连续流反应器中油酸无溶剂合成9,10- 二羟基硬脂酸Synthesis of 9,10-dihydroxystearic acid from oleic acid in a continuous flow reactor without solvent
2023
张铭远,邓林江,陈治家,钮腾飞 ZHANG Mingyuan，DENG Linjiang，CHEN Zhijia，NIU Tengfei
为改善现有9,10-二羟基硬脂酸合成存在的反应不连续、反应时间过长等问题,以油酸为原料，过氧化氢为氧化剂，在连续流反应器中合成9,10-二羟基硬脂酸，对催化剂进行了筛选，并对合成工艺条件进行单因素实验优化。结果表明，9，10-二羟基硬脂酸，合成的最佳工艺条件为以磷钨酸为催化剂、不使用溶剂、30%过氧化氢与油酸物质的量比3∶ 1、反应温度60 ℃、催化剂用量10%（以油酸质量计）、反应时间23.6 min，在此条件下油酸转化率为91.2%，9,10-二羟基硬脂酸选择性为82.6%。该方法解决了传统间歇釜式反应器中制备9,10-二羟基硬脂酸时反应时间长、工艺烦琐等问题，且绿色环保。In order to improve the existing problems in the synthesis of 9,10-dihydroxystearic acid of discontinuous reaction and long reaction time, 9,10-dihydroxystearic acid was synthesized in a continuous flow reactor with oleic acid as the starting material, hydrogen peroxide as the oxidant.After screening catalyst, the synthesis process conditions were optimized by single factor experiment.The results showed that the optimal conditions for the synthesis of 9,10-dihydroxystearic acid were obtained as follows: with phosphotungstic acid as the catalyst, molar ratio of 30% H2O2 to oleic acid 3∶ 1, reaction temperature 60 ℃, catalyst dosage 10% of oleic acid mass, reaction time 23.6 min, and no solvent. Under these conditions, the conversion rate of oleic acid and the selectivity of 9,10-dihydroxystearic acid were 912% and 82.6%, respectively. By utilizing this system, the difficulties associated with the production of 9,10-dihydroxystearic acid in the conventional batch reactor, such as long reaction time and complex processes, were resolved. Additionally, this system is environmentally benign and green.
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