层状铝钛硅酸盐Al-JDF-L1的合成与表征  

Synthesis and Characterization of Layered Alumino-Titanosilicate Al-JDF-L1

作　　者：孙月桥[1] 刘显灵[1] 杜夏梅[1] 张舒冬[2] 储刚[1] 金英杰[1] 

机构地区：[1]辽宁石油化工大学化学化工与环境学部石油化工学院,辽宁抚顺113001 [2]中国石化抚顺石油化工研究院,辽宁抚顺113001

出　　处：《石油化工》2013年第6期597-603,共7页Petrochemical Technology

基　　金：辽宁省自然科学基金项目(200922180);国家自然科学基金项目(21171083)

摘　　要：采用Na2O-TiO2-Al2O3-SiO2-KF-H2O无机体系,在190℃、120h下水热合成出结晶性层状铝钛硅酸盐(Al-JDF-L1)。用XRD、SEM、低温N2吸附-脱附和多重EDX分析表征了产物的晶相、组成和孔结构。表征结果显示,Al-JDF-L1具有与层状钛硅酸盐JDF-L1相同的晶相、形貌结构和微孔吸附性能。当结晶产物的骨架Al/Ti原子比为0.07时,Al(Ⅲ)以AlO4四面体形式嵌入Al-JDF-L1晶体结构,形成单一相Al-JDF-L1层状晶体;当骨架Al/Ti原子比增至0.37时,Al-JDF-L1层状晶体是合成产物的主要晶相,并伴生六方结构的毛沸石竞争相。此外,1.78%(w)甲基纤维素辅助合成的Al-JDF-L1试样(骨架Al/Ti原子比为0.35)具有皱缩的表面层理结构和尺度分布较宽(2.4～35nm)的层间孔,其附加的BJH比表面积和孔隙率明显增加。Novel crystalline alumino-titanosilicates with layered structure,namely microporous molecular sieves Al-JDF-L1,were hydrothermally synthesized at 190 ℃ for 120 h in Na2O-TiO2-Al2O3-SiO2-KF-H2O inorganic systems,and characterized by means of XRD,SEM,N2 adsorption-desorption and multiple EDX.The layered Al-JDF-L1 crystals showed the same crystal phase,morphological structure and microporous sorption capacity as layered titanosilicate JDF-L1,and the multiple EDX data concerning crystal compositions provided the evidence of aluminum substitution in the form of tetrahedron in Al-JDF-L1 when the Al/Ti atomic ratio of Al-JDF-L1 crystals was about 0.07.When the Al/Ti atomic ratio increased to 0.37,Al-JDF-L1 crystals as dominant phase formed with the intergrowth of a little competing hexagonal erionite.Furthermore,an isostructural analogue with Al/Ti atomic ratio 0.35 prepared with 1.78%（w） methyl cellulose-containing initial gel was confirmed to feature a wrinkled,laminated structure,which created additional mesoporosity with interlamellar distances of 2.4-35 nm and an increased BJH specific surface area.

关 键 词：水热合成 Al-JDF-L1分子筛 同晶取代 铝钛硅酸盐 层状结构 

分 类 号：TQ424.25[化学工程]