甲醇鈉之製備與其與二氯甲烷之液-固相轉移催化甲氧基取代; The preparation of Sodium Methoxide and the S-L Phase-Transfer Catalyzed Methoxy Substitution of Dichloromethane.

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题名:	甲醇鈉之製備與其與二氯甲烷之液-固相轉移催化甲氧基取代;The preparation of Sodium Methoxide and the S-L Phase-Transfer Catalyzed Methoxy Substitution of Dichloromethane.
作者:	王冠文;Guan-Wun Wang
贡献者:	化學工程與材料工程研究所
关键词:	甲醇鈉;二氯甲烷;甲氧基取代;相轉移催化;Methoxy Substitution;Dichloromethane;Sodium Methoxide;Phase-Transfer Catalyzed
日期:	2009-06-09
上传时间:	2009-09-21 12:31:17 (UTC+8)
出版者:	國立中央大學圖書館
摘要:	本研究在探討甲醇鈉之製備與其及二氯甲烷之液-固相轉移催化甲氧基取代。理論推究兩相中之物理與化學程序，得知溶劑之種類與劑量、相轉移催化劑種類與劑量、攪拌速度以及反應溫度為影響總反應速率及產物分佈的因素，並遂一實驗求得最適反應條件如下：甲醇鈉之製備：在甲醇1.2 mol、氫氧化鈉1 mol、催化劑（BzBu3NCl）劑量為甲醇的10％、氯化鈣0.1 mol、反應溫度50℃及攪拌速度200 rpm等條件下，反應八小時，抽氣過濾後，再以100?150℃蒸出甲醇則可得甲醇鈉固體約20 g（收率約60％）。二甲氧基甲烷之製備有以下兩種方法： I. 在甲醇鈉2 mol、二氯甲烷1 mol、溶劑THF約為0.6 mol、催化劑（BzBu3NCl）劑量為甲醇鈉的10％、反應溫度50℃及攪拌速度200 rpm等條件下於250mL之三頸圓底燒瓶，反應約一天半，可得二甲氧基甲烷產率達90％以上。 II. 在甲醇2.2 mol、氫氧化鈉3.2 mol、二氯甲烷1 mol、溶劑THF約為0.6 mol、催化劑（BzBu3NCl）劑量為甲醇的10％、反應溫度50℃及攪拌速度200rpm等條件下，反應約三小時，可得二甲氧基甲烷產率約85％。 The preparation of sodium methoxide and the phase-transfer catalyzed methoxy substitution of dichloromethane were studied. The physical and chemical processes were considered to derive the overall production rate equation for methylal. The factors (the types and amounts of the solvents, the kinds and amounts of phase-transfer catalysts, the stirring speed and the reaction temperature) affecting the overall reaction rate and the product distributed were studied. The results can be explained with the overall rate equation. Sodium methoxide was prepared as follows: methanol 1.2 mol, sodium hydroxide 1 mol and phase-transfer catalyst (BzBu3NCl) amounts of 10% methanol, reaction temperature 50℃and stirring speed 200 rpm. Reaction time about 8 hours, vacuum-filter and distillation in 100~150℃, we can recycle methanol and obtain pure sodium methoxide solid. The dimethoxymethane was synthesized by method I and method II. Method I: sodium methoxide 2 mol, dichloromethane 1 mol, solvent (THF) 0.6 mol and phase-transfer catalyst (BzBu3NCl) amounts of 10% sodium methoxide, reaction temperature 50℃and stirring speed 200 rpm. Reaction time about 30 hours, we can obtain about 90% dimethoxymethane. Method II: methanol 2.2 mol, sodium hydroxide 3.2 mol, dichloromethane 1 mol, solvent (THF) 0.6 mol and phase-transfer catalyst (BzBu3NCl) amounts of 10% methanol, reaction temperature 50℃and stirring speed 200 rpm. Reaction time about 3 hours, we can obtain about 50% dimethoxymethane.
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