b轴取向透明Silicalite-1分子筛膜的制备研究
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摘要
开发一种在透明载璃片载体上合成致密透明连续的b轴定向Silicalite-1分子筛膜的方法。首先对载体进行预处理,再结合原位水热合成法,合成出致密连续的b轴定向的Silicalite-1分子筛膜。研究改变载体的预处理方式、晶化时间、合成液配比等条件对分子筛膜合成的影响。采用X射线衍射(XRD)和扫描电镜(SEM)对膜的定向性和晶体形貌进行表征。通过XRD和SEM图可以看出,在晶化温度180oC,晶化时间48 h,以乙醇溶液进行载体预处理的条件下,合成出的分子筛膜为连续致密的,且定向性较好。
In this paper, a dense and continuous b-oriented Silicalite-1 zeolite film was synthesized on transparent glass substrate. The substrate was firstly treated with piranha solution, then it was transformed into Silicalite-1 zeolite synthesis solution to obtain oriented film. The effect of pre-treatment method, the crystallization time,the composition of the synthesis solution were investigated. The crystallinity and morphology of the oriented film was examined by X-ray diffraction(XRD) and scanning electron microscopy(SEM). It can be concluded that the best synthesis parameter is the crystallization temperature of 180 o C, crystallization time of 48 h, substrate pretreated with ethanol. A continuous, dense Silicalite-1 film was prepared with better orientation.
In this paper, a dense and continuous b-oriented Silicalite-1 zeolite film was synthesized on transparent glass substrate. The substrate was firstly treated with piranha solution, then it was transformed into Silicalite-1 zeolite synthesis solution to obtain oriented film. The effect of pre-treatment method, the crystallization time,the composition of the synthesis solution were investigated. The crystallinity and morphology of the oriented film was examined by X-ray diffraction(XRD) and scanning electron microscopy(SEM). It can be concluded that the best synthesis parameter is the crystallization temperature of 180 o C, crystallization time of 48 h, substrate pretreated with ethanol. A continuous, dense Silicalite-1 film was prepared with better orientation.
引文
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[12]Motuzas J,Julbe A,Noble R D,et al.Rapid synthesis of oriented Silicalite-1 membranes by microwave-assisted hydrothermal treatment[J].Microporous and Mesoporous Materials,2006,92(1-3):259-269.
[13]XU X,YANG W,Liu J,et al.Fast formation of Na A zeolite membrane in the microwave field[J].Chinese Science Bulletin,2000,45(13):1 179-1 181.
[14]WANG Z,YANY.Controlling crystal orientation in zeolite MFI thin films by direct in situ crystallization[J].Chemistry of materials,2001,13(3):1 101-1 107.
[2]蒋海洋.分子筛膜的制备和新型分子筛膜反应器[D].天津大学,2004.
[3]石义平.定向Silicalite-1分子筛膜的合成[J].膜科学与技术,2008,28(4):9-13.
[4]刘赞,王新忠,陈爱民.分子筛膜分离技术的研究进展[J].工业水处理,2006,26(11):12-15.
[5]TAVOLARO A,DRIOLI E.Zeolite membranes[J].Advanced Materials,1999,11(12):975-996.
[6]YAN Y,DAVIS M E,GAVALAS G R.Preparation of zeolite ZSM-5 membranes by in situ crystallization on porousα-Al2O3[J].Industrial&Engineering Chemistry Research,1995,34(5):1 652-1 661.
[8]LEE J S,LEE Y J,TAE E L,et al.Synthesis of zeolite as ordered multicrystal arrays.[J].Science,2003,301(5634):818-821.
[9]YAN Y,AND Z W.Controlling Crystal Orientation in Zeolite MFI Thin Films by Direct In Situ Crystallization[J].Chemistry of Materials,2001,13(3):1 101-1 107.
[10]LIU Y,LI Y,YANG W.Fabrication of highly b-oriented MFI film with molecular sieving properties by controlled in-plane secondary growth.[J].Journal of the American Chemical Society,2010,132(6):1 768-1 769.
[11]LL X,YAN Y,WANG Z.Continuity control of b-oriented MFI zeolite films by microwave synthesis[J].Industrial&Engineering Chemistry Research,2010,49(12):5 933-5938.
[12]Motuzas J,Julbe A,Noble R D,et al.Rapid synthesis of oriented Silicalite-1 membranes by microwave-assisted hydrothermal treatment[J].Microporous and Mesoporous Materials,2006,92(1-3):259-269.
[13]XU X,YANG W,Liu J,et al.Fast formation of Na A zeolite membrane in the microwave field[J].Chinese Science Bulletin,2000,45(13):1 179-1 181.
[14]WANG Z,YANY.Controlling crystal orientation in zeolite MFI thin films by direct in situ crystallization[J].Chemistry of materials,2001,13(3):1 101-1 107.