不同载体钯催化剂的结构表征及其在笼形叔胺脱N-苄基上的应用

以γ Al2O3、木质活性炭、煤质活性炭为载体,以氯化钯为前体制备了Pd(OH)2/Al2O3、Pd(OH)2/C催化剂,并用X射线衍射、透射电镜和X射线光电子能谱等技术对这些催化剂进行了结构表征。以六苄基六氮杂异伍兹烷(HBIW)的脱苄反应为例,研究了不同载体Pd(OH)2催化剂对笼形叔胺N 苄基脱苄反应的活性,分析了影响催化剂活性的各种因素。实验结果表明,当催化剂用量为HBIW质量的0 2%(以Pd计)时,氢解产品四乙酰基二苄基六氮杂异伍兹烷(TADBIW)的收率可达88%,其中以煤质活性炭为载体的催化剂已用于HBIW氢解脱苄的20kg级放大实验,TADBIW产品收率为82%。

Studies of Different Supported Palladium Catalysts for Debenzylation of the Caged Tertiary Amine

The catalysts Pd(OH)_2/Al_2O_3 and Pd(OH)_2/C were prepared using γ-Al_2O_3 and carbon as the supported materials and PdCl_2 as the precursor.These catalyst samples were characterized by XRD,TEM and XPS techniques.Debenzylation of hexabenzylhexaazaisowurtzitane(HBIW) served as example for studying the activities of these supported catalysts in debenzylation of caged tertiary amines.The results showed that the use of 0.2% Pd(based on HBIW) gave the hydrogenolysis product tetraacetyldibenzylhexaazaisowurtzitane(TADBIW) in 88% yield.In addition,the catalysts supported on the coal materials have been applied to the scale-up pilot of hydrogenolysis of 20 kg HBIW and the yield of TADBIW reached 82%.