CN116590091A - Grape seed oil extraction method and extraction device - Google Patents
Grape seed oil extraction method and extraction device Download PDFInfo
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- CN116590091A CN116590091A CN202310529695.1A CN202310529695A CN116590091A CN 116590091 A CN116590091 A CN 116590091A CN 202310529695 A CN202310529695 A CN 202310529695A CN 116590091 A CN116590091 A CN 116590091A
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- 238000000605 extraction Methods 0.000 title claims abstract description 84
- 239000008169 grapeseed oil Substances 0.000 title claims abstract description 53
- 238000000926 separation method Methods 0.000 claims abstract description 84
- 235000014787 Vitis vinifera Nutrition 0.000 claims abstract description 36
- 241000219095 Vitis Species 0.000 claims abstract description 33
- 235000009754 Vitis X bourquina Nutrition 0.000 claims abstract description 33
- 235000012333 Vitis X labruscana Nutrition 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 22
- 229940087559 grape seed Drugs 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 abstract description 27
- 235000019198 oils Nutrition 0.000 abstract description 27
- 239000002253 acid Substances 0.000 abstract description 21
- 239000010779 crude oil Substances 0.000 abstract description 10
- 238000007670 refining Methods 0.000 abstract description 9
- 150000002978 peroxides Chemical class 0.000 abstract description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 abstract description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 abstract description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005642 Oleic acid Substances 0.000 abstract description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 abstract description 4
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 4
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- 238000012360 testing method Methods 0.000 description 7
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
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- 229930003268 Vitamin C Natural products 0.000 description 3
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- 239000003513 alkali Substances 0.000 description 3
- 238000009874 alkali refining Methods 0.000 description 3
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- 238000004332 deodorization Methods 0.000 description 3
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- 235000021588 free fatty acids Nutrition 0.000 description 3
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- 235000021313 oleic acid Nutrition 0.000 description 3
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- 229940046009 vitamin E Drugs 0.000 description 3
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
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- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
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- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241000931143 Gleditsia sinensis Species 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 235000021360 Myristic acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
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- QYSXJUFSXHHAJI-XFEUOLMDSA-N Vitamin D3 Natural products C1(/[C@@H]2CC[C@@H]([C@]2(CCC1)C)[C@H](C)CCCC(C)C)=C/C=C1\C[C@@H](O)CCC1=C QYSXJUFSXHHAJI-XFEUOLMDSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
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- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000004042 decolorization Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- IKGXIBQEEMLURG-NVPNHPEKSA-N rutin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-NVPNHPEKSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000011514 vinification Methods 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000019166 vitamin D Nutrition 0.000 description 1
- 239000011710 vitamin D Substances 0.000 description 1
- 150000003710 vitamin D derivatives Chemical class 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
- 229940046008 vitamin d Drugs 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
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Classifications
-
- 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
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a grape seed oil extraction method and an extraction device, and belongs to the technical field of oil extraction. The method comprises the following steps: (1) grape seed pretreatment; (2) crushing; (3) extraction; the extraction method comprises the following steps: placing crushed grape seeds into an extraction kettle, and opening supercritical CO 2 A system; when each device reaches the preset parameter value, the CO is started 2 Gas cylinder, control CO 2 Flow rate, extraction kettle pressure; separating the temperature and the pressure of the kettle I; separating kettle II temperature and pressure; and separating the grape seed oil by a rectifying column after extraction. The crude oil with low oleic acid value can be obtained by controlling the pressure in the separation kettle. Compared with the existing method for preparing grape seed oil, the oil prepared by the invention has lower saponification value, acid value and peroxide value, can maintain the original nutritive value of the oil to the maximum extent, and has no oilSubsequent refining treatment is required.
Description
Technical Field
The invention relates to the technical field of grease extraction, in particular to an extraction method and extraction equipment of grape seed oil.
