Characterization of Mixing Performance in a Microreactor and its Application to the Synthesis of Porous Coordination Polymer Particles
Characterization of Mixing Performance in a Microreactor and its Application to the Synthesis of Porous Coordination Polymer Particles
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DOI：
10.4164/sptj.52.382
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发表时间：
2015-07
影响因子：
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通讯作者：
Satoshi Watanabe;Shuji Ohsaki;Akiko Fukuta;T. Hanafusa;K. Takada;Hideki Tanaka;T. Maki;K. Mae;M. Miyahara
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文献类型：
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作者：
Satoshi Watanabe;Shuji Ohsaki;Akiko Fukuta;T. Hanafusa;K. Takada;Hideki Tanaka;T. Maki;K. Mae;M. Miyahara
摘要本文通过碘化物/碘酸盐化学测试反应，定量评价了自制中心碰撞式微反应器的混合性能，并将其应用于多孔配位聚合物（PCPs）或金属有机骨架（MOFs）的亚类分子筛咪唑骨架-8（ZIF-8）的合成。化学测试反应表明，该微反应器具有优异的混合性能，其特征混合时间短于1 ms，比间歇式反应器和毫米级Y形混合器快约100倍。利用快速均匀混合的优点，该微反应器通过简单地混合硝酸锌和2-甲基咪唑的水溶液成功地制备了具有高重现性的ZIF-8颗粒。在室温下的合成产生具有倒角立方体形状的ZIF-8颗粒，而5 °C的较低温度产生乌藨子型球形颗粒。结果表明，所制备的ZIF-8纳米粒子的BET比表面积约为1500 m2/g，并表现出由ZIF-8骨架结构转变引起的门吸附行为。
Abstract Here we quantitatively evaluated the mixing performance of a tailor-made microreactor with central-collision type through the iodide/iodate chemical test reaction, and applied the microreactor to the synthesis of zeolitic imidazolate framework-8 (ZIF-8), which is a subclass of porous coordination polymers (PCPs) or metal organic frameworks (MOFs). The chemical test reaction demonstrated excellent mixing performance of the microreactor with a characteristic mixing time shorter than 1 ms, which is approximately 100 times faster than those of a batch reactor and a millimeter-sized Y-shaped mixer. Taking advantage of the rapid and uniform mixing, the microreactor successfully produced ZIF-8 particles with high reproducibility by simply mixing aqueous solutions of zinc nitrate and 2-methylimidazole. The synthesis at room temperature resulted in ZIF-8 particles with chamfered cube shape, while a lower temperature of 5 °C produced raspberry-type spherical particles. We confirmed that prepared ZIF-8 particles have BET surface area of ∼1500 m 2 /g and exhibit the gate adsorption behavior caused by the structural transition of the ZIF-8 framework.