酸功能化磷钨钒杂多酸离子液体的合成及其酯催化性能研究
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摘要
采用酸化萃取-离子交换法合成了三种季胺类磷钨钒杂多酸离子液体催化剂,对其进行了红外和紫外表征,考察了各催化剂对氯乙酸和正戊醇的酯化反应性能和重复使用性能。结果表明,三种催化剂的催化酯化性能依次为[TEAPS]_5PW_(10)V_2O_(40)>[TEAPS]_6PW_9V_3O_(40)>[TEAPS]_4PW_(11)VO_(40)。在催化剂用量0.2g,带水剂用量10mL,反应温度140℃,醇酸比1.2:1的反应条件下,催化剂[TEAPS]_5PW_(10)V_2O_(40)性能最佳,其酯化率高达98.75%,具有便于回收、重复使用性能好的特点。
Three kinds of quaternary amines phosphotunstovanadium heteropoly acid ionic liquid catalysts are synthesized by stepwise acidification-ether extraction and ion exchange method. The catalysts are characterized by Fourier transform spectrophotometry(FT-IR) and UV-Vis spectrophotometry(UV). The catalytic ability and reusability are evaluated in esterfication of chloroacetic acid and n-pemyl alcohol. The results show that the catalytic ability order of prepared catalysts is listed as follow:[TEAPS]_5PW_(10)V_2O_(40)>[TEAPS]_6PW_9V_3O_(40)>[TEAPS]_PW_(11)VO_(40). Under the optimized condition, i.e. the amount of catalyst is 0.2 g, water carrier is 10 mL, reaction temperature is 140℃, the ratio of alcohol to acid is 1.3/1, the [TEAPS]_5PW_(10)V_2O_(40) exhibits the best catalytic performance with esterification rate 98.75%, and has good recovery ability and reusability.
Three kinds of quaternary amines phosphotunstovanadium heteropoly acid ionic liquid catalysts are synthesized by stepwise acidification-ether extraction and ion exchange method. The catalysts are characterized by Fourier transform spectrophotometry(FT-IR) and UV-Vis spectrophotometry(UV). The catalytic ability and reusability are evaluated in esterfication of chloroacetic acid and n-pemyl alcohol. The results show that the catalytic ability order of prepared catalysts is listed as follow:[TEAPS]_5PW_(10)V_2O_(40)>[TEAPS]_6PW_9V_3O_(40)>[TEAPS]_PW_(11)VO_(40). Under the optimized condition, i.e. the amount of catalyst is 0.2 g, water carrier is 10 mL, reaction temperature is 140℃, the ratio of alcohol to acid is 1.3/1, the [TEAPS]_5PW_(10)V_2O_(40) exhibits the best catalytic performance with esterification rate 98.75%, and has good recovery ability and reusability.
引文
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[3]吴庆银,柳云骐,唐瑜.现代无机合成与制备化学[M].北京:化学工业出版社,2010.
[4]王军.离子液体的性能及应用[M].北京:中国纺织出版社,2006.
[5]马青,童金辉,宿玲弟,等.物理化学学报[J].,2016,32(12): 2961-2967.
[6]Domaille, P. J.; Hervéa, G.; Téazéa, A. Vanadium (V) substituted dodecatungstophosphates Inorg. Synth., 2007, 27: 96-104.
[7] Leng Y, Wang J, Zhu D R, et al. Heteropolyanion-based ionic liquids:Reaction-induced self seperation catalysts for esterification Angew. Chem. Int. Ed,2009, 48:168–171.
[8] Wu X, Huang T, Tong X, et al. Thermoregulated polyoxometalate-based ionic-liquid gel electrolytes[J]. Rsc Advances, 2015, 5(28):21973-21977.
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