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A novel method to synthesize high performance silicalite-1 membrane

机译：合成高性能silicalite-1膜的新方法

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摘要

Silicalite-1 membranes supported on macroporous alumina tubes for hydrogen separation were successfully prepared by a specific synthesis protocol called counter-diffusion hydrothermal crystallization (CDHC). This method introduced silica source (tetraethyl orthosilicate, TEOS) and template agent (tetra-propyl ammonium bromide, TPABr) from opposite directions of the support wall, overwhelming the conventional in situ hydrothermal crystallization (ISHC). After an optimization process, the optimum molar composition of silicon precursor was 1SiO2:0.135Na2O:100H2O:2EtOH and that of template precursor was 1.5TPABr:100H2O. XRD and SEM analysis showed the as-prepared membranes were typical silicalite-1 membranes with high internal crystalline order as well as dense and continuous surface morphology. Single-gas permeation tests indicated the membrane prepared with optimized recipe combined high H2 permeance (1.24 x 10~(-6) mol m~(-2) s~(-1) Pa~(-1)) and good H2 selectivity (α_(H2/SF_6) = 155) at room temperature, 0.1 MPa pressure drop. Moreover, the consumption of template in this novel method was about one third of that used in conventional hydrothermal synthesis. This concept can also be extended to other many types of zeolite membranes.
机译：通过称为反扩散水热结晶（CDHC）的特定合成规程成功地制备了支撑在大孔氧化铝管上用于氢分离的Silicalite-1膜。该方法从支撑壁的相反方向引入了二氧化硅源（原硅酸四乙酯，TEOS）和模板剂（四丙基溴化铵，TPABr），使传统的原位水热结晶法（ISHC）不堪重负。经过优化处理后，硅前驱体的最佳摩尔组成为1SiO2：0.135Na2O：100H2O：2EtOH，模板前驱体的最佳摩尔组成为1.5TPABr：100H2O。 XRD和SEM分析表明，所制备的膜是典型的silicalite-1膜，具有较高的内部结晶顺序以及致密和连续的表面形态。单气体渗透测试表明，采用优化配方制备的膜结合了较高的H2透过率（1.24 x 10〜（-6）mol m〜（-2）s〜（-1）Pa〜（-1））和良好的H2选择性（在室温，0.1 MPa压降下α_（H2 / SF_6）= 155）。而且，在这种新方法中，模板的消耗量约为常规水热合成所用模板量的三分之一。该概念还可以扩展到其他许多类型的沸石膜。

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