CN1310903C - Method for extracting natural vitamin E from vegetable oil and fat refining and deodorizing distillate - Google Patents
Method for extracting natural vitamin E from vegetable oil and fat refining and deodorizing distillate Download PDFInfo
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- CN1310903C CN1310903C CNB200510114851XA CN200510114851A CN1310903C CN 1310903 C CN1310903 C CN 1310903C CN B200510114851X A CNB200510114851X A CN B200510114851XA CN 200510114851 A CN200510114851 A CN 200510114851A CN 1310903 C CN1310903 C CN 1310903C
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Abstract
The invention discloses a method for extracting natural vitamin E from the refined off-odor distillate of vegetable fat. The invention comprises the steps as follow: (1) acid removing through distillation, the refined off-odor distillate of vegetable fat is distillated to remove the fatty acid in a condition of a vacuum degree ranging from 0.5 Pa to 50 Pa, a temperature ranging from 117 DEG C to 190 DEG C and a linear velocity of 3m/s to 5m/s; (2) esterification reaction; (3) cold decantation, in which most of sterols are separated out; (4) filtering and separating to remove the sterols; (5) dehydration; and (6) molecular distillation, the dehydrated liquid is processed with four stages of molecular distillation under different temperatures and vacuum degrees so as to obtain natural vitamin E. The invention separates and removes the fatty acid from the refined off-odor distillate through distillation, and then produces the fatty acid methyl ester through the one-off esterification reaction. The technology has the advantages of reducing the one-off esterification process, decreasing the assistant material consumption and the energy consumption, reducing the production cost and increasing the yield.
Description
Technical field
The present invention relates to a kind of method of from vegetable oil and fat refining and deodorizing distillate, extracting natural VE.
Background technology
Modern medicine confirms that vitamin-E has stronger physiologically active, and it can control the generation of intravital lipid peroxide, therefore has the function that delays senility.
Vegetable oil and fat refining and deodorizing distillate is the by product of oil and fat refining, contains abundant natural VE and plant sterol, is the high quality raw material of extraction and separating natural vitamin E and plant sterol.Except that the plant sterol of natural VE that contains 2%-10% and 5%-15%, major part is free fatty acids and neutral oil in the vegetable oil and fat refining and deodorizing distillate, and free fatty acid content is 30%-50%, and the content of neutral oil is 20%-30%.Traditional technology will be carried out fatization twice to vegetable oil and fat refining and deodorizing distillate, earlier free lipid acid in the deodorization distillate is carried out esterification, again the neutral oil in the deodorization distillate carry out lactideization, free fatty acids and neutral oil all are transformed into fatty acid methyl ester, carry out operations such as cold analysis, sterols separated, molecular distillation separation of fatty acids methyl esters again, the significant difference of boiling point between this technology utilization fatty acid methyl ester and the natural VE and being separated.And the free fatty acids in the actual deodorization distillate can utilize the difference of boiling point under uniform pressure fully and lipid acid is removed in advance, carry out the disposable esterification of neutral oil again, avoid twice esterification, thereby can save solvent, catalyzer and the consumption of water power vapour, the treatment capacity of the esterification cold analysis of identical scale is strengthened, reduce production costs simultaneously.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate is provided.
Technical scheme of the present invention is summarized as follows:
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate and to be removed free fatty acids under vacuum tightness 0.5Pa～50Pa, temperature are 117 ℃～190 ℃, the condition of linear velocity 3m/s～5m/s;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol or ethanol: sodium hydroxide is 30: 6～15: 1～3 to carry out esterification, 2 hours～10 hours reaction times;
(3) cold analysis, mother liquor after the esterification is carried out cold analysis, low whipping speed is 20rpm～40rpm, be cooled fast to 60 ℃ with 5 ℃～10 ℃/h, drop to 40 ℃ with 0.5 ℃～2 ℃/h again, drop to 0 ℃～5 ℃ with 0.5 ℃～1.5 ℃/h again, stop to stir, be incubated 24 hours～48 hours, most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under 500Pa～3000Pa isolated liquid to be carried out processed at 100 ℃～120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.08MPa～-0.099MPa, 100 ℃～120 ℃
Secondary: 5Pa～100Pa, 120 ℃～180 ℃
Three grades: 0.5Pa～5Pa, 160 ℃～170 ℃
Level Four: 0.5Pa～5Pa, 170 ℃～190 ℃
Obtain fatty acid methyl ester at secondary, obtain natural VE in level Four.
