PDF (1236K)
摘要
研究了二聚酸二缩水甘油酯及其改性胺环氧固化剂的制备工艺,制得具有增韧作用的环氧树脂固化剂。采用羧酸-环氧氯丙烷(ECH)酯化、闭环二步法合成二聚酸二缩水甘油酯,其最佳合成工艺条件为:催化剂为四丁基溴化铵且用量为二聚酸(DA)质量的2%,酯化反应温度为90℃,DA:ECH(摩尔比,下同)=1:10,环化反应温度为55℃,NaOH质量分数为30%,DA:NaOH=1:4。将制得的缩水甘油酯与异佛尔酮二胺进行胺化反应得到改性胺固化剂,其与环氧树脂618固化产物的冲击强度为29.6kJ/m2,体现出优异的增韧效果。
Abstract
The preparation process of dimer acid diglycidyl ester and its modified amine epoxy curing agent was investigated,and the epoxy resin curing agent with toughening effect was prepared.Dimer acid diglycidyl ester was prepared by using two-step synthesis of carboxylic acid-epichlorohydrin esterification and dehydrohalogenation.The optimum synthesis conditions were as follows:tetrabutylammonium bromide was used as catalyst and its amount was 2% of DA weight.The esterification reaction temperature was 90℃,DA:ECH(molar ratio)=1:10,the cyclization reaction temperature was 55℃.the concentration of sodium hydroxide(NaOH) was 30% (weight),DA:NaOH(molar ratio)=1:4.The obtained glycidyl ester and isophorone diamine were subjected to amination reaction to obtain modified amine curing agent.The impact strength of product cured by epoxy resin 618 and the modified amine curing agent was 29.6kJ/m2,which showed that the curing agent had excellent toughening effect.
关键词
缩水甘油酯
/
改性胺固化剂
/
环氧树脂
/
增韧
Key words
glycidyl ester
/
modified amine curing agent
/
epoxy resin
/
toughening
二聚酸二缩水甘油酯及其改性胺环氧固化剂的制备[J].
化工新型材料, 2019, 47(1): 177-180 DOI:
[1] 朱思巧,梁兵,王长松,等.含磷阻燃环氧树脂固化剂研究进展[J].化工新型材料,2016,44(8):17-19.
[2] 肖艳.环氧树脂分类、应用领域及市场前景[J].化学工业,2014,32(9):19-24.
[3] 李娟,郭杰,刘青.环氧树脂固化剂研究新进展[J].化工新型材料,2017,45(3):31-33.
[4] 陈燕青,周孜,朱新宝.第十九次全国环氧树脂应用技术学术交流会暨学会华南地区分会第一届学术交流会论文集[C].广州:第十九次全国环氧树脂应用技术学术交流会暨学会华南地区分会第一届学术交流会,2016.
[5] 唐一林,江成真,朱红军.一种二聚酸缩水甘油酯的合成方法:中国,103570918A[P].2014-02-12.
[6] 聂小安,王定选.C36二聚酸二缩水甘油酯型环氧树脂的合成[J].热固性树脂,1997,12(3):11-16.
[7] 余磊,刘安昌.对苯二甲酸二缩水甘油酯的合成[J].广东化工,2009,36(6):26-28,252.
基金资助
上海市教育基金(LM201713);上海应用技术大学绿色涂料协同创新平台建设资助(3921NH166015)
