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摘要缩水甘油醚在工业上广泛用于环氧树脂的稀释剂。目前缩水甘油醚的生产工艺主要采用二步法，所得产品的有机氯含量较高，难以达到电子等应用领域的要求，因此，低氯和无氯法合成缩水甘油醚的绿色合成工艺研究越来越受到关注。本文在调研文献的基础上，分别采用H2O2和mCPBA为氧化剂，探索环氧化烯丙基醚合成缩水甘油醚的绿色方法。找到了一种能够有效催化H2O2环氧化的催化剂，即经过NaOH改性的TS-1分子筛，合成苄基缩水甘油醚和正丁基缩水甘油醚的产率分别达到48.78%和25.45%，但是采用该方法合成双酚A二缩水甘油醚较为困难。对mCPBA环氧化合成缩水甘油醚的方法进行了探索并采用正交实验法对工艺条件进行优化，该方法能够顺利合成苄基缩水甘油醚和正丁基缩水甘油醚，但是对双酚A二烯丙基醚的环氧化主要得到单边环氧化产物。另外，本文还通过制备负载型固体碱NaOH-TiO2，并用该固体碱替代传统方法使用的NaOH溶液来探索合成双酚A二缩水甘油醚DGEBA的绿色工艺，并通过设计正交试验对实验条件进行优化，但是，该方法得到的DGEBA产品纯度较低，品质不好，工艺条件有待进一步探索。21681
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关键词 缩水甘油醚，H2O2，mCPBA，固体碱
毕业论文设计说明书（论文）外文摘要
Title A study on the green synthetic technology of glycidyl ether
Abstract
Glycidyl ether has been widely used as epoxy resins diluent in industry . Currently glycidyl ether has been mainly produced by two-step process, the resulting product’s organochlorine value is generally high , which is difficult to meet the requirements of the electronics industry and other fields , so increasing attention has been concentrated on the green synthesis study of low chlorine and no chlorine synthesis of glycidyl ether . In this paper , based on the research of literatures, H2O2 and mCPBA were used as oxidant to explore the green synthesis of glycidyl ether . TS-1 zeolite modified by NaOH was found to be a new effective catalyst in epoxidation of allyl ether with H2O2 ,resultantly benzyl glycidyl ether and n-butyl glycidyl ether were obtained with their yield 48.78% and 25.45% respectively , but this method for the synthesis of bisphenol A diglycidyl ether was difficult. Epoxidation synthesis method with mCPBA was explored using orthogonal experimental to optimize conditions for the process, benzyl glycidyl ether and n-butyl glycidyl ether were successfully synthesized, but as for bisphenol A diallyl ether, epoxidized product was mainly mono glycidyl ether of bisphenol A. In addition, solid base NaOH-TiO2 was prepared to replace NaOH solution in traditional method to explore the green synthesis of DGEBA , and the conditions for the process were optimized through orthogonal experimental. However, the purity and epoxy value of DGEBA obtained by this method was poor, the process conditions were expected to be explored further.
Keywords glycidyl ether, H2O2, mCPBA, solid base
目次
1 绪论 1
1.1 缩水甘油醚简介 1
1.2 缩水甘油醚的生产方法 2
1.2.1 一步法 2
1.2.2 二步法 2
1.2.3 固碱法 3
1.2.4 氧化法 3
1.2.5 其他方法 4
1.3 烯烃环氧化方法简介 4
1.3.1 以H2O2为氧化剂 5
1.3.2 以过氧酸为氧化剂 7
1.4 过氧化氢加合物简介 7