CN104611124A - Method for extracting oil from perilla seeds by squeezing and supercritical CO2 extraction technology - Google Patents
Method for extracting oil from perilla seeds by squeezing and supercritical CO2 extraction technology Download PDFInfo
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- CN104611124A CN104611124A CN201510001014.XA CN201510001014A CN104611124A CN 104611124 A CN104611124 A CN 104611124A CN 201510001014 A CN201510001014 A CN 201510001014A CN 104611124 A CN104611124 A CN 104611124A
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- perilla seed
- extraction
- oil
- supercritical
- squeezing
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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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
-
- 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
Abstract
The invention provides a method for extracting oil from perilla seeds by a combined squeezing and supercritical CO2 extraction technology. According to the method, firstly, performing low-temperature squeezing on perilla seeds to obtain perilla seed oil and perilla seed meals, and controlling the oil content in the seed meals; secondly, pulverizing the seed meals, and mixing the pulverized seed meals with a filler; thirdly, further extracting residuary oil from the seed meals through a supercritical CO2 extraction technology, wherein the extraction rate of the perilla seed oil is 90.9-98.3%. In the method, the pretreatment squeezing process can solve the problems that materials are accumulated and caked and channeling is generated, so that the extraction rate of the oil is increased, and the method is suitable for industrial and large-scale production.
Description
Technical field
The present invention relates to a kind of method that perilla seed carries oil, particularly one squeezing and supercritical CO
2the method of Purple Perilla Seed Oil is extracted in extraction.
Background technology
Purple Perilla Seed Oil, is obtained by the mature seed of medicinal plant purple perilla, and be a kind of natural fats and oils of high degree of unsaturation, major ingredient is alpha-linolenic acid, and its content is close to 50%.Purple Perilla Seed Oil protects the liver, antithrombotic, reducing blood-fat, hypotensive, vision protection, raising intelligence, antidotal effect, and have restraining effect to anaphylaxis and inflammation.
Method mainly physical squeezing method and the organic solvent extractionprocess of industrial extraction Purple Perilla Seed Oil.Physical squeezing method is separated from raw material by oil by mechanical pressure, and by a kind of method of physical method by oil refining, but this method oil yield is lower; Organic solvent extractionprocess utilizes similar dissolve mutually theory, is extracted by the oil in perilla seed with organic solvents such as sherwood oil, methyl alcohol, ether.In the oil that this method usual is produced, Determination of Residual Organic Solvents is high, large to harm, and extraction time is long, aftertreatment is loaded down with trivial details.
Supercritical CO is adopted in patent CN95109379
2abstraction technique carries oil to perilla seed, has groped processing parameter.This technique is by supercritical CO
2contact with material, extraction oil, then make supercutical fluid become common gases by decompression, cooling, and oil separated out, thus reach the object of separating-purifying.Supercritical CO
2abstraction technique, can overcome the shortcoming of organic solvent extractionprocess, and organic solvent-free remains, and nontoxic, extraction time is short, and extract is best in quality, and at utmost can keep the advantages such as raw-material effective constituent.The technique of the single use supercritical extraction Purple Perilla Seed Oil of current report is comparatively simple, and laboratory is feasible, but can't meet the demand of industrialization, large-scale production, and reason is as follows:
1. the technique with laboratory is different, and the enforcement of industrialization, mass-producing will focus on economic benefit, and reduce costs as far as possible and generate profit maximization, therefore its extraction yield should reach more than 90%, uses single milling process or supercritical CO
2extraction process is difficult to reach, or cost is higher.
2. perilla seed oleaginousness is generally 47-50%, because oleaginousness is high, pulverizes at supercritical CO
2easily pile up caking in equipment, be unfavorable for extraction.At supercritical CO in the past
2the relevant report of perilla seed pre-treatment is had no in the patent of extraction Purple Perilla Seed Oil.
3. when mass-producing is amplified, have scale effect, material is more, more easily piles up caking, produces channel, is unfavorable for supercritical extraction.Do not consider large-scale production in patent in the past and research, do not mention the effective means solving channel yet.
