CN104611124B - Purple perilla seed is through squeezing and supercritical CO2The method that extraction carries oil - Google Patents
Purple perilla seed is through squeezing and supercritical CO2The method that extraction carries oil Download PDFInfo
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- CN104611124B CN104611124B CN201510001014.XA CN201510001014A CN104611124B CN 104611124 B CN104611124 B CN 104611124B CN 201510001014 A CN201510001014 A CN 201510001014A CN 104611124 B CN104611124 B CN 104611124B
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- purple perilla
- perilla seed
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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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
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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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention proposes a kind of by squeezing and supercritical CO2The method that abstraction technique is combined extraction Purple Perilla Seed Oil, this method is that purple perilla seed first is carried out into cold pressing, obtains Purple Perilla Seed Oil and the purple perilla seed dregs of rice, controls oil content in the purple perilla seed dregs of rice, then mixed after the purple perilla seed dregs of rice are crushed with filler and pass through supercritical CO2Abstraction technique further extracts remaining oil in the purple perilla seed dregs of rice, and the recovery rate of gained Purple Perilla Seed Oil is 90.9 98.3%.Pre-treatment expressing process of the present invention can solve the problems, such as solid accumulation caking in extraction process, produce channel, so as to improve the recovery rate of oil, suitable for industrialization, the production of scale.
Description
Technical field
The present invention relates to a kind of method that purple perilla seed carries oil, more particularly to a kind of squeezing and supercritical CO2Extraction extraction is purple
The method of perilla oil.
Background technology
Purple Perilla Seed Oil, obtained by the mature seed of medicinal plant purple perilla, be a kind of natural oil of high degree of unsaturation, mainly
Composition is alpha-linolenic acid, and its content is close to 50%.Purple Perilla Seed Oil have liver protection, antithrombotic, reducing blood lipid, hypotensive, protection eyesight, carry
The effect of high intelligence, anti-aging, and have inhibitory action to allergic reaction and inflammation.
The method of industrial extraction Purple Perilla Seed Oil is mainly physical squeezing method and organic solvent extractionprocess.Physical squeezing method is
Oil is separated from raw material by mechanical pressure, and with physical method by a kind of method of oil refining, but this method oil yield
It is relatively low；Organic solvent extractionprocess utilizes similar compatibility principle, with organic solvents such as petroleum ether, methanol, ether by purple perilla seed
Oil extract comes out.Determination of Residual Organic Solvents height, harm to the human body are big in the oil that the usual method is produced, and extraction time length,
Post-process cumbersome.
Supercritical CO is used in patent CN951093792Abstraction technique carries out carrying oil to purple perilla seed, has groped technological parameter.
The technique is by supercritical CO2Contacted with material, extraction oil, then supercritical fluid is become common gases by depressurizing, cooling,
And make oily precipitation, so as to reach the purpose of separating-purifying.Supercritical CO2Abstraction technique, organic solvent extractionprocess can be overcome
Shortcoming, organic solvent-free residual, nontoxic, extraction time is short, and extract is best in quality, and can at utmost keep having for raw material
The advantages that imitating composition.The technique for the single use supercritical extract Purple Perilla Seed Oil reported at present is simpler, and laboratory is feasible, but also
Can not meet the needs of industrialization, large-scale production, reason is as follows：
1. different with the technique in laboratory, industrialization, the implementation of scale will focus on economic benefit, reduce into as far as possible
This simultaneously generates profit maximization, therefore its recovery rate should reach more than 90%, use single milling process or supercritical CO2
Extraction is extremely difficult to, or cost is higher.
2. purple perilla seed oil content is generally 47-50%, because oil content is high, crush in supercritical CO2Easily accumulated in equipment
Caking, is unfavorable for extracting.In conventional supercritical CO2Extract the related report that purple perilla seed pre-treatment is had no in the patent of Purple Perilla Seed Oil
Road.
3. scale is amplified, there is enlarge-effect, material is more, easier accumulation caking, produces channel, is unfavorable for super face
Boundary extracts.Large-scale production is not considered in conventional patent and research, does not also refer to solving the effective means of channel.
