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ZSM-5、ZSM-35和ZSM-39沸石多孔材料的合成与表征
The Synthesis and Charaterization of Porous Materials ZSM-5,ZSM-35 and ZSM-39 Zeolites
【作者】 厉学武;
【导师】 董晋湘;
【作者基本信息】 太原理工大学 , 工业催化, 2005, 硕士
【摘要】 规整多孔材料因具有均一的孔道、可以调控的晶体形貌、尺寸以及容积等,所以在催化、离子交换、吸附等方面已经被广泛应用,其合成、特性与应用研究,成为国际上的热点研究课题之一。本文系统考察了氟离子对蒸气相合成ZSM-35沸石的影响,报道了ZSM-39沸石在蒸气相中的合成规律以及过渡金属在蒸气相中合成ZSM-35沸石过程中的作用。 首先,在F--SiO2-Al2O3-H2O的反应体系中,通过选择合适的反应物组成、晶化温度和反应时间系统考察了氟离子对合成ZSM-35沸石的影响。采用XRD、SEM、TG-DTA、氮吸附、FT-IR以及NMR分析技术对合成的ZSM-35沸石样品进行了表征,结果表明凝胶组成为40NH4F-13.58SiO2-Al2O3-57.36H2O,液相组成为
【Abstract】 Ordered porous materials have been intensively applied in many fields such as adsorption, ion exchange, and catalysis owing to their uniformity of pore system, modification of pore size, volume, crystal morphology and so forth. Recently, the synthesis, characteristic and application about ordered porous materials became hot topic on the international. In this paper, effects of fluoride ion on the synthesis of ZSM-35 zeolite were investigated by vapor phase transport method. Additionally, the roles of transition metals in synthesis of ZSM-35 zeolite were systematically investigated and the synthesis of ZSM-39 zeolite using vapor phase transport method was reported.Firstly, the effects of fluoride ion in the crystallization system of F--SiO2-Al2O3-H2O were systematically studied using vapor phase transport method by means of the selectivity of reaction compositions, synthesis conditions such as crystallization time and temperature. Thesamples synthesized were characterized by the XRD, NMR, SEM, nitrogen adsorption, TG-DTA and FT-IR. The experiment results showed that ZSM-35 zeolite was synthesized when the chemical compositions of gels were 40NH4F-13.58SiO2-Al2O3-57.36H2O by vapor phase transport method, the compositions of liquid reaction mixtures was EDA/H2O=1.32, crystallization temperature and time were 493 K and 15 days respectively, the experiment results showed that fluoride ion played the roles of improving crystal size, increasing ZSM-35 zeolite surface area and framework Si/Al ratio.Secondly, we systematically investigated roles of transition-metal ion (such as Cr3+, Mn2+, Co3+, Cu2+, Zn2+, Pb2+) in the synthesis of ZSM-35 zeolite using vapor phase transport method. Samples synthesized were characterized by the XRD, FT-IR, UV-vis and SEM. The experiment results showed that Mn2+, Co3+, Cu2+, Zn2+ and Pb2+ could only alter the crystal size, crystal morphology and relative crystallinity of ZSM-35 zeolite, whereas the introduction of Cr3+ makes reaction compositions forming ZSM-5 zeolite instead of ZSM-35 zeolite. It implies that Cr3+ plays the roles that induced synthesis compositions to produce ZSM-5 zeolite, chromium was incorporated framework of ZSM-5 zeolite, altered the compositions of ZSM-5 zeolite synthesized; meanwhile ZSM-5 zeolite synthesized possessed high relative crystallinity, good crystal morphology and uniform crystal size.Lastly, we reported the synthesis of microporous ZSM-39 zeolite in the crystallization system of F"-SiO2-H2O using vaporphase transport method by using ?-propylamine as template agent, fumed silicate as silica source and ammonium fluoride as mineralizing agent. The samples synthesized were characterized by the XRD, SEM and FT-IR. The experiment results proved that ZSM-39 zeolite with high relative crystallinity, good crystal morphology and large crystal size was obtained from the reaction system of NH4F-Si2O-6.7H2O when the reaction time and temperature were 15 days and 493 K respectively.
【Key words】 vapor phase transport method; zeolite; synthesis; characterization;
- 【网络出版投稿人】 太原理工大学 【网络出版年期】2006年 02期
- 【分类号】O643.36
- 【被引频次】3
- 【下载频次】1036