CN113881494A - Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology - Google Patents

Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology Download PDF

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CN113881494A
CN113881494A CN202111320279.8A CN202111320279A CN113881494A CN 113881494 A CN113881494 A CN 113881494A CN 202111320279 A CN202111320279 A CN 202111320279A CN 113881494 A CN113881494 A CN 113881494A
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extraction
rapeseed
kettle
pressure
rapeseeds
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Inventor
杨再文
冉义斌
罗晓琴
余鹏
刘杰
杨易
周孝红
赵娅
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Guizhou Huiteng Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/108Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/008Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Fats And Perfumes (AREA)

Abstract

The scheme discloses a method for producing strong aromatic rapeseed oil by a supercritical fluid extraction technology in the field of rapeseed oil processing, which comprises the following steps: the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, and putting the screened rapeseeds into a baking and frying machine, wherein the frying temperature is 100-200 ℃, the frying time is 1-3 h, and the rotating speed is 14-28 r/min; step two: crushing rapeseeds to obtain rapeseed powder; placing the mixture into a supercritical extraction kettle, setting the extraction temperature to be 15-40 ℃, starting a pressure pump to enable the extraction pressure to be 20-50 MPa, setting the pressure value of a separation kettle I and the separation kettle II to be 6-15 MPa, setting the separation temperature to be 20-55 ℃, and carrying out static extraction for 120-300 min to obtain extracted crude oil and slag; step three: extracting the crude oil to a separation kettle I and a separation kettle II to obtain rapeseed crude oil; step four: closing the pressurizing pump; step five: standing the rapeseed crude oil for 24-28 h to obtain the strong-flavor rapeseed oil. The method in the scheme can obtain the high-quality fragrant rapeseed oil.

