1. Icing up splitting up
Liquify 200kg of phytosterol oleate (the content of stigmasterol is 15.58%) in 1000L ethyl acetate, mix at 65 ° C up until the phytosterol oleate is totally dissolved, after that move it to a freezer as well as freeze it at -20 ° C Freeze for 8 hrs. The clear liquid obtained by cold splitting up went through vacuum purification to recoup ethyl acetate to acquire 32.71 kg of crude product of Stigmasterol Sigma oleate.
2. Saponification response
Add 300 L of 5% NaOH ethanol solution with a mass portion of 5% to the unrefined item of Stigmasterol Sigma oleate obtained in step 1, and also accomplish saponification reaction at 80 ° C., as well as the response time is 4 hours.
3. Solid-liquid splitting up
After the saponification reaction, include 300L NaCl saturated aqueous service to the saponification fluid, and also wait until sodium oleate is totally sped up from the saponification liquid, and make use of a tympanic filter press to divide the saponification product at 6kPa to acquire a stigmasterol ethanol remedy. After that the gotten Stigmasterol Sigma ethanol option went through vacuum purification to recuperate ethanol to get 32.52 kg of Stigmasterol Sigma crude item with a pureness of 62.25%.
4. Crystallization and also purification
Include the crude stigmasterol to 200L n-butanol, mix at 55 ° C till the crude stigmasterol is entirely dissolved, then lower the temperature level to 25 ° C at a cooling price of 4 ° C/hour, stir at 15 rpm, and maintain growing crystals at a consistent temperature level for 12 hrs, adopt drum membrane filter press to accomplish solid-liquid splitting up under 6kPa, get stigmasterol filter cake 31.87 kg, the pureness of Stigmasterol Sigma is 73.22%. The filtrate is distilled to recover n-butanol as well as sterol, and the solvent is recycled.
5. Recrystallization and purification
Step 4 was duplicated as soon as, and the resulting filter cake was vacuum-dried at 60 ° C. to obtain a stigmasterol product with a purity of 98.26%, and a return of 90.32%.