The content of the invention
The purpose of the present invention is by squeezing and supercritical CO2Abstraction technique is combined, and acquisition recovery rate is 90.9-98.3%
Purple Perilla Seed Oil.Pre-treatment expressing process can solve the problems, such as solid accumulation caking in extraction process, produce channel, so as to improve
The recovery rate of Purple Perilla Seed Oil.
The technical scheme is that first squeezed purple perilla seed, Purple Perilla Seed Oil and the purple perilla seed dregs of rice are obtained, then by purple perilla
The seed dregs of rice are crushed, and are then mixed with filler, finally with supercritical CO2Abstraction technique enters remaining oil in the purple perilla seed dregs of rice
Onestep extraction comes out.
Comprise the following steps：
1. purple perilla seed is squeezed, pressing temperature is controlled at 30-50 DEG C, and squeezing draws Purple Perilla Seed Oil and the purple perilla seed dregs of rice；
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 10-40 mesh, obtains purple perilla seed dregs of rice powder；
3. taking purple perilla seed dregs of rice powder to be mixed with uniform filling, it is put into extraction kettle material barrel, the body of purple perilla seed dregs of rice powder and filler
Product is than being 1:1-1:2.5, material barrel is put into supercritical CO2In the extraction kettle of equipment, the Stress control of extraction kettle is in 15-
28MPa, temperature control is at 35-45 DEG C；
4. Purple Perilla Seed Oil is with CO2Fluid enters separating still by pipeline, and the temperature control of separating still is divided at 40-50 DEG C
From 150min；Through above-mentioned squeezing, crushing, supercritical CO2Extraction, isolated Purple Perilla Seed Oil.
1. middle purple perilla seed squeezing oil yield be 20-35% to step, and oil content is controlled in 15-30% in the purple perilla seed dregs of rice.
Supercritical CO2The separating pressure of extraction is 7-9MPa.
Supercritical CO2The extraction yield of extraction is 83.3-94.7%.
Purple perilla seed is through squeezing and supercritical CO2After extraction carries oil, purple perilla seed oil-containing recovery rate is 90.9-98.3%.
CS-E-3, CS-E-5, CS-E-8 or CS-E-10.
Effect of the invention is that：
1. the present invention proposes a kind of squeezing and supercritical CO2The method for the extraction Purple Perilla Seed Oil that abstraction technique is combined.
2. pre-treatment squeezing puies forward oily process and solves purple perilla seed because of the high directly crushing extraction of oil content easily accumulation caking, generation
Channel is unfavorable for the problem of extraction.
3. the purple perilla seed dregs of rice oil content by squeezing is effectively controlled, make in production process shared by supercritical extract process
Time is greatly shortened, and overall oily cost is put forward so as to reduce.
4. the relatively single milling process of this method or single CO2Supercritical extraction has high oil extract rate, can
Industrialization, scale are implemented.
Embodiment
Embodiment 1
The oil extracting methods of purple perilla seed are:
1. purple perilla seed under the conditions of 30 DEG C, squeezes out 20% Purple Perilla Seed Oil, and obtains the purple perilla seed dregs of rice, contain in the purple perilla seed dregs of rice
Fuel-flow control is for 30%.
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 10 mesh, obtains purple perilla seed dregs of rice powder；
It is put into 3. 300g purple perilla seed dregs of rice powder is mixed with uniform filling in material barrel, the volume ratio of purple perilla seed dregs of rice powder and filler
For 1:1, filler selects the CS-E-3 of stainless steel, and material barrel is put into supercritical CO2In the extraction kettle of equipment, extraction is opened
Kettle intake valve, with booster pump by CO2Continual to squeeze into extraction kettle, the temperature of extraction kettle is 35 DEG C, pressure 15MPa, is made
Purple Perilla Seed Oil is dissolved in supercritical CO2In fluid, there is Purple Perilla Seed Oil to be extracted out after 10min；
4. opening separator intake valve, Purple Perilla Seed Oil is with CO2Separating still is entered by pipeline, by the temperature control of separating still
System pressure 7MPa, makes CO at 40 DEG C2Separated with Purple Perilla Seed Oil, obtain 75g Purple Perilla Seed Oil after 150min in the separator,
The extraction yield of Purple Perilla Seed Oil is 83.3%.
