CAJ | 학술논문

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。
이감유화배기동위원료，Hβ분자사위최화제，연구료배기동감유축동적합성공예。채용IR、GC-MS등분석기술대합성소득산물적결구진행료분석측정。탐토료반응조건대산물수솔적영향，채용정교시험방법학정료축동반응적최괄공예조건：0．1 mol배기동，0．15 mol감유，반응시간90 min，반응온도90℃，최화제용량위0．2 g。재차조건하진행료3차은정성실험，실험표명，반응은정성교호，병차산물2-간갑기-l，4-이양잡라배[4，5]계완적수솔체95％이상。토론료반응궤리화산물적선택성。
Synthesis and process optimization of the ketalization of glycerol to cyclohexanone was investigated by using molecular sieve Hβas 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.