以TMAOH为添加剂制备高孔隙率纳米MIL-101(Cr)

Facile Synthesis of High Porous Nano-MIL-101(Cr) with the Addition of TMAOH

为改进纳米MIL-101(Cr)的制备方法,采用水热合成法和改进的溶剂置换法,并在反应过程中添加四甲基氢氧化铵(TMAOH),制备得到粒径均一、孔隙率较高的纳米MIL-101(Cr),并通过粉末X射线衍射(PXRD)、扫描电子显微镜(SEM)、热重分析(TG)、CHN元素分析以及N2吸附脱附实验,对纳米MIL-101(Cr)进行了表征。实验结果表明:采用改进后的溶剂置换法洗涤产物,大大地缩短了后处理时间;当TMAOH的添加量为1mmol,可制备得到粒径约为93nm、BET比表面积约为3500m2/g的纳米MIL-101(Cr);经PXRD、SEM、TG、CHN元素分析以及N2吸附脱附实验可知产物不仅纯度高,而且具有极高的孔隙率。此方法可以简单、高效地制备纳米MIL-101(Cr),从而拓宽其应用范围。

In order to improve the preparation method, nano-sized MIL-101（Cr） was synthesized with the addition of tetramethylammonium hydroxide（TMAOH）through hydrothermal method and improved solvent replacement method. The obtained nano-MIL-101 （Cr） was of uniform particle size and high porosity. The synthesized MIL-101（Cr） was characterized by PXRD、SEM、TG、CHN and N2 adsorption measurements. The results revealed that the improved solvent replacement method greatly shortened the post-treatment time. When the TMAOH was added with an amount of 1 mmol, the nano-MIL-101 （Cr） with a particle diameter about 93 nm and a BET surface area about 3 500 m2 /g could be prepared. PXRD, SEM, TG, CHN elemental analysis and N2 adsorption desorption experiments showed that the product was not only of great purity, but also of very high porosity. The new method could be used to prepare nano-MIL-101 （Cr） in a simple and efficient way to expand its application prospect.