Vacuum tightness can be selected 5Pa～40Pa in step (1), and vacuum tightness is 10Pa～30Pa preferably, and best vacuum tightness is 15Pa～20Pa.
Temperature can be controlled at 130 ℃～170 ℃ in step (1), and best temperature is 140 ℃～160 ℃.
Distillation plant can select conventional underpressure distillation device in step (1), is preferably short-distance distiller.
Linear velocity is 4m/s in step (1).
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate of the present invention is that the lipid acid in the deodorization distillate is separated removal by distillating method, carry out disposable lactide reaction then and generate fatty acid methyl ester, this technology has reduced esterification process one time, the consumption of subsidiary material and the consumption of the energy have been reduced, reduce production cost, improved output.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 0.5Pa, temperature are 117 ℃, the condition of linear velocity 4m/s and to be removed lipid acid in short-distance distiller;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol: sodium hydroxide is to carry out esterification, 4 hours reaction times at 30: 6: 1;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 20rpm, is cooled fast to 60 ℃ with 5 ℃/h, drops to 40 ℃ with 1 ℃/h again, drops to 5 ℃ with 1 ℃/h again, stops to stir, and is incubated 24 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 2000Pa isolated liquid to be carried out processed at 120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.095MPa, 120 ℃
Secondary: 30Pa, 150 ℃
Three grades: 3Pa, 160 ℃
Level Four: 2Pa, 180 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains vitamin-E at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Embodiment 2
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 5Pa, temperature are 130 ℃, the condition of linear velocity 3m/s and to be removed lipid acid in the underpressure distillation device;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol: sodium hydroxide is to carry out esterification, 2 hours reaction times at 30: 15: 3;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 40rpm, is cooled fast to 60 ℃ with 10 ℃/h, drops to 40 ℃ with 0.5 ℃/h again, drops to 0 ℃ with 0.5 ℃/h again, stops to stir, and is incubated 36 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 3000Pa isolated liquid to be carried out processed at 100 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.08MPa, 100 ℃
Secondary: 5Pa, 120 ℃
Three grades: 0.5Pa, 160 ℃
Level Four: 0.5Pa, 170 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains natural VE at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Embodiment 3
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 50Pa, temperature are 190 ℃, the condition of linear velocity 5m/s and to be removed lipid acid in short-distance distiller;
(2) esterification, by weight the mother liquor that step (1) is obtained: ethanol: sodium hydroxide is to carry out esterification, 10 hours reaction times at 30: 10: 2;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 30rpm, is cooled fast to 60 ℃ with 7 ℃/h, drops to 40 ℃ with 2 ℃/h again, drops to 3 ℃ with 1.5 ℃/h again, stops to stir, and is incubated 48 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 500Pa isolated liquid to be carried out processed at 110 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.099MPa, 110 ℃
Secondary: 100Pa, 180 ℃
Three grades: 5Pa, 170 ℃
Level Four: 5Pa, 190 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains natural VE at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Embodiment 4
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 40Pa, temperature are 140 ℃, the condition of linear velocity 4m/s and to be removed lipid acid in short-distance distiller;
(2) esterification, by weight the mother liquor that step (1) is obtained: ethanol: sodium hydroxide is to carry out esterification, 6 hours reaction times at 30: 6: 2;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 20rpm, is cooled fast to 60 ℃ with 5 ℃/h, drops to 40 ℃ with 1 ℃/h again, drops to 5 ℃ with 1 ℃/h again, stops to stir, and is incubated 24 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 2000Pa isolated liquid to be carried out processed at 120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.095MPa, 120 ℃
Secondary: 30Pa, 150 ℃
Three grades: 3Pa, 160 ℃
Level Four: 2Pa, 180 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains natural VE at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Embodiment 5
