以粒径为0.3~0.4μm的α-Al2O3为原料,通过悬浮液真空抽吸法,制备出平均孔径约为70 nm的完整无缺陷的片状α-Al2O3支撑体;以仲丁醇铝为前驱体,采用颗粒溶胶路线制备出稳定的Boehmite溶胶,以此溶胶采用浸浆法,在制备的α-Al2O3支撑体上制备出完整无缺陷的γ-Al2O3中孔膜,并考察了烧成温度对γ-Al2O3中孔膜性能的影响。结果表明,本文制备出的γ-Al2O3膜的孔径约为3 nm,对PEG的截留分子量为2800~5300,纯水渗透通量为11.5~25.9 L·m^-2·h^-1[7.6×10^5Pa,(14±1)℃]。说明在孔径为70 nm左右的载体上直接制备孔径为3 nm的完整的中孔膜是可行的。
Starting from alumina with particle size of 0.3-0.4 /2m, disk α-Al2O3 supports were prepared via colloidal filtration with a mean pore size of ca. 70 nm as determined by Hg intrusion method. The polished supports with mirror-like surface were used for mesoporous membrane preparation. A stable Boehmite sol with a mean particle size of about 20 nm was successfully synthesized with aluminium secbutoxide (ALSB) as a precursor through particle colloidal sol-gel route. Defect-free γ-Al2O3 mesoporous membranes with pore size of ca. 3 nm superimposed on the disk α-Al2O3 supports were then prepared by dip-coating with the Boehmite sol and subsequently calcined in a temperature range of 400-800℃. The molecular weight cut-off (MWCO) for PEG and the flux for pure water of these membranes are 2800- 5300and 11. 5-25.9 L· m^-2 - h^- 1 [7.6×10^5 Pa, (14±1)℃], respectively, which confirms the integrity of the mesoporous membranes. The results presented in this paper provide a feasible method for the preparation of defect-free mesoporous membranes with a pore size of about 3 nm directly by coating onto macroporous Al2O3 support with a pore size of about 70 nm.