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%.
A kind of processing approach of removing Stigmasterol Sigma from soybean oil deodorization distillate, specifically comprises the steps:
1) Ultrasonic saponification response: According to the weight quantity proportion of 1:19, the deodorised extract of soybean oil, the n-butanol option with a focus of 85%, as well as the alkaline service combined with KOH and NaOH analytically pure in an amount accounting for 25% of the whole remedy quantity After securing, ultrasonically blend at a power of 250W, a frequency of 50Hz, as well as a temperature of 45 ° C for 35 mins, and then represent saponification as well as precipitation at a temperature level of 75 ° C for 4 hrs to acquire a saponification mixture A;
2) Separation and also removal: Centrifuge the saponification combination A at a speed of 3500r/min while it is hot, and vacuum cleaner filter, cool down the filtrate in a natural state, and afterwards return the filtrate to the cyclic ultrasonic saponification response procedure for cyclic extraction;
3) Purification by recrystallization: Add 3 times of n-butanol with a focus of 85% to the suction filtrate, and also after the power is 250W, the regularity is 50Hz, and also the temperature level is 50 ° C, after ultrasonic dissolution for 30min, include 0.8 g of bit size to the blend. It is 10μm stigmasterol fine powder, mixed as well as mixed evenly at the speed of 200r/min, then promptly moved to the temperature level of 25 ° C, stirred at the speed of 100r/min, cooled and crystallized, vacuum cleaner filteringed system, and after that repeated the recrystallization purification step 3 The 2nd time, vacuum-dry as well as grind the obtained suction filtrate at a temperature level of 25 ° C to acquire Stigmasterol Sigma; the suction filtrate n-butanol can be reused.