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 30Pa, temperature are 160 ℃, the condition of linear velocity 4m/s and to be removed lipid acid in short-distance distiller;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol: sodium hydroxide is to carry out esterification, 3 hours reaction times at 30: 6: 1;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 20rpm, is cooled fast to 60 ℃ with 5 ℃/h, drops to 40 ℃ with 1 ℃/h again, drops to 5 ℃ with 1 ℃/h again, stops to stir, and is incubated 24 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 2000Pa isolated liquid to be carried out processed at 120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.095MPa, 120 ℃
Secondary: 30Pa, 150 ℃
Three grades: 3Pa, 160 ℃
Level Four: 2Pa, 180 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains natural VE at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Embodiment 6
A kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate comprises the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate under vacuum tightness 40Pa, temperature are 170 ℃, the condition of linear velocity 4m/s and to be removed lipid acid in short-distance distiller;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol: sodium hydroxide is to carry out esterification, 4 hours reaction times at 30: 8: 1;
(3) cold analysis is carried out cold analysis with the mother liquor after the esterification, and low whipping speed is 30rpm, is cooled fast to 60 ℃ with 5 ℃/h, drops to 40 ℃ with 1 ℃/h again, drops to 5 ℃ with 1 ℃/h again, stops to stir, and is incubated 24 hours, and most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under the 2000Pa isolated liquid to be carried out processed at 120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.095MPa, 120 ℃
Secondary: 30Pa, 150 ℃
Three grades: 3Pa, 160 ℃
Level Four: 2Pa, 180 ℃
Obtain fatty acid methyl ester at secondary, three grades of overhead products return secondary, and to distill to guarantee that fatty acid methyl ester obtains natural VE at the level Four overhead product in the natural VE below 100ppm, to steam residual thing once more be residual oil.
Claims (8)
1, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate is characterized in that comprising the steps:
(1) distillation depickling is distilled material plant oil and fat refining deodorization distillate and to be removed lipid acid under vacuum tightness 0.5Pa～50Pa, temperature are 117 ℃～190 ℃, the condition of linear velocity 3m/s～5m/s;
(2) esterification, by weight the mother liquor that step (1) is obtained: methyl alcohol or ethanol: sodium hydroxide is 30: 6～15: 1～3 to carry out esterification, 2 hours～10 hours reaction times;
(3) cold analysis, mother liquor after the esterification is carried out cold analysis, low whipping speed is 20rpm～40rpm, be cooled fast to 60 ℃ with 5 ℃～10 ℃/h, drop to 40 ℃ with 0.5 ℃～2 ℃/h again, drop to 0 ℃～5 ℃ with 0.5 ℃～1.5 ℃/h again, stop to stir, be incubated 24 hours～48 hours, most sterols are separated out;
(4) filtering separation is removed sterol;
(5) dehydration is under 500Pa～3000Pa isolated liquid to be carried out processed at 100 ℃～120 ℃ in vacuum tightness;
(6) molecular distillation, the liquid after will dewatering under different temperature and the vacuum tightness carries out the level Four molecular distillation, and condition at different levels is as follows:
One-level :-0.08MPa～-0.099MPa, 100 ℃～120 ℃
Secondary: 5Pa～100Pa, 120 ℃～180 ℃
Three grades: 0.5Pa～5Pa, 160 ℃～170 ℃
Level Four: 0.5Pa～5Pa, 170 ℃～190 ℃
Obtain fatty acid methyl ester at secondary, obtain natural VE in level Four.
2, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 1, the vacuum tightness that it is characterized in that described step (1) is 5Pa～40Pa.
3, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 2, the vacuum tightness that it is characterized in that described step (1) is 10Pa～30Pa.
4, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 3, the vacuum tightness that it is characterized in that described step (1) is 15Pa～20Pa.
5, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 1, the temperature that it is characterized in that described step (1) is 130 ℃～170 ℃.
6, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 5, the temperature that it is characterized in that described step (1) is 140 ℃～160 ℃.
7, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 1 is characterized in that distillation plant is a short-distance distiller.
