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化学工业与工程 2014, Vol. 31 Issue (5) :31-36    DOI: doi: 10.13353/j.issn.1004.9533.2014.05.006
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乙二醇二缩水甘油醚的合成及表征
张娅,许涌深,邱守季,杨磊
(天津大学化工学院,天津 300072)
Preparation and Characterization of Glycol Diglycidyl Ether
 ZHANG  Ya, XU  Yong-Shen, QIU  Shou-Ji, YANG  Lei
(School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China)

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摘要 以乙二醇和环氧氯丙烷(ECH)为原料,三氟化硼乙醚络合物为催化剂,合成了乙二醇二缩水甘油醚。通过正交试验的实验方法研究了原料配比、催化剂用量、开环反应温度以及闭环反应时间对产物收率和环氧指数的影响,并且用气相色谱、傅里叶红外光谱和核磁氢谱对产物进行了分析和表征。对正交实验的进一步验证和优化表明,乙二醇二缩水甘油醚的最适宜制备条件为:n(ECH)/n(乙二醇)为2.2,催化剂用量为乙二醇质量的0.5%,开环反应温度为50 ℃,闭环反应时间为1 h。最适宜工艺条件下合成产物的各项技术指标均优于工业生产技术指标。
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张娅
许涌深
邱守季
杨磊
关键词乙二醇二缩水甘油醚   合成   表征     
Abstract: Glycol diglycidyl ether was synthesized based on the reaction of ethylene glycol with epichlorohydrin(ECH), using boron trifluoride ether complex as catalyst. The condition of the reaction that affected the epoxy index (EI) and yield of the product, such as the molar ratio of raw material, the amount of catalyst, etherification temperature and the cyclization time were investigated by orthogonal tests. The products were characterized by GC, FTIR spectra and 1H spectra. It has shown by verifying and further optimizing the results of the orthogonal tests that the optimal preparation conditions for glycol diglycidyl ether are 2.2 of the mole ratio between ECH and ethylene glycol, 0.5% of the amount of catalyst (based on the quality of ethylene glycol), 50 ℃ of the etherification temperature and 1 h of the cyclization time. Compared with the traditional process conditions,the reaction time is shorter and the reaction temperature is lower. The result has shown that the technical index of the products is excellent.
Keywordsglycol diglycidyl ether   synthesis   characterization     
Received 2013-03-05;
Corresponding Authors: 许涌深,E-mail:yongshen@tju.edu.cn。     Email: yongshen@tju.edu.cn
About author: 张娅(1987-),女,硕士研究生,现从事精细化工中间体材料和表面活性剂的研究。
引用本文:   
张娅, 许涌深, 邱守季, 杨磊.乙二醇二缩水甘油醚的合成及表征[J].  化学工业与工程, 2014,31(5): 31-36
ZHANG Ya, XU Yong-Shen, QIU Shou-Ji, YANG Lei.Preparation and Characterization of Glycol Diglycidyl Ether[J].  Chemcial Industry and Engineering, 2014,31(5): 31-36
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