CN104651037A - Method for extracting oil and protein in silybum marianum kernels by subcritical fluid - Google Patents
Method for extracting oil and protein in silybum marianum kernels by subcritical fluid Download PDFInfo
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- CN104651037A CN104651037A CN201410021739.0A CN201410021739A CN104651037A CN 104651037 A CN104651037 A CN 104651037A CN 201410021739 A CN201410021739 A CN 201410021739A CN 104651037 A CN104651037 A CN 104651037A
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- silybum marianum
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to a method for extracting oil and protein in silybum marianum kernels by subcritical fluid. The method is characterized by comprising the following steps: (1) screening dried silybum marianum kernels, removing impurities, and peeling hulls by virtue of a peeling machine to obtain silybum marianum kernels; (2) rolling or extruding and grinding the silybum marianum kernels; (3) putting the ground silybum marianum kernels and an extraction solvent into a subcritical fluid extraction kettle for continuous extraction to obtain extracting liquid; (4) gasifying the extracting solvent by means of pressure reduction and temperature increase in an evaporation system to separate the extracting solvent from the extracting liquid so as to obtain silybum marianum kernel oil; (5) keeping the solid in the extraction kettle as the silybum marianum protein. Compared with supercritical extraction, the method has the advantages of low equipment investment and low production state stress, and is suitable for industrial large-scale production. Compared with a traditional process for preparing oil and protein, the method has the advantages of simple process flow, high yield, good quality of oil and protein, environmental friendliness and no pollution.
Description
Technical field
The present invention relates to the treatment process of a kind of Silymarin, particularly relate to a kind of method of grease and albumen in subcritical fluid extraction silybum marianum seeds, belong to Vegetable oil lipoprotein and protein extraction isolation technique.
Background technology
Silymarin, has another name called for water flies pheasant, Milk Thistle, and be composite family Silybum plant, English formal name used at school is Herba Silybi, latin name Silyum marianum.Originating in Mediterranean, the western grass in Asia also has wild distribution, is life in 2 years or annual herb plant, now Europe, Asia, and Africa, all there is cultivation in South and North America.
Silymarin is a kind of excellent cash crop and oilseed plant, and fruit or title seed have good health protection effect.Phase later 1960s, the scientists being representative with West Germany H Wanger finds and confirms the extract of Silymarin seed---silymarin has nutrition, protect the liver, protect the health-care effect of liver, and safe without toxic side effect, therefore, the plant utilization of Silymarin is carried out widely in the whole world, China introduces Silymarin seed from West Germany at that time the beginning of the seventies in last century, after experiment in cultivation success, the medicinal health research of Silymarin and establishing in large scale advance rapidly, like this, this color of silybum marianum seed oil is pale yellow, bright, outward appearance and mouthfeel be the new oil product also output along with a large amount of production of silymarin all well., main containing unsaturated fatty acids in silybum marianum seed oil, wherein containing a large amount of oleic acid, linolic acid and a small amount of linolenic acid, eicosanoic acid etc. (for details see attached table 1).As everyone knows, unsaturated fatty acids is very useful to human body, particularly double bond unsaturated fatty acids is combined formed ester and easily transports with cholesterol, metabolism and excretion, therefore silybum marianum seed oil can reduce cholesterol and the triglyceride level of exogenous hyperlipidaemia, can the atherosis and fatty liver of prevention of arterial.
The method producing silybum marianum seed oil at present mainly contains mechanical cold-press and solvent extraction method.Machinery cold-press oil yield is low, the wasting of resources is large, the grease of about 10% has all been stayed in the silybum marianum seed dregs of rice, solvent extraction method, oil yield is high, but dissolvent residual in oil is also high, high temperature leaches the also serious quality reducing oil simultaneously, these two kinds of techniques all cannot by the albumen sepn in silybum marianum seed out simultaneously, and quality proteins a large amount of in silybum marianum seed is all contained in the silybum marianum seed dregs of rice, only can use as cheap feed.
Subcritical fluid extraction is the new extraction and separation technology grown up in recent years, and contrast tradition produces grease and protein Process, and have technique simple, recovery rate is high, good product quality, pollution-free, many advantages such as no solvent residue.Contrast supercritical extraction technology, it is few that it has facility investment, and production status pressure is low, is easy to many advantages such as control.
In view of the foregoing, China's subcritical fluid extraction technological invention patent in recent years continues to bring out, as 2001.8.2 invention disclosed patent (ZL01108701.3) provides a kind of method of extracting pyrethrin by using subcritical liquified petroleum gas, 2008.4.16 invention disclosed patent (200610104744.3) provides a kind of subcritical fluid extraction solvent and extracting process, 2012.06.20 invention disclosed patent (201110374434.4) provides the method for a Subcritical fluid extraction Seabuckthorm Seed Oil, and 2012.08.22 invention disclosed patent (201210138610.9) adopts subcritical extraction method to extract the method etc. of woodfrog egg oil, these type of research and development are a lot of, research and development space is wide, be expected to become the direction of extraction and separation technology progress instantly.But investigate according to applicant: present stage adopts subcritical fluid extraction technology, is suitable for large-scale industrial production, extracting and separating goes out grease and albumen two products in silybum marianum seed while that particularly a technical process being got off, still belong to blank.