Description

Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology
Technical Field
The invention relates to the field of rapeseed oil processing, in particular to a method for producing strong-flavor rapeseed oil by a supercritical fluid extraction technology.
Background
Rapeseed oil plays an important role in edible vegetable oil of residents in China, not only wins nutritionists and consumers with excellent edible quality, but also is popular with growers due to the status, effect and benefit in crop rotation.
The extraction method commonly used by the rapeseed oil at present comprises a solvent extraction method, an ultrasonic extraction method, a microwave extraction method, an enzyme extraction method and the like. Although the extraction method such as solvent extraction method has high extraction rate, it has inevitable defects that solvent remains, and in the case of heat-sensitive food, heating may cause qualitative changes of some unsaturated fatty acids, such as DHA, ARA and other chemical substances. Along with the improvement of living standard, people have higher and higher requirements on the nutritional quality, sensory quality and freshness of the rapeseed oil, and the rapeseed oil obtained by solvent leaching is difficult to meet the requirements, so that a low-temperature organic solvent-free extraction technology is gradually valued by people. At present, the low-temperature and solvent residue-free high-new extraction separation technology mainly comprises a supercritical extraction fluid technology, an aqueous enzymatic technology, a superfine grinding technology, a molecular distillation technology and the like.
The principle of the supercritical carbon dioxide extraction separation process is that the supercritical carbon dioxide has a special dissolving effect on certain special natural products, and the relation between the dissolving capacity and the density of the supercritical carbon dioxide, namely the influence of pressure and temperature on the dissolving capacity of the supercritical carbon dioxide is utilized to carry out the supercritical carbon dioxide extraction separation process. The supercritical carbon dioxide is contacted with the substance to be separated, so that the components with different polarity, boiling point and molecular weight are selectively extracted in turn.
Disclosure of Invention
The invention aims to provide a method for producing strong-flavor rapeseed oil by a supercritical fluid extraction technology, and provides a method for extracting the rapeseed oil by supercritical carbon dioxide, which has the advantages of low treatment temperature, no solvent residue, no pollution, less nutrient loss and the like.
The method for producing the strong aromatic rapeseed oil by the supercritical fluid extraction technology comprises the following steps:
the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, and putting the screened rapeseeds into a baking and frying machine, wherein the frying temperature is 100-200 ℃, the frying time is 1-3 h, and the rotating speed is 14-28 r/min;
step two: crushing the fried rapeseeds to obtain rapeseed powder; placing rapeseed powder into a supercritical extraction kettle, setting the supercritical extraction kettle on a computer, setting the extraction temperature to be 15-40 ℃, starting a pressure pump to enable the extraction pressure to be 20-50 MPa, setting the pressure value of a separation kettle I and the separation kettle II to be 6-15 MPa and the separation temperature to be 20-55 ℃ for standby, and then carrying out static extraction for 120-300 min to obtain extracted crude oil and slag;
step three: extracting crude oil to a separation kettle I and a separation kettle II, and collecting the extracted crude oil in the separation kettle I and the separation kettle II separately every 30min to obtain rapeseed crude oil;
step four: after the pressure maintaining time is over, closing the pressure pump and the supercritical carbon dioxide inlet valve to enable the reading of a pressure gauge in the extraction kettle to be 0;
step five: standing the rapeseed crude oil for 24-28 h, filtering and removing large particle impurities of the rapeseed crude oil by using plate and frame equipment to obtain the strong-flavor rapeseed oil.
The beneficial effect of this scheme: the rapeseed is fried by adopting a frying machine, so that the problems of coking and gelatinization of the rapeseed and the condition of time and labor waste in operation are solved, the quality of the product is ensured, and the production cost is reduced; the advantages of supercritical carbon dioxide extraction are mainly as follows: 1) critical temperature and critical pressure (Tc is 31.1 ℃, Pc is 7.38MPa), the operation condition is mild, and the damage to the effective components is less; 2) carbon dioxide can be considered a non-toxic, inexpensive solvent similar to water; 3) the carbon dioxide is stable, non-toxic, non-combustible, safe and environment-friendly in the using process, and can avoid the oxidation of products; 4) the carbon dioxide does not contain nitrate and harmful heavy metals in the extract, and has no residue of harmful solvent; 5) during supercritical carbon dioxide extraction, the extracted substances can be separated out by reducing the pressure or increasing the temperature without repeated extraction operation, so that the process of multiple times of extraction is reduced, and the steps are simplified; the two are combined with each other to obtain the rapeseed oil with low treatment temperature, no solvent residue, no pollution and less nutrient loss.
Further, the crushed grain size of the rapeseeds crushed in the step two is 20-40 meshes.
Further, the initial frequency of the pressure pump in the second step is 10-15 Hz, and the pressure is artificially and slowly increased during the pressurization, so that the pressure is finally up to 20-50 MPa.
Further, in the pressure relief process in the fourth step, the pressure relief is artificially and slowly carried out. If the pressure is directly released, the rape seed powder can easily run into the separation kettle along with the supercritical carbon dioxide penetrating through the plug net, so that the pipeline pollution is caused.
Further, in the pressure relief process in the fourth step, the pressure relief speed in the extraction kettle is 0.001-0.10 MPa/s.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
example 1: a method for producing strong aromatic rapeseed oil by a supercritical fluid extraction technology comprises the following specific operation steps:
