CN113817539B - Method for extracting peanut meal oil by utilizing low-temperature continuous phase change - Google Patents
Method for extracting peanut meal oil by utilizing low-temperature continuous phase change Download PDFInfo
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- CN113817539B CN113817539B CN202111032559.9A CN202111032559A CN113817539B CN 113817539 B CN113817539 B CN 113817539B CN 202111032559 A CN202111032559 A CN 202111032559A CN 113817539 B CN113817539 B CN 113817539B
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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
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the field of vegetable oil extraction, and particularly relates to a method for extracting peanut meal oil by utilizing low-temperature continuous phase change. The invention takes peanut meal as a raw material, and is added into an extraction kettle after being crushed, and adopts a low-temperature continuous phase change extraction technology in combination with ethanol leaching, and the conditions are as follows: peanut meal: ethanol (m: V=1:1-1:3) is leached for 1-3h, the extraction temperature is 40-65 ℃, the extraction pressure is 0.3-1.0 Mpa, the extractant is compressed into liquid, the liquid flows through an extraction kettle at the flow rate of 60-80L/h, the continuous extraction is carried out for 30-110 min, the peanut meal oil is extracted, and then the peanut meal oil enters an analysis tank, the analysis temperature is 50-80 ℃, and the analysis pressure is 0.1-0.4 Mpa. The extraction process disclosed by the invention has the advantages of keeping water-soluble and fat-soluble component substances to the greatest extent on the basis of ensuring the extraction rate of more than 95%, being safe and efficient, having no solvent residue, and being high in quality of the obtained peanut meal oil product and capable of realizing industrialized development.
Description
Technical Field
The invention belongs to the field of vegetable oil extraction, and particularly relates to a method for extracting peanut meal oil by utilizing low-temperature continuous phase change.
Technical Field
Peanut is one of the most important oil-based commercial crops in China, and the total annual yield is about 1334.1 ten thousand t, and is the first in the world. The peanut meal is a byproduct obtained by taking shelled peanuts as a raw material and extracting grease, has light brown or dark brown color, has light peanut fragrance, is small blocks or powder, and contains a small amount of peanut shells. The peanut meal which is left after oil pressing is about 900 ten thousand t each year, has rich nutrition, complete amino acid types, high protein content and 47% -55% crude protein content, belongs to complete protein, is inferior to soybean protein in plant protein, but is easier to absorb than soybean protein, contains less anti-nutritional factors, is easy to digest and absorb by human body, and can be used as a source for supplementing nutrition for human body. The method is a problem which is worthy of being taken into consideration in terms of how to reasonably develop and utilize low-value peanut meal with rich nutrition and rich resources and to improve the high-value utilization value of the peanut meal.
The peanut meal can be roughly classified into two types according to the different pressing processes, namely, hot pressed peanut meal and cold pressed peanut meal. Compared with hot pressed peanut meal, the cold pressed peanut meal can effectively avoid the problem of harmful substance residue caused by direct contact with chemical substances in the traditional oil preparation and refining process, well protect the components of oil, protein, sugar, lipid substances, mineral substances and the like in oil materials which are easy to damage at high temperature, and ensure the development and utilization value of the cake meal. However, the peanut oil obtained by the low-temperature squeezing method has low aromatic components, so that the requirements of consumers are difficult to reach, and the market share is low; and the utilization of cold pressed cake in China is still in the primary stage. The peanut meal in China is mainly prepared from hot pressed peanuts. After high-temperature squeezing, maillard reaction can be carried out on the peanuts, so that the peanut oil with strong aroma flavor is obtained. However, the high temperature causes serious deformation of protein and has certain influence on the nutritive value, so the peanut meal is commonly used for animal feed, the high-value utilization rate is low, and the protein resource is greatly wasted.
Secondly, the peanut meal contains trace beneficial substances which are difficult to dissolve in water, such as peanut flavone and the like. The substances are rich in content and have important biological activity on human bodies, but are mainly in peanut meal. Therefore, the extraction of the substances from the peanut meal plays a key role in developing high-quality peanut meal oil and realizing high-value utilization of the peanut meal. At present, related researches on extracting active substances from peanut meal at home and abroad are few, and the method mainly comprises simple ethanol leaching, and has low extraction efficiency and high time cost. Therefore, a medium and high-efficiency extraction and separation method needs to be developed, and the method has important significance for developing high-quality peanut meal oil.
