Synthesis of tetragonal sulfated zirconia via a novel route for biodiesel production
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摘要: 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 (NH3-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.Abstract: 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.
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Key words:
- tetragonal sulfated zirconia /
- impregnating /
- crystalline zirconia /
- transesterification /
- biodiesel
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Figure 1 XRD patterns of all the samples including calcined samples (SCZ-300, SCZ-400, SCZ-500) and as-synthesized sample CZ
Figure 5 EDS of the prepared sulfated zirconia catalysts
(a): SCZ-300; (b): SCZ-400; (c): SCZ-500
Table 1 Textrual properties of the CZ and SCZ samples
Sample Calcination temperature t/℃ ABET /(m2·g-1) CZ － 450 SCZ-300 300 141 SCZ-400 400 156 SCZ-500 500 66 
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Table 2 Acid properties of the different SCZ samples
Sample Peak temperature t/℃ Area under NH3-TPD peaks (a.u./mg) Total NH3-TPD peak area (a.u./mg) SCZ-300 234 553 0.08 0.09 0.17 SCZ-400 309 601 0.05 0.29 0.34 SCZ-500 309 602 0.62 0.53 1.15
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Table 3 Catalytic results obtained over the SCZ catalysts
Sample Reaction temperature t/℃ Reaction time t/h FAME yield w/% SCZ-300 150 6 1.8 SCZ-400 150 6 7.1 SCZ-500 150 6 84.6
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