离子液体催化合成乙二醇丁醚醋酸酯.pdf

第22卷第6期
化学研究
中国科技核心期刊
011年11月
C HEMICAL RESEARCH
hxy@henu.edu.cn
离子液体催化合成乙二醇丁醚醋酸酯
俊江,李春海,马丽群,钱繞
(广'东石油化工学院化学与生命科学系,广东茂名525000
摘要:以乙二醇单了醚和冰醋酸为原料,在离子液体N-甲基叱咯烷酮硫酸氢盐([ Hnmp HSO)催化下,合成
了乙二醇丁醚階酸.考察了催化剂用量、物料配比、反应时间、带水剂等因素对反应收率的影响.利用气相色
谱仪分析了产物的纯度;利用核磁共振谱仪和质谱仪表征了产物的结构.结果表明,合成产物的纯度大于
99.0%,[Hnmp]HSo)4对合成乙二醇丁醚醋酸酯有良好的催化活性;在催化剂用量为反应物料总质量的6%,乙
二醇单丁隣用量为11.8g,乙二醇单丁瞇与冰醋酸的物质的量之比为1:2,回流时间为3h,帯水剂环已烷用量
为15mL的反应条件下,产物收率达94.66;且催化剂重复使用5次仍保持较高活性
关词:N-甲基吡咯煷硫酸盐;离子液体;乙二醇丁讚酸酯;催化合成
中图分类号:TQ633
文献标志码:A
文章编号:1008-1011(2011106-0046-03
Synthesis of 2-butoxyethyl acetate in the presence
of ionic liquid catalyst
TENG Jun-jiang, LI Chun-hai, MA Li-qun, QIAN Jian
Department of Chemistry and Life Science, Guangdon Institute of Petrchemical Tech ology
Abstract: Ethylene glycol monobutyl ether and acetic acid were used as the starting materials to
synthesize 2-butoxyethyl acetate in the presence of ionic liquid 1-methyl 2 pyrrolidinone hydro-
sulfate as a catal yst. The influence of synthetic conditions such as dosage of catalyst, ratio of
acid to alcohol, reaction time and water stripping agent on yield were investigated. The purity
of as-synthesized product was determined by gas chromatographic analysis; and its structure
a characterized by means of nuclear magnetic resonance spectroscopy and mass spectrome
try. Results show that as-synthesized product has a purity of above 99.0%. lonic liquid 1
methyl-2 -pyrrolidinone hydrosulfate exhibits excellent catalytic activity for the synthesis of 2
butoxyethyl acetate. Target product 2-butoxyethyl acetate is obtained at a yield of.6%
when the dosage of catalyst(s. lota] mass of reactants), amount of ethylene glycol monobutyl
ether, molar ratio of ethylene glycol monobutyl ether to acetic acid, refluxing time, and dosage
of cyclohexane are kept as 6%, 11.8 g, 1: 2, 3 h, and 15 ml, respectively. Besides, the cata
rst can bc reused for five times without significant loss in yield
Keywords: I-methyl-2-pyrrolidinone hydrosulfate; ionic liquid; 2-butoxyethyl acetate; catalytic
synthesi
乙二醇丁醚猎酸酯又名丁基溶纤剂醋酸酯,是一种具有多官能团的高沸点溶剂,被广泛用于金属、家具
啧漆和凃刷漆等髙档油漆的溶剂以及造纸上浆涂料的溶剂,此外可用作乳胶漆的助聚结剂,它对多种漆有着
优良的溶解性能,使它在多彩涂料和乳液涂料中获得了广泛的应用12.全球醇醋酸酯较大的生产国是
收稿臼期;
基金项目:茂名市重点科技计项日(10A18)
作者简介:俊江(1979一),男,讲师,博士生,主要从事精细有机合成及工业催化方面的研究,E- mail: tengjunjiang(@sohu,conm