Summary of the invention
Object of the present invention is just the above-mentioned technical problem solving prior art existence, by research and lot of experiments screening repeatedly, provides a kind of method of grease and albumen in subcritical fluid extraction silybum marianum seeds.
For achieving the above object, this subcritical fluid extraction that the present invention provides is separated the method for grease and albumen in silybum marianum seeds, is characterized in comprising the following steps.
(1) seed shell is peelled off after the silybum marianum seed screening and removing impurities of drying through machinery of peeling off.Obtain silybum marianum seeds.
(2) silybum marianum seeds is rolled or attrition crushing.
(3) by the silybum marianum seeds of fragmentation and solvent by 1: 1-1: 20 quality volume to put in subcritical abstraction still the continuous extraction of adverse current gradient 1-20 time. each 10-150min. obtains extracting solution, and extraction process is aided with ultrasonic wave and stirring.
(4) extraction liquid obtained enters vapo(u)rization system through pipeline.Utilization decompression temperature-rising method makes the solvent gasification separation in extraction liquid, and separating pressure is 0.1-2.0mpa.Separation temperature is 0-90 DEG C, and reuse after the solvent of gasification enters compression cycle system, the extraction liquid separating solvent is silybum marianum seed oil, and the solids stayed in extraction kettle is silybum marianum protein.
For realizing object of the present invention better, the solvent in described step (3) refers to butane, propane, dme, Trimethylmethane, liquefied petroleum gas (LPG), any one in 1.1.1.2-Tetrafluoroethane.
For realizing object of the present invention better, in described step (3), extraction conditions refers to that extraction temperature is 5----85 DEG C.Extracting pressure is 0.15-3.0mpa, and extraction flow is 10-160L/h.
Compared with prior art, the invention has the beneficial effects as follows.
Present invention process process is simple, and easy handling controls, and extraction recovery rate improves, and quality product improves, and can be separated acquisition two kinds of products simultaneously.
Solvent for use transforms through liquid state → gaseous state → liquid circulation, recycle, loss be few, pollution-free,
Have production status pressure low compared with supercritical extraction process, device fabrication cost is low, is suitable for large-scale commercial production application.
Extracting and separating is thorough, fat content≤1% in extract remainder silybum marianum protein.Dissolvent residual≤50ppm in silybum marianum seed oil.
Extraction time is short, extraction temperature is low.Fully remain the activeconstituents of silybum marianum seed oil and silybum marianum protein.
Embodiment
Embodiment 1: make extraction solvent with butane.
(1) the silybum marianum seed mechanical descaling of will mix through screening, dry nothing.Obtain silybum marianum seeds.
(2) silybum marianum seeds is ground (squeezing) fragmentation.
(3) the feed liquid quality volume silybum marianum seeds of fragmentation and extraction solvent butane being pressed 1:20 drops in subcritical fluid extraction still, extraction temperature 5 DEG C, extracting pressure 0.8mpa, extraction solvent flow is adverse current gradient continuous extraction 10 times under the condition of 80L/h, each 75min is extracted liquid, and extraction process is aided with ultrasonic wave and stirring.
(4) extraction liquid is transported to vapo(u)rization system, utilize decompression temperature-rising method, the butane gasifying in extraction liquid is separated, separating pressure is 0.4mpa, separation temperature is 10 DEG C, and the butane of gasification enters compression cycle system Posterior circle and utilizes, and the extraction liquid isolating butane is silybum marianum seed oil.
(5) namely the solids stayed in extraction kettle is silybum marianum protein.In order to make butane Quick-gasifying residual in albumen, Pressure Drop in still be risen to 10 DEG C to 0.4mpa temperature.Receive residual to the greatest extent butane, extraction completes; Clean out silybum marianum protein in still, extraction kettle enters next production cycle.
Embodiment 2: make extraction solvent with dme.
(1) to extract--the pre-treatment of silybum marianum seeds is as embodiment 1.
(2) the feed liquid quality volume pressing 1:5 through pretreated silybum marianum seeds and extraction solvent dme is dropped in subcritical fluid extraction still, extraction temperature 20 DEG C, extracting pressure 0.15mpa, extraction solvent flow is under the condition of 40L/h, adverse current gradient continuous extraction 15 times, each 30min.Be extracted liquid, extraction process is aided with ultrasonic wave and stirring.
