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摘要：邻甲氧基苯酚作为一种重要的化工原料,已经非常广泛地利用在医药、香料合成等工业生产中。目前工业上主要是以邻氨基苯甲醚为原料合成邻羟基苯甲醚，对它的色谱分析方法有很多，常用气相色谱分析,测定方法快速、简单、方便。气相色谱分析一般采用柱前衍生法,衍生试剂有醋酐、三氟醋酐、四甲基硅醚等。气相色谱分析法法虽然操作方便，但对高含量的样品分析准确度不高，而液相色谱分析“四高”的特点决定了液相色谱更为合适。由于内标法中进样量的变化和色谱条件的微小变化对结果影响不大。本论文采用对甲苯酚为内标物，采用高效液相色谱内标法分析，用甲醇水体系作流动相，V(甲醇)/V(质量分数为0.5%的乙酸水溶液)=50：50流速0.8mL/min；紫外检测波长为280nm；柱温为25℃,检测邻羟基苯甲醚取得了较为满意的结果。20998
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毕业论文关键词：高效液相色谱法；气相色谱法；内标法；邻羟基苯甲醚；对甲苯酚
Synthesis and Quality Control of
2-Methoxyphenol
Abstract：Guaiacol (o-methoxyphenol) is an important chemical raw material, in medicine, it is widely used in synthesis of perfume. Industry was the main o-anisidine as raw material for the synthesis of guaiacol, the method with o-anisidine as raw material, the diazo reaction with sodium nitrite in acidic aqueous solution at low temperature,, generated diazonium salt drip into the hydrolysate (boiling in acid aqueous solution containing copper sulfate catalyst hydrolysis of crude phenol), with water steam steaming by solvent extraction, distillation from guaiacol purity greater than 99%. Chromatographic analysis of it there are a lot of methods, analysis of commonly used gas chromatography method for the determination of simple, fast, convenient, and much of this literature. Gas chromatography using pre column derivatization with acetic anhydride, derivatization reagent, three fluorine acetic anhydride, four trimethylsilyl ether etc.. But more troublesome, need strict anhydrous conditions of acetic anhydride. Three fluorine acetic anhydride activity is high, but the price is more expensive.The samples with relatively high content of gas chromatographic method for the analysis of accuracy is not high, and the characteristics of liquid chromatography, high speed, high efficiency is high, high sensitivity and high content by HPLC is appropriate. Method for analysis of selection of internal standard method is best, because the internal standard method is little effect on the change of sample volume change and the chromatographic conditions on the results. Using hydroquinone as internal standard substance, using high performance liquid chromatography internal standard method for the determination of guaiacol and achieved satisfactory results.
KeyWords：High performance liquid chromatography;gas chromatography； internal standard method; salicylic ether; hydroquinone
目 录
摘要 Ⅰ
Abstract Ⅱ
目录 Ⅲ
1 绪论 1
1.1 课题背景 1
1.2 课题的内容和意义 1
2 文献综述 2
2.1 邻羟基苯甲醚简介 2
2.2 邻羟基苯甲醚的文献合成方法 2
2.3 基本反应机理 2
2.4 气相色谱法简介 3
2.5 高效液相色谱法简介 4
3 邻羟基苯甲醚的合成工艺研究 6
3.1 本文所选的合成路线 6
3.2 实验所需试剂及仪器 6
3.3 实验过程 7
3.3.1 邻甲羟基苯重氮盐的制备 7
3.3.2 邻甲羟基苯重氮盐的水解 7
3.4实验结果 7
4 邻羟基苯甲醚的质量控制 10
4.1 邻羟基苯甲醚的气相色谱分析 10
4.1.1 实验部分 12
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