Background
Grape seeds account for about 5% of the weight of wine grapes and are a resource by-product produced in wine production. The planting area of the wine grapes in Shandong province exceeds 52.23 mu (25.13 mu in the home and 27.1 mu in the outside port base), the yield of the wine grapes is approximately 55 ten thousand tons, and the yield of grape seeds per year is approximately 3 ten thousand tons. The grape seed oil contains 14% -18% of a large amount of unsaturated fatty acid, palmitic acid, stearic acid, oleic acid, linoleic acid and the like, also contains trace linolenic acid, lauric acid, myristic acid and the like, contains more than 18 amino acids, has higher content of K, na, ca, fe, zn, mn and other nutrient elements in mineral elements, and also contains abundant vitamin A, vitamin D, vitamin E, vitamin P and other components. The grape seed oil contains abundant vitamin E, which is a famous antioxidant, and can prevent various diseases and keep skin and muscle healthy. The grape seed oil contains procyanidine (OPC), which is the substance with the strongest antioxidant and free radical scavenging ability found in the nature at present, and has antioxidant activity 50 times of vitamin E and 20 times of vitamin C, and can prevent various diseases, especially cardiovascular diseases, care skin and prevent aging. One of the effects of OPC is to protect vitamin C from oxidative inactivation before reaching the site of onset. OPC is therefore also referred to as a vitamin C potentiator.
The offal of grape wine making processing is mainly grape skin and grape seeds, wherein the grape seeds account for 4% -7% of the weight of the fresh fruits. Grape seeds mainly come from offal of grape processing enterprises (such as winery and the like), a large number of grape seeds can be generated in the wine production process, and if the grape seeds are not utilized, the grape seeds not only pollute the environment, but also cause the waste of active ingredients.
Currently, the extraction methods of industrial grape seed oil include a pressing method and an immersion method. The squeezing method is used as an ancient mechanical oil extraction method, the equipment and the process are simple, but the squeezing method is adopted because grape seeds are hard, the oil yield is low, and the energy consumption is high. The dipping method has high oil yield, but the process flow is complicated, the product has solvent residues, the natural characteristic of the grease is difficult to ensure, and the requirement on the subsequent processing technology is high. Meanwhile, the acid value is high when crude oil is obtained by a pressing method or an impregnation method, and further refining is needed to reduce the acid value. This undoubtedly increases the grease extraction process and will result in a loss of most of the nutrients.
The novel extraction method of grape seed oil comprises microwave method, ultrasonic solvent extraction method and supercritical CO 2 Extraction method, etc. At present, the single report of the extraction method is more, the research on the grape seed oil yield is more, and the research on the grape seed oil quality such as acid value reduction, peroxide value and the like is less.
Disclosure of Invention
Aiming at the defects existing in the prior art for extracting grape seed oil, the invention provides an extraction method and extraction equipment for grape seed oil, so as to solve the technical problems. The invention optimizes the supercritical CO 2 Extraction process, research of separation pressure on supercritical CO 2 The effect of acid value of extracted grape seed oil is improved by supercritical CO 2 The quality of the grape seed oil is extracted, so that the refined grape seed oil reaches the national grade I grape seed oil standard.
The technical scheme of the invention is as follows:
the grape seed oil extracting process includes the following steps:
(1) Grape seed pretreatment
Taking grape seeds after brewing, naturally airing and air-drying, controlling the moisture content of the grape seeds to be less than 3%, and removing impurities; washing with water, and oven drying at 80deg.C.
(2) Crushing
Treating the dried grape seeds in the step (1) at a low temperature of-80 ℃ for 2 hours; crushing the seeds by a crusher, separating the crushed seeds by a cyclone separator to obtain kernels, and crushing the kernels to 40-60 meshes at a low temperature (4 ℃) for later use; because grape seed oil is mainly stored in the seed kernel, pigment content (polyphenol) in the seed shell is higher, the extraction rate of grape seed oil is influenced, the quality (color, acid value and peroxide value) of the grape seed oil is greatly influenced, and the yield and quality of the grape seed oil can be greatly improved through low-temperature shelling treatment.
(3) Extraction
Supercritical CO is carried out on the crushed grape seeds 2 Extracting; the method comprises the following steps: placing crushed grape seeds into an extraction kettle, and opening supercritical CO 2 System, set up CO 2 A cylinder pressure value; simultaneously starting a cooler and a high-pressure system; setting parameters of an extraction kettle, a separation kettle I and a separation kettle II; when each device reaches the preset parameter value, the CO is started 2 Gas cylinder, control CO 2 The flow rate is 50L/h, the pressure of the extraction kettle is 20-40 MPa, the extraction time is 40-60 min, and the temperature of the extraction kettle is 35-50 ℃; the temperature of the separation kettle I is 55 ℃ and the pressure is 8-16 MPa; the temperature of the separation kettle II is 40 ℃ and the pressure is 8-16 MPa.