The existing process for extracting the cake residue mainly comprises an extraction method, a water-enzyme method and a supertechnologySonic assisted extraction and supercritical extraction. The extraction method can simplify the subsequent complicated refining process of the grease, shortens the production period and reduces the refining loss, is an extraction method with potential industrialization value, but has the problems of solvent residue and toxicity, and the protein in the meal is seriously denatured, so that the development and the utilization of the protein are greatly limited. The aqueous enzymatic process is considered to be a very potential green, high quality oil extraction technology, but lacks a highly targeted enzyme preparation, and the high cost of commercial enzyme preparations and the high hydrolysis of proteins limit the industrial development of aqueous enzymatic residue extraction. The ultrasonic-assisted extraction method greatly shortens the extraction time, and the extraction reagent can be recovered, has low cost and achieves the purposes of high efficiency and energy conservation, but the method has not wide application in cake residue. Supercritical CO 2 The technology for extracting peanut meal oil is a good extraction technology, can not only improve the yield of products and directly obtain essential oil products, but also has no solvent residue, can furthest reserve the activity of nutrient components in the essential oil products, is an environment-friendly novel technology, but has the advantages of expensive equipment, higher energy consumption, high pressure required in the process and inapplicability to large-scale production.
CN111440658A discloses a process for extracting butane from peanut meal, which mainly comprises the steps of firstly crushing peanut raw materials, sieving to obtain peanut meal powder, pressurizing butane gas into butane liquid, mixing with ethanol and the peanut meal powder, extracting to obtain solid peanut meal and leached oil, wherein the solid peanut meal is desolventized to obtain finished product meal, and carrying out reduced pressure distillation on the leached oil to separate butane gas and ethanol, thus obtaining grease. The process flow is simple and safe to operate, fewer auxiliary raw materials are used, the energy consumption is low, the prepared peanut oil is clear, active substances in the product are reserved, the nutritive value is high, and the utilization rate and the added value of the peanut meal are improved. However, the process needs to be extracted in steps, materials need to be transferred, and the operation complexity is increased.
CN 103937614A discloses a leaching solution for extracting grease from sunflower seed oil meal, which comprises, by weight, 100 parts of ethanol, 20-26 parts of 1, 4-butanediol, 15-20 parts of methyl acetate, 2-7 parts of hydroxyethylidene diphosphonic acid, 1-3 parts of sodium carbonate, 0.2-3 parts of cellulase and 0.08-0.5 part of sodium iso-vitamin C. The leaching solution for extracting the grease from the sunflower seed oil meal provided by the invention is used for further leaching according to the characteristics of the oil meal after the sunflower seeds are pressed, and the obtained grease has high yield and can be industrially applied. However, the use of a large amount of organic solvents is easy to destroy the protein structure of the meal, and whether the solvent removal is complete or not directly influences the quality of the meal oil.
CN104257882a discloses a method for simultaneously extracting and separating grease, chlorogenic acid and total flavonoids from medlar dreg, which is characterized in that (1) medlar dreg is extracted by supercritical carbon dioxide extraction technology to obtain medlar oil; (2) Taking medlar dreg after oil extraction, and carrying out supercritical carbon dioxide extraction by taking ethanol as an entrainer to obtain an extract for later use; (3) Subjecting the supercritical carbon dioxide extract to macroporous adsorbent resin, preferably D101 macroporous adsorbent resin, sequentially eluting with water, 10-15% (v/v) (preferably 15%) and 65-75% (v/v) (preferably 70%) ethanol, collecting ethanol eluate of each concentration, concentrating, and drying to obtain chlorogenic acid and total flavonoids. However, the existing supercritical carbon dioxide extraction technology is high in price, low in factory industrialization degree and difficult to popularize and use.
Therefore, how to reduce the damage to the effective components and improve the yield of peanut meal oil is a relatively popular research subject in the years. The Chinese patent with publication number of CN103349849A discloses a multifunctional continuous phase change extraction device, and the extraction technology has wide application range of solvent extraction, safety and continuity of supercritical dynamic extraction, and much lower equipment cost and operation cost than the supercritical extraction device, can completely extract at one time, can realize industrialization, and can realize omnibearing efficient extraction of natural products. The technical principle is that the grease is extracted dynamically and efficiently by utilizing the two-phase change of the extractant under different pressures and temperatures and the strong penetrability of the extractant under a certain pressure. The low temperature is continuously reflected in the process that the extraction solvent is compressed into liquid under the condition that the critical pressure and the critical temperature are lower than the extraction solvent, the liquid flows through the extraction kettle to extract the materials, then the phase is changed into gas in the analysis kettle, the extracted materials fall into the analysis kettle, the analyzed gas is compressed into liquid again and flows through the extraction kettle again, and the process temperature is much lower than the conventional oil refining temperature; compared with the common solvent extraction method, the method has the advantages of remarkably improved yield and purity, greatly shortened time, and no harmful solvent