N′,N-二-(2-羟乙基)-草酰胺的制备方法研究
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摘要
以甲醇为溶剂,草酸二乙酯与单乙醇胺为原料制备了N′,N-二-(2-羟乙基)-草酰胺,并对其进行红外光谱分析。研究溶剂用量、反应物配比、反应温度与保温时间对N′,N-二-(2-羟乙基)-草酰胺产率的影响。结果表明:最佳工艺条件为甲醇作溶剂,甲醇与草酸二乙酯质量比=5∶1,反应物摩尔比n(草酸二乙酯)∶n(单乙醇胺)=1∶2.3,反应温度为70℃,保温时间1.5h,此时N′,N-二-(2-羟乙基)-草酰胺产率达到97.1%。
N′,N-bis(2-hydroxyethyl)oxamide was prepared from diethyl oxalate and monoethanolamine in the presence of methanol as solvent.The structure of product was characterized by FT-IR.The effects of solvent amount,reaction temperature and holding time,reactant ratio on the yield were discussed.The results showed that optimum conditions for reaction were obtained:methanol as solvent,mass ratio of methanol to diethyl oxalate=5∶1;molar ratio of diethyl oxalate to monoethanolamine=1∶2.3;reaction temperature=70℃,holding time 1.5 h.The yield was 97.1%.
N′,N-bis(2-hydroxyethyl)oxamide was prepared from diethyl oxalate and monoethanolamine in the presence of methanol as solvent.The structure of product was characterized by FT-IR.The effects of solvent amount,reaction temperature and holding time,reactant ratio on the yield were discussed.The results showed that optimum conditions for reaction were obtained:methanol as solvent,mass ratio of methanol to diethyl oxalate=5∶1;molar ratio of diethyl oxalate to monoethanolamine=1∶2.3;reaction temperature=70℃,holding time 1.5 h.The yield was 97.1%.
引文
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[2]Zarzyka I,Naróg D,Stagraczyński R.Polyurethane foams with the contribution of products of hydroxyalkylation of N,N′-bis(2-hydroxyalkyl)oxamides with alkylene carbonates-obtaining and properties[J].Journal of Applied Polymer Science,2012,124(1):755-764.
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[4]刘生鹏,童身毅.2,2′-双(2-唑啉)的合成[J].精细石油化工进展,2001,2(12):12-14.
[5]钱震宇,郭宝华,史建中,等.双恶唑啉扩链尼龙1010[J].高分子学报,2004(4):506-510.
[6]Dong W,Zou B,Ma P,et al.Influence of phthalic anhydride and bioxazoline on the mechanical and morphological properties of biodegradable poly(lactic acid)/poly[(butylene adipate)-co-terephthalate]blends[J].Polymer International,2013,62(62):1783-1790.
[7]陈玉君,何国山,陈仕国,等.双唑啉化合物增容PET/PA66共混体系的研究[J].塑料工业,2002,30(5):13-15.
[8]钱震宇,郭宝华,徐军,等.尼龙1010扩链反应的动力学模型和分析[J].高分子学报,2004(4):511-517.
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[10]De Beukeleer S H J,Desseyn H O,Perlepes P S.Synthesis,spectroscopy and thermal analysis of nickel(Ⅱ),palladium(Ⅱ)and copper(Ⅱ)complexes with N,N′-bis(2-hydroxyethyl)-oxamide[J].Transition Metal Chemistry,1994,19(5):542-547.
[11]王玉环,刘书志.N′,N-二-(2-羟乙基)-乙二酰胺的合成工艺研究[J].河北化工,2009,32(11):21-23.
[12]王顶.PET的反应挤出扩链及扩链剂的合成研究[D].大连:大连理工大学,2005.