Further, in the step (2), grape seeds are crushed to 60 meshes.
Further, in the step (3), the pressure of the extraction kettle is 30MPa.
Further, the pressure of the separation kettle I is 13MPa.
Further, the pressure of the separation kettle II is 9MPa.
An extraction device for extracting grape seed oil comprises CO 2 The device comprises a gas cylinder, a cooler, a raw material tank, a carrying agent storage tank, an extraction kettle, a separation kettle I and a separation kettle II; the CO 2 The gas cylinder is connected with the first purifier; the first purifier is connected with the cooler; the cooler is connected with the pipeline of the carrying agent storage tank in parallel and then connected with the mixing kettle; the mixing kettle is connected with the second purifier; the purifier is connected with the extraction kettle; the extraction kettle is connected with the separation kettle I; the separation kettle I is connected with the separation kettle II; and the separation kettle II is connected with the rectifying column.
The beneficial effects of the invention are as follows:
the invention adopts supercritical CO 2 Extracting oil from grape seed oil by using an extraction method, and controlling the pressure in a separation kettle to obtain crude oil with low acid value. Compared with the new solvent and hydraulic method for preparing grape seed oil, the supercritical extraction oil has higher iodine value, lower saponification value, acid value, peroxide value and supercritical CO 2 The extraction method can maximallyThe original nutritive value of the grease is maintained, no solvent residue exists, and the subsequent refining treatment (degumming, alkali refining, deodorization and other processes) is not needed. Thus, supercritical CO 2 The extracted grape seed oil is superior to a solvent extraction method, can meet the development requirements of pure natural food and skin care base oil products, and has good development and application prospects.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic diagram of the reaction apparatus of example 1.
FIG. 2 is a graph showing the effect of pressure in separation vessel I on acid value of grape seed oil in example 1.
FIG. 3 is a graph showing the effect of pressure in separation tank II on acid value of grape seed oil in example 1.
In the figure, 1-CO 2 The device comprises a gas cylinder, a first 2-purifier, a 3-cooler, a 4-carrying agent storage tank, a 5-raw material tank, a 6-mixing kettle, a second 7-purifier, an 8-extraction kettle, a 9-separation kettle I, a 10-separation kettle II and an 11-rectification column.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
As shown in FIG. 1, an extraction apparatus for extracting grape seed oil comprises CO 2 Gas cylinder 1, cooler 3, raw material tank 5, carrying agent storage tank 4, extraction kettle 8 and separation kettleI9 and a separation kettle II 10; the CO 2 The gas cylinder 1 is connected with the first purifier 2; the first purifier 2 is connected with the cooler 3; the cooler 3 is connected with a pipeline of the carrying agent storage tank 4 in parallel and then connected with the mixing kettle 6; the mixing kettle 6 is connected with a second purifier 7; the second purifier 7 is connected with the extraction kettle 8; the extraction kettle 8 is connected with the separation kettle I9; the separation kettle I9 is connected with the separation kettle II 10; the separation kettle II 10 is connected with the rectifying column 11.
Example 2
In the apparatus of example 1, for supercritical CO 2 Pressure of extraction separation kettle I and pressure of separation kettle II are researched
In CO 2 Under the condition that the conditions such as the flow rate, the extraction pressure, the extraction time, the extraction kettle temperature, the separation kettle I and the separation kettle II are unchanged, the pressures of the separation kettle I and the separation kettle II are researched, the influence of the pressure changes of the separation kettle I and the separation kettle II on the acid value of the grape seed oil is researched respectively, and the optimal separation kettle pressure is determined through a combined test.
(1) Pressure study of separation kettle I
Setting CO 2 The flow rate is 50L/h, the extraction kettle pressure is 30MPa, the extraction time is 60min, the extraction kettle temperature is 45 ℃, the separation kettle I temperature is 55 ℃, the separation kettle II temperature is 40 ℃, the separation kettle II pressure is 8MPa, and the rectification column pressure is 4MPa. And respectively researching the influence of the pressure of the separation kettle I on the acid value of the grape seed oil when the pressure of the separation kettle I is 8MPa, 10MPa, 12MPa, 14MPa and 16MPa. The specific results are shown in FIG. 2.