the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, putting the screened rapeseeds into a drying and frying machine with a production model of ziboshunda 200, wherein the frying temperature is 150 ℃, the frying time is 2h, and the rotating speed is 21 r/min;
step two: crushing the fried rapeseeds with the granularity of 30 meshes to obtain rapeseed powder; placing rapeseed powder into a supercritical extraction kettle, setting the frequency of an initial pressure pump on a computer to be 12Hz and the extraction temperature to be 25 ℃, starting the pressure pump, setting the pressure values of a separation kettle I and a separation kettle II to be 10MPa and the separation temperature to be 32 ℃ for standby during the period, performing static extraction for 210min, and artificially and slowly increasing the pressure during pressurization to ensure that the extraction pressure is 30MPa to obtain extracted crude oil and slag;
step three: extracting crude oil to a separation kettle I and a separation kettle II, and collecting the extracted crude oil in the separation kettle I and the separation kettle II separately every 30min to obtain rapeseed crude oil;
step four: after the pressure maintaining time is over, closing the pressure pump and the supercritical carbon dioxide inlet valve, taking the pressure relief speed in the kettle to be 0.005MPa/s, and allowing the reading of a pressure gauge in the extraction kettle to be 0;
step five: standing the crude rapeseed oil for 26 hours, and filtering and removing large-particle impurities of the crude rapeseed oil by using plate-and-frame equipment to obtain the strong-flavor rapeseed oil.
Example 2: a method for producing strong aromatic rapeseed oil by a supercritical fluid extraction technology comprises the following specific operation steps:
the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, putting the screened rapeseeds into a drying and frying machine with a production model of ziboshunda 200, wherein the frying temperature is 100 ℃, the frying time is 1h, and the rotating speed is 14 r/min;
step two: crushing the fried rapeseeds, wherein the crushing particle size is 20 meshes, so as to obtain rapeseed powder; placing rapeseed powder into a supercritical extraction kettle, setting the frequency of an initial pressure pump on a computer to be 10Hz and the extraction temperature to be 15 ℃, starting the pressure pump, setting the pressure values of a separation kettle I and a separation kettle II to be 8MPa and the separation temperature to be 20 ℃ for standby during the period, performing static extraction for 120min, and artificially and slowly increasing the pressure during pressurization to ensure that the extraction pressure is 20MPa to obtain extracted crude oil and slag;
step three: extracting crude oil to a separation kettle I and a separation kettle II, and collecting the extracted crude oil in the separation kettle I and the separation kettle II separately every 30min to obtain rapeseed crude oil;
step four: after the pressure maintaining time is over, closing the pressure pump and the supercritical carbon dioxide inlet valve, and ensuring the pressure relief speed in the extraction kettle to be 0.001MPa/s and the reading of a pressure gauge in the extraction kettle to be 0;
step five: standing the rapeseed crude oil for 24 hours, and filtering and removing large-particle impurities of the rapeseed crude oil by using plate-and-frame equipment to obtain the strong-flavor rapeseed oil.
Example 3: a method for producing strong aromatic rapeseed oil by a supercritical fluid extraction technology comprises the following specific operation steps:
the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, putting the screened rapeseeds into a drying and frying machine with a catastrogen production model number of 200, wherein the frying temperature is 200 ℃, the frying time is 3h, and the rotating speed is 28 r/min;
step two: crushing the fried rapeseeds, wherein the crushing particle size is 40 meshes, so as to obtain rapeseed powder; placing rapeseed powder into a supercritical extraction kettle, setting the frequency of an initial pressure pump on a computer to be 15Hz and the extraction temperature to be 40 ℃, starting the pressure pump, setting the pressure values of a separation kettle I and a separation kettle II to be 15MPa and the separation temperature to be 55 ℃ for standby during the period, performing static extraction for 300min, and artificially and slowly increasing the pressure during pressurization to ensure that the extraction pressure is 50MPa, so as to obtain extracted crude oil and slag;
step three: extracting crude oil to a separation kettle I and a separation kettle II, and collecting the extracted crude oil in the separation kettle I and the separation kettle II separately every 30min to obtain rapeseed crude oil;
step four: after the pressure maintaining time is over, closing the pressure pump and the supercritical carbon dioxide inlet valve, and ensuring the pressure relief speed in the extraction kettle to be 0.10MPa/s and the reading of a pressure gauge in the extraction kettle to be 0;
step five: standing the rapeseed crude oil for 28h, filtering and removing large-particle impurities by using plate-and-frame equipment to obtain the strong-flavor rapeseed oil.
Comparative example: selecting rapeseeds, adopting No. six light gasoline solvent naphtha to fully soak a grease raw material, then extracting at high temperature, and processing by a 'six-threshing' process to obtain the rapeseeds.
The quality indexes of the oil products obtained by extraction in example 1, example 2 and example 3, such as sensory, nutrient and heavy metal, are tested.
1. Experimental materials: strong-flavor rapeseed oil obtained in example 1, example 2 and example 3.
2. The experimental method comprises the following steps: and detecting according to the corresponding national standard of the people's republic of China.
And detecting the sensory and fatty acid compositions of the extracts in the separation kettle I and the separation kettle II to obtain the following data:
Figure BDA0003345343670000041
Figure BDA0003345343670000051
and (4) conclusion: the comparison shows that the data of the examples 1, 2 and 3 are superior to those of the comparative example, the comparative example also contains No. six light gasoline solvent naphtha residues, the crude oil prepared by leaching contains more non-fat components, has dark color and poor quality, and the rapeseed oil obtained by the examples has five solvent residues, no pollution and less nutrient loss.

