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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%.
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