As can be seen from FIG. 2, the oleic acid value of separation vessel I decreases as the pressure of separation vessel I increases. The analysis reason is that the pressure of the separation kettle I is increased, and the extracted grape seed oil is treated by CO 2 The dissolving capacity of the oil and CO in the separation kettle I is increased, and the oil and CO in the separation kettle I are separated 2 The separation rate of the fluid is smaller than that of free fatty acid and CO 2 The separation rate of the fluid results in less precipitation of free fatty acids in the separation vessel I, and the acid value of the oil in the separation vessel I is correspondingly reduced.
(2) Pressure study of separation still II
Setting CO 2 The flow rate is 50L/h, the pressure of the extraction kettle is 30MPa, the extraction time is 60min, the temperature of the extraction kettle is 45 ℃, and the separation is carried outThe temperature of the kettle I is 55 ℃, the pressure of the separation kettle I is 12MPa, the temperature of the separation kettle II is 40 ℃, and the pressure of the rectifying column is 4MPa. And respectively researching the influence of the pressure of the separation kettle II on the acid value of the grape seed oil when the pressure of the separation kettle II is 6MPa, 7MPa, 8MPa, 9MPa and 10 MPa. The specific results are shown in FIG. 3.
As can be seen from FIG. 3, as the pressure of separation tank II increases, the oleic acid value of separation tank II decreases. The analysis reason is that the pressure of the separation kettle II is increased, and the extracted grape seed oil is subjected to CO 2 The dissolving capacity of the oil and CO in the separation kettle II is increased 2 The separation rate of the fluid is reduced, and free fatty acid is less precipitated in the separation kettle II, so that the acid value of oil in the separation kettle II is reduced.
(3) Supercritical CO 2 Process optimization for reducing acid value of grape seed oil by extraction technology
Setting CO 2 The flow rate is 50L/h, the extraction kettle pressure is 30MPa, the extraction time is 60min, the extraction kettle temperature is 45 ℃, and the separation kettle I temperature is 55 ℃; the temperature of the separation kettle II is 40 ℃, and the pressure of the rectifying column is 4MPa. And respectively setting the pressure of the separation kettle I to 11MPa, 12MPa and 13MPa, and setting the pressure of the separation kettle II to 8MPa, 9MPa and 10MPa, so as to carry out a combined test. The test results are shown in Table 1.
TABLE 1 results of the combined tests
From the combined test results, the acid value of the grape seed oil obtained by the separation kettle I is 0.567mgKOH/g at the same extraction conditions, the pressure of the separation kettle I is 13MPa, and the pressure of the separation kettle II is 9MPa.
Example 3
The grape seed oil extracting process includes the following steps:
(1) Grape seed airing
Taking grape seeds after brewing, naturally airing and air-drying, and removing impurities for standby, wherein the total weight of the grape seeds is 10kg.
(2) Crushing
Pulverizing grape seeds in the step (1) to 60 meshes for later use.
(3) Extraction
Supercritical CO is carried out on the crushed grape seeds 2 Extracting; wherein CO is 2 The flow rate is 50L/h, the pressure of the extraction kettle is 13MPa, the extraction time is 60min, and the temperature of the extraction kettle is 45 ℃.
The temperature of the separation kettle I is 55 ℃ and the pressure is 9MPa; the temperature of the separation kettle II is 40 ℃ and the pressure is 8MPa.
Grape seed oil yield was calculated according to the following formula:
1.62kg of grape seed oil was finally obtained, grape seed oil yield=16.2%.
Comparative example 1
The grape seed oil is prepared by adopting a hydraulic cold pressing process, and the specific steps are as follows:
(1) Taking 40kg of dried grape seeds, screening to remove impurities, and crushing to 60 meshes;
(2) And (5) loading the crushed grape seeds into a squeezer for squeezing. The squeezing pressure is 40MPa, the squeezing chamber temperature is 50 ℃, and the squeezing time is 60min. 3.08kg of grape seed oil crude oil is obtained, and the crude oil yield=7.7%.
