Journal of Petrochemical Universities

Journal of Petrochemical Universities ›› 2014, Vol. 27 ›› Issue (3): 41-47.DOI: 10.3969/j.issn.1006-396X.2014.03.010

Previous Articles     Next Articles

Preparation of HY/MCM41 Composite and Application in Adsorption Desulfurization

  

  1. (1.Key Laboratory of Petrochemical Catalytic Science and Technology, Liaoning Shihua University, Fushun Liaoning 113001, China; 2. College of Chemistry & Chemical Engineering, China University of Petroleum, Qingdao Shandong 266555, China)
  • Received:2014-01-03 Revised:2014-04-18 Published:2014-06-25 Online:2014-06-16

HY /MCM - 4 1分子筛的制备及改性后在吸附脱硫中的应用

于文宇1,  阮艳军1,  秦玉才1, 2,  尹 锋1,  范跃超1,  宋丽娟1, 2   

  1. ( 1. 辽宁石油化工大学辽宁省石油化工催化科学与技术重点实验室, 辽宁抚顺1 1 3 0 0 1;
    2. 中国石油大学( 华东) 化学化工学院, 山东青岛2 6 6 5 5 5)
  • 通讯作者: 宋丽娟 ( 1 9 6 2 - ) , 女, 教授, 博士, 从事新型催化材料及清洁油品生产新工艺研究; E - m a i l : l s o n g 5 6@2 6 3. n e t 。
  • 作者简介:于文宇 ( 1 9 8 8 - ) , 男, 硕士研究生, 从事清洁燃料生产的研究; E - m a i l : y u w e n y u 0 9 0 7@1 6 3. c o m。
  • 基金资助:
    国家自然科学基金 ( 2 0 9 7 6 0 7 7, 2 1 0 7 6 1 0 0) ;国家重点基础研究发展规划 ( 9 7 3计划) ( 2 0 0 7 C B 2 1 6 4 0 3) ; 中国石油化
    工股份有限公司抚顺石油化工研究院项目资助 ( 1 0 0 1 0 1 0 2 - 1 2 - Z C 0 6 1 3 - 0 0 3 8) ; 中国石油天然气股份有限公司石油化工研究院
    项目资助 ( 1 0 - 0 1 A - 0 1 - 0 1 - 0 1) 。

Abstract: HY/MCM41 mesomicroporous composite materials composed of a core of HY zeolite and a thin layer of MCM41 have been synthesized by the overgrown crystallization. The samples were characterized by means of Xray diffraction (XRD), N2 adsorptiondesorption, scanning electron microscope (SEM), transmission electron microscope (TEM), Pyridine in situ infrared (PyIR) and Intelligent Gravimetric Analyzer (IGA) instruments. It was found that the composite material exhibited both properties of mesoporous MCM41 and microporous HYzeolite sieves. Adsorptive desulfurization performances of Ce ion supported over the synthesized composites as a sulfur adsorbent were evaluated. It was found that when the adsorbent was prepared by a solidstate grinding method with sulfur capacity of 1.81 mg/g can be obtained. While for the liquid ion exchange method, only 1.32 mg/g sulfur capacity can be reached. Through the batch methods it is found that for the former modified adsorbents the desulfurization degree can be reached to 90.6% while the latter only 81.2%. It also can be found that the Brnsted (B) acid of the adsorbent inhibited the adsorption desulfurization whereas the Lewis (L) acid, especially weak L acid, had a positive effecton adsorption desulfurization.

Key words: HY/MCM41,    ,  Composite molecular sieve,    , Adsorptive desulfurization,    ,  Sulfur capacity

摘要: 采用附晶生长法合成了 HY /MCM - 4 1复合分子筛, 利用 X射线衍射仪( XR D) 、 N2 吸附脱附、 扫描电 镜( S EM) 、 透射电镜( T EM) 、 智能重量分析仪( I GA) 、 吡啶原位红外( P y - I R) 等技术对其物化性质进行了表征, 发现 HY /MCM - 4 1复合分子筛具有微孔和介孔的双重孔道分布, 且形貌为核壳结构。通过对金属C e离子改性制得吸附 剂的吸附脱硫性能考察, 发现固相研磨法改性的吸附剂在空速为5h-1时吸附穿透硫容量可达1. 8 1m g / g, 大于液相 离子交换法改性的吸附剂吸附穿透硫容量1. 3 2m g / g。采用静态间歇法时, 固相改性的吸附剂的脱硫率可达 9 0 . 6%, 高于液相改性的吸附剂脱硫率8 1. 2%。同时发现, 吸附剂表面的B酸对吸附脱硫有着抑制作用, 而L酸尤 其是弱的L酸的酸量与吸附脱硫性能有着正相关关系。

关键词: HY /MCM - 4 1,    ,  , 复合分子筛,    ,  , 吸附脱硫,   ,  , 硫容量

Cite this article

Yu Wenyu, Ruan Yanjun, Qin Yucai,et al. Preparation of HY/MCM41 Composite and Application in Adsorption Desulfurization[J]. Journal of Petrochemical Universities, 2014, 27(3): 41-47.

于文宇, 阮艳军, 秦玉才. HY /MCM - 4 1分子筛的制备及改性后在吸附脱硫中的应用[J]. 石油化工高等学校学报, 2014, 27(3): 41-47.