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Bronsted-Lewis双酸性离子液体催化合成对苯二甲酸二(二乙二醇丁醚)酯
引用本文:胡兵,谈继淮,谢冰雪,张海飞,尹佳伟,朱新宝.Bronsted-Lewis双酸性离子液体催化合成对苯二甲酸二(二乙二醇丁醚)酯[J].精细化工,2015,32(8).
作者姓名:胡兵  谈继淮  谢冰雪  张海飞  尹佳伟  朱新宝
作者单位:南京林业大学化学工程学院,江苏 南京 210037,南京林业大学化学工程学院,江苏 南京 210037,南京林业大学化学工程学院,江苏 南京 210037,南京林业大学化学工程学院,江苏 南京 210037,南京林业大学化学工程学院,江苏 南京 210037,南京林业大学化学工程学院,江苏 南京 210037
基金项目:江苏省产学研前瞻性研究项目(NO.BY2014006-03)
摘    要:制备了具有不同SnCl2摩尔分数的Bronsted-Lewis双酸性离子液体3-(1-吡啶基)丙磺酸-氯化亚锡离子液体(3-(1-Py)-(CH2)3-SO3H]Cl-xSnCl2),x为Lewis所占的摩尔分数。用吡啶探针红外光谱作为表征手段,比较了不同x值催化剂的酸性强度变化,并将其应用于对苯二甲酸二(二乙二醇丁醚)酯的合成反应。考察了x值、原料配比、催化剂用量、带水剂用量、反应时间等因素对酯化率的影响,并对精制产品用1HNMR进行结构表征。结果表明,当x=0.5时,该离子液体的催化活性最高。以3-(1-Py)-(CH2)3-SO3H]Cl-0.5SnCl2为催化剂,对苯二甲酸(PTA)和二乙二醇丁醚(DGBE)的摩尔配比n(DGBE):n(PTA)=2.3:1,催化剂用量为4.0%(PTA质量),带水剂正丁醚用量为60.0%(PTA质量),反应时间为2.5h,搅拌转速300r/min时,产品的酯化率高达99.43%。催化剂在不进行任何处理的情况下,可以循环使用5次。 关键词:双酸性离子液体;对苯二甲酸; 二乙二醇丁醚 ;对苯二甲酸二(二乙二醇丁醚)酯;增塑剂

关 键 词:双酸性离子液体  对苯二甲酸    二乙二醇丁醚    对苯二甲酸二(二乙二醇丁醚)酯  增塑剂
收稿时间:4/3/2015 12:00:00 AM
修稿时间:6/1/2015 12:00:00 AM

Synthesis of Di(2-(2-butoxyethoxy)ethanol) Terephthalate by Bronsted-Lewis Acidic Ionic Liquid
HU Bing,TAN Ji-huai,XIE Bing-xue,ZHANG Hai-fei,YIN Jia-wei and ZHU Xin-bao.Synthesis of Di(2-(2-butoxyethoxy)ethanol) Terephthalate by Bronsted-Lewis Acidic Ionic Liquid[J].Fine Chemicals,2015,32(8).
Authors:HU Bing  TAN Ji-huai  XIE Bing-xue  ZHANG Hai-fei  YIN Jia-wei and ZHU Xin-bao
Affiliation:College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China,College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China,College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China,College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China,College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China,College of Chemical Engineering , Nanjing Forestry University , Nanjing 210037 , China
Abstract:Bronsted-Lewis acidic ionic liquids 3-(1-Py)-(CH2)3-SO3H]Cl-xSnCl2 wi-th different mole fractions of SnCl2 was prepared(where x is the mole fractio-ns of the Lewis acid).The acidity of the group was characterized and compare-d to each other by means of FTIR in virtue of pyridine molecular probe,the d-ual acidic ionic liquids were then employed to the synthesis reaction of di(2-(2-butoxyethoxy)ethanol) terephthalate.The influences of catalyst type and amount,ratio of reactants,dosage of water-entrainer,reaction temperature,reaction time we-re investigated .In addition,the target product by 1HNMR .The results show that 3-(1-Py)-(CH2)3-SO3H]Cl-0.5SnCl2 had the highest catalytic activity.With 3-(1-Py)-(CH2)3-SO3H]Cl-0.5SnCl2 as catalyst,the optimal reaction conditions were as follows:n(DGBE):n(PTA)=2.3:1,catalyst (4.0% of mass of PTA),water-entrainer (60.0% of mass of PTA),reaction time (2.5h) and the speed stirring was 300r/min.the esterification rate was 99.43%.Catalyst in the case of without any proc-essing, can be recycled five times.
Keywords:Bronsted-Lewis acidic ionic liquid  2-(2-butoxyethoxy)ethanol  di(2-(2-butoxyethoxy)ethanol) terephthalate  plasticizer
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