杯[4]芳烃磺酸催化合成苯甲醛甘油缩醛  

CATALYTIC SYNTHESIS OF BENZALDEHYDE GLYCEROL ACETAL BY ACID CALIX[4]ARENE

作　　者：高良军[1] 杨星[2] 陈平[2] 

机构地区：[1]浙江海洋学院石化与能源工程学院,浙江舟山316000 [2]辽宁石油化工大学化学与材料科学学院,辽宁抚顺113001

出　　处：《精细石油化工》2016年第2期5-10,共6页Speciality Petrochemicals

基　　金：教育部科学技术研究重点项目(No.209031)

摘　　要：以杯[4]芳烃磺酸为催化剂,以甘油和苯甲醛为原料进行缩合反应,得到2-苯基-1,3-二氧六环-5-醇和4-羟甲基-2-苯基-1,3-二氧戊环的混合物。考察了原料配比、催化剂用量、反应时间、油浴温度、带水剂的量及种类对苯甲醛转化率的影响。结果表明,杯[4]芳烃磺酸是合成苯甲醛甘油缩醛的高效催化剂,反应的适宜条件为:n(苯甲醛)∶n(甘油)=1∶1.1,催化剂的质量为反应物总质量的0.1%,15mL甲苯为带水剂(占反应物总质量的1.26%),130℃反应1h,苯甲醛的转化率为98.35%,主产物2-苯基-1,3-二氧六环-5-醇的选择性为73.94%。p-Sulfonic acid Calix[4]arene was used as the catalyst by the condensation of glycerol with benzaldehyde to obtain mixtures of 5-hydroxy-2-phenyl-1,3-dioxan and 4-hydroxymethy-2-phenyl-1,3-dioxolane.Effects of molar ratio of the reactants,catalyst amount,reaction time,oil bath temperature,the volume and kinds of water carrying agent on conversion of benzaldehyde have been optimized.The optimal conditions were as follows：molar ratio of benzaldehyde to glycerol is 1∶1.1,catalyst amount was 0.1% of reactant amount,15 mL toluene was used as water carrying agent（toluene amount was 1.26% of reactant amount）and reacted at 130 ℃ for 1h.The conversion of benzaldehyde is 98.35%,the selectivity of 5-hydroxy-2-phenyl-1,3-dioxan is 73.94%.

关 键 词：磺酸 苯甲醛甘油缩醛 甘油 苯甲醛 

分 类 号：TQ244.1[化学工程—有机化工]