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以磷钨钼杂多酸作催化剂,在超声条件下,以正丁醇和冰醋酸为原料,合成乙酸正丁酯。首先制备了催化剂磷钨钼杂多酸,并对其进行了IR和XRD表征,证明了所制备的磷钨钼杂多酸催化剂具有Keggin的结构。进一步较系统地研究了酯化反应中催化剂焙烧温度、催化剂用量、带水剂种类与用量、醇酸摩尔比、反应时间等对酯化率的影响。结果表明,反应的适宜条件为:在20 kHz,1.0 W/cm2的超声条件下,催化剂焙烧温度为400℃,用量为0.6 g,带水剂为甲苯,用量为10 mL,反应温度为120℃,n(正丁醇)∶n(乙酸)=1.5∶1(乙酸用量为0.4mol),反应时间60 min,酯化率可达99.3%。
With n-butanol and glacial acetic acid as raw materials, n-butyl acetate was synthesized with heteropolyphosphoric-tungstophosphoric acid as catalyst under ultrasonic condition. First, a catalyst of heteropolyphosphoric acid was prepared and characterized by IR and XRD. It was proved that the heteropolyacid catalyst possesses Keggin structure. The effect of catalyst calcination temperature, amount of catalyst, type and amount of water-carrying agent, mole ratio of alkyd and reaction time on the esterification rate was studied systematically. The results showed that the suitable conditions for the reaction were as follows: the calcination temperature was 400 ℃, the dosage was 0.6 g, the water-bearing agent was toluene, the dosage was 10 mL and the reaction temperature was 120 ℃ under ultrasonic wave of 1.0 W / cm2 at 20 kHz , n (n - butanol): n (acetic acid) = 1.5:1 (the amount of acetic acid 0.4mol), the reaction time 60 min, esterification rate of 99.3%.