Summary of the invention
The object of the invention is squeezing and supercritical CO
2abstraction technique combines, and obtaining extraction yield is the Purple Perilla Seed Oil of 90.9-98.3%.Pre-treatment expressing process can solve solid accumulation caking in extraction process, produce the problem of channel, thus improves the extraction yield of Purple Perilla Seed Oil.
Technical scheme of the present invention is first squeezed by perilla seed, obtains Purple Perilla Seed Oil and the perilla seed dregs of rice, then pulverized by the perilla seed dregs of rice, then mix with filler, finally use supercritical CO
2oil remaining in the perilla seed dregs of rice extracts by abstraction technique further.
Comprise the following steps:
1. squeezed by perilla seed, pressing temperature controls at 30-50 DEG C, and squeezing draws Purple Perilla Seed Oil and the perilla seed dregs of rice;
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 10-40 order, obtains perilla seed dregs of rice powder;
3. get perilla seed dregs of rice powder to mix with uniform filling, put into extraction kettle material barrel, the volume ratio of perilla seed dregs of rice powder and filler is 1:1-1:2.5, and material barrel is put into supercritical CO
2in the extraction kettle of equipment, the pressure-controlling of extraction kettle is at 15-28MPa, and temperature controls at 35-45 DEG C;
4. Purple Perilla Seed Oil is with CO
2fluid enters into separating still by pipeline, and the temperature of separating still controls at 40-50 DEG C, is separated 150min; Through above-mentioned squeezing, pulverizing, supercritical CO
2extraction, separation obtain Purple Perilla Seed Oil.
Step 1. middle perilla seed squeezing oil yield is 20-35%, and in the perilla seed dregs of rice, oleaginousness controls at 15-30%.
Supercritical CO
2the separating pressure of extraction is 7-9MPa.
Supercritical CO
2the percentage extraction of extraction is 83.3-94.7%.
Perilla seed is through squeezing and supercritical CO
2after oil is carried in extraction, perilla seed oil-containing extraction yield is 90.9-98.3%.
CS-E-3, CS-E-5, CS-E-8 or CS-E-10.
Effect of the present invention is:
1. the present invention proposes a kind of squeezing and supercritical CO
2the method of the extraction Purple Perilla Seed Oil that abstraction technique combines.
2. pre-treatment squeezing is put forward oily process and is solved perilla seed and directly pulverize extraction because oleaginousness is high and easily pile up caking, produce the problem that channel is unfavorable for extraction.
3. the perilla seed dregs of rice oleaginousness through squeezing is effectively controlled, and the time shared by supercritical extraction operation in production process is shortened greatly, thus reduces and overall carry oily cost.
4. the milling process that present method is relatively single or single CO
2supercritical extraction has high oily extraction yield, can industrialization, mass-producing implement.
Embodiment
Embodiment 1
The oil extracting methods of perilla seed is:
1. perilla seed is under 30 DEG C of conditions, squeezes out the Purple Perilla Seed Oil of 20%, and obtains the perilla seed dregs of rice, and in the perilla seed dregs of rice, oleaginousness controls be 30%.
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 10 orders, obtains perilla seed dregs of rice powder;
3. mixed with uniform filling by 300g perilla seed dregs of rice powder and put into material barrel, the volume ratio of perilla seed dregs of rice powder and filler is 1:1, and the CS-E-3 of stainless steel selected by filler, and material barrel is put into supercritical CO
2in the extraction kettle of equipment, open extraction kettle intake valve, with topping-up pump by CO
2continually squeeze in extraction kettle, the temperature of extraction kettle is 35 DEG C, and pressure is 15MPa, makes Purple Perilla Seed Oil be dissolved in supercritical CO
2in fluid, Purple Perilla Seed Oil after 10min, is namely had to be extracted out;
4. open separator intake valve, Purple Perilla Seed Oil is with CO
2enter into separating still by pipeline, the temperature of separating still controlled at 40 DEG C, pressure is 7MPa, makes CO
2be separated with Purple Perilla Seed Oil, obtain the Purple Perilla Seed Oil of 75g after 150min in the separator, the percentage extraction of Purple Perilla Seed Oil is 83.3%.
