摘要:δ-十一内酯为酯类香料,具有内酯类香料的一些共有的特点,同时也有其独特的地方,具有强烈的果香香气,桃子和杏仁样香韵,是最常用的内酯香料之一。常用于紫丁香、桂花、茉莉等日用香精的调配。也常用于桃子、牛奶、奶油、黄油等食用香精的调配。本论文以2-正己基环戊酮为初始原料,经过Baeyer-villiger氧化反应制备了δ-十一内酯,筛选了反应所需的氧化剂和碱,并详细研究了反应物摩尔配比、反应时间等条件对制备δ-十一内酯的影响,当反应物(2-正己基环戊酮):氧化剂(间氯过氧苯甲酸):碱(碳酸氢钠粉末)的摩尔比为1:1:3,室温搅拌8h时,最终产物δ-十一内酯的得率是99.164%。δ-十一内酯的结构经核磁共振氢谱、质谱和红外光谱的确证,具有强烈的奶油样脂肪气息,桃子样香韵等香气特征。该优化的工艺条件对进一步研究内酯类香料化合物的制备具有一定的理论参考价值,对δ-十一内酯的中试和工业化生产也可提供实际应用价值。62230
毕业论文关键字:香精调配,δ-十一内酯;内酯香料化合物;Baeyer-Viliger氧化反应
Study on Preparation of Undecanolactone
Abstract:Undecanolactone as a member of the lactone perfume, it also has some common features of the lactone perfume, it also has its unique place, with strong fruity aroma, peach and almond like incense rhyme, is one of the most commonly used lactone perfume. Commonly used in lilac, osmanthus, jasmine and other fragrances blending. Is also commonly used in peaches, milk, cream, butter and other edible flavor blending. This thesis with 2-hexyl cyclopentanone as the raw material, by using Baeyer-Villiger oxidation reaction to prepared undecanolactone, Then selecting the required oxidant and alkali of the reaction, and a detailed study on the reactant molar ratio, reaction time of preparing Undecanolactone.When the molar ratio of the reactant (2-hexyl cyclopentanone):oxidant (metachloroperbenzoic acid):thealkali (sodium bicarbonate powder) is 1:1:3,stirring at room temperature for 8h, the final product of undecanolactone yield is 99.164%.structure of undecanolactone was confirmed by nuclear magnetic resonance hydrogen spectrum, mass spectrometry and infrared spectroscopy,it has strong butter-like fat flavor, peach like aroma ect aroma characteristics. The optimized process conditions for further study on compounds of lactones aroma with certain theory reference value, pilot and industrial production of undecanolactone can also provide practical application value.
KeyWords:Flavour blending;Undecanolactone;Compound of lactones perfume;Baeyer-Viliger oxidation reaction
目 录
1 前言 1
1.1.1 香料概述 1
1.1.2 香料现状 1
1.1.3 内酯类香料化合物的简介 1
1.1.4 关于本课题的研究现状 2
1.2本课题主要研究的内容 4
1.3 本课题研究的目的及意义 4
2 实验方法和实验内容 5
2.1 反应机理 5
2.2 实验内容 6
2.2.1 δ-十一内酯 6
2.2.2 实验所用材料试剂 6
2.2.3 实验所用仪器 7
2.2.5 反应条件的确立 8
2.2.6 柱层析过程