多级孔无铝Beta分子筛的合成与表征
Synthesis and Characterization of Hierarchical Aluminum Free Beta Zeolite
摘要
Abstract
The influence of various parameters upon the physical state of precursor and crystallization of alu-minum-free Beta zeolite were investigated in fluoride media. X-Ray diffraction(XRD) analysis showed that H2 O/SiO2 molar ratio in the precursor played an important role in the viscosity of precursor and the crystallization of aluminum-free Beta zeolite. High H2O/SiO2 molar ratio(>10) was benefited to the precur-sor's viscosity but inhibited the crystallization process of aluminum-free Beta zeolite. While, high crystalline aluminum-free Beta zeolite with polyhedron or sphere morphology in micrometer scale could be obtained in the presence of nucleation promoter( GeO2 ) and crystallization promoter such as ClO-4 and PO3-4 at 150 ℃ for 4 d, even though H2 O/SiO2 molar ratio was high to 20-30. The analysis of thermogravimetry and energy dispersive spectrometry proved that small amount of ClO-4 and PO3-4 maybe incorporated into the channel of Beta zeolite and influenced the thermal decomposition process of template ( tetraethyl ammonium cation ) . Further charac-terization for the morphology, crystalline and pore structure of the resultant aluminu-free Beta zeolite were carried out by environmental scanning electron microscope(SEM), transmission electron microscope(TEM), selected-area electron diffraction ( SAED ) and nitrogen adsorption-desorption isotherm. The results indicate that the obtained aluminum-free Beta zeolite is hierarchical structure, which constructed by nanoparticles or nanosheets. The mesoporous pore size is in the range of 3. 4-3. 8 nm.关键词
高水硅比/晶化条件/多级孔结构/无铝Beta分子筛Key words
High H2 O/SiO2 molar ratio/Crystallization parameter/Hierarchical structure/Aluminum free Beta zeolite分类
化学化工引用本文复制引用
翁强,陈沛,赵凤起,高红旭,陈新兵,安忠维..多级孔无铝Beta分子筛的合成与表征[J].高等学校化学学报,2014,(2):215-223,9.基金项目
教育部长江学者和创新团队发展计划(批准号:IRT1070)、陕西省重点科技创新团队(批准号:2012KCT-21)、陕西省自然科学基金(批准号:2012JM2002)、陕西省科技攻关项目(批准号:2012K08-09)、中央高校团队项目(批准号:GK261001108, GK261001009)和中央高校基本科研业务费专项资金(批准号:GK201101003, GK201302036, GK201302037)资助.@@@@Supported by the Changjiang Scholars and Innovative Research Team in University, China(No. IRT1070), the Key Science & Technology Innovation Team of Shaanxi Province, China(No.2012KCT-21), the Natural Science Foundation of Shaanxi Province, China(No.2012JM2002), the Key Science and Technology Program of Shaanxi Province, China(No.2012K08-09), the State Education Ministry for the Research Team of Central Universities, China(Nos. GK261001108, GK261001009), and the State Education Ministry Fundamental Research Funds for the Central Universities, China(Nos. GK201101003, GK201302036, GK201302037) (批准号:IRT1070)