蓖麻油缩水甘油醚合成工艺研究

摘要

Using castor oil and epoxy chloropropane( ECH) as the main raw materials under the alkali condition, a novel castor oil glycidyl ether ( COGE) was synthesized through two steps, namely open loop and closed loop reaction. The effects of process conditions on epoxy values were investigated. The results showed that the highest epoxy value the product achieved was 1. 56 mmol/g under the condition that the open loop reaction was set at 0. 4% catalyst dosage,3. 5 molar ratio of ECH and castor oil, and reaction temperature at 60 ℃ for 5 h, and as well as the close-loop reaction was set 0. 4% catalyst dosage, 1. 1 molar ratio of NaOH and ECH, and reaction temperature at 60 ℃ for 6 h. The chemical structure of the castor oil glycidyl ether was characterized by FT-IR and 1H NMR. TGA analysis showed that castor oil glycidyl ether had good thermal stability at high temperature. Viscosity test showed that the product could reduce the viscosity of epoxy resin.%以蓖麻油、环氧氯丙烷( ECH)和液碱为主要原料,经二步法开环闭环反应合成了蓖麻油缩水甘油醚( COGE),研究了开环、闭环工艺条件对产物环氧值的影响。结果表明,开环催化剂三氟化硼-二乙基醚用量0.4%,ECH与蓖麻油的物质的量比3.5∶1,反应温度60℃,反应时间5 h；闭环催化剂四甲基氯化铵用量0.4%,反应时间6 h,反应温度60℃,NaOH与ECH物质的量比1.1∶1时产物环氧值最高为1.56 mmol/g。采用红外光谱(FT-IR)、核磁共振氢谱(1H NMR)表征了合成产物的化学结构,热失重(TG)分析表明蓖麻油缩水甘油醚具有优良的高温热稳定性,黏度测试表明该产物可以降低环氧树脂的黏度,加入量15%时,黏度降低46%。