(3) Refining:
a. hydration degumming: coarse filtering the crude oil, heating the crude oil to 65 ℃ after filtering, adding 1%o phosphoric acid solution, and stirring at 60rpm for 30min; then adding 70 ℃ water, and stirring for 30min at 30 rpm; stopping stirring, and standing for sedimentation for 4 hours; discharging the settled phospholipids from the cone bottom of the degumming device;
b. alkali refining deacidification: heating the degummed oil in the previous step to 65 ℃, adding NaOH at 60rpm, and stirring at 30rpm for 30min; wherein the alkali dosage is as follows: naOH (kg) =7.13×10-4×oil weight×acid number; standing after stirring, naturally settling for 4 hours, and discharging settled Chinese honeylocust from the cone bottom of the deacidification equipment;
c. washing: heating the alkali oil refining obtained in the previous step to 80-85 ℃, adding 8% of water by weight of the alkali oil refining at 60rpm, and stirring at 30rpm for 30min; stopping stirring, naturally settling for 2 hours, and discharging wastewater from the cone bottom;
d. adsorption decolorization: heating the grease in the previous step to 120-130 ℃ under-0.08 MPa for dehydration; adding neutral activated clay accounting for 1-3% of the weight of the grease after dehydration, stirring for 30min at 40rpm, filtering with a plate frame to obtain decolorized oil, and pumping the decolorized oil into a deodorizing tank.
e. Vacuum deodorization: heating the decolorized oil obtained in the previous step to 150 ℃ under the condition of-0.08 MPa; then heating to 240 ℃, preserving heat for 2 hours, and then reducing the oil temperature to below 70 ℃;
f. dewaxing at low temperature: controlling the rotating speed to 45rpm, reducing the temperature of the deodorizing oil in the last step to 8 ℃ in a gradient cooling mode, and maintaining for 12 hours; then adding diatomite filter aid accounting for 2% of the weight of the deodorized oil, uniformly stirring, and filtering by adopting a plate frame to obtain 2.78kg of clear finished grape seed oil, wherein the grape seed oil yield is=6.95%.
Comparative example 2
The grape seed oil is prepared by adopting a hydraulic hot pressing process, and the specific steps are as follows:
(1) Taking 40kg of dried grape seeds, screening to remove impurities, and crushing to 60 meshes;
(2) Steaming, wherein the steaming temperature is 110 ℃, and the steaming time is 60min; cooling to room temperature after steaming;
(3) And (5) loading the cooled grape seeds into a squeezer for squeezing. The squeezing pressure is 40MPa, the squeezing chamber temperature is 50 ℃, and the squeezing time is 60min. 4.88kg of grape seed oil crude oil is obtained.
(4) Refining: the refining method was the same as that of comparative example 2. 4.28kg of finished grape seed oil is obtained, and the recovery rate is 87.7%.
Test case
The main indexes of the crude oil and the finished oil prepared in example 2 and comparative example 2 were measured, wherein moisture and volatiles were measured: is executed according to GB/T5528-2008. Determination of acid value: performed as per GB/T5530-2005. Peroxide value measurement: performed as per GB/T5538-2005. Transparency, odor, taste measurement: is executed according to GB/T5525-2008. The specific results are shown in Table 2 below:
TABLE 2 determination of main index of oil product
As can be seen from the results of the test in Table 2, the present invention uses supercritical CO 2 Extracting oil from grape seed oil by using an extraction method, and controlling the pressure in a separation kettle to obtain crude oil with low acid value. Compared with the new solvent and hydraulic method for preparing grape seed oil, the supercritical extraction oil has higher iodine value, lower saponification value, acid value, peroxide value and supercritical CO 2 The extraction method can keep the original nutritive value of the grease to the maximum extent, has no solvent residue, and does not need subsequent refining treatment (degumming, alkali refining, deodorization and other processes).
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. The extraction method of the grape seed oil is characterized by comprising the following steps of:
(1) Grape seed pretreatment
Taking grape seeds after brewing, naturally airing and air-drying, controlling the moisture content of the grape seeds to be less than 3%, and removing impurities; washing with water, and oven drying at 80deg.C;
(2) Crushing
Treating the dried grape seeds in the step (1) at a low temperature of-80 ℃ for 2 hours; crushing the seeds by a crusher, separating the crushed seeds by a cyclone separator to obtain kernels, and crushing the kernels to 40-60 meshes at the temperature of 4 ℃ for later use;
(3) Extraction
Supercritical CO is carried out on the crushed grape seeds 2 Extracting; the method comprises the following steps: placing crushed grape seeds into an extraction kettle, and opening supercritical CO 2 System, set up CO 2 A cylinder pressure value; simultaneously starting a cooler and a high-pressure system; setting parameters of an extraction kettle, a separation kettle I and a separation kettle II; when each device reaches the preset parameter value, the CO is started 2 Gas cylinder, control CO 2 The flow rate is 50L/h, and the pressure of the extraction kettle is 20-40 MPa; the temperature of the separation kettle I is 55 ℃ and the pressure is 8-16 MPa; the temperature of the separation kettle II is 40 ℃ and the pressure is 8-16 MPa; and separating the grape seed oil by a rectifying column after extraction.
