Method for preparing high-purity stigmasterol from phytosterol oleate
A technology of phytosterol oleate and stigmasterol oleate, which is applied in the direction of steroids and organic chemistry, can solve the problems of many times of crystallization and complicated process, and achieve simple operation steps, full utilization and less times of crystallization Effect
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Embodiment 1
[0024] 1. Freezing separation
[0025] Dissolve 200kg of phytosterol oleate (the content of stigmasterol is 15.58%) in 1000L ethyl acetate, stir at 65°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer and freeze it at -20°C Freeze for 8 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 32.71 kg of crude stigmasterol oleate.
[0026] 2. Saponification reaction
[0027] Add 300 L of 5% NaOH ethanol solution with a mass fraction of 300 L to the crude stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C., and the reaction time is 4 hours.
[0028] 3. Solid-liquid separation
[0029] After the saponification reaction, add 300L NaCl saturated aqueous solution to the saponification liquid, and wait until sodium oleate is completely precipitated from the saponification liquid, and use a tympanic filter press to separate the saponificati...
Embodiment 2
[0035] 1. Freezing separation
[0036] Dissolve 100g of phytosterol oleate (the content of stigmasterol is 15.58%) in 400mL of ethyl acetate, stir and dissolve at 65°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer, and store it at -20 Freeze and separate at ℃ for 10 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 18.57 g of crude stigmasterol oleate.
[0037] 2. Saponification reaction
[0038] Add 185 mL of 5% NaOH ethanol solution to the crude product of stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C., and the reaction time is 3 hours.
[0039] 3. Solid-liquid separation
[0040] After the saponification reaction, add 185mL NaCl saturated aqueous solution to the saponification solution, and wait until sodium oleate is completely precipitated from the saponification solution, use a tympanic filter press to separate th...
Embodiment 3
[0046] 1. Freezing separation
[0047] Dissolve 100g of phytosterol oleate (the content of stigmasterol is 15.58%) in 800mL of ethyl acetate, stir at 60°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer, and freeze it at -20°C Freeze for 5 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 19.38 g of crude stigmasterol oleate.
[0048] 2. Saponification reaction
[0049] Add 95 mL of 8% NaOH ethanol solution with a mass fraction of 8% to the crude stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C. for 5 hours.
[0050] 3. Solid-liquid separation
[0051] After the saponification reaction, add 190mL NaCl saturated aqueous solution to the saponification solution, and wait until sodium oleate is completely precipitated from the saponification solution, use a tympanic filter press to separate the saponification product at 6kPa to ...
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