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研究了一种无催化剂条件下,以低浓度过氧化氢氧化油酸制备反-9,10-二羟基硬脂酸的方法。考察了不同载氧剂、反应时间、物料质量比、过氧化氢的滴加温度、反应温度、分离纯化条件等因素对收率的影响。较佳的工艺条件为:以甲酸为载氧剂,反应时间5 h,m(油酸)∶m(过氧化氢)∶m(甲酸)=8∶7∶5,过氧化氢的滴加温度为30~35℃,反应温度为60~65℃,将混合产物与乙酸乙酯按体积比1∶4进行分离纯化。在该条件下,该工艺顺利完成了500 L反应釜中试。结果显示,反-9,10-二羟基硬脂酸的收率可达92%。用IR及GC-MS对产品结构进行了表征,其质量分数可达95%以上。
A method for preparing trans-9,10-dihydroxystearic acid by oleic acid oxidation at a low concentration of hydrogen peroxide under a catalyst-free condition was studied. The effects of different oxygen carriers, reaction time, material mass ratio, dropping temperature of hydrogen peroxide, reaction temperature, separation and purification conditions on the yield were investigated. The optimum conditions were as follows: formic acid as oxygen carrier, reaction time 5 h, m (oleic acid): m (hydrogen peroxide): m (formic acid) = 8: Is 30-35 DEG C and the reaction temperature is 60-65 DEG C, and the mixed product and the ethyl acetate are separated and purified in a volume ratio of 1: 4. Under this condition, the process successfully completed the 500 L reactor pilot. The results showed that the yield of trans-9,10-dihydroxystearic acid was 92%. The structure of the product was characterized by IR and GC-MS. The mass fraction of the product was more than 95%.