基于桐油的环氧沥青增容剂的合成与表征

Synthesis and Characterization of Epoxy Asphalt Compatibilizer Based on Tung Oil

以桐油和环氧树脂为原料,通过皂化、酯化和环氧化三步反应制备了环氧沥青增容剂。研究了反应温度、反应时间、催化剂用量和反应物投料比等对各步反应的影响。结果表明:当皂化温度为70℃,回流时间为2 h,桐油与氢氧化钠的摩尔比为1∶3.6时,桐油反应转化率为76.3%;当反应温度为100℃,反应时间为5 h,环氧树脂与桐油酸的摩尔比为1∶2,环氧树脂与甲苯的质量比为1∶2时,四正丁基溴化铵用量为反应物质量的2.5%时,酯化产物具有较低的环氧值0.544 mol/100 g;环氧化反应的最优工艺条件为:反应温度60℃,反应时间45 min,双氧水与甲酸、桐油酸酯树脂的摩尔比为3∶1∶1,硫酸的用量为桐油酸酯质量分数的1.5%。通过傅立叶变换红外光谱分析并确认了各步目标产物的结构。

Epoxy asphalt compatibilizer was prepared with tung oil and epoxy resin as precursors by three steps of saponification, esterification and epoxidation reactions. The effects of reaction temperature, reaction time, catalyst dosage and reactant feed ratio on each reaction were investigated. The results show that the conversion rate of tung oil was 76.3%, in mole ratio of tung oil to sodium hydroxide 1 ： 3.6, at 70 ℃ for 2 h. The esterified product has a lower epoxy value of 0.544 mol/100g at 100 ℃ for 5 h, in the molar ratio of epoxy resin to eleostearic acid 1 ： 2, the mass ratio of epoxy resin to toluene 1 ： 2, the amount of catalyst of 2.5% of the mass of reactants. The optimal conditions for the epoxidation process are found in molar ratio of hydrogen peroxide to formic acid and tung oleate resin 3 ： 1 ： 1, at 60 ℃for 45 rain, the concentrated sulfuric acid of 1.5% of the mass of tung oleate resin. The structures of the compounds were confirmed by Fourier transform infrared spectroscopy.