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晶种和晶化模式对金属有机骨架MI L-101合成的影响

         

摘要

In order to enhance the yield of metal-organic framework MIL-101,seed crystals method and dynamic hydrothermal crystallization method were involved to synthesize MIL-101.The static hydrothermal crystalliza-tion method was also involved to compare with the dynamic hydrothermal crystallization method.The influence of seed crystals and crystallization mode on the yield and grain size of MIL-1 0 1 was investigated by using X-Ray Diffraction (XRD),Scanning Electron Microscope (SEM)and N2 physical adsorption.The result showed that MIL-101 powders as seed crystals were dissolved into appropriate structural unit as a growth core of MIL-101 crystal during the synthesis of MIL-101.Consequently,the crystallization introduction period was shortened and the yield of MIL-1 0 1 was enhanced.Crystallization mode affected the yield and grain size of MIL-1 0 1 .The yield of MIL-101 synthesized by dynamic crystallization method was higher than static crystallization method,which were increased with the increasing of stirring speed when it is lower than 200 r/min.The grain size of MIL-101synthesized by dynamic crystallization method was less than static crystallization,which was decreased with the increasing of stirring speed.%采用晶种导向法、静态水热晶化法和动态水热晶化法合成金属有机骨架 MIL-101,通过 XRD、SEM、N2物理吸附等表征方法考察了晶种和晶化模式对MI L-101产物收率和晶粒尺寸的影响。结果表明, MI L-101原粉作为晶种在合成过程中可溶解成(或解离成)适当的结构单元作为晶体生长核心,缩短晶化诱导期,提高产物收率。晶化模式影响 MI L-101产物的收率和晶粒尺寸。动态晶化合成的 MI L-101产物收率较静态晶化产物收率高,搅拌速率小于200 r/min时收率随搅拌速率增加而增加。动态晶化合成的MI L-101产物晶粒尺寸较静态晶化产物晶粒尺寸小,随搅拌速率增加而减小。

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