Co-reporter:Kun Jiao, Xiangyu Xu, Zhi Lv, Jiaqing Song, Mingyuan He, Hermann Gies
Microporous and Mesoporous Materials 2016 Volume 225() pp:98-104
Publication Date(Web):1 May 2016
DOI:10.1016/j.micromeso.2015.11.043
•Nanosized Silicalite-1 with high crystallinity was synthesized in fluoride media.•Fluorine source, F/SiO2 ratio, reaction condition and silica source were studied.•Content of Si–OH in the surface of silica source affects the size and crystallinity.This paper reports on the successful crystallization of monodisperse, highly crystalline, nanosized zeolite Silicalite-1 crystals in fluoride media by using an active silica gel as silica source and tetrapropylammonium fluoride as structure directing agent. The synthesis procedure is hydrothermal dynamic crystallization. The silica/water ratio and synthesis temperature were reduced to optimize the number of crystal nuclei and control the rate of crystallization for obtaining nanosized zeolite crystals. Meanwhile, F− ions were used to partly replace OH− ions in the synthesis system to obtain zeolite products with high crystallinity. Analytical results of XRD-, SEM-, Dynamic Light Scanning- (DLS) IR-, Simultaneous Thermal Analysis- (STA) and N2 adsorption and desorption experiments show that the average particle size of zeolite Silicalite-1 product is about 45 nm and shows high crystallinity. The F− containing Silicalite-1 zeolite sample was compared with an industrial ZSM-5 zeolite sample and it shows obvious advantages in both reduced particle size and enhanced crystallinity.A nanosized F-containing Silicalite-1 zeolite with high crystallinity and high thermal stability was synthesized by dynamic hydrothermal synthesis and the main factor was the concentration of Si–OH in the surface of silica source.
Co-reporter:Zhengjia Li, Kun Jiao, Xiangyu Xu, Jiaqing Song
Microporous and Mesoporous Materials 2014 Volume 199() pp:7-10
Publication Date(Web):15 November 2014
DOI:10.1016/j.micromeso.2014.06.021
•A facile synthesis of the zeolitic precursor PLS-4 was reported.•Layered products have been obtained, due to the hydrogen bonding of hydroxyl groups.•Three new morphologies have been obtained.•This is the first directed synthesis of Al-PLS-4 zeolitic precursor.A novel synthetic route to the layered material PLS-4 has been developed using amorphous silica as the silica source and ethyldimethylethanolammonium fluoride as the organic structure-directing agent. This reaction can proceed under high concentration conditions utilizing quaternary ammonium fluoride salt rather than ammonium fluoride or hydrofluoric acid. By introducing aluminum, alkali metal and alkaline earth metal into the aforementioned system, three new morphologies have been obtained. Products were fully characterized using powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and nitrogen adsorption analyses.Graphical abstract