以二苯甲酮（BP）和水合肼为原料合成二苯甲酮腙（BPH），探讨了催化剂种类、催化剂用量、原料配比、溶剂种类等因素对产物收率及色泽的影响，并对产物进行 IR 和 HPLC 表征和成本核算。结果表明：常规低沸点溶剂更合适，高沸点溶剂会使副产物增多，影响产品质量；离子液体作催化剂能大大缩短反应时间；最佳合成条件为：离子液体催化剂用量为 BP 质量的2％、n（水合肼）∶n（BP）＝2.8∶1、无水乙醇为溶剂、反应时间3 h、温度控制在回流状态下。从工业成本角度考虑，最佳合成条件为：冰乙酸催化剂用量为 BP 质量的2％、n（水合肼）∶n（BP）＝2.8∶1、无水甲醇为溶剂、反应时间9 h、温度控制在回流状态下。%Using benzopnenone and hydrazine hydrate as raw materials,benzophenone hydrazone was syn-thesized.The effects of type and dosage of catalyst,molar ratio of raw materials,type of solvent on the yield and color of the product were studied.The product was characterized by IR and HPLC.The cost was calculated as well.Results showed that,the conventional low-boiling point solvent was more suitable,the introduction of high-boiling point solvent would increase the amount of byproducts.And ionic liquid catalyst could greatly shorten reaction time.The optimum synthetic conditions were as follows:the amount of ionic liquid catalyst was 2%,the molar ratio of hydrazine hydrate to BP was 2.8∶1,solvent was absolute ethanol and reaction time was 3 h,the reaction temperature was refluxing temperature.The more economical and energy efficient synthetic conditions were as follows:the amount of acetic acid catalyst was 2%,the molar ratio of acetic acid to BP was 2.8∶1,solvent was absolute methanol and reaction time was 9 h,the reaction temperature was refluxing tem-perature.
展开▼
