反-9,10-二羟基硬脂酸的合成

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。

Synthesis of trans-9,10-Dihydroxystearic Acid

Trans-9,10-Dihydroxystearic acid was synthesized with oleic acid as the raw material and hydrogen peroxide as the oxidant without catalyst.The effects of factors such as different oxygen carrier,reaction time,ratio of raw materials,the temperature of trickling hydrogen peroxide,reaction temperature and crystallization condition on the yield were discussed.The results showed that formic acid was a oxygen carrier,reaction time was 5 h,m(oleic acid)∶m(hydrogen peroxide)∶m(formic acid)=8∶7∶5,the temperature of trickling hydrogen peroxide was between 30～35 ℃,and reaction temperature was between 60～65 ℃.Under the optimal conditions,500 L reactor pilot test was successfully carried out.The yield reached 92% and the mass percent of product was over 95%.The structure of product was characterized by IR and GC-MS.