2,4,6-三甲基酚觸媒氧化反應之研究

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Title:	2,4,6-三甲基酚觸媒氧化反應之研究
Authors:	劉邦毅
Contributors:	李國禎 Kuo-Tseng Li 東海大學化學工程與材料工程學系
Keywords:	2;4;6-三甲基酚;氧化反應
Date:	2000
Issue Date:	2011-07-26T03:45:10Z (UTC)
Abstract:	本論文目的在於篩選適當之觸媒以將2,4,6-三甲基酚選擇性氧化成3,5-二甲基-4-羥基苯甲醛，並且選擇較佳之觸媒以探討各種反應條件，包括：反應溫度、添加劑種類及濃度、氧氣壓力、溶劑種類、觸媒及反應物濃度等的改變，對反應物之轉化率和產物之產率及選擇率的影響，此外亦探討此選擇性氧化反應之反應動力學。實驗結果顯示，除了文獻上已揭示過的銅觸媒外，本研究發現鐵之氯化物及溴化物觸媒亦具有不錯的選擇性氧化反應之催化性能。對於銅觸媒，50℃~70℃的反應溫度是較佳的操作條件；對於鐵觸媒，70℃~90℃則能夠得到較好的反應結果。反應中加入某些適當的添加劑能明顯加快反應速率，對於CuCl觸媒而言，加入neocupr、DMF、acetone oxime的添加物，能得到不錯的效果；對於FeCl2觸媒而言，加入acetone oxime可明顯增加反應速率。增加反應壓力對反應速率有明顯的增進，但對產率則沒有太大的影響。使用不同的醇當溶劑，發現醇的直鏈愈長，愈不利於此一氧化反應。觸媒和反應物濃度的影響，在2,4,6-TMP /觸媒之莫耳比= 1 / 0.05時，是一最佳操作條件。在動力學方面，FeCl2觸媒之2,4,6-三甲基酚選擇性氧化反應為一次反應，其活化能為E1 = 65.1 KJ/mole，E2 = 33.2 KJ/mole。 This thesis study catalysts used for the selective oxidation of 2,4,6-trimethylphenol to 3,5-dimethyl-4-hydroxybenzaldehyde by molecular oxygen in a batch reactor。A variety of reaction conditions were investigated including reaction temperature、 additives types and their concentration、oxygen pressure、solvent、catalyst and reactant concentration，to study their influence on the conversion、yield and selectively。 In addition to the copper catalysts revealed in the literature，we found that iron chloride and iron bromine catalyst are also good catalysts。For copper catalysts，the temperature range of 50~70℃ exhibited better reaction results；For iron catalysts，70~90℃ had better results。The addition of some suitable additives significantly increased reaction rate。For CuCl catalyst，the addition of neocupr、DMF、acetone oxime had good effect。For FeCl2 catalyst，the addition of acetone oxime had not only increased reaction rate dramatically，but also improved yield at higher temperature。 The increase of reaction pressure increased the reaction rate，but did not affect yield。It was found that the reaction results deteriorated with the use of longer chain alcohol as solvent。 As to the effect of catalyst and reactant concentration，the 2,4,6-TMP/ catalyst molar ratio to 1 / 0.05 exhibited the best reaction results。 The results of kinetics study showed that the selective oxidation of 2,4,6-TMP was first order reaction and the activation energies were E1 = 65.1 KJ/mole，E2 = 33.2 KJ/mole。
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