TGDDM环氧树脂的合成研究

Study on synthesis of TGDDM epoxy resin

以4,4′-二氨基二苯甲烷(DDM)与环氧氯丙烷(ECH)为原料,乙醇为稀释剂进行开环反应,再在碱性条件下进行环化反应,合成TGDDM环氧树脂,并用红外光谱进行表征。结果表明,较优工艺条件为:开环反应温度为60℃,反应时间15 h,n(ECH)∶n(DDM)=4.3∶1,DDM加料温度为50℃,环化反应温度为50℃,反应时间1 h,n(NaOH)∶n(DDM)=4.5∶1,氢氧化钠浓度为30%,此时目标产物TGDDM的收率为94%,环氧值为0.870 mol/100 g,无机氯含量为6.12 mg/kg,易皂化氯含量为114 mg/kg。

TGDDM epoxy resin was synthesized with 4,4′-diaminodiphenylmethane(DDM)and epichlorohydrin(ECH)as raw materials,ethanol as diluent by ring-opening reaction,followed by cyclization under alkaline conditions.The product was characterized by infrared spectroscopy.The results showed that the optimal conditions were as follows:the ring-opening reaction temperature is 60℃,the ring-opening reaction time is 15 h,n(ECH)∶n(DDM)=4.3∶1,the DDM addition temperature is 50℃,the cyclization reaction temperature is 50℃,the cyclization reaction time is 1 h,n(NaOH)∶n(DDM)=4.5∶1,and the concentration of sodium hydroxide is 30%.Under the optimum conditions,the yield of TGDDM is 94%,the epoxy value is 0.870 mol/100 g,the inorganic chlorine content is 6.12 mg/kg,and the easily saponifiable chlorine content is 114 mg/kg.