摘要
采用水热法制备了结晶良好的层状α-Zr(HPO_4)_2(α-ZrP)化合物,并利用XRD、SEM、FT-IR、TG、NH_3-TPD等技术表征了样品的物相、结晶度、热稳定性及表面酸性等;以α-蒎烯异构化为模型反应表征了样品的酸催化活性.结果表明:采用水热法可以制备出物相单一且具有良好结晶度和热稳定性的层状α-Zr(HPO_4)_2;磷酸浓度对α-ZrP的物相、结晶度有明显影响,水热条件对其表面酸性影响较大;在磷酸浓度为8M,P∶Zr(摩尔比)=3∶1,180℃下水热24 h制备的α-ZrP样品同时具有弱酸性位和中强度酸性位,150℃下反应4 h后α-蒎烯的转化率可达88.31%,具有较强的酸催化活性,异构化主产物对伞花烃的选择性高达69.45%
α-Zr( HPO4)2with good crystallinity is successfully synthesized by hydrothermal method and the acid catalytic activity of α-ZrP as catalyst is investigated by using α-pinene Isomerization as probe reaction.The phase,crystallinity,thermal stability and surface acidity of samples are then characterized by X-ray diffraction( XRD),Scanning electron microscope( SEM),Fourier transform infrared spectra( FT-IR),thermogravimetry( TG) and NH3 temperature programmed desorption( NH3-TPD). The results show that α-ZrP synthesized by hydrothermal method has good crystallinity and thermostability,and that the phase,crystallinity and surface acidity are impacted obviously by concentration of phosphoric acid and hydrothermal conditions respectively. The weak and moderate intensity acid sites are produced on α-ZrP when the concentration of phosphoric acid is 8 mol/L,the mole ratio of P to Zr is 3∶ 1 under 180 ℃ for 24 h. After reacting at 150 ℃ for 4 h,α-pinene enjoys a high conversion( 88. 31%),and the main product is p-cymene with the mass fraction of69. 45%.
作者
司甜
祝琳华
何艳萍
SI Tian ZHU Linhua HE Yanping(Faculty of Chemical Engineering, Kunming University of Science and Technology, Kunming 650500, Chin)
出处
《昆明理工大学学报(自然科学版)》
CAS
2017年第1期98-104,共7页
Journal of Kunming University of Science and Technology(Natural Science)
基金
国家自然科学基金项目(6492-20110038)
云南省教育厅科学研究基金项目(2014Y079)