超声波辅助活性炭负载杂多酸盐催化合成尼泊金丁酯

CATALYTIC SYNTHESIS OF BUTYL PARABEN WITH ACTIVATED CARBON SUPPORTED HETEMPOLY COMPOUND BY ULTRASONIC ASSISTED METHOD

以对羟基苯甲酸和正丁醇为原料,活性炭负载Keggin型杂多酸盐[(CH_2)_5NH_2]_4SiMo_(12)O_(40)为催化剂,在超声波辐射下合成尼泊金丁酯。考察了催化剂用量、原料配比、超声波辐射功率及辐射时间对尼泊金丁酯收率的影响。结果表明:超声波辐射下活性炭负载Keggin型杂多酸盐[(CH_2)_5NH_2]_4SiMo_(12)O_(40)具有良好的催化活性。较佳工艺条件为:对羟基苯甲酸4.14 g(0.03 mo1),酸醇摩尔比1.0:2.0,环己烷40 mL,催化剂7g,450 W超声波辐射20 min。尼泊金丁酯收率达到97%以上。

The butyl paraben was synthesized with p-hydroxy benzoic acid and n-butanol by ultrasonic assisted method, with activated carbon supported keggin-structured hetempoly compound, [-（CH2）5NH2]4SiMo12040, as catalysts. Effects of catalyst dosage, molar ratios of the reactants, ul-trasonic wave power and radiation time were investigated. The results showed that the catalytic activi-ty is good under ultrasonic and the optimal conditions were determined as follows： p-hydroxy benzoic 4.14 g （0.03 mol）, mole ratio of p-hydroxy benzoic acid to n-butanol 1.0 ： 2.0, cyclohexane 40 mL, catalyst 7 g as well as radiation time 20 min with the ultrasonic wave power of 450 W. Under these conditions, the yield of butyl paraben was up to 97%.