Claims (5)

1. A method for producing strong aromatic rapeseed oil by a supercritical fluid extraction technology is characterized by comprising the following steps:
the method comprises the following steps: preparing rapeseeds, screening the rapeseeds, and putting the screened rapeseeds into a baking and frying machine, wherein the frying temperature is 100-200 ℃, the frying time is 1-3 h, and the rotating speed is 14-28 r/min;
step two: crushing the fried rapeseeds to obtain rapeseed powder; placing rapeseed powder into a supercritical extraction kettle, setting the supercritical extraction kettle on a computer, setting the extraction temperature to be 15-40 ℃, starting a pressure pump to enable the extraction pressure to be 20-50 MPa, setting the pressure value of a separation kettle I and the separation kettle II to be 6-15 MPa and the separation temperature to be 20-55 ℃ for standby, and then carrying out static extraction for 120-300 min to obtain extracted crude oil and slag;
step three: extracting crude oil to a separation kettle I and a separation kettle II, and collecting the extracted crude oil in the separation kettle I and the separation kettle II separately every 30min to obtain rapeseed crude oil;
step four: after the pressure maintaining time is over, closing the pressure pump and the supercritical carbon dioxide inlet valve to enable the reading of a pressure gauge in the extraction kettle to be 0;
step five: standing the rapeseed crude oil for 24-28 h, filtering and removing large particle impurities of the rapeseed crude oil by using plate and frame equipment to obtain the strong-flavor rapeseed oil.
2. The method for producing highly aromatic rapeseed oil by using the supercritical fluid extraction technology according to claim 1, wherein the method comprises the following steps: and the crushed grain size of the rapeseeds crushed in the second step is 20-40 meshes.
3. The method for producing highly aromatic rapeseed oil by using the supercritical fluid extraction technology according to claim 2, characterized in that: and the initial frequency of the pressure pump in the second step is 10-15 Hz, and the pressure is artificially and slowly increased during pressurization to finally reach 20-50 MPa.
4. The method for producing highly aromatic rapeseed oil by using the supercritical fluid extraction technology according to claim 3, wherein the method comprises the following steps: in the pressure relief process in the fourth step, the pressure relief is artificially and slowly carried out.
5. The method for producing highly aromatic rapeseed oil by using the supercritical fluid extraction technology according to claim 4, wherein the method comprises the following steps: in the pressure relief process of the fourth step, the pressure relief speed in the extraction kettle is 0.001-0.10 MPa/s.
CN202111320279.8A 2021-11-09 2021-11-09 Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology Pending CN113881494A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070002911A (en) * 2005-06-30 2007-01-05 주식회사 유맥스 Edible oil containing high content of tocopherol produced by using super critical fluid and process for production thereof
CN107927199A (en) * 2017-11-08 2018-04-20 广东金妮宝科技发展有限公司 Low acid number vegetable seed ready-mixed oil of a kind of high oleic acid and preparation method thereof
CN109536273A (en) * 2018-10-12 2019-03-29 贵州航天乌江机电设备有限责任公司 The technique of fatty acid substance in a kind of supercritical fluid extraction sesame
CN111019755A (en) * 2019-12-11 2020-04-17 甘肃金浩生物科技有限公司 Flaxseed oil CO2Supercritical extraction separation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070002911A (en) * 2005-06-30 2007-01-05 주식회사 유맥스 Edible oil containing high content of tocopherol produced by using super critical fluid and process for production thereof
CN107927199A (en) * 2017-11-08 2018-04-20 广东金妮宝科技发展有限公司 Low acid number vegetable seed ready-mixed oil of a kind of high oleic acid and preparation method thereof
CN109536273A (en) * 2018-10-12 2019-03-29 贵州航天乌江机电设备有限责任公司 The technique of fatty acid substance in a kind of supercritical fluid extraction sesame
CN111019755A (en) * 2019-12-11 2020-04-17 甘肃金浩生物科技有限公司 Flaxseed oil CO2Supercritical extraction separation method

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