双子二醇中间体的制备与表征

摘要

In order to obtain high-purity ethylene glycol diglycidyl ether(EGDGE) as spacer,the purification of EGDGE was completed using vacuum distillation to cut fraction.Then the dimer gemini-diol intermedium was synthesized by ring opening reaction.The effects of different conditions on gemini-diol yield were considered.The structures of the spacer EGDGE and gemini-diol were characterized by IR and chromatograph mass spectrometer.The results show that the EGDGE's boiling point is 116-119 ℃ (666.6 Pa) and purity is 94.51％.The optimum reaction conditions are that reaction temperature is 100 ℃,the catalyst is the compound of KOH and phosphorus triphenyl whose mass fraction is 0.25％,and reaction time is 3-5 h.The ultimate yield of gemini-diol is 88.2％.The molecular structure of the sample is the same as that of the designed.%为得到纯度较高的乙二醇二缩水甘油醚作为联接基,利用减压蒸馏切割馏分对其进行提纯,通过开环反应与壬基酚合成一种双子二醇中间体.考虑不同合成条件对双子二醇收率的影响.利用红外光谱和色质联用仪对联接基和双子二醇进行结构表征.结果表明:乙二醇二缩水甘油醚的沸点为116～ 119℃(666.6 Pa),纯度为94.51％；当反应温度100 ℃、催化剂KOH0.25％与三苯基膦0.25％复配、反应时间3～5h时,双子二醇的产率达88.2％；化合物结构与所设计的分子结构相同.