Synthesis of metal-organic frameworks by continuous flow
Synthesis of metal-organic frameworks by continuous flow
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DOI：
10.1039/c4gc00313f
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发表时间：
2014-08-01
期刊：
影响因子：
9.8
通讯作者：
Schroeder, Martin
中科院分区：
文献类型：
--
作者：
Bayliss, Peter A.;Ibarra, Ilich A.;Schroeder, Martin
本文描述了一种仅以水为反应介质且仅需短停留时间的金属有机骨架合成的连续流工艺。这为结合绿色化学的许多原理的材料的放大提供了一条新的途径。通过连续流动反应合成MIL-53(Al)，该工艺仅需要5-6分钟，时空产率为1300 kg m(-3) d（-1）。我们已经证明了用这种方法合成了500g MIL-53(Al)，可以通过简单地在反应器中添加金属盐和配体的进一步溶液来进一步放大。该产品比商业生产的MOF样品具有更高的表面积和更好的颜色。此外，还开发了一种利用超临界乙醇从MIL-53（Al）的孔内提取对苯二甲酸的新方法，代表了一种从多孔宿主中活化和去除底物的新方法。
A continuous flow process for the synthesis of a metal-organic framework using only water as the reaction medium and requiring only short residence times is described. This affords a new route to scale-up of materials incorporating many of the principles of Green Chemistry. The process is demonstrated by the synthesis MIL-53(Al) via continuous flow reaction requiring only 5-6 minutes with a space time yield of 1300 kg m(-3) d(-1). We have demonstrated the synthesis of 500 g of MIL-53(Al) using this process, which can be scaled-up further by simply feeding further solutions of metal salt and ligand through the reactor. The product has a higher surface area and a better colour than a commercially produced sample of this MOF. In addition, a new and effective method for the extraction of terephthalic acid from within the pores of MIL-53(Al) using supercritical ethanol has been developed, representing a new methodology for activation and removal of substrates from porous hosts.