Production of multiple unsaturated fatty acid phytosterin ester
A technology of unsaturated fatty acid and phytosterol ester, applied in the field of preparation of food additives, can solve the problems of harsh operating conditions, difficult industrialized production and the like, and achieves the effects of low requirements on reaction conditions, simple process, high content and reaction yield
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Embodiment 1
[0039] Embodiment 1: the preparation of fatty acid methyl ester
[0040] Take 100kg of sunflower oil (in which linoleic acid: 69%, oleic acid: 21%) mixed with 200kg of methanol, heat up to reflux at 70°C, add 50kg of sodium methoxide dropwise, and complete the dropwise addition within 30min. The reaction was maintained at this temperature for 3hr. Use TLC to monitor the degree of completion of the reaction during the reaction. After the reaction is completed, add 300kg of deionized water, leave it to separate after slight stirring, remove the lower hydration layer, and then wash with 300kg of deionized water to neutrality. The washed oil layer was degassed and dried under vacuum conditions to obtain 85.1 kg of fatty acid methyl esters with a conversion rate of 98% and a yield of 95%. The fatty acid composition was analyzed by GC. The specific results are shown in Table 1.
Embodiment 2
[0041] Embodiment 2: the preparation of crude polyunsaturated fatty acid phytosterol ester
[0042] Get 10kg phytosterol (beta-sitosterol: 48.2%, stigmasterol: 25.7%, campesterol: 24.0%, brassicasterol: 1.5%) and the fatty acid methyl ester of 40kg above-mentioned preparations are mixed and be warmed up to 110 ℃, dissolve phytosterol , after heating up, the reactant was vacuum-dried, and the vacuum degree reached -0.09Mpa, and kept for 1hr. After the dehydration was completed, 12 kg of 35% sodium methoxide solution was added dropwise. The mixture was maintained at 130° C. for 3.5 hours under a vacuum of 30 Pa until the reaction was complete. The degree of completion of the reaction could be monitored by TLC. The methanol produced during the reaction could be recovered and concentrated. After the reaction was completed, the temperature of the reaction solution was lowered to 80°C, the vacuum was broken, the catalyst was quenched with 40kg of deionized water, and the reaction s...
Embodiment 3
[0044] Embodiment 3: the refining of polyunsaturated fatty acid phytosterol ester
[0045] Heat 17.0kg of the yellow crude phytosterol fatty acid ester obtained above to melt at 100°C, add 150g of activated clay and 150g of activated carbon, vacuumize and stir for 1.0hr, then filter, then put the filtered product into the reaction kettle, and add After 150g of activated clay, 150g of diatomaceous earth, and 100g of activated carbon, keep a vacuum of -0.08MPa, stir at 110°C for 0.5hr, and obtain 15.8kg of light yellow to white plants with phytosterol esters obtained after filtration through conventional deodorization steps. Sterol fatty acid esters that are free-flowing fluids above 35°C. The content of various sterols and fatty acids can be analyzed by gas chromatography, and the specific results are shown in Table 1.
[0046] Fatty acid and sterol composition analysis in table 1 starting reactant and product
[0047] linseed oil
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