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作 者:陈加伟[1] 陈慧如[1] 漆虹[1] 徐南平[1]
机构地区:[1]南京工业大学膜科学技术研究所、材料化学工程国家重点实验室,江苏南京210009
出 处:《化工学报》2013年第11期4060-4067,共8页CIESC Journal
基 金:国家自然科学基金项目(20906047,21276123);国家高技术研究发展计划项目(2012AA03A606);江苏省高校自然科学研究计划项目(11KJB530006);江苏省“六大人才高峰”项目;材料化学工程国家重点实验室自主课题(ZK201002)~~
摘 要:以五正丁氧基铌为前驱体,通过溶胶-凝胶法制备出稳定的Nb2O5聚合溶胶,详细考察了溶胶制备过程参数(体系酸度、水解比、反应温度、反应时间和螯合剂用量)对溶胶尺寸、稳定性以及制备重复性的影响。采用平均粒径为4.8nm的Nb2O5溶胶,通过浸浆法在平均孔径为3nm的γ-Al2O3中孔膜上制备出Nb2O5微孔膜。利用TG、XRD、NH3吸附-脱附、CO2吸附、吡啶吸附傅里叶变换红外光谱(Py-IR)和单组分气体渗透实验等手段对Nb2O5粉体及微孔膜的性能进行了表征,结果表明:在200℃、0.3MPa条件下,350℃烧成的微孔Nb2O5膜对H2的渗透率和H2/CO2的理想分离因子分别为3.1×10-9 mol·m-2·s-1·Pa-1和21。此外,微孔Nb2O5膜经150kPa的水蒸气处理8h后,膜的渗透性能以及H2/CO2理想选择性基本保持不变。Polymeric Nb2O5 sols were successfully synthesized via sol-gel process by using niobium penta(n)butoxide as a precursor.Effects of synthesis parameters,including pH of system,hydrolysis ratio,reaction temperature,reaction time and chelating agent,on the state and size of Nb2O5 sols were investigated in detail.Microporous Nb2O5 membranes were deposited on defect-free γ-alumina membranes with an average pore size of ca.3 nm,by using polymeric Nb2O5 sol with an average size of 4.8 nm.The properties of Nb2O5 powder and the supported Nb2O5 membranes were characterized by TG,XRD,NH3 adsorption-desorption,CO2 adsorption,Fourier-transform infrared spectroscopy of pyridine adsorption(Py-IR)and single gas permeance test.Results showed that the single hydrogen permeance and H2/CO2 permselectivity of 350℃-calcined microporous Nb2O5 membrane were 3.1×10-9 mol·m-2·s-1·Pa-1 and 21,respectively,measured at 200℃ and 0.3 MPa.The single gas permeance and H2/CO2 permselectivity of the membrane remained fairly stable after in-situ exposure to 150 kPa steam for 8 h.
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