近临界水中薯蓣皂苷水解生成薯蓣皂苷元的工艺研究

Technology of Diosgenin Production by Dioscin Hydrolysis in Subcritical Water

薯蓣皂苷元是合成甾体激素类药物和甾体避孕药的重要中间体,传统工艺采用盐酸水解法将黄姜中的薯蓣皂苷水解生成薯蓣皂苷元,反应时间4h,最大收率为1.78%。该工艺反应时间长,耗水量大,对环境污染严重。今研究了无催化剂条件下,近临界水中薯蓣皂苷水解成薯蓣皂苷元的工艺,分别考察了反应温度、反应压力、反应时间等因素对薯蓣皂苷元收率的影响。研究结果表明,近临界水解法工艺简单,反应时间短,对环境友好,在较佳工艺条件下:P=25.0MPa,T=260℃,t=10min,薯蓣皂苷元收率为1.46%。

Diosgenin is one of the very important chemical intermediates for synthesis of steroid hormone medicine and steroid contraceptive. The traditional technology of diosgenin production is using hydrochloric acid to hydrolyze dioscin, the hydrolysis time needed is 4 h and the maximum diosgenin yield is 1.78%. The long reaction time, large amount of water consumption and heavy environmental pollution are the main shortcomings of the traditional technology. In this paper, the proposed diosgenin production process of conducting dioscin hydrolysis in subcritical water without catalyst was studied. The effects of hydrolysis temperature, pressure and time on the yield of diosgenin were investigated. The experimental results show that the proposed process has the adventages of simple technology, shorter reaction time and being friendly to environment. The suitable hydrolysis conditions found are as follows： reaction pressure 25.0 MPa, temperature 260℃ and reaction time 10 min. Under above conditions, the yield of diosgenin is 1.46%