石油炼制与化工 ›› 2015, Vol. 46 ›› Issue (8): 76-80.

• 基础研究 • 上一篇    下一篇

W-SBA-15的制备及其吸附脱氮性能研究

唐磊,纪桂杰,沈健   

  1. 辽宁石油化工大学石油化工学院
  • 收稿日期:2015-01-29 修回日期:2015-03-24 出版日期:2015-08-12 发布日期:2015-07-27
  • 通讯作者: 沈健 E-mail:412128550@qq.com

STUDY ON W-SBA-15 PREPARATION AND ITS ADSORPTIVE DENITRIFICATION PERFORMANCE

  • Received:2015-01-29 Revised:2015-03-24 Online:2015-08-12 Published:2015-07-27

摘要: 分别以钨酸钠和钨酸铵为钨源、以正硅酸乙酯为硅源,分别采用直接合成法和后合成法制得W-SBA-15(x)和W/SBA-15(x)(x表示硅钨摩尔比),采用XRD,BET,NH3-TPD等分析手段对样品进行表征,并考察不同制备方法、不同WO3负载量以及焙烧温度、焙烧时间对样品吸附脱氮效果的影响。结果表明:直接合成法制备的W-SBA-15(20)和后合成法制备的W/SBA-15(20)都能很好地保留SBA-15的介孔结构,而直接合成法制备的W-SBA-15(10)使分子筛的有序结晶度明显变差;W-SBA-15(20)相对于W/SBA-15(20)和W-SBA-15(10)具有更好的吸附能力;当焙烧温度为550 ℃、焙烧时间为6h时,所制W-SBA-15(20)吸附剂的吸附脱氮效果最好,在反应温度为140 ℃、反应时间为30min、剂油质量比为1:30的条件下,对喹啉十二烷模拟油的脱氮率为66.32%,饱和吸附量为25.66 mg/g。

Abstract: W-SBA-15(x) was synthesized by direct synthesis method using tetraethoxysilane (TEOS) as silica source and Na2WO4 as W source, (x represent the mole ratio of W and Si). The W/SBA-15(x) was prepared by post-synthesis method using prepared SBA-15 and ammonium tungstate solution. The samples were characterized by XRD, BET, and NH3-TPD. Effect of preparation method, WO3 loadings, calcination temperature and time on the performance of adsorptive denitrification was investigated. The results show that the mesoporous structure of SBA-15 can well be remained by both direct synthesis and post-synthesis methods. The ordered crystallinity of W-SBA-15(10) is worse. The denitrification performance of W-SBA-15(20) is better than W/SBA-15(20) and W-SBA-15 (10). The denitrification performance of W-SBA-15(20) is the best when the adsorbent was calcined at 550 ℃ for 6 h. At the adsorption conditions of 140 ℃, 30 min and absorbent/oil ratio of 1:30, the denitrification rate of model oil quinoline solution in dodecane, reaches 66.32% and the saturated absorption capacity is 25.66 mg/g.