Perilla seed is through squeezing, pulverizing, supercritical CO
2after extraction, separation, the extraction yield of oil is 90.9%.
Embodiment 2
The oil extracting methods of perilla seed is:
1. perilla seed squeezes out the Purple Perilla Seed Oil of 25% under 40 DEG C of conditions, and obtains the perilla seed dregs of rice, and in the perilla seed dregs of rice, oleaginousness controls 25%.
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 20 orders, obtains perilla seed dregs of rice powder;
3. 300g perilla seed dregs of rice powder is mixed with uniform filling and put into material barrel, material barrel is put into supercritical CO
2in the extraction kettle of equipment, the volume ratio of perilla seed dregs of rice powder and filler is 1:1.5, and the CS-E-8 of stainless steel selected by filler, opens extraction kettle intake valve, with topping-up pump by CO
2continually squeeze in extraction kettle, the temperature of extraction kettle is 40 DEG C, and pressure is 23MPa, makes Purple Perilla Seed Oil be dissolved in supercritical CO
2in fluid, Purple Perilla Seed Oil after 10min, is namely had to be extracted out;
4. open separator intake valve, Purple Perilla Seed Oil is with CO
2enter into separating still by pipeline, the temperature of separating still controlled at 45 DEG C, pressure is 8MPa, makes CO
2be separated with Purple Perilla Seed Oil, obtain the Purple Perilla Seed Oil of 62.8g after 150min in the separator, the percentage extraction of Purple Perilla Seed Oil is 83.7%.
Perilla seed is after squeezing, pulverizing, SCF-CO 2, separation, and the extraction yield of oil is 93%.
Embodiment 3
The oil extracting methods of perilla seed is:
1. perilla seed is after 45 DEG C of mechanical low-temperature are cold rolling, squeezes out the Purple Perilla Seed Oil of 30%, and obtains the perilla seed dregs of rice, and in the perilla seed dregs of rice, oleaginousness controls 20%.
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 20 orders, obtains perilla seed dregs of rice powder;
3. mixed with uniform filling by 300g perilla seed dregs of rice powder and put into material barrel, the volume ratio of perilla seed dregs of rice powder and filler is 1:2, and filler is CS-E-10, and material barrel is put into supercritical CO
2in the extraction kettle of equipment, open extraction kettle intake valve, with topping-up pump by CO
2continually squeeze in extraction kettle, the temperature of extraction kettle is 45 DEG C, and pressure is 25MPa, makes Purple Perilla Seed Oil be dissolved in supercritical CO
2in fluid, Purple Perilla Seed Oil after 10min, is namely had to be extracted out;
4. open separator intake valve, Purple Perilla Seed Oil is with CO
2enter into separating still by pipeline, the temperature of separating still controlled at 50 DEG C, pressure is 9MPa, makes CO
2be separated with Purple Perilla Seed Oil, obtain the Purple Perilla Seed Oil of 52.5g after 150min in the separator, the percentage extraction of Purple Perilla Seed Oil is 87.5%.
Perilla seed is after squeezing, pulverizing, SCF-CO 2, separation, and the extraction yield of oil is 96%.
Most preferred embodiment:
The oil extracting methods of perilla seed is:
1. perilla seed is after 50 DEG C of mechanical low-temperature are cold rolling, squeezes out the Purple Perilla Seed Oil of 30%, and obtains the perilla seed dregs of rice, and in the perilla seed dregs of rice, oleaginousness controls 20%.
