Preparation and shaping of solid acid SO42-/TiO2 and its application for esterification of propylene glycol monomethyl ether and acetic acid

doi:10.1016/j.cjche.2016.11.006

›› 2017, Vol. 25 ›› Issue (9): 1207-1216.DOI: 10.1016/j.cjche.2016.11.006

• Catalysis, kinetics and reaction engineering • 上一篇下一篇

Preparation and shaping of solid acid SO₄^2-/TiO₂ and its application for esterification of propylene glycol monomethyl ether and acetic acid

Zhixian Huang, Yixiong Lin, Ling Li, Changshen Ye, Ting Qiu

School of Chemical Engineering, Fuzhou University, Fuzhou 350116, China

收稿日期:2016-09-14 修回日期:2016-11-18 出版日期:2017-09-28 发布日期:2017-10-11
通讯作者: Ting Qiu,E-mail:tingqiu@fzu.edu.cn
基金资助:
Supported by the National Natural Science Foundation of China (21306025, 21576053) and the International Science & Technology Cooperation Program of China (2013DFR90540).

Preparation and shaping of solid acid SO₄^2-/TiO₂ and its application for esterification of propylene glycol monomethyl ether and acetic acid

Zhixian Huang, Yixiong Lin, Ling Li, Changshen Ye, Ting Qiu

School of Chemical Engineering, Fuzhou University, Fuzhou 350116, China

Received:2016-09-14 Revised:2016-11-18 Online:2017-09-28 Published:2017-10-11
Supported by:
Supported by the National Natural Science Foundation of China (21306025, 21576053) and the International Science & Technology Cooperation Program of China (2013DFR90540).

摘要/Abstract

摘要： The solid acid SO₄^2-/TiO₂ was prepared by immersion method and applied for synthesis of propylene glycol methyl ether acetate (PMA) through esterification reaction of propylene glycol monomethyl ether (PM) and acetic acid (HAc). The optimal catalyst preparation condition was determined by orthogonal analysis of parameters in a five-factor and four-level test. The obtained solid acid catalysts were characterized in detail by means of X-ray powder diffraction, thermogravimetry, pyridine adsorbed IR analysis, scanning electron microscopy, and BET surface area method. Synthesis of PMA was studied in this paper through experimental investigation of reaction conditions such as temperature, molar ratio of reactants, catalyst dosage and agitation speed. Based on its possible reaction mechanism, a pseudo-homogeneous kinetic model was established and its activation energies E_a⁺ and E_a^-, 65.68×10³ J·mol^-1 and 57.78×10³ J·mol^-1, were estimated. To prepare shaped solid acid catalyst SO₄^2-/TiO₂, the shaping method of impregnation-shaping-impregnation was applied. The optimal molding formulation of solid acid catalyst, obtained from the orthogonal test, was found to be binder 7 wt%, reinforcing agent 20 wt%, pore forming material 2.5 wt%, and lubricant 4 wt%. The results of performance test of catalyst demonstrated that the shaped solid acid catalyst exhibited high activity and stability.

关键词: Propylene glycol methyl ether acetate, Solid acid, Shaping, Kinetic modeling

Abstract: The solid acid SO₄^2-/TiO₂ was prepared by immersion method and applied for synthesis of propylene glycol methyl ether acetate (PMA) through esterification reaction of propylene glycol monomethyl ether (PM) and acetic acid (HAc). The optimal catalyst preparation condition was determined by orthogonal analysis of parameters in a five-factor and four-level test. The obtained solid acid catalysts were characterized in detail by means of X-ray powder diffraction, thermogravimetry, pyridine adsorbed IR analysis, scanning electron microscopy, and BET surface area method. Synthesis of PMA was studied in this paper through experimental investigation of reaction conditions such as temperature, molar ratio of reactants, catalyst dosage and agitation speed. Based on its possible reaction mechanism, a pseudo-homogeneous kinetic model was established and its activation energies E_a⁺ and E_a^-, 65.68×10³ J·mol^-1 and 57.78×10³ J·mol^-1, were estimated. To prepare shaped solid acid catalyst SO₄^2-/TiO₂, the shaping method of impregnation-shaping-impregnation was applied. The optimal molding formulation of solid acid catalyst, obtained from the orthogonal test, was found to be binder 7 wt%, reinforcing agent 20 wt%, pore forming material 2.5 wt%, and lubricant 4 wt%. The results of performance test of catalyst demonstrated that the shaped solid acid catalyst exhibited high activity and stability.

Key words: Propylene glycol methyl ether acetate, Solid acid, Shaping, Kinetic modeling

Zhixian Huang, Yixiong Lin, Ling Li, Changshen Ye, Ting Qiu. Preparation and shaping of solid acid SO₄^2-/TiO₂ and its application for esterification of propylene glycol monomethyl ether and acetic acid[J]. , 2017, 25(9): 1207-1216.

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Preparation and shaping of solid acid SO₄^2-/TiO₂ and its application for esterification of propylene glycol monomethyl ether and acetic acid

Preparation and shaping of solid acid SO₄^2-/TiO₂ and its application for esterification of propylene glycol monomethyl ether and acetic acid

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