CN102229641A - Method for extracting phytosterol from deodorized distillate of vegetable oil - Google Patents
Method for extracting phytosterol from deodorized distillate of vegetable oil Download PDFInfo
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- CN102229641A CN102229641A CN2011101049971A CN201110104997A CN102229641A CN 102229641 A CN102229641 A CN 102229641A CN 2011101049971 A CN2011101049971 A CN 2011101049971A CN 201110104997 A CN201110104997 A CN 201110104997A CN 102229641 A CN102229641 A CN 102229641A
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- solid acid
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- plant sterol
- alcohol
- ethanol
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Abstract
The invention belongs to the technical field of biochemical engineering, and particularly relates to a method for extracting phytosterol from a deodorized distillate of vegetable oil. The technical scheme is as follows: the process comprises the following steps: 1. esterification: calculating the theoretical dosage of alcohol according to the content of free fatty acid in the deodorized distillate, wherein the actual dosage of the added alcohol is 1-8 times of the theoretical dosage; solid acid is used as a catalyst, the dosage of the solid acid is 0.5-3% (mass percentage content) of the actual dosage of alcohol, the solid acid is stirred and reacted for 0.5-3 hours at the reflux temperature of 50-95 ℃, and water is added after the reaction is finished; 2. filtering; 3. cold separation: carrying out cold precipitation at 5-35 ℃ for 1-10 hours to obtain phytosterol crystals; 4. washing and drying: washing the filtrate with a mixed solvent of ethanol and acetone, and drying to obtain the white phytosterol, wherein the volume ratio of the ethanol to the acetone is 1-10: 10-1. The invention has the beneficial effects that: simple chemical process, simple operation, no pollution and low cost.
Description
Technical field
The invention belongs to technical field of biochemical industry, relate in particular to a kind of from the vegetable oil deodorized method that slips out thing extraction plant sterol.
Background technology
The vegetable oil deodorized main component that slips out thing is free fatty acids, neutral grease, natural VE and plant sterol etc.Existingly mainly contain two kinds from the method for wherein extracting plant sterol: a kind of strong acid, highly basic of being to use is as catalyzer, free fatty acids and neutral grease are changed into fatty acid ester after, isolate plant sterol again, referring to Chinese patent CN1074217A.Its defective is, strong acid, alkali corrosion are strong on the one hand, equipment material is had relatively high expectations, and the aftertreatment more complicated, unfavorable to environment; This on the other hand comparatively loaded down with trivial details as the chemical technology of catalyzer with strong acid, highly basic.Another kind method is to utilize lipase to replace conventional strong acid, highly basic as catalyzer, referring to Chinese patent CN1563399A.Its defective is that the lipase price is higher, and suitability for industrialized production acquires a certain degree of difficulty.
Summary of the invention
For addressing the above problem, it is easy, lower-cost from the vegetable oil deodorized method that slips out thing extraction plant sterol that the present invention proposes a kind of technological process.
Technical scheme of the present invention is: a kind of from the vegetable oil deodorized method that slips out thing extraction plant sterol, its processing step comprises: (1) esterification: the content that slips out free lipid acid in the thing according to deodorization, calculate the theoretical consumption of alcohol, the theoretical consumption and the free fatty acids mass ratio of alcohol are 1:1, and the actual consumption that adds alcohol is 1～8 times of theoretical consumption; Use the solid acid as catalyst, consumption is 0.5～3%(quality percentage composition of actual pure consumption), 50～95 ℃ of following stirring reactions of reflux temperature 0.5～3 hour, reaction added entry after finishing, and the weight that adds entry is with actual to add pure weight identical.(2) filter: by filtering solid acid and reaction system are separated, solid acid is waited until next time and is used.(3) cold analysis: after the reaction system filtering solid acid catalyst after the esterification, after 1～10 hour, plant sterol is separated out with needle-like, sheet or Powdered crystal 5～35 ℃ of cold analysis, and vacuum filtration or centrifugation can get the plant sterol crystal.(4) washing and drying: the mixed solvent washing with ethanol and acetone leaches thing, in 80～100 ℃ of oven dry of temperature, obtains white plant sterol, and the volume ratio of ethanol and acetone is 1～10:10～1.
Solid acid is a kind of acid Lewis acid stronger than 100% sulfuric acid.Reaction finishes the back only needs filter operation can realize and the separating of reaction system.Process is easy, pollution-free, and have making simply, advantage such as not water funk, high temperature resistant, be a kind of very promising " green " commercial catalysts.Solid acid can be formed by various safe powder formulation organic complexes, can replace the use of acid in a lot of fields, and solid acid is a powder formulation, has transportation safety, carrying, advantage such as easy to use.
Beneficial effect of the present invention is: chemical technology is simple, and is easy and simple to handle, pollution-free, and cost is low.
Embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1: slip out from the soybean oil deodorization and extract plant sterol the thing, processing step is as follows:
(1) esterification: the soybean oil deodorization slips out thing 300 g, and wherein, containing free fatty acids is 46.7%(quality percentage composition), slip out in the thing content of free lipid acid according to deodorization, calculating the actual consumption that adds alcohol is 140ml.Use solid acid SO
4 2-/ Z
rO
2-Al
2O
3Make catalyzer, consumption is 1.3g, and 75 ℃ of following stirring reactions of reflux temperature 2 hours, reaction finished the back and adds 140ml water.
(2) filter: by filtering solid acid and reaction system are separated, solid acid is waited until next time and is used.
(3) cold analysis: after the reaction system filtering solid acid catalyst after the esterification, after 6 hours, plant sterol is separated out with needle-like, sheet or Powdered crystal 20 ℃ of cold analysis, and vacuum filtration or centrifugation can get the plant sterol crystal.
(4) washing and drying: leach thing twice with the ethanol of volume ratio 1:3 and the mixed solvent washing of acetone,, obtain white plant sterol 26.5g in 90 ℃ of oven dry of temperature.
Claims (1)
1. one kind slips out the method that thing extracts plant sterol from vegetable oil deodorized, it is characterized in that its processing step comprises:
(1) esterification: slip out in the thing content of free lipid acid according to deodorization, calculate the theoretical consumption of alcohol, theoretical consumption and the free fatty acids mass ratio of alcohol are 1:1, and actual to add pure consumption be 1～8 times of theoretical consumption; Use the solid acid as catalyst, consumption is 0.5～3%(quality percentage composition of actual pure consumption), 50～95 ℃ of following stirring reactions of reflux temperature 0.5～3 hour, reaction added entry after finishing, and the weight that adds entry is with actual to add pure weight identical;
(2) filter: by filtering solid acid and reaction system are separated, solid acid is waited until next time and is used;
(3) cold analysis: after the reaction system filtering solid acid catalyst after the esterification, after 1～10 hour, plant sterol is separated out with needle-like, sheet or Powdered crystal 5～35 ℃ of cold analysis, and vacuum filtration or centrifugation can get the plant sterol crystal;
(4) washing and drying: the mixed solvent washing with ethanol and acetone leaches thing, in 80～100 ℃ of oven dry of temperature, obtains white plant sterol, and the volume ratio of ethanol and acetone is 1～10:10～1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110104997.1A CN102229641B (en) | 2011-04-26 | 2011-04-26 | Method for extracting phytosterol from deodorized distillate of vegetable oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110104997.1A CN102229641B (en) | 2011-04-26 | 2011-04-26 | Method for extracting phytosterol from deodorized distillate of vegetable oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102229641A true CN102229641A (en) | 2011-11-02 |
| CN102229641B CN102229641B (en) | 2013-09-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201110104997.1A Active CN102229641B (en) | 2011-04-26 | 2011-04-26 | Method for extracting phytosterol from deodorized distillate of vegetable oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861036A (en) * | 2014-02-24 | 2015-08-26 | 上海兰蒂斯生物医药科技有限公司 | Extract for prevention and treatment of prostatic diseases and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101331149A (en) * | 2005-11-08 | 2008-12-24 | 科学与工业研究会 | A process for the preparation of high purity phytosterols from deodourizer distillate from vegetable oils |
| CN101822978A (en) * | 2010-04-07 | 2010-09-08 | 代斌 | Catalyst for integrative conversion of rapeseed oil deodorizer distillate and preparation method thereof |
| CN101985460A (en) * | 2010-08-10 | 2011-03-16 | 江南大学 | Method for preparing phytosterol ester |
-
2011
- 2011-04-26 CN CN201110104997.1A patent/CN102229641B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101331149A (en) * | 2005-11-08 | 2008-12-24 | 科学与工业研究会 | A process for the preparation of high purity phytosterols from deodourizer distillate from vegetable oils |
| CN101822978A (en) * | 2010-04-07 | 2010-09-08 | 代斌 | Catalyst for integrative conversion of rapeseed oil deodorizer distillate and preparation method thereof |
| CN101985460A (en) * | 2010-08-10 | 2011-03-16 | 江南大学 | Method for preparing phytosterol ester |
Non-Patent Citations (1)
| Title |
|---|
| 曹崇江 等: "Al、Ga促进SO42-/ZrO2的合成及其对酯化反应的催化作用", 《应用化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861036A (en) * | 2014-02-24 | 2015-08-26 | 上海兰蒂斯生物医药科技有限公司 | Extract for prevention and treatment of prostatic diseases and preparation method thereof |
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| CN102229641B (en) | 2013-09-11 |
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Address after: 272400 No. 263 Jianshe South Road, Jiaxiang County, Jining City, Shandong Province Patentee after: SHANDONG JIAGUAN GRAIN OIL INDUSTRY GROUP Co.,Ltd. Address before: 272400 No. 263 Jianshe South Road, Jiaxiang County, Jining City, Shandong Province Patentee before: JIAXIANG JIAGUAN GREASE CHEMICAL Co.,Ltd. |