采用超声波辅助法用一水合醋酸铜、五水合硫酸铜、二水合氯化铜、三水合硝酸铜四种铜盐分别和均苯三酸反应快速制备金属有机框架化合物HKUST-1,探讨了铜盐、三乙胺、超声波作用功率、反应时间、溶剂的配比、加料顺序等因素对HKUST-1产率的影响。结果表明,适宜的反应条件为:醋酸铜8.62 mmol,均苯三酸4.76 mmol,分别溶解于24 m L体积比为1:1:1的水、N,N-二甲基甲酰胺、乙醇的混合溶剂中,将两种反应物混合后,添加1 m L三乙胺,在300 W超声功率间歇式(超声2 s,关3 s)作用下反应30 min,可得到产率为99.1%的HKUST-1,所得产物通过XRD、IR进行表征并验证。
Cu(OAc)2·H2O, Cu SO4·5H2O, Cu Cl2·2H2O and Cu(NO3)2·3H2O were individually reacted with benzenetricarboxylic acid under ultrasonication for rapid synthesis of metal-organic framework HKUST-1. The effects of cupric salts, triethylamine, ultrasonic power, reaction time, solvent ratio and reactant addition sequence on the yield of HKUST-1 were investigated. The optimized condition for the preparation of HKUST-1 was found as: Cu(OAc)2·H2O(8.62 mmol) and benzenetricarboxylic acid(4.76 mmol) were firstly individually dissolved in the mixtures of H2 O, DMF and ethanol(volume ratio 1:1:1), and the resulted solutions were then mixed together and triethylamine(1 m L) was added. The mixture was then ultrasonicated for 30 min under intermittent ultrasonication(work 2 s, pause 3 s) to generate HKUST-1 with a yield of 99.1%. The samples were characterized by XRD and IR.