三氢化铝的一锅法制备与表征

发布时间：2018-02-13 10:31

  本文关键词： 三氢化铝 α-三氢化铝 固相真空法 固相甲苯法 浆液法 一步法　出处：《哈尔滨工业大学》2015年硕士论文　论文类型：学位论文

【摘要】：本文系统综述了Al H3的合成及应用研究现状。提出一种改进型的制备方法:(1)在制备Al H3乙醚络合物过程中直接用含有Li Cl沉淀的Al H3乙醚络合物进行脱醚转晶,得到固相产物;(2)对固相产物进行洗涤,除去Li Cl杂质并对α-Al H3进行稳定化处理。此种不需过滤Li Cl的方法被我们称为“一锅法”。根据Al H3乙醚络合物所处的状态和环境,将Al H3的“一锅法”合成细化成固相真空法、固相甲苯法以及浆液法并分别进行研究。最后还研究了Al H3的“一步法”合成。通过固相真空法,将含有Li Cl的固体Al H3醚合物在真空条件下进行转晶,XRD和IR等测试结果表明改变Li BH4用量以及转晶温度、转晶时间等反应条件,利用固相真空法制备出了单一晶型的α-Al H3:当没有Li BH4参与反应且Li Al H4:Al Cl3摩尔比为4:1时,单一晶型α-Al H3所需的转晶温度为77~80℃,转晶时间为2~3 h;当有Li BH4参与反应且Li Al H4:Al Cl3:Li BH4摩尔比为4:1:0.5时,单一晶型α-Al H3所需的转晶温度为80~85℃,转晶时间为1~2 h。通过固相甲苯法,将含有Li Cl的固体Al H3醚合物在甲苯中进行转晶,XRD和IR等测试结果表明改变转晶温度、转晶时间等反应条件,利用固相甲苯法也制备出了单一晶型的α-Al H3:当Li Al H4:Al Cl3:Li BH4摩尔比为4:1:1时,理想转晶温度和时间分别为80~85℃和1.5~2 h。此种方法制备的单一晶型的α-Al H3氢含量为8.8~8.9wt%。通过浆液法,将Al H3乙醚络合物溶液浓缩后,置于甲苯条件下进行转晶,改变转晶温度以及实验流程,确定了浆液法制备α-Al H3的合适条件。XRD结果表明产物为单一晶型的α-Al H3;TG测试表明失重量与理论值10.1wt%相当,且产物的初始分解温度高达176℃。类似于浆液法,一步法是直接用Li Al H4和Al Cl3在90~100℃的甲苯中直接制备非溶剂化的α-Al H3。实验结果表明样品是直径为10~50μm的大颗粒,分解温度在170℃,含氢量高达10%。综合对比四种方法的结果,浆液法合成的α-Al H3呈直径10~50μm的大颗粒,测试结果表明制备的α-Al H3的生成热焓值为11.9 k J/mol,失重率高达10wt%,均与理论值相一致,因此更适合单一晶型α-Al H3的制备。
[Abstract]:In this paper, the synthesis and application of Al H 3 are reviewed systematically. An improved preparation method: 1) in the process of preparing Al H 3 ether complex, it is directly used to deether transprystallization with Al H 3 ether complex containing Li Cl precipitation. The solid product is washed, the impurity of Li Cl is removed and 伪 -Al H 3 is stabilized. This method, which does not require filtration of Li Cl, is called "one pot process." according to the state and environment of the Al H 3 ether complex, The "one pot" synthesis of Al H 3 was refined into solid phase vacuum method, solid phase toluene method and slurry method, respectively. Finally, the "one step" synthesis of Al H 3 was also studied. The results of XRD and IR measurements of solid Al H 3 ether complexes containing Li Cl in vacuum show that the amount of Li BH4 and the reaction conditions such as temperature and time of transition are changed. The single crystalline 伪 -Al H 3 was prepared by solid phase vacuum method. When there was no Li BH4 in the reaction and the mole ratio of Li Al H 4 to Al Cl3 was 4: 1, the transition temperature of 伪 -Al H 3 was 7780 鈩，

本文编号：1507953