8, a kind of method of extracting natural VE from vegetable oil and fat refining and deodorizing distillate according to claim 1 is characterized in that described linear velocity is 4m/s.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200510114851XA CN1310903C (en) | 2005-06-28 | 2005-11-18 | Method for extracting natural vitamin E from vegetable oil and fat refining and deodorizing distillate |
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| CN200510014056 | 2005-06-28 | ||
| CN200510014056.3 | 2005-06-28 | ||
| CNB200510114851XA CN1310903C (en) | 2005-06-28 | 2005-11-18 | Method for extracting natural vitamin E from vegetable oil and fat refining and deodorizing distillate |
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| CN1775771A CN1775771A (en) | 2006-05-24 |
| CN1310903C true CN1310903C (en) | 2007-04-18 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101607977B (en) * | 2009-06-12 | 2011-06-29 | 天津工业大学 | Method for extracting and purifying natural phytosterol from oil deodorization distillate residual oil and technique thereof |
| CN103467432B (en) * | 2013-09-16 | 2016-08-17 | 四川省仁德制药有限公司 | A kind of method extracting vitamin E from deodorizer distillate of idesia polycarpa oil |
| CN103571633B (en) * | 2013-11-15 | 2015-09-16 | 潘见 | Esterification-ultra-high voltage Crystallization Separation the method for one vegetable oil overhead product |
| CN103965155B (en) * | 2014-04-15 | 2018-10-16 | 江苏玺鑫维生素有限公司 | A kind of preparation process of natural VE |
| CN107474093B (en) * | 2017-08-23 | 2019-07-23 | 福建省格兰尼生物工程股份有限公司 | A kind of method of deodorization distillate continuous production VE, sterol, methyl esters, glycerol, squalene and high-boiling components |
| CN107722093B (en) * | 2017-09-28 | 2020-11-10 | 沧州市宝来金康生物科技股份有限公司 | Process for extracting sterol from vegetable oil deodorizer distillate |
| CN108299373B (en) * | 2018-05-07 | 2021-01-12 | 宜春大海龟生命科学有限公司 | Method for extracting natural vitamin E from rice bran oil deodorizer distillate |
| CN112159384A (en) * | 2020-09-07 | 2021-01-01 | 山西农业大学 | Soybean vitamin E extraction device and extraction method |
| CN112941126A (en) * | 2021-04-01 | 2021-06-11 | 福建省格兰尼生物工程股份有限公司 | Method for extracting soybean vitamin E from non-soybean deodorized distillate |
| CN112920155A (en) * | 2021-04-01 | 2021-06-08 | 福建省格兰尼生物工程股份有限公司 | Method for extracting alpha vitamin E from deodorized distillate |
| CN114686297A (en) * | 2022-04-01 | 2022-07-01 | 中粮工科(西安)国际工程有限公司 | Method for efficiently retaining natural VE and phytosterol in walnut oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037769C (en) * | 1993-01-14 | 1998-03-18 | 清华大学 | Process for extracing vitamin E and sterol from by-product after refining vegetable oil |
| CN1418877A (en) * | 2002-12-06 | 2003-05-21 | 武汉凯迪精细化工有限公司 | Process for extracting vitamin E from plant-oil debrominated distillate |
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2005
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1037769C (en) * | 1993-01-14 | 1998-03-18 | 清华大学 | Process for extracing vitamin E and sterol from by-product after refining vegetable oil |
| CN1418877A (en) * | 2002-12-06 | 2003-05-21 | 武汉凯迪精细化工有限公司 | Process for extracting vitamin E from plant-oil debrominated distillate |
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Assignee: China Grains and Oils Group Corporation Agricultural Science and Technology Co., Ltd. Assignor: Tian Ke Ke (Tianjin) Biological Engineering Co., Ltd. Contract fulfillment period: 2008.9.20 to 2014.9.19 contract change Contract record no.: 2008110000192 Denomination of invention: Method for extracting natural vitamin E from vegetable oil and fat refining and deodorizing distillate Granted publication date: 20070418 License type: Exclusive license Record date: 20081212 |
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Address after: Second Street 300457 Tianjin City Development Zone No. 2 Building No. 2 villa Wanlian Patentee after: COFCO Tianke Bioengineering (Tianjin) Co., Ltd. Address before: Second Street 300457 Tianjin City Development Zone No. 2 Building No. 2 villa Wanlian Patentee before: Zhonggu Tianke (Tianjin) Bioengineering Co., Ltd. |
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