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對羥基苯甲醚合成工藝研究

時間:2019-04-30 22:23來源:畢業論文
對氨基苯甲醚硫酸鹽配置溫度50-55℃,重氮化溫度為 25±3℃, 五水硫酸銅濃度40%,水解反應溫度為 75±3℃水解反應時加入重氮液等體積甲苯作為萃取劑的最佳工藝條件下,對氨基苯甲醚的

摘要:對羥基苯甲醚是醫藥、農藥、香料等精細化工產品的重要中間體及原料。目前,國內外都將對羥基苯甲醚合成作為研究熱點之一。以對氨基苯甲醚為原料通過重氮化再水解的方法制備的對羥基苯甲醚成本低廉、反應條件溫和且產率高,具有良好的發展前景。本文主要研究用對氨基苯甲醚為原料合成對羥基苯甲醚的工藝優化,通過氣相色譜法對反應液進行分析,對比分析采用水蒸氣蒸餾合成對甲氧基苯酚和甲苯萃取條件下水解反應合成對甲氧基苯酚的反應選擇性,并考察了溫度、CuSO4濃度和甲苯用量對水解反應的影響。實驗結果表明,在 w(對氨基苯甲醚 ):w(水):w(硫酸,98%)為 1:10:1.25,對氨基苯甲醚硫酸鹽配置溫度50-55℃,重氮化溫度為 25±3℃, 五水硫酸銅濃度40%,水解反應溫度為 75±3℃水解反應時加入重氮液等體積甲苯作為萃取劑的最佳工藝條件下,對氨基苯甲醚的產率明顯提高, 目標化合物通過GC分析確證。本文對精制過程中,減壓蒸餾后的釜底殘留液中的主要成分進行分離,并通過用核磁氫譜鑒定其結構。本文有效地提出來一條綠色環保的重氮鹽水解方法。本文所用的合成工藝較為新穎,和已經成熟的合成工藝不同,需要通過不斷的探索研究來優化,希望能給對羥基苯甲醚合成工藝提供一條新的途徑。35048
畢業論文關鍵詞:對氨基苯甲醚; 對羥基苯甲醚; 重氮鹽的水解;工藝改進
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.

源¥自%六:維;論-文'網=www.aftnzs.live


KeyWords:Para amino benzene ether; Para hydroxy benzene ether; Hydrolysis of heavy nitrogen salt; Technological improvement
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1 前言    1
1.1 對羥基苯甲醚簡介    1
1.2 對羥基苯甲醚的性質    1 對羥基苯甲醚合成工藝研究:http://www.aftnzs.live/huaxue/20190430/32828.html
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