Purple perilla seed is through squeezing, crushing, supercritical CO2After extraction, separation, oily recovery rate is 90.9%.
Embodiment 2
The oil extracting methods of purple perilla seed are:
1. purple perilla seed squeezes out 25% Purple Perilla Seed Oil under the conditions of 40 DEG C, and obtains the purple perilla seed dregs of rice, contain in the purple perilla seed dregs of rice
Fuel-flow control is 25%.
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 20 mesh, obtains purple perilla seed dregs of rice powder；
It is put into 3. 300g purple perilla seed dregs of rice powder is mixed with uniform filling in material barrel, material barrel is put into supercritical CO2If
In standby extraction kettle, the volume ratio of purple perilla seed dregs of rice powder and filler is 1:1.5, filler selects the CS-E-8 of stainless steel, opens
Extraction kettle intake valve, with booster pump by CO2Continual to squeeze into extraction kettle, the temperature of extraction kettle is 40 DEG C, and pressure is
23MPa, Purple Perilla Seed Oil is set to be dissolved in supercritical CO2In fluid, there is Purple Perilla Seed Oil to be extracted out after 10min；
4. opening separator intake valve, Purple Perilla Seed Oil is with CO2Separating still is entered by pipeline, by the temperature control of separating still
System pressure 8MPa, makes CO at 45 DEG C2Separated with Purple Perilla Seed Oil, obtain 62.8g purple perilla seed after 150min in the separator
Oil, the extraction yield of Purple Perilla Seed Oil is 83.7%.
Purple perilla seed is through squeezing, crush, SCF-CO 2, after separation, oily recovery rate is 93%.
Embodiment 3
The oil extracting methods of purple perilla seed are:
1. purple perilla seed after 45 DEG C of mechanical low-temperature cold rollings, squeezes out 30% Purple Perilla Seed Oil, and obtains the purple perilla seed dregs of rice, purple
Oil content control is 20% in the Perillaseed dregs of rice.
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 20 mesh, obtains purple perilla seed dregs of rice powder；
It is put into 3. 300g purple perilla seed dregs of rice powder is mixed with uniform filling in material barrel, the volume ratio of purple perilla seed dregs of rice powder and filler
For 1:2, filler CS-E-10, material barrel is put into supercritical CO2In the extraction kettle of equipment, extraction kettle intake valve is opened, with increasing
Press pump is by CO2Continual to squeeze into extraction kettle, the temperature of extraction kettle is 45 DEG C, pressure 25MPa, is dissolved in Purple Perilla Seed Oil
Supercritical CO2In fluid, there is Purple Perilla Seed Oil to be extracted out after 10min；
4. opening separator intake valve, Purple Perilla Seed Oil is with CO2Separating still is entered by pipeline, by the temperature control of separating still
System pressure 9MPa, makes CO at 50 DEG C2Separated with Purple Perilla Seed Oil, obtain 52.5g purple perilla seed after 150min in the separator
Oil, the extraction yield of Purple Perilla Seed Oil is 87.5%.
Purple perilla seed is through squeezing, crush, SCF-CO 2, after separation, oily recovery rate is 96%.
Most preferred embodiment：
The oil extracting methods of purple perilla seed are:
1. purple perilla seed after 50 DEG C of mechanical low-temperature cold rollings, squeezes out 30% Purple Perilla Seed Oil, and obtains the purple perilla seed dregs of rice, purple
Oil content control is 20% in the Perillaseed dregs of rice.
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 40 mesh, obtains purple perilla seed dregs of rice powder；
It is put into 3. 300g purple perilla seed dregs of rice powder is mixed with uniform filling in material barrel, the volume ratio of purple perilla seed dregs of rice powder and filler
For 1:2.5, filler selects CS-E-8, and material barrel is put into supercritical CO2In the extraction kettle of equipment, extraction kettle intake valve is opened,
With booster pump by CO2Continual to squeeze into extraction kettle, the temperature of extraction kettle is 45 DEG C, pressure 28MPa, makes Purple Perilla Seed Oil molten
Solution is in supercritical CO2In fluid, there is Purple Perilla Seed Oil to be extracted out after 10min；
4. opening separator intake valve, Purple Perilla Seed Oil is with CO2Separating still is entered by pipeline, by the temperature control of separating still
System pressure 9MPa, makes CO at 50 DEG C2Separated with Purple Perilla Seed Oil, obtain 56.8g purple perilla seed after 150min in the separator
Oil, the extraction yield of Purple Perilla Seed Oil is 95%.
