环氧脱水蓖麻油的制备工艺研究  

Synthesis Process of Epoxidized Dehydrated Castor Oil

作　　者：黄旭娟 刘鹤[1,2,3,4] 商士斌[1,2,3,4,5] 齐帆[1,2,3,4] 

机构地区：[1]中国林业科学研究院林产化学工业研究所 [2]生物质化学利用国家工程实验室 [3]国家林业局林产化学工程重点开放性实验室 [4]江苏省生物质能源与材料重点实验室,江苏南京210042 [5]中国林业科学研究院林业新技术研究所,北京1000912

出　　处：《林产化学与工业》2015年第4期41-47,共7页Chemistry and Industry of Forest Products

基　　金：国家自然科学基金资助项目(31200446);江苏省自然科学基金资助项目(BK2012063);中国林科院林业新技术所基本科研业务费专项资金(CAFINT2012C05)

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1 100.0 mP a·s,DCO黏度为299.5 mP a·s,EDCO黏度为1 896.0 mP a·s;产品的热稳定性顺序为EDCO>DCO>CTO。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 UF-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 1 100.0, 299.5 and 1 896.0 mPa·s, respectively. TG analysis demonstrated that the descending order of thermal stability of the products was EDCO 〉 DCO 〉 CTO.

关 键 词：过氧乙酸 环氧化 环氧脱水蓖麻油 

分 类 号：TQ35[化学工程] TQ645