2. The extraction method according to claim 1, wherein in the step (2), grape seeds are crushed to 60 mesh.
3. The extraction method according to claim 1, wherein the extraction time is 40 to 60 minutes.
4. The extraction process according to claim 1, wherein the extraction kettle temperature is 35-50 ℃.
5. The extraction process of claim 1, wherein the extraction tank pressure is 30MPa.
6. The extraction process according to claim 1, wherein the pressure in the separation vessel I is 13MPa.
7. The extraction method according to claim 1, wherein the pressure of the separation tank II is 9MPa.
8. An extraction apparatus for carrying out the extraction process of claim 1, comprising CO 2 The device comprises a gas cylinder, a cooler, a raw material tank, a carrying agent storage tank, an extraction kettle, a separation kettle I and a separation kettle II; the CO 2 The gas cylinder is connected with the first purifier; the purifier I and the coolerConnecting; the cooler is connected with the pipeline of the carrying agent storage tank in parallel and then connected with the mixing kettle; the mixing kettle is connected with the second purifier; the purifier is connected with the extraction kettle; the extraction kettle is connected with the separation kettle I; the separation kettle I is connected with the separation kettle II; and the separation kettle II is connected with the rectifying column.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105482893A (en) * | 2015-10-28 | 2016-04-13 | 广州中大南沙科技创新产业园有限公司 | Supercritical CO2 extraction method for tuber onion seed oil |
| CN107011986A (en) * | 2017-05-12 | 2017-08-04 | 江苏金洲粮油食品有限公司 | A kind of preparation method of grape-kernel oil |
| CN107418722A (en) * | 2017-05-18 | 2017-12-01 | 毕节市中药产业发展办公室 | Use supercritical CO2Extract Rosa roxburghii seed oil |
| CN111175218A (en) * | 2020-03-23 | 2020-05-19 | 河南理工大学 | Supercritical carbon dioxide extraction-permeability testing device and method |
| CN112587554A (en) * | 2020-12-15 | 2021-04-02 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with gastric mucosa protecting effect, and its preparation method and equipment |
| CN114836258A (en) * | 2022-04-20 | 2022-08-02 | 宁夏松海盛华农林科技开发有限公司 | Method for extracting grape seed oil by using grape seeds after brewing |
| CN115261120A (en) * | 2022-08-15 | 2022-11-01 | 宁夏皇蔻生物科技有限公司 | Method for preparing grape seed oil by using grape seeds and product |
-
2023
- 2023-05-11 CN CN202310529695.1A patent/CN116590091A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105482893A (en) * | 2015-10-28 | 2016-04-13 | 广州中大南沙科技创新产业园有限公司 | Supercritical CO2 extraction method for tuber onion seed oil |
| CN107011986A (en) * | 2017-05-12 | 2017-08-04 | 江苏金洲粮油食品有限公司 | A kind of preparation method of grape-kernel oil |
| CN107418722A (en) * | 2017-05-18 | 2017-12-01 | 毕节市中药产业发展办公室 | Use supercritical CO2Extract Rosa roxburghii seed oil |
| CN111175218A (en) * | 2020-03-23 | 2020-05-19 | 河南理工大学 | Supercritical carbon dioxide extraction-permeability testing device and method |
| CN112587554A (en) * | 2020-12-15 | 2021-04-02 | 福建仙芝楼生物科技有限公司 | Ganoderma spore oil with gastric mucosa protecting effect, and its preparation method and equipment |
| CN114836258A (en) * | 2022-04-20 | 2022-08-02 | 宁夏松海盛华农林科技开发有限公司 | Method for extracting grape seed oil by using grape seeds after brewing |
| CN115261120A (en) * | 2022-08-15 | 2022-11-01 | 宁夏皇蔻生物科技有限公司 | Method for preparing grape seed oil by using grape seeds and product |
Non-Patent Citations (1)
| Title |
|---|
| 李大婧, 刘荣, 王萍: "超临界CO_2萃取玉米黄色素的试验研究", 中国粮油学报, no. 05, 30 October 2005 (2005-10-30), pages 35 - 39 * |
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