One-pot synthesis of SO42-/Zr-PHTS via hydrothermal method and their catalytic behavior

doi:10.3969/j.issn.0438-1157.2012.11.022

Abstract

Abstract: Mesoporous sulfated Zr-PHTS(SO₄^2-/Zr-PHTS)solid acid was prepared by using P123(EO₂₀PO₇₀EO₂₀)as a structure directing agent via the one-pot hydrothermal process in lower concentration sulfuric acid solution.These prepared samples were characterized by powder X-ray diffraction(XRD),TEM,N₂ sorption isotherms,Py-FTIR spectra,and NH₃-TPD.The characterization results showed that the obtained samples possessed well-ordered hexagonal mesostructure,and all the samples had weak and medium acidity dominated by Lewis acid sites according to the analysis of pyridine adsorption and NH₃-TPD.With the increase of Si/Zr molar ratio,specific surface areas relatively little varied and acidity was obviously reduced,but pore volume and pore diameter were not severely affected.In addition,the SO₄^2-/Zr-PHTS catalyst showed good performance in the THF polymerization reaction,and such result could be related to the mesoporous structure and surface acidity.

Key words: SO₄^2-/Zr-PHTS, hydrothermal synthesis, solid acid, tetrahydrofuran, polymerization

摘要： 在低酸度硫酸体系中,以P123(EO₂₀PO₇₀EO₂₀)为模板剂水热法一步合成硫酸化锆掺杂PHTS固体酸催化剂(SO₄^2-/Zr-PHTS),利用XRD、TEM、N₂吸附-脱附以及NH₃-TPD、Py-FTIR等手段对其进行表征。结果表明,SO₄^2-/Zr-PHTS具有有序的六方相介孔结构,具有以L酸为主的弱、中强度的酸性中心;随着硅锆摩尔比的增加,其酸量逐渐减少,比表面积逐渐增加,孔容、孔径无显著变化。SO₄^2-/Zr-PHTS在催化四氢呋喃聚合中表现出良好的反应性能,推测固体酸的表面酸性和孔结构决定着催化四氢呋喃聚合的反应性能。

关键词: SO₄^2-/Zr-PHTS, 水热合成, 固体酸, 四氢呋喃, 聚合

CLC Number:

O643.32

HAN Yanhui, JIA Zhiqi, GE Yuanyuan, ZHAO Yongxiang. One-pot synthesis of SO₄^2-/Zr-PHTS via hydrothermal method and their catalytic behavior[J]. CIESC Journal, 2012, 63(11): 3531-3536.

韩艳辉, 贾志奇, 盖媛媛, 赵永祥. 水热一步法合成SO₄^2-/Zr-PHTS及其催化性能[J]. 化工学报, 2012, 63(11): 3531-3536.

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One-pot synthesis of SO₄^2-/Zr-PHTS via hydrothermal method and their catalytic behavior

水热一步法合成SO₄^2-/Zr-PHTS及其催化性能

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