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固体酸催化15-羟基十五烷酸甲酯合成环十五内酯的研究

Study on Synthesis of Cyclopentadecanolide Catalyzed by Solide Acid from Methyl 15-Hydroxypentadecanate

【作者】 赖芳

【导师】 刘雄民;

【作者基本信息】 广西大学 , 林产化学加工工程, 2006, 硕士

【摘要】 环十五内酯是一种重要的大环麝香,它广泛用于香水、香精、化妆品、食品、医药等领域。以蒜头果油为原料,经皂化、酸化及溶剂结晶制得二十四碳-15-烯酸,再经臭氧化—还原、酸化、甲酯化反应生成15-羟基十五烷酸甲酯,在固体酸催化下合成环十五内酯。主要研究内容为: (1) 开展了固体酸催化15-羟基十五烷酸甲酯合成环十五内酯的研究,结果表明NaY、NH4Y、HY型沸石分子筛均能催化15-羟基十五烷酸甲酯转化为环十五内酯,此研究未见相关文献报道。 (2) 实验考察了NH4Y型沸石分子筛的焙烧温度、焙烧时间、颗粒粒度的大小对15-羟基十五烷酸甲酯合成环十五内酯的影响。NH4Y型沸石分子筛颗粒直径小于0.074mm,在550℃焙烧3h后,对15-羟基十五烷酸甲酯的催化效果较好。 (3) 优化了固体酸催化15-羟基十五烷酸甲酯合成环十五内酯的反应条件,在15-羟基十五烷酸甲酯的用量为2.0mmol的条件下,底物浓度为0.07mol·L-1环己烷溶剂用金属钠进行脱水,固体酸HY型沸石分子筛用量为2.0g,在90℃下反应15h时,环十五内酯产率为2.23%。 (4) 对NaY、NH4Y、HY型沸石分子筛进行了阳离子交换和脱铝的改性研究。HY型沸石分子筛经过0.05MNH4Cl溶液90℃进行阳离子交换4次,每次交换1h,再550℃焙烧3h得到的沸石分子筛催化效果较好;HY型沸石分

【Abstract】 Cyclopentadecanolide is an important macrocycle musk. It is widely used in perfume, cosmetic, food, and medical industry. Starting from cis-tetracos-15-enoic acid, obtained from malania oleifera oil through saponification, acidification and solvent crystallization, cyclopentadecanolide was synthesized with catalyzing by solid acid from methyl 15-hydroxypentadecanate, which obtained from cis-tetracos-15-enoic acid through several steps, such as ozonization-reductation, acidification, methyl esterification. The contents were as follows:Cyclopentadecanolide was synthesized from methyl15-hydroxypentadecanate catalyzed by solid acid had been investigated. NaY zeolite, NH4Y zeolite, and HY zeolite all showed obviously capacity to catalyze the reaction, which was unreported.The effect of roasting temperature, roasting time, and grain size of NH4Y zeolite on synthesis of cyclopentadecanolide from methyl 15-hydroxypentadecanate had been studied. The result demonstrated the

  • 【网络出版投稿人】 广西大学
  • 【网络出版年期】2006年 12期
  • 【分类号】TQ225.24
  • 【下载频次】118
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