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Synthesis, Characterization and Esterification Application of Acid-Functionalized Ternary Heteropolyanion-Based Ionic Liquids with Temperature-Responsive Behaviour
Author NameAffiliationE-mail
YAN Jing-Sen School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China yanjs910@163.com 
AI Li-Mei School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China  
WANG Qiang School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China  
WANG Ze-Qing School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China  
E Yong-Sheng School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China  
LIU Hai-Bin School of Biomedical & Chemical Engineering, Liaoning Institute of Science and Technology, Benxi, Liaoning 117004, China  
Abstract: A series of vanadium-substituted ternary heteropoly acids with Keggin structure were synthesized by acidification-ether extraction method. Furthermore, the heteropolyanion-based ionic liquids with functional sulfonic acid group,[PyPs]3+nPW12-nVnO40 (n=1, 2, 3), were synthesized by an ion exchange method. The products were characterized by nuclear magnetic resonance spectroscopy (NMR), element analysis, Fourier transform infrared spectrophotometry (FT-IR), UV-Vis spectrophotometry, X-ray diffraction (XRD), thermogravimetry-differential scanning calorimetry (TG-DSC) and potentiometric titration measurements. The catalytic ability and reusability of the ionic liquid catalysts were evaluated in esterification reaction of chloroacetic acid with n-pentyl alcohol. The results show that the ionic liquid catalyst was an amorphous structural compound with temperature responsive characteristics, in which Keggin structure and high acid strength of ionic liquid catalyst remain. The catalyst formed a homogeneous mixture with the reactants at the reaction temperature, but precipitated with biphase separation when the reaction ends and reaction temperature was lowered, and so could be easily separated from the products by a simple filtration. Sulfonic acid functionalized heteropolyanion-based ionic liquids exhibited higher ester catalytic activity than heteropoly acids and unsulfonated heteropolyanion-based ionic liquids. Under the optimized reaction conditions, the conversion rate of[PyPS]4PW11VO40 (PyPS is 1-(3-sulfonate) propyl pyridine) to chloroacetic acid could reach 97.6%, and the conversion rate was 91.9% after repeated reaction four times, but the structure of the catalyst had no change significantly.
Keywords: catalysis  esterification  heteropoly acid  temperature-responsive ionic liquid  synthesis  characterization
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YAN Jing-Sen,AI Li-Mei,WANG Qiang,WANG Ze-Qing,E Yong-Sheng,LIU Hai-Bin.Synthesis, Characterization and Esterification Application of Acid-Functionalized Ternary Heteropolyanion-Based Ionic Liquids with Temperature-Responsive Behaviour[J].Chinese Journal of Inorganic Chemistry,2018,34(12):2179-2187.
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Chinese Journal of Inorganic Chemistry