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Catalytic synthesis of chloroacetates with thermoregulated ionic liquids based on vanadium-substituted polyoxometalate

机译:基于钒取代的多金属氧酸盐的热调节离子液体催化合成氯乙酸盐

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A series of polyoxometalate-based ionic liquid (POM-IL) catalysts with functional sulfonic acid groups, [TEAPS] _(3+ n ) PW _(12? n ) V _( n ) O _(40) ( n = 1, 2, 3) were synthesized and characterized by nuclear magnetic resonance spectroscopy (NMR), Fourier transform infrared spectrophotometry (FT-IR), UV-Vis spectrophotometry (UV), potentiometric titration and thermogravimetry-differential scanning calorimetry (TG-DSC). The catalytic ability and reusability of the POM-IL catalysts were evaluated on esterification of chloroacetic acid and n -amyl alcohol. The optimum reaction conditions, 0.2 g of the catalyst amount, 10 mL of water carrier, 140 °C of reaction temperature, and 1.2/1 of the molar ratio of alcohol/acid, were obtained by an orthogonal test. [TEAPS] _(5) PW _(10) V _(2) O _(40) was found to be the best active catalyst with an esterification rate of 98.75% and could be reused five times without significant decrease in activity. The ionic liquid acted as a temperature-responsive catalyst, forming a homogeneous mixture with the reactants at reaction temperature, and could be precipitated and separated from products when the reaction ends at ambient temperature. Therefore, an environmentally friendly and highly efficient approach for the synthesis of chloroacetates is provided.
机译:一系列具有官能磺酸基团的多金属氧酸盐基离子液体(POM-IL)催化剂,[TEAPS] _(3+ n)PW _(12?n)V _(n)O _(40)(n = 1 (2、3)被合成并通过核磁共振波谱法(NMR),傅立叶变换红外分光光度法(FT-IR),紫外-可见分光光度法(UV),电位滴定和热重-差示扫描量热法(TG-DSC)进行表征。在氯乙酸和正戊醇的酯化反应中评估了POM-IL催化剂的催化能力和可重复使用性。通过正交试验获得最佳反应条件,催化剂量为0.2g,水载体为10mL,反应温度为140℃,醇/酸的摩尔比为1.2 / 1。发现[TEAPS] _(5)PW _(10)V _(2)O _(40)是最佳的活性催化剂,其酯化率为98.75%,可以重复使用五次而活性没有明显降低。离子液体充当温度响应型催化剂,在反应温度下与反应物形成均匀的混合物,并且当反应在环境温度下结束时可能从产物中沉淀并分离出来。因此,提供了一种环保且高效的氯乙酸酯合成方法。

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