关于金属有机框架化合物MIL-125的合成？现在在尝试制备 MIL-125，我按照文献上的方法试了几次，制备出的都是白色粉末状态的产物，没有晶体出现，XRD的峰值很弱。原料是： 钛酸异丙酯 （ 四异丙氧基钛 ）； 对苯二甲酸 ；DMF；甲醇。溶剂用的都是国药的。反应温度是150℃，用的是15ml的反应釜，反应15小时。不知道哪里出问题了，还请各位大神不吝赐教。原文：MIL-125??or??Ti8O8(OH)4[O2C-C6H4-CO2]6? ? was??obtained??starting??from??1.5??mmol??of terephthalic??acid??or??1,4??Benzenedicarboxylic??acid??(250??mg)??(Aldrich,??98??%),??1??mmol??of titanium isoproproxide Ti(OiPr)4 (0.3 ml) (Acros Organics, 98%), introduced in a solution of 4.5??ml??of??dimethylformamide??(Acros??Organics,??extra-dry)??and??0.5??ml??of??dry??methanol (Aldrich, 99.9%). The mixture was stirred gently during 5 minutes at room temperature and then further introduced in a 23 ml Teflon liner and then put into a metallic PAAR digestion bomb at 150°C during15 hours. Back to room temperature, the white solid was recovered by r filtration, washed twice with aceton and dried under air at room temperature. The free solvant was removed by calcination at 200°C overnight during 12 hours.??（J. AM. CHEM. SOC. 2009, 131, 10857–10859 9 10857）查看更多7个回答 . 11人已关注
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