(3) extraction liquid of acquisition is transported to vapo(u)rization system, utilize decompression temperature-rising method, make the dme gasification separation in extraction liquid, separating pressure is 0.1mpa, and separation temperature is 30 DEG C, and dme is separated with extraction liquid, obtains silybum marianum seed oil.
(4) Pressure Drop in extraction kettle is risen to 30 DEG C to 0.1mpa temperature, receive the gasification dme remained in the greatest extent in silybum marianum protein; Clean out silybum marianum protein in still, namely one takes turns extraction production completes.
Embodiment 3: make extraction solvent with Trimethylmethane.
(1) to extract--the pre-treatment of silybum marianum seeds is as embodiment 1.
(2) the feed liquid quality volume pressing 1:1 through pretreated silybum marianum seeds and extraction solvent Trimethylmethane is dropped in subcritical fluid extraction still, extraction temperature 35 DEG C, extracting pressure 2.3mpa, extraction solvent flow is under the condition of 120L/h, adverse current gradient continuous extraction 5 times, each 120min.Be extracted liquid, extraction process is aided with ultrasonic wave and stirring.
(3) extraction liquid of acquisition is transported to vapo(u)rization system, utilize decompression temperature-rising method, make the Trimethylmethane gasification separation in extraction liquid, separating pressure is 1.0mpa, and separation temperature is 45 DEG C, and Trimethylmethane is separated with extraction liquid, both obtains silybum marianum seed oil.
(4) by Pressure Drop in extraction kettle to 1.0mpa, temperature increase to 45 DEG C, receives the gasification Trimethylmethane that remains in the greatest extent in silybum marianum protein, cleans out silybum marianum protein in still, and one takes turns extraction produces and namely completes.
Embodiment 4: make extraction solvent with propane.
(1) to the pre-treatment of the sub-benevolence of extract-Silymarin as embodiment 1.
(2) the feed liquid quality volume pressing 1:15 through pretreated silybum marianum seeds and extraction solvent propane is dropped in subcritical abstraction still.Extraction temperature 55 DEG C, extracting pressure 1.8mpa.Under the condition of extraction solvent flow 160L/h, adverse current gradient extracts 1 time, and the time is 150min, is extracted liquid, and extraction process is aided with ultrasonic wave and stirring.
(3) extraction liquid of acquisition is transported to vapo(u)rization system, utilize decompression temperature-rising method, make the propane gasification separation in extraction liquid, separating pressure is 1.2mpa, and separation temperature is 60 DEG C, and propane is separated with extraction liquid, both obtains silybum marianum seed oil.
(4) by Pressure Drop in extraction kettle to 1.2mpa temperature increase to 60 DEG C, receive the gasification propane that remains in the greatest extent in silybum marianum protein; Clean out silybum marianum protein in still, namely one takes turns extraction production completes.
Embodiment 5: make extraction solvent with liquefied petroleum.
(1) to the pre-treatment of extract-silybum marianum seeds as embodiment 1.
(2) the feed liquid quality volume pressing 1:10 through pretreated silybum marianum seeds and extraction solvent liquefied petroleum is dropped in subcritical abstraction still, extraction temperature 85 DEG C, extracting pressure 3.0mpa, under the condition of extraction solvent flow 10L/h, adverse current gradient continuous extraction 20 times, each time is 10min, and extraction process is aided with ultrasonic wave and stirring.
(3) extraction liquid of acquisition is transported to vapo(u)rization system, utilize the method that decompression heats up that the liquefied petroleum gasification in extraction liquid is separated, separating pressure 2.0mpa, separation temperature is 90 DEG C, and liquefied petroleum is separated with extraction liquid, obtains silybum marianum seed oil.
(4) by Pressure Drop in extraction kettle to 2.0mpa temperature increase to 90 DEG C, receive and remain in the greatest extent the gasification liquefied petroleum of silybum marianum protein; Clean out silybum marianum protein in still, namely one takes turns extraction production completes.
Embodiment 6: make extraction solvent with 1.1.1.2 mono-Tetrafluoroethane (hereinafter referred to as Tetrafluoroethane).
(1) to the pre-treatment of extract-silybum marianum seeds as embodiment 1.
(2) the feed liquid quality volume pressing 1:2.5 through pretreated silybum marianum seeds and extraction solvent Tetrafluoroethane is dropped in subcritical abstraction still, extraction temperature 45 DEG C, extracting pressure 1.3mpa, under the condition of extraction solvent flow 100L/h, adverse current gradient continuous extraction 12 times, each 50min is extracted liquid, and extraction process is aided with ultrasonic wave and stirring.
(3) extraction liquid of acquisition is transported to vapo(u)rization system, utilize heating under reduced pressure method that the Tetrafluoroethane in extraction liquid is separated with extraction liquid, separating pressure is 0.5mpa, and separation temperature is 55 DEG C, and Tetrafluoroethane is separated with extraction liquid, obtains silybum marianum seed oil.
