Sakai Motomu, Yasuda Noriyuki, Tsuzuki Yuto, Matsukata Masahiko
Research Organization for Nano & Life Innovation, Waseda University;
Department of Applied Chemistry, Waseda University.
J Vis Exp. 2020 Feb 22(156). doi: 10.3791/60500.
Membrane separation has drawn attention as a novel-energy saving separation process. Zeolite membranes have great potential for hydrocarbon separation in petroleum and petrochemical fields because of their high thermal, chemical, and mechanical strength. A *BEA-type zeolite is an interesting membrane material because of its large pore size and wide Si/Al range. This manuscript presents a protocol for *BEA membrane preparation by a secondary growth method that does not use an organic structure-directing agent (OSDA). The preparation protocol consists of four steps: pretreatment of support, seed preparation, dip-coating, and membrane crystallization. First, the *BEA seed crystal is prepared by conventional hydrothermal synthesis using OSDA. The synthesized seed crystal is loaded on the outer surface of a 3 cm long tubular α-Al2O3 support by a dip-coating method. The loaded seed layer is prepared with the secondary growth method using a hydrothermal treatment at 393 K for 7 days without using OSDA. A *BEA membrane having very few defects is successfully obtained. The seed preparation and dip-coating steps strongly affect the membrane quality.
膜分离作为一种新型节能分离工艺已引起关注。沸石膜因其高热稳定性、化学稳定性和机械强度,在石油和石化领域的烃类分离中具有巨大潜力。BEA 型沸石由于其孔径大、硅铝比范围宽,是一种有趣的膜材料。本论文介绍了一种通过二次生长法制备 BEA 膜的方案,该方法不使用有机结构导向剂(OSDA)。制备方案包括四个步骤:载体预处理、晶种制备、浸涂和膜结晶。首先,使用 OSDA 通过传统水热合成法制备 BEA 晶种。通过浸涂法将合成的晶种负载在 3 cm 长的管状 α-Al2O3 载体的外表面。使用水热处理法在 393 K 下处理 7 天,不使用 OSDA,采用二次生长法制备负载晶种层。成功获得了缺陷极少的 BEA 膜。晶种制备和浸涂步骤对膜质量有很大影响。