化工学报 ›› 2016, Vol. 67 ›› Issue (7): 2880-2886.DOI: 10.11949/j.issn.0438-1157.20160104

• 分离工程 • 上一篇    下一篇

吡啶基聚合离子液体的制备及其对油中噻吩硫的吸附性能

李春喜1,2, 许慧慧1,2, 朱学习1,2, 陆颖舟2, 孟洪2   

  1. 1. 北京化工大学化工资源有效利用国家重点实验室, 北京 100029;
    2. 北京化工大学化学工程学院, 北京 100029
  • 收稿日期:2016-01-25 修回日期:2016-03-30 出版日期:2016-07-05 发布日期:2016-07-05
  • 通讯作者: 李春喜
  • 基金资助:

    国家自然科学基金项目(21376011)。

Synthesis of pyridinium based polymerized ionic liquid and its adsorptive desulfurization performance for thiophenic sulfurs from oil

LI Chunxi1,2, XU Huihui1,2, ZHU Xuexi1,2, LU Yingzhou2, MENG Hong2   

  1. 1. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China;
    2. College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029, China
  • Received:2016-01-25 Revised:2016-03-30 Online:2016-07-05 Published:2016-07-05
  • Supported by:

    supported by the National Natural Science Foundation of China (21376011).

摘要:

以4-乙烯基吡啶(VP)和1,4-对二氯苄(PXDC)为原料,通过自由基聚合和季铵化交联反应,制得了一种高度交联的离子液体聚合物——PVP-PXDC。采用凝胶渗透色谱法、元素分析法、红外光谱分析法、扫描电镜、热重分析及比表面积分析等分析方法对离子聚合物的组成、结构、形貌、热稳定性及比表面积、孔结构参数等进行了表征,并考察了吸附剂的脱硫性能。结果表明,先通过聚合得到重均分子量16万以上的PVP线性聚合物,再在DMF溶剂中按VP与PXDC摩尔比2:1加入交联剂,可得到平均孔径为17.8 nm聚合离子液体介孔材料,其热分解温度在250℃以上,比表面积为56.9 m2·g-1。在油/剂质量比50:1和30℃条件下,其对1000 mg·kg-1模型油中二苯并噻吩(DBT)、苯并噻吩(BT)和噻吩(T)的吸附量分别为5.65、5.48和4.53 mg S·g-1,远高于常规吡啶基离子液体,吸附等温线符合Freundlich方程。

关键词: 4-乙烯基吡啶, 聚合离子液体, 吸附剂, 脱硫, 噻吩硫

Abstract:

By using 4-vinyl pyridine (VP) and p-xylylene dichloride (PXDC), a PVP-PXDC, a highly crosslinked polymerized ionic liquid, was synthesized through radical polymerization and quaternary crosslinking reaction. In terms of composition, structure, morphology, thermal stability, specific surface area and pore structure of the ionic liquid polymer, it has been characterized by techniques of gel permeation chromatography, elemental analysis, infrared spectroscopy, scanning electron microscopy, thermo gravimetric analyzer and N2-adsorption, respectively, followed by the performance evaluation as adsorbent for desulfurization. It showed that the mesoporous ionic liquid polymer features 17.8 nm of average pore size, 56.9 m2·g-1 of specific area of and above 250℃ of decomposition temperature. The ionic liquid polymer was achieved by synthesis of the linear PVP polymer (160000 of weight-based mean molecular weight) followed by crosslinking with PXDC at molar ratio of VP/PXDC of 2:1 in DMF solvent. Its adsorption capacities for 1000 mg·kg-1 DBT, BT and T in a representative oil, are 5.65, 5.48 and 4.53 mg S·g-1 at 303 K and mass ratio of oil/adsorbent of 50:1, respectively, which are much higher than those of conventional pyridinium based ionic liquids. Moreover, the adsorption isotherms follow Freundlich equation.

Key words: 4-vinyl pyridine, poly ionic liquid, adsorbent, desulfurization, thiophenic sulfur

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