环己酮乙二醇缩酮的催化合成研究  

Study of catalytic synthesis of cyclohexanone ethylene ketal

作　　者：邓斌[1,2] 陈劲翔[3] 张晓军[2] 徐安武[2] 

机构地区：[1]湘南学院化学与生命科学系,湖南郴州423000 [2]中国科技大学合肥微尺度物质科学国家实验室,安徽合肥230026 [3]中国矿业大学化学与环境工程学院,北京100083

出　　处：《日用化学工业》2010年第2期104-107,143,共5页China Surfactant Detergent & Cosmetics

基　　金：国家自然科学基金资助项目(20971118);湖南省自然科学基金资助项目(07JJ3017);湖南省教育厅重点资助科研项目(08A065)

摘　　要：采用沉淀-浸渍法制备了固体超强酸S2O82-/SnO2-SiO2催化剂,用于以环己酮和乙二醇为原料制备合成香料环己酮乙二醇缩酮的反应中。探讨了催化剂对缩酮反应的催化活性,较系统地考察了带水剂种类及用量、醇酮摩尔比、催化剂用量、反应时间对产品收率的影响,并用正交试验对反应条件进行了优化。实验结果表明,固体超强酸S2O82-/SnO2-SiO2是合成环己酮乙二醇缩酮的良好催化剂,在n(乙二醇)∶n(环己酮)=1.6∶1(0.32 mol∶0.2 mol),催化剂用量为反应物总质量的1.0%,带水剂环己烷用量8.0 mL,反应1.5 h的条件下,环己酮乙二醇缩酮收率可达97.2%。固体超强酸S2O82-/SnO2-SiO2催化剂的稳定性良好,在重复使用6次后环己酮乙二醇缩酮收率为90.1%;经傅里叶变换红外光谱和气相色谱-质谱分析表明,产物为环己酮乙二醇缩酮,纯度达99%以上。Aroma compound cyclohexanone ethylene ketal was synthesized from cyclohexanone and glycol as starting material with S2O8^2-/SnO2 -SiO2 solid super- acid as catalyst. The catalyst was prepared by precipitation -impregnation method. Factors that affect product yield were investigated. Orthogonal designed experiment was used to optimize reaction conditions. Experimental results showed that S2O8^2-/SnO2 -SiO2 solid super - acid was an excellent catalyst. With conditions of n （ glycol ） ： n （ cyclohexanone ） = 1.6 ： 1.0 （0. 32 mol： 0. 2 mol） ;catalyst dosage of 1.0% （w） of the total reactants;8.0 mL of cyclohexane as water - stripping agent and reaction time 1.5 h; the yield of cyclohexanone ethylene ketal could achieve 97.2%. Stabhity and repeatability of the S2O8^2-/SNO2 - SiO2 catalyst were examined. The yield of cyclohexanone ethylene ketal kept at 90. 1% after being re - used for six times. The product was characterized by means of FTIR and GC - MS. Purity of the product achieves higher than 99%.

关 键 词：环己酮乙二醇缩酮 固体超强酸 催化合成 

分 类 号：TQ234.2[化学工程—有机化工] TQ655