二苯甲酰甲烷制备工艺的优化

Optimization of the preparation process of dibenzoylmethane

本文选用Claisen缩合反应以甲氧基钠催化苯乙酮与苯甲酸酯反应制备二苯甲酰甲烷(DBM).对反应物的用量及添加方式的探讨,确定了一种产率优良的制备工艺,在该工艺条件下讨论了苯甲酸酯添加比例对产物收率的影响.相比于已有工艺,本实验的方案在较低的反应物添加比例下取得了更高的收率.将反应放大10倍,收率稳定.此外,本实验简化了副产NaCl的回收提纯工艺,整体工艺无废水产生,有效解决了废固NaCl的回收再用问题.

In this paper,the Claisen condensation reaction is used to prepare dibenzoylmethane(DBM)by reacting acetophenone and benzoate with sodium methoxide.The amount of reactant and the way of adding were discussed.A kind of preparation process with good yield was deter-mined.Under the condition of this process,the influence of the proportion of benzoate adding on the yield of the product was discussed.Compared with the existing process,the experimental scheme achieved a higher yield at a lower ratio of reactants.The reaction was magnified 10 times and the yield was stable.In addition,this experiment simplifies the recovery and purification process of by-product NaCl,the whole process has no waste water,and effectively solves the problem of recovery and reuse of waste solid NaCl.