以二乙胺为模板剂,利用微波辅助水热合成法制备了SAPO-11晶体,研究了水热温度和时间对合成产物晶体结构性质的影响。采用XRD、FT-IR、SEM、BET和NH3-TPD等手段对SAPO-11晶体的物相组成、骨架结构、微观形貌、孔结构及表面酸性进行了分析表征。研究结果表明,不同水热条件对SAPO-11晶体结构性质影响较大。反应温度低于180℃时,合成样品仅存SiO2物相,无SAPO-11晶相生成；反应温度高于200℃时,部分SAPO-11晶体二次生长致使晶粒均匀度和比表面积大幅下降；反应时间大于1 h时,SAPO-11晶体生长易转晶生成少量AlPO4-5和CFSAPO-1(C)杂晶相；在反应温度200℃,反应时间1 h条件下制备得到的纯相SAPO-11球形晶粒表面具有弱酸特征,比表面积、孔容和平均孔径分别达199.4 m2·g-1,0.15 cm3·g-1和2.92 nm。
Effect of various reaction temperature and time on crystal structure properties of SAPO-11 synthesized from diethylamine template via microwave-assisted hydrothermal route was investigated in this paper. These obtained products were characterized by XRD, FT-IR, SEM, BET and NH3-TPD techniques to investigate their crystalline phase, skeletal structure, morphology, pore structure and surface acidity. The results indicate that different hydrothermal conditions pose significant impact on the structure properties of the synthesized products. Only SiO2 phase but no SAPO-11 crystalline phase existed in the product synthesized when the reaction temperature below 180 ℃, and the SAPO-11 with rather small specific surface area and inhomogeneity in crystal size was also obtained when the reaction temperature higher than 200 ℃. A small amount of AlPO4-5 and CFSAPO-1 ( C ) miscellaneous crystal phases are derived from SAPO-11 crystal when the reaction time over 1 h. The product with pure SAPO-11 phase and spherical crystalline grains was eventually and successfully synthesized at 200℃ for 1 h via microwave-assisted hydrothermal route, and the SAPO-11 possessed distinct physicochemical properties with the weak acid on the surface, high specific surface area of 199. 4 m2·g-1, pore volume of 0. 15 cm3 ·g-1 and average pore diameter of 2. 92 nm.
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