Hβ分子筛催化合成环己酮甘油缩酮及工艺优化  

Synthesis and Process Optimization of Ketalization of Glycerol to Cyclohexanone Using Molecular Sieve Hβ as Catalysts

作　　者：陆禹吉 王成章[2,3] 高勤卫[1] 叶建中[2,3] 陶冉[2,3] 

机构地区：[1]南京林业大学化学工程学院,江苏南京210037 [2]中国林业科学研究院林产化学工业研究所,国家林业局林产化学工程重点开放性实验室 [3]江苏省生物质能源与材料重点实验室,江苏南京210042

出　　处：《生物质化学工程》2014年第4期7-12,共6页Biomass Chemical Engineering

基　　金：国际合作与交流项目(S2012GR0138)

摘　　要：以甘油和环己酮为原料,Hβ分子筛为催化剂,研究了环己酮甘油缩酮的合成工艺。采用IR、GC-MS等分析技术对合成所得产物的结构进行了分析测定。探讨了反应条件对产物收率的影响,采用正交试验方法确定了缩酮反应的最适工艺条件:0.1 mol环己酮,0.15 mol甘油,反应时间90 min,反应温度90℃,催化剂用量为0.2 g。在此条件下进行了3次稳定性实验,实验表明,反应稳定性较好,并且产物2-羟甲基-l,4-二氧杂螺环[4,5]癸烷的收率达95%以上。讨论了反应机理和产物的选择性。Synthesis and process optimization of the ketalization of glycerol to cyclohexanone was investigated by using molecular sieve Hβ as catalysts. The structure of the product was identified by IR and GC-MS spectrum. Influence of reaction condition on the yield of the product was examined. The optimum synthesis conditions were determined based on the orthogonal test results as follows： amount of cyclohexanone was 0. 1 mol,amount of glycerol was 0. 15 mol,reaction time was 90 min,reaction temperature was 90 ℃,and amount of catalysts was 0. 2 g. Three experiments were carried out under these conditions. A good stability was obtained. The yield of the product 2-methylol-1,4-dioxaspiro[4,5]decane could reach more than 95%. Reaction mechanism and selective of product were discussed.

关 键 词：环己酮 甘油 HΒ分子筛 缩酮反应 正交试验 机理 

分 类 号：O643.32[理学—物理化学]