制备一系列硅胶(SiO2)负载的磷钨酸铯盐催化剂,将其用于香兰素与1,2-丙二醇的缩合反应,合成香兰素丙二醇缩醛,考察催化剂中Cs^+取代数、磷钨酸铯盐负载量、催化剂用量、1,2-丙二醇与香兰素摩尔比及反应时间对缩合反应的影响.结果表明:磷钨酸铯盐的Cs^+取代数为2.5、负载量为40%时催化剂活性最高;在反应温度368K、n(1,2-丙二醇)/n(香兰素)=2.4、催化剂用量占反应体系质量分数1.5%、带水剂苯的用量30mL、回流反应3h的条件下,香兰素的转化率达到86.6%,香兰素丙二醇缩醛的选择性为100%.
A series of cesium phosphotungstate catalysts supported on silica gel ( SiO2 ) were prepared and used to catalyze the condensation reaction of vanillin with 1,2-propanediol into vanillin propylene glycol acetal. Effects of substituted number of Cs^+ , loading of cesium phosphotungstate, catalyst amount, mole ratio of 1,2-propanediol to vanillin, and reaction time on the reactivity were investigated. Results showed that the catalyst with Cs ^+ substituted number of 2.5, and Cs salt loading of 40% exhibited the highest activity. Under optimal reaction conditions, i. e. , reaction temperature 368 K, mole ratio of 1,2-pro- panediol to vanillin 2.4, catalyst mass fraction in reaction medium 1.5 % , 30 mL benzene as water removal additive, and reaction time 3 h, the conversion of vanillin was 86.6% and the selectivity for vanillin propylene glycol aeetal was 100%.