Purple perilla seed is through squeezing, crushing, supercritical CO2After extraction, separation, oily recovery rate is 98.3%.
Claims (3)
1. purple perilla seed is through squeezing and supercritical CO2The method that extraction carries oil, comprises the following steps：
1. purple perilla seed is squeezed, pressing temperature is controlled at 30-50 DEG C, and squeezing draws Purple Perilla Seed Oil and the purple perilla seed dregs of rice；Purple perilla
Seed squeezing oil yield be 20-35%, and oil content is controlled in 15-30% in the purple perilla seed dregs of rice；
2. being crushed the purple perilla seed dregs of rice with pulverizer, smashing fineness is 10-40 mesh, obtains purple perilla seed dregs of rice powder；
3. taking purple perilla seed dregs of rice powder to be mixed with uniform filling, it is put into extraction kettle material barrel, the volume ratio of purple perilla seed dregs of rice powder and filler
For 1:1-1:2.5, material barrel is put into supercritical CO2In the extraction kettle of equipment, the Stress control of extraction kettle is in 15-28MPa, temperature
Degree control is at 35-45 DEG C；Filler material is stainless steel, and filler specification is：CS-E-3, CS-E-5, CS-E-8 or CS-E-10；
4. Purple Perilla Seed Oil is with CO2Fluid enters separating still by pipeline, and the temperature control of separating still is at 40-50 DEG C, separation
150min；Through above-mentioned squeezing, crushing, supercritical CO2Extraction, isolated Purple Perilla Seed Oil；Supercritical CO2The separating pressure of extraction
For 7-9MPa.
2. purple perilla seed according to claim 1 is through squeezing and supercritical CO2The method that extraction carries oil, it is characterised in that：It is super to face
Boundary CO2The extraction yield of extraction is 83.3-94.7%.
3. purple perilla seed according to claim 1 is through squeezing and supercritical CO2The method that extraction carries oil, it is characterised in that：Purple perilla
Seed is through squeezing and supercritical CO2After extraction carries oil, purple perilla seed oil-containing recovery rate is 90.9-98.3%.
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| CN106957717A (en) * | 2016-01-11 | 2017-07-18 | 徐蕴山 | A kind of meter of dregs of rice supercritical extract method for producing oil and its rice dregs of rice of manufacture oil and the degreasing rice dregs of rice |
| CN106858083A (en) * | 2017-02-23 | 2017-06-20 | 西南大学 | A kind of feed for improving milk production of cow and coffin hardness and preparation method thereof |
| CN109010577A (en) * | 2017-06-09 | 2018-12-18 | 邹玮 | A kind of hippophae rhamnoides compositions and preparation method thereof of anticoagulation platelet aggregation-against antithrombotic |
| CN109735404B (en) * | 2019-01-11 | 2021-05-28 | 澳宝化妆品（惠州）有限公司 | Solid washing composition containing perilla seed extract and preparation method thereof |
| CN111518613A (en) * | 2020-04-29 | 2020-08-11 | 幺麻子食品股份有限公司 | Blending production process of zanthoxylum oil |
| CN112760164A (en) * | 2020-12-29 | 2021-05-07 | 黑龙江珍爱生物科技有限公司 | Extraction method for effectively removing residual oil in perilla meal |
| CN117603758A (en) * | 2023-11-23 | 2024-02-27 | 哈尔滨工业大学 | Cold pressing-supercritical combined extraction elytrigia repens kernel oil and preparation method and application thereof |
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| WO2008020865A1 (en) * | 2006-08-18 | 2008-02-21 | Semo Milling, Llc | Power production using grain fractionation products |
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| CN1208758A (en) * | 1998-07-02 | 1999-02-24 | 湖北李时珍保健油总公司 | Purple perilla oil and method for preparing same |
| CN101338246A (en) * | 2008-08-08 | 2009-01-07 | 铁岭三能科技有限公司 | Process for preparing hazelnut oil |
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