【摘要】 研究了以苯甲酰氯和间苯二酚为原料、液碱为除酸剂,酯化合成然后精制得间苯二酚单苯甲酸酯的工艺.研究了酯化反应中温度、物料配比、pH、间苯二酚水溶液的浓度和反应时间等条件对反应的影响,获得了较佳的酯化工艺条件:苯甲酰氯与间苯二酚的摩尔比为1.15∶1;pH值为7.5;反应温度为25℃;反应时间为1.5 h;间苯二酚溶液的质量分数为10%.酯化反应收率为88.6%.考察了结晶溶剂配比、温度对产品质量和收率的影响,经实验评估得到了较佳的结晶工艺条件:结晶溶剂甲苯的体积(/mL)与初产物的质量(/g)之比为2.5∶1,结晶温度为30℃,结晶收率为95.0%.优化工艺条件下产品的总收率为84.2%.更多还原

【Abstract】 A new process for preparation of resorcinol monobenzoate starting from benzoyl chloride and resorcinol by esterification,extraction and crystallization was studied. The influence of temperature,pH,reaction time,resorcinol solution concentration and molar ratio of reactants on the yield of esterification was investigated. The optimum reaction conditions were evaluated and selected as follows: the molar ratio of benzoyl chloride to resorcinol was 1. 15 ∶ 1,the pH value was 7. 5,reaction temperature was 25 ℃,reaction time was1. 5 h,resorcinol solution concentration was 10%,under the optimum condition the yield of esters was about88. 6%. The dosage of crystallization solvent and the temperature of crystallization were experimented also.The results of the experiments showed that the temperature of crystallization was 30 ℃. The ratio of solvent and reaction product was 2. 5 ∶ 1. The yield of esterification product was about 95. 0%. The total yield was84. 2%.更多还原