将过硫酸铵浸渍于直接合成的纳米氧化锆晶体表面,经300-500℃高温焙烧处理获得硫化氧化锆催化剂。采用X射线衍射(XRD)、氮气吸附-脱附、氨气程序升温脱附(NH_3-TPD)、傅里叶红外光谱(FT-IR)、扫描电镜(SEM)和能谱仪(EDS)等分析手段对催化剂的结构性能进行了表征。结果表明,所有的催化剂均展现出纯四方相结构和高的结晶度。其中,经500℃热处理获得的催化剂拥有最高的硫含量和酸性位,将其应用于大豆油与甲醇酯交换反应合成生物柴油,获得了脂肪酸甲酯收率高达84.6%的催化效果,进一步表明该催化剂表面存在优越的超强酸位。
The sulfated zirconia was prepared by directly impregnating ammonium persulphate on the crystalline zirconia and followed by the calcination temperatures of 300-500℃.The structural properties of the catalysts were characterized by X-ray diffraction (XRD), N2 adsorption-desorption, ammonia temperature programmed desorption (NH3-TPD), Fourier transform infrared spectroscopy (FT-IR) and a scanning electron microscope (SEM) equipped with an energy dispersive spectroscope (EDS).The experiment results demonstrated that the catalysts presented the tetragonal structure of zirconia and high crystallinity.The catalyst calcined at 500℃ possessed the highest sulfur content and acidic sites in the catalysts.The catalyst exhibited high catalytic activity in transesterification of soybean oil with methanol.The yield of biodiesel achieved 84.6% because of the preferable super-acid sites on the surface of the catalyst.