micro water
synthesis
