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公开(公告)号：KR1019940002715B1
公开(公告)日：1994-03-31
申请号：KR1019910020481
申请日：1991-11-18
Applicant: 한국과학기술연구원
IPC: C07D311/72
Abstract: The tocopherol is separated and purifyed by (a) adding organic solvent of n-hexane, n-heptane, acetone or methylethylketone into the soybean oil distillate and removing the crystallized sterol of the mixture by filtering, (b) methylesterifying the obtained fatty acid by reflux at 60-80 deg.C with 35 % HCl catalyst, (c) dissolving in lower alcohol, adsorbing it into alkaline anion exchange resin and purifying with lower alcohol contg. acetic acid, formic acid, oxalic acid or succinic acid, (d) recirculating the esterifyed product in a molecular distillator to obtain the final product.
Abstract translation: 通过（a）将正己烷，正庚烷，丙酮或甲基乙基酮的有机溶剂加入大豆油馏出物中并通过过滤除去混合物的结晶固醇，分离出生育酚，（b）将所得脂肪酸甲酯化为 用35％HCl催化剂在60-80℃回流，（c）溶解在低级醇中，吸附到碱性阴离子交换树脂中，用低级醇进行纯化。 乙酸，甲酸，草酸或琥珀酸，（d）将酯化产物在分子蒸馏器中再循环以获得最终产物。
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公开(公告)号：KR1019930010024A
公开(公告)日：1993-06-21
申请号：KR1019910020481
申请日：1991-11-18
Applicant: 한국과학기술연구원
IPC: C07D311/72
Abstract: 본 발명은 대두유 탈취 부산물로부터 천연토코페롤을 분리, 정제함에 있어서, 대두유 탈취부산물을 지용성 유기용매로 용해시키고, 물, 알코올 또는 물을 함유한 알코올을 첨가하여 스테롤 혼합물을 제거하고, 얻어진 잔류지방산을 메틸 에스테르화 시킨다음, 이를 유극성 유기용매에 용해하여 염기성 음이온교환수지에 유입시켜서 산성유기용매로 용출하는 것을 특징으로 하는 대두유 탈취 부산물로부터 고순도의 천연 토코페롤을 고수율로 분리, 정제하는 방법이다.
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Patent Agency Ranking
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公开(公告)号：KR1019920005695B1
公开(公告)日：1992-07-13
申请号：KR1019900012985
申请日：1990-08-22
Applicant: 한국과학기술연구원
IPC: C11B7/00
Abstract: A process for separating and concentrating sterol and tocopherol from deodorized distillate of soybean oil comprises (A) adding mixed solvent of n-hexane and 50 % (V/V) methanol to soybean oil distillate, (B) cooling the mixture to 5 deg.C -10 deg.C to separate sterol first, (C) methyl esterifying the mixture from which sterol is removed, (D) recirculating esterified product in a molecular distiller at 100-130 deg.C and 10-2 - 10-4 torr to remove fatty acid methyl ester, and (D) recirculating again it at 170-200 deg.C and 10-2 - 10-4 torr to separate and concentrate tocopherol. The mixing ratio of n-hexane to methanol is 10:1, and addition amount of mixed solvent is 2 or 3 times the amount of soybean oil distillate.
Abstract translation: 从大豆油的除臭馏分中分离和浓缩固醇和生育酚的方法包括（A）向大豆油馏出物中加入正己烷和50％（V / V）甲醇的混合溶剂，（B）将混合物冷却至5℃。 （C）甲基酯化除去固醇的混合物，（D）在100-130℃和10-2-10-4托的分子蒸馏器中再循环酯化产物 去除脂肪酸甲酯，和（D）再次在170-200℃和10-2-10-4托再循环以分离和浓缩生育酚。 正己烷与甲醇的混合比为10:1，混合溶剂的添加量为豆油馏出物的2〜3倍。
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公开(公告)号：KR1019930005415B1
公开(公告)日：1993-06-21
申请号：KR1019910001231
申请日：1991-01-25
Applicant: 한국과학기술연구원
IPC: C07D311/72
Abstract: The tocopherol is purifyed by (a) adding mixed solvent of n- hexane and 50 % (v/v) methanol into the soybean oil distillate, (b) removing the sterol of the mixt. by filtering, cooling the filtered soln., and re-filtering, (c) methyl esterifying the mixt. from which sterol is removed, (d) recirculating esterified product at 100-130 deg.C and 10-3-10-4 torr in the molecular distillator to remove fatty acid methyl ester, (e) concentrating the obtd. soln. contg. 50-55 % tocopherol and dissolving in the lower alcohol (I), (f) adsorbing it into alkaline anion exchange resin, and purifying with the (I) contg. 5-10 % acetic acid, and (g) dissolving the purifyed tocopherol in the (I) and passing through cation exchange resin to obtain the final product.
Abstract translation: 生育酚通过（a）将正己烷和50％（v / v）甲醇的混合溶剂加入大豆油馏出物中，（b）除去混合物的固醇来纯化。 通过过滤，冷却过滤的溶胶，并重新过滤，（c）甲基酯化混合物。 （d）在分子蒸馏器中在100-130℃和10-3-10-4乇下再循环酯化产物以除去脂肪酸甲酯，（e）浓缩该物质。 SOLN。 contg。 50-55％生育酚溶于低级醇（I）中，（f）将其吸附到碱性阴离子交换树脂中，用（I） 5-10％乙酸，和（g）将纯化的生育酚溶解在（I）中并通过阳离子交换树脂以获得最终产物。
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