(4) by Pressure Drop in extraction kettle to 0.5mpa temperature increase to 55 DEG C, receive and remain in the greatest extent the gasification Tetrafluoroethane of silybum marianum protein, clean out silybum marianum protein in still, one takes turns extraction produces and namely completes.
Claims (3)
1. subcritical fluid extraction is separated a method for grease and albumen in silybum marianum seeds, comprises the following steps:
(1) peel off seed shell by after the silybum marianum seed screening and removing impurities of drying through machinery of peeling off, obtain silybum marianum seeds;
(2) silybum marianum seeds is rolled or attrition crushing;
(3) silybum marianum seeds of fragmentation and solvent to be put in subcritical abstraction still the continuous extraction of adverse current gradient 1-20 time by the quality volume of 1 ﹕ 1 ~ 1 ﹕ 20, each 10-150min, is extracted liquid, and extraction process is aided with ultrasonic wave and stirring;
(4) extraction liquid obtained enters vapo(u)rization system through pipeline, utilization decompression temperature-rising method makes the solvent gasification separation in extraction liquid, separating pressure is 0.1-2.0mpa, separation temperature is 0-90 DEG C, reuse after the solvent gasified enters compression cycle system, the extraction liquid separating solvent is silybum marianum seed oil, and the solids stayed in extraction kettle is silybum marianum protein.
2. a kind of subcritical fluid extraction according to claim 1 is separated the method for grease and albumen in silybum marianum seeds, it is characterized in that: the solvent in described step (3) is butane, propane, dme, Trimethylmethane, liquefied petroleum gas (LPG), 1.1.1.2---any one in Tetrafluoroethane.
3. a kind of subcritical fluid extraction according to claim 1 is separated the method for grease and albumen in silybum marianum seeds, it is characterized in that: in described step (3), extraction conditions refers to that extraction temperature is 5----85 DEG C, extracting pressure is 0.15-3.0mpa, and extraction flow is 10-160L/h.
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| CN201410021739.0A CN104651037A (en) | 2014-01-17 | 2014-01-17 | Method for extracting oil and protein in silybum marianum kernels by subcritical fluid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106310708A (en) * | 2016-10-14 | 2017-01-11 | 江西中烟工业有限责任公司 | Method for obtaining wolfberry fruit extract through multistage countercurrent extraction by adopting centrifugal extractor |
| CN107653062A (en) * | 2017-09-01 | 2018-02-02 | 湖南中医药大学 | A kind of method of subcritical abstraction Rhus fruit grease |
| CN108175026A (en) * | 2018-03-12 | 2018-06-19 | 黑龙江军门现代农业发展有限公司 | A kind of Silybum Marianum Gaertn Seed Oil solid beverage of brain tonic and intelligence development and preparation method thereof |
| CN109054990A (en) * | 2018-08-27 | 2018-12-21 | 浙江工业大学 | The method that one-step method efficiently prepares fish orgotein and cod-liver oil |
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| CN102260589A (en) * | 2011-06-24 | 2011-11-30 | 江苏江大源生态生物科技有限公司 | Method for preparing silybum marianum oil |
| CN102924438A (en) * | 2012-10-30 | 2013-02-13 | 晨光生物科技集团股份有限公司 | Method for extracting silymarin and silybum mariamum oil from silybum mariamum seed |
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| US20110027396A1 (en) * | 2007-12-23 | 2011-02-03 | Euromed Sa | Novel milk thistle extract, method for the production, and use |
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| CN101810350A (en) * | 2010-04-20 | 2010-08-25 | 江苏大学 | Method for comprehensive utilization of silybum marianum seeds |
| CN102260589A (en) * | 2011-06-24 | 2011-11-30 | 江苏江大源生态生物科技有限公司 | Method for preparing silybum marianum oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106310708A (en) * | 2016-10-14 | 2017-01-11 | 江西中烟工业有限责任公司 | Method for obtaining wolfberry fruit extract through multistage countercurrent extraction by adopting centrifugal extractor |
| CN107653062A (en) * | 2017-09-01 | 2018-02-02 | 湖南中医药大学 | A kind of method of subcritical abstraction Rhus fruit grease |
| CN108175026A (en) * | 2018-03-12 | 2018-06-19 | 黑龙江军门现代农业发展有限公司 | A kind of Silybum Marianum Gaertn Seed Oil solid beverage of brain tonic and intelligence development and preparation method thereof |
| CN109054990A (en) * | 2018-08-27 | 2018-12-21 | 浙江工业大学 | The method that one-step method efficiently prepares fish orgotein and cod-liver oil |
| CN109054990B (en) * | 2018-08-27 | 2022-04-08 | 浙江工业大学 | Method for efficiently preparing fish liver protein and fish liver oil by one-step method |
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