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为了获得高性能Silicalite-1沸石膜,采用提拉法在大孔α-Al2O3载体上制备了Silicalite-1/TiO2复合过渡层,再在此过渡层上水热合成Silicalite-1沸石膜。探讨了过渡层中Silicalite-1晶种对成膜性能的影响,并采用XRD、SEM和单组分气体渗透测试对Silicalite-1沸石膜进行表征。结果表明,采用该方法合成得到了典型的Silicalite-1沸石膜,没有其它杂晶出现,同时缩短了传统水热合成法的成膜周期。所得Silicalite-1沸石膜层薄而致密,晶粒小而均匀,没有大的缺陷,紧密围绕载体表面生长。在25℃、0.1 MPa条件下,该Silicalite-1沸石膜的H2渗透速率为1.0×10-6mol/(m2.s.Pa),H2/SF6理想分离因数达到205.4;在200℃、0.1 MPa条件下,H2渗透速率达到2.1×10-6mol/(m2.s.Pa),H2/N2理想分离因数达到3.5。
In order to obtain high-performance Silicalite-1 zeolite membrane, Silicalite-1 / TiO2 composite transition layer was prepared on the macroporous α-Al2O3 support by Czochralski method. Hyd Silicite-1 zeolite membrane was hydrothermally synthesized on this transition layer. The effect of Silicalite-1 seeds in the transitional layer on the film-forming properties was discussed. Silicalite-1 zeolite membranes were characterized by XRD, SEM and single component gas permeation test. The results show that the typical Silicalite-1 zeolite membrane synthesized by this method has no other miscellaneous crystals and shortens the film-forming cycle of traditional hydrothermal synthesis. The obtained Silicalite-1 zeolite film is thin and dense, with small and uniform grains, no big defects and closely surrounding the surface of the carrier. The H2 permeation rate of this Silicalite-1 zeolite membrane was 1.0 × 10-6mol / (m2.s.Pa) at 25 ℃ and 0.1 MPa, and the ideal separation factor of H2 / SF6 was 205.4. Under the conditions of 200 ℃ and 0.1 MPa H2 permeation rate reached 2.1 × 10-6mol / (m2.s.Pa), H2 / N2 ideal separation factor reached 3.5.