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摘要：对羟基苯甲醚是医药、农药、香料等精细化工产品的重要中间体及原料。目前，国内外都将对羟基苯甲醚合成作为研究热点之一。以对氨基苯甲醚为原料通过重氮化再水解的方法制备的对羟基苯甲醚成本低廉、反应条件温和且产率高，具有良好的发展前景。本文主要研究用对氨基苯甲醚为原料合成对羟基苯甲醚的工艺优化，通过气相色谱法对反应液进行分析，对比分析采用水蒸气蒸馏合成对甲氧基苯酚和甲苯萃取条件下水解反应合成对甲氧基苯酚的反应选择性，并考察了温度、CuSO4浓度和甲苯用量对水解反应的影响。实验结果表明，在 w(对氨基苯甲醚 )：w（水）：w(硫酸，98%)为 1:10:1.25，对氨基苯甲醚硫酸盐配置温度50-55℃，重氮化温度为 25±3℃, 五水硫酸铜浓度40%，水解反应温度为 75±3℃水解反应时加入重氮液等体积甲苯作为萃取剂的最佳工艺条件下，对氨基苯甲醚的产率明显提高， 目标化合物通过GC分析确证。本文对精制过程中，减压蒸馏后的釜底残留液中的主要成分进行分离，并通过用核磁氢谱鉴定其结构。本文有效地提出来一条绿色环保的重氮盐水解方法。本文所用的合成工艺较为新颖，和已经成熟的合成工艺不同，需要通过不断的探索研究来优化，希望能给对羟基苯甲醚合成工艺提供一条新的途径。35048
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毕业论文关键词：对氨基苯甲醚; 对羟基苯甲醚; 重氮盐的水解；工艺改进
An Study on Synthesizing Process of p-Hydroxyanisole
Abstract:p-Hydroxyanisole is a kind of important pharmaceutical intermediates and raw materials,which has important significance in the pharmaceutical industry. Nowadays, the process of methoxyphenol has become an research hotspot at home and abroad . Used P-anisidine as the raw meterials through the way of diazotization and hydrolyzation to process the methoxyphenol,which is low cost, mild reaction conditions and high productivity . This paper studies in the use of optimization for the synthesis of amino anisole hydroxyanisole technology and comparative analysis of synthesis to hydrolysis by steam distillation under -methoxy- phenol and toluene extraction conditions selective synthesis reaction of p-methoxyphenol. Examining the temperature, concentration of CuSO4 and amount of toluene effects on hydrolysis reaction.Optimizing the reaction conditions by multiple parallel experiments and analyzing the isomerization product by gas chromatography.Experimental results show that in W (p-aminoanisole) : W (water), W (sulfuric acid, 98%) for 1:10:1. 25,temperature on the allocation of amino benzene methyl ether sulfate from 50 to 55 ℃,diazotization temperature of 25 ± 3 ℃, blue copper pentahydrate initial concentration of 40% ,hydrolysis Reaction temperature of 75 ± 3 °C,When hydrolitic reaction joins volume toluene and so on diazonium fluid to take the extracting agent the best technological conditions , the amino benzene methyl ether yield increased significantly, the target was confirmed by GC analysis.In this paper, refining process, vacuum distillation after the bottom of the main components of liquid residue were separated, and through the use of NMR to identify its structure.This paper effectively bring up a green diazonium salt water solution method.In this paper, the synthesis process is relatively novel,which is different from some mature synthetic process.This need optimizes through the unceasing exploration research, hoping it can give the hordenine methyl ether synthesis craft to provide a new way.
KeyWords：Para amino benzene ether; Para hydroxy benzene ether; Hydrolysis of heavy nitrogen salt; Technological improvement
目 录
摘要..I
Abstract..II
目录..III
1 前言 1
1.1 对羟基苯甲醚简介 1
1.2 对羟基苯甲醚的性质 1
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