微波辅助合成法制备金属有机骨架材料MOF-5的研究  

Preparation of metal-organic framework materials MOF-5 via microwave assisted method

作　　者：梁淑君[1] 韩海军[2] 翟燕[1] 李歆[1] 

机构地区：[1]太原工业学院材料工程系,山西太原030008 [2]太原工业学院机械工程系,山西太原030008

出　　处：《现代化工》2017年第3期137-140,共4页Modern Chemical Industry

基　　金：山西省高校科技研究开发项目(20121030);山西省回国留学人员科研资助项目(2012-107);山西省重点扶持学科建设经费资助

摘　　要：以六水合硝酸锌和对苯二甲酸为原料,N,N-二甲基甲酰胺(DMF)为溶剂,通过微波辅助合成的方法制备了金属有机骨架MOF-5晶体。采用X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、热失重(TG)和扫描电子显微镜(SEM)等对晶体的表面形貌、晶体结构及热稳定性等进行了表征。结果佳合成工艺条件:反应温度为130℃,反应时间为60 min,微波辐射功率为100 W,此时合成的MOF-5晶体为规则的立方体结构,粒径均匀,大小约在20~40μm。反应温度升高或降低均不利于合成规则形态的晶体;反应时间太短,晶体产率太低,延长反应时间对晶体的结构与性能影响不大,但会使产率提高;微波辐射功率对晶体的表面形貌、结构和性能有较大影响。With zinc nitrate hexahydrate and terephthalic acid as raw materials,N,N-dimethyl formamide（ DMF）as solvent,the metal organic skeleton MOF-5 crystals are prepared by microwave assisted synthesis method. The surface morphology,crystalline structure and thermal stability of the MOF-5 crystals have been characterized by X-ray diffraction（ XRD）,Fourier transform infrared spectroscopy（ FT-IR）,thermal gravity（ TG） and scanning electron microscope（ SEM）. The results show that the best synthesis conditions are： 130℃ of reaction temperature,60 minutes of reaction time and 100 W of microwave radiation power. The obtained MOF-5 crystal is a regular cubic structure with uniform crystal grain size. The size is about 20- 40 μm. Increasing or reducing reaction temperature is unfavorable to the process of crystal synthesis. When the reaction time is too short,the yield of the crystals is too low. Through prolonging the reaction time results in slightly effect on the structure and performance but leads to an increase the yield of crystals.Microwave radiation power has a great influence on surface morphology,structure and properties of the MOF-5 crystals.

关 键 词：金属有机骨架 MOF-5 微波辅助 合成法 

分 类 号：O614[理学—无机化学]