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采用平行反应器,以苯甲醛、氯仿为原料,以氢氧化钠为碱剂,十六烷基三甲基溴化铵(CTMAB)和β-环糊精(β-CD)复合催化剂为相转移催化剂合成了扁桃酸.通过测熔点和IR分析对产物进行了表征.采用单因素实验法研究了相转移催化剂种类、反应物的摩尔配比、反应时间、反应温度、催化剂用量等对产物产率的影响.在单因素实验的基础上,根据Box-Benhnken设计原理,设计三因素三水平响应面分析法,建立二次多项式回归方程的预测模型,获得最佳工艺参数:反应温度80℃,反应时间2.16 h,催化剂用量7.54%(CTMAB占5.37%,β-CD占2.17%),摩尔比n(苯甲醛)n(氯仿)=1 1.38.在此条件下通过曲面响应法预测的扁桃酸的理论产率为63.16%,实际测得扁桃酸的产率均值为63.00%,与理论预测值基本相符.
Using parallel reactors, benzaldehyde and chloroform as raw materials, and sodium cetyltrimethylammonium bromide (CTMAB) and β-cyclodextrin (β-CD) as phase transfer agent Catalyst was used to synthesize mandelic acid.The product was characterized by measuring the melting point and IR.The single factor experiment was used to study the effects of the type of phase transfer catalyst, molar ratio of reactants, reaction time, reaction temperature, catalyst dosage, Based on the single-factor experiment, the three-factor three-level response surface analysis method was designed according to the Box-Benhnken design principle, and the prediction model of the quadratic polynomial regression equation was established to obtain the optimum process parameters: reaction temperature 80 ℃, reaction The time of 2.16 h, the amount of catalyst 7.54% (CTMAB accounted for 5.37%, β-CD accounted for 2.17%), the molar ratio of n (benzaldehyde) n (chloroform) = 1 1.38 under this condition predicted by the curved surface of mandelic acid The theoretical yield was 63.16%. The mean yield of mandelic acid actually measured was 63.00%, basically in line with the theoretical predictions.