摘要
以酸化的凹凸棒石黏土为载体,用浸渍法制备了凹凸棒石负载磷钨酸催化剂,并采用XRD、IR和紫外可见分光光度法等手段对催化剂进行了表征。将此用做合成苹果酯的催化剂,考察了反应物的摩尔比、催化剂用量、带水剂用量、反应时间和反应温度等各种因素对苹果酯收率的影响。实验结果表明,凹凸棒石负载磷钨酸催化剂催化活性良好,结构稳定且能够重复使用,并得到较佳工艺条件:n(乙酰乙酸乙酯)∶n(乙二醇)=1.0∶1.5,催化剂用量为2 g,带水剂苯为50 mL,110℃下反应180 min,苹果酯收率可达89.7%。
Using acid -treated attapulgite clay as supporter, attapulgite clay supported phosphotungstic acid catalyst were prepared through impregnation method, and characterized by XRD, IR and UV spectrophotometry. Such catalyst was used for synthesis of fructone. Effects of molar ratio of ethyl acetoacetate to glycol, the dosage of catalyst, the dosage of water stripping agent, the reaction time, the reaction temperature on the esterification yield were investigated. The experimental results showed that attapulgite clay supported phosphotungstic acid catalyst has good catalytic activity, structural stability, and can be reused. Optimum conditions for the synthesis are : molar ratio of ethyl acetoacetate to glycol is 1.0:1.5 ; the dosage of catalyst is 2 g; the amount of benzene as water stripping agent is 50 mL; the reaction time is 3 h; the reaction temperature is 110 ℃. Its yield achieves higher than 89.7%.
出处
《日用化学工业》
CAS
CSCD
北大核心
2008年第6期386-389,412,共5页
China Surfactant Detergent & Cosmetics
关键词
香料
苹果酯
磷钨酸
凹凸棒石
乙酰乙酸乙酯
乙二醇
fragrance
fructone
phosphotungstic acid
attapulgite
ethyl acetoacetate
glycol