环氧亚麻油增塑剂的优化合成与表征

Optimized Synthesis and Characterization of Epoxidized Linseed Oil Plasticizer

在磷酸催化下,甲酸和双氧水生成过氧甲酸,再以过氧甲酸作为环氧化剂,对亚麻油进行环氧化反应。利用正交试验优化反应条件,研究了原料亚麻油的级别和加料方式对环氧化反应的影响。结果表明:影响亚麻油环氧化反应的因素主次顺序为磷酸用量>双氧水用量>甲酸用量>反应温度,最佳反应条件为m亚麻油∶m磷酸∶m双氧水∶m甲酸=1∶0.01∶1.55∶0.29。采用滴加磷酸、双氧水及甲酸三者混合物的加料方式,加料温度为65℃,反应温度为68℃,反应时间为3 h,产物环氧值达8.10%。红外光谱分析表明,亚麻油经环氧化反应成功地合成了环氧亚麻油,热重/差热分析证明,制备的环氧亚麻油具有较好的热稳定性。

Epoxidation of linseed oil with peroxyformic acid generated by the reaction of formic acid and hydrogen peroxide in the presence of phosphoric acid as the catalyst was studied, and the optimized reaction conditions were also obtained by the application of orthogonal experimental method. Impacts of raw linseed oil level and feeding methods on the epoxidation of linseed oil were also investigated in this paper. The results showed that factors affecting the epoxidation of linseed oil were in the order of the amount of phosphoric acidhydrogen peroxideformic acidreaction temperature. The epoxy value of the final product could reach 8.10% under the following optimized conditions： mlinseed oil：mphosphoric acid：mhydrogen peroxide：mformic acid=1∶0.01∶1.55∶0.29, using the feeding method of dropping the mixture of phosphoric acid/hydrogen peroxide/formic acid to the reactor under 65 ℃, reaction temperature was 68 ℃ and time was 3 h. FTIR analysis showed the successfully synthesized of epoxidized linseed oil by the epoxidation reaction and thermogravimetric analysis/differential thermal analysis（TG/DTA）proved good thermal stability of the epoxidized linseed oil obtained.