环氧脱水蓖麻油的制备工艺研究
Synthesis Process of Epoxidized Dehydrated Castor Oil
-
摘要: 以蓖麻油(CTO)为原料,先制备脱水蓖麻油(DCO),再以磷酸为催化剂,过氧乙酸为氧化剂,进行环氧化反应制备环氧脱水蓖麻油(EDCO),通过单因素和正交试验优化不同条件对产品环氧值的影响。结果表明,制备EDCO较佳工艺条件为反应温度30 ℃、反应时间3.5 h、DCO与过氧乙酸物质的量之比5.5:1、磷酸用量0.5%,此条件下所得EDCO的环氧值达到4.82%。采用FT-IR和 1H NMR 表征了蓖麻油、脱水蓖麻油以及环氧脱水蓖麻油的化学结构,结果证实EDCO中C=C被环氧化后基本消失,生成了环氧键。通过黏度测定、热重分析(TG)等方法对产品的性能进行了分析,得到CTO黏度为1100.0 mPa·s,DCO黏度为299.5 mPa·s,EDCO黏度为1896.0 mPa·s;产品的热稳定性顺序为EDCO> DCO> CTO。Abstract: Dehydrated castor oil(DCO) was firstly prepared by using castor oil(CTO) as raw material via dehydration reaction, and epoxidized dehydrated castor oil(EDCO) was synthesized using phosphoric acid as catalyst and acetic acid peroxide as the oxidant by epoxidation reaction afterwards. The influences of different parameters on the epoxy value of EDCO were investigated through single factor and orthogonal experiments. The results indicated that the optimal preparation conditions of EDCO were 3.5 h reaction time, 30 ℃ reaction temperature, 5.5:1 molar ratio of peracetic acid to DCO and 0.5% phosphoric acid dosage. The epoxy value of EDCO could be up to 4.82% under these conditions. In addition, the chemical structures of CTO, DCO, and EDCO were characterized by FT-IR and 1H NMR . It was confirmed that the C=C double bonds in EDCO almost disappeared and the epoxy bonds were formed during the epoxidation. The properties of the products were also studied by viscosity measurement and thermogravimetric analysis(TG). Viscosity measurement showed that the viscosities of CTO, DCO, and EDCO were 1100.0, 299.5 and 1896.0 mPa·s, respectively. TG analysis demonstrated that the descending order of thermal stability of the products was EDCO> DCO> CTO.