Method for extracting plant sterol from fatty acid or methyl ester pitch from distillate
A technology for phytosterols and fatty acids, applied in the field of oleochemical industry, can solve the problems of difficulty in large-scale industrial production, low sterol yield, large solvent loss, etc. Effect
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Embodiment 1
[0016] Example 1: Cottonseed oil fatty acid distillation blackfoot, the sterol content measured by gas chromatography is 11.5%. Weigh 60 grams of the black foot, put it in a saponification tank, add 30 milliliters of water to dilute and stir evenly, add 80 milliliters of 20% sodium hydroxide aqueous solution, saponify at 95 ° C for 16 hours, release alkali precipitation waste water, and then add 100 milliliters of water, After stirring evenly, add 100 ml of 40% calcium chloride aqueous solution, heat up to 70-80° C., react for 3 hours, discharge, wash with water, and dry to obtain 67 grams of dry calcium soap powder. Use 300 milliliters of acetone to boil and extract for 1 hour, let stand, remove the supernatant, repeat the extraction twice, combine the extracts, evaporate the acetone to obtain 7.5 grams of crude sterols, with a purity of 84.2%, and a sterol extraction yield of 91.5 %.
Embodiment 2
[0017] Example 2: Weigh 200 grams of waste oil fatty acid distillation black foot, put it in a saponification tank, add 250 milliliters of 30% sodium hydroxide aqueous solution, heat in an oil bath at 120° C., and saponify for 24 hours. Add 350 ml of 20% calcium chloride solution, react in an oil bath at 100°C for 4 hours, filter, wash with water, and dry in an oven at 105°C for 5 hours to obtain 212 grams of calcium soap. Add 2 liters of acetone, and extract in a boiling water bath under reflux for 2 hours. After removing the acetone solvent from the extracted clear liquid, 9.2 grams of crude sterols are obtained. The content of sterol in the waste oil fatty acid distillation is 4.4%, the purity of crude sterol is 82.7%, and the extraction yield of sterol is 86.5% as measured by gas chromatography.
Embodiment 3
[0018] Example 3: Weigh 98.5 grams of soybean oil deodorization distillate fatty acid methyl ester distilled black foot, put it in a saponification tank, add 150 ml of 30% sodium hydroxide solution, saponify at 95 ° C for 24 hours, add 30% calcium chloride aqueous solution 100 ml, filtered after reacting for 3 hours, washed with water until neutral, and dried in an oven at 105°C until the water content was below 3%, to obtain 94 grams of calcium soap.
[0019] Weigh 20 grams of calcium soap and extract with 100 milliliters of acetone under reflux for 1 hour, repeat the extraction once more, combine the extracts, and evaporate the acetone to obtain 4.9 grams of crude sterols. The content of nigra sterol is 21.7%, the purity of crude sterol is 84.4%, and the extraction yield of sterol is 90.9% as measured by gas chromatography.
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