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 40 orders, obtains perilla seed dregs of rice powder;
3. mixed with uniform filling by 300g perilla seed dregs of rice powder and put into material barrel, the volume ratio of perilla seed dregs of rice powder and filler is 1:2.5, and CS-E-8 selected by filler, and material barrel is put into supercritical CO
2in the extraction kettle of equipment, open extraction kettle intake valve, with topping-up pump by CO
2continually squeeze in extraction kettle, the temperature of extraction kettle is 45 DEG C, and pressure is 28MPa, makes Purple Perilla Seed Oil be dissolved in supercritical CO
2in fluid, Purple Perilla Seed Oil after 10min, is namely had to be extracted out;
4. open separator intake valve, Purple Perilla Seed Oil is with CO
2enter into separating still by pipeline, the temperature of separating still controlled at 50 DEG C, pressure is 9MPa, makes CO
2be separated with Purple Perilla Seed Oil, obtain the Purple Perilla Seed Oil of 56.8g after 150min in the separator, the percentage extraction of Purple Perilla Seed Oil is 95%.
Perilla seed is through squeezing, pulverizing, supercritical CO
2after extraction, separation, the extraction yield of oil is 98.3%.
Claims (6)
1. perilla seed is through squeezing and supercritical CO
2the method of oil is put forward in extraction, comprises the following steps:
1. squeezed by perilla seed, pressing temperature controls at 30-50 DEG C, and squeezing draws Purple Perilla Seed Oil and the perilla seed dregs of rice;
2. pulverized by the perilla seed dregs of rice with pulverizer, smashing fineness is 10-40 order, obtains perilla seed dregs of rice powder;
3. get perilla seed dregs of rice powder to mix with uniform filling, put into extraction kettle material barrel, the volume ratio of perilla seed dregs of rice powder and filler is 1:1-1:2.5, and material barrel is put into supercritical CO
2in the extraction kettle of equipment, the pressure-controlling of extraction kettle is at 15-28MPa, and temperature controls at 35-45 DEG C;
4. Purple Perilla Seed Oil is with CO
2fluid enters into separating still by pipeline, and the temperature of separating still controls at 40-50 DEG C, is separated 150min; Through above-mentioned squeezing, pulverizing, supercritical CO
2extraction, separation obtain Purple Perilla Seed Oil.
2. method according to claim 1, is characterized in that: step 1. middle perilla seed squeezing oil yield is 20-35%, and in the perilla seed dregs of rice, oleaginousness controls at 15-30%.
3. perilla seed according to claim 1 is through squeezing and supercritical CO
2the method of oil is put forward in extraction, it is characterized in that: supercritical CO
2the separating pressure of extraction is 7-9MPa.
4. perilla seed according to claim 1 is through squeezing and supercritical CO
2the method of oil is put forward in extraction, it is characterized in that: supercritical CO
2the percentage extraction of extraction is 83.3-94.7%.
5. perilla seed according to claim 1 is through squeezing and supercritical CO
2the method of oil is put forward in extraction, it is characterized in that: perilla seed is through squeezing and supercritical CO
2after oil is carried in extraction, perilla seed oil-containing extraction yield is 90.9-98.3%.
6. method according to claim 1, is characterized in that: filler material is stainless steel, and filler specification is: CS-E-3, CS-E-5, CS-E-8 or CS-E-10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510001014.XA CN104611124B (en) | 2015-01-05 | 2015-01-05 | Purple perilla seed is through squeezing and supercritical CO2The method that extraction carries oil |
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|---|---|---|---|
| CN201510001014.XA CN104611124B (en) | 2015-01-05 | 2015-01-05 | Purple perilla seed is through squeezing and supercritical CO2The method that extraction carries oil |
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| CN104611124B CN104611124B (en) | 2017-11-14 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN109735404A (en) * | 2019-01-11 | 2019-05-10 | 澳宝化妆品（惠州）有限公司 | A kind of solid detergent composition and preparation method thereof containing purple common perilla seed |
| 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109735404A (en) * | 2019-01-11 | 2019-05-10 | 澳宝化妆品（惠州）有限公司 | A kind of solid detergent composition and preparation method thereof containing purple common perilla seed |
| 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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