摘要
通过探索温度、加碱方式、碱用量等因素对合成四溴双酚A二缩水甘油醚(DGEBA)的影响,优化出较好的合成条件.较理想的合成条件如下:两步加碱,第一步为催化剂量的碱,先于70℃醚化0.5h,然后升温至100~105℃醚化1.5h;第二步增加碱用量,闭环反应3h.采用FT-IR、^1H—NMR和热分析等对之进行表征.分析结果显示:产品纯度较高,没有未反应的TBBPA,环氧端基的特征吸收峰十分明显;热稳定性较高,热分解温度高于300℃.
The parameters of the polymerization reaction (such as reaction temperature, reaction time, addition way of the alkali, the amount of the alkali used) were investigated to optimize the good synthesis procedure of tetrabromobiphenol-A type diglycidly ether(DGEBA). The optimal synthesis routes of DGEBA was described as follows: the addition of alkali was performed by two steps, the catalysis amount alkali was used in first step, etherification proceeded at 70℃ over a period of 0.5 h at first, then enhanced the temperature to 100t 105 ℃ and continued etherifying for an additional 1.5 h; in the second step, the amount of alkali equivalent to that of TBBPA was charged, the mixture maintained at 100~105 ℃ over a 3h period. The product's characteristics was provided through Fourier transform infrared spectroscopy, proton nuclear magnetic resonance and thermal gravimetric analysis. The product with high purity (containing no TBBPA)exhibited good stability, its thermal decomposition temperature is over 300 ℃.
出处
《河南大学学报(自然科学版)》
CAS
北大核心
2006年第1期44-49,共6页
Journal of Henan University:Natural Science
基金
河南省科技厅普通攻关项目(0424270119)
河南省教育厅自然基金资助(2000150026)
关键词
缩水甘油醚
四溴双酚A
环氧氯丙烷
反应性阻燃剂
Diglycidyl ether
Tetrabromobiphenol A
Eipchlorohydrin
Reactive flame retardant