节点文献
1,1,2,2-四对羟基苯基乙烷四缩水甘油醚环氧树脂的合成
Synthesis of 1,1,2,2-Tetrakis(Hydroxyphenyl) Ethane Tetraglycidyl Ether Epoxy Resin
【摘要】 将1,1,2,2-四对羟基苯基乙烷与环氧氯丙烷在醚化催化剂四乙基溴化铵和溶剂异丙醇存在下,先进行醚化反应,然后加入适量的NaOH进行环氧化脱氯反应,再经水洗、分离、精制,得到1,1,2,2-四对羟基苯基乙烷四缩水甘油醚环氧树脂(PGEE)。研究了原料配比、反应时间和温度对PGEE环氧值和可水解氯含量的影响。实验结果表明,当环氧氯丙烷与1,1,2,2-四对羟基苯基乙烷摩尔比为21、1,1,2,2-四对羟基苯基乙烷与NaOH摩尔比为1∶4.0、醚化温度85℃、醚化时间4h、环氧化温度70℃、环氧化时间2.5h时,所得PGEE环氧值为0.51m ol,可水解氯质量分数为1.92×10-4,收率为57.5%。经傅里叶变换红外光谱和核磁共振表征,初步确认合成的产品为PGEE。
【Abstract】 1,1,2,2-tetrakis(hydroxyphenyl) ethane tetraglycidyl ether epoxy resin(PGEE) was synthesized from 1,1,2,2-ttrakis(hydroxyphenyl) ethane and epichlorohydrin with tetraethylammonium bromide as etherification catalyst,sodium hydroxide as epoxidation catalyst and isopropanol as solvent.The raw PGEE resin was then treated in following water washing,vacuum disillation and recrystallization to obtain pure PGEE.Effects of reactant ratio,reaction time and temperature on hydrolysable chlorine content and epoxy value of synthesized PGEE were investigated.Under appropriate conditions: mole ratio of 1,1,2,2-tetrakis(hydroxyphenyl) ethane to epichlorohydrin 21,mole ratio of 1,1,2,2-tetrakis(hydroxyphenyl) ethane to sodium hydroxide 1 ∶4.0,etherification temperature 85 ℃,etherification time 4 h,epoxidation temperature 70 ℃ and epoxidation time 2.5 h,the epoxy value and yield of PGEE,and mass fraction of hydrolysable chlorine in it are 0.51 mol,57.5% and 1.92×10-4,respectively.Structure of the synthesized PGEE was preliminary identified by means of FTIR,1H NMR and 13C NMR.
- 【文献出处】 石油化工 ,Petrochemical Technology , 编辑部邮箱 ,2007年05期
- 【分类号】TQ323.5
- 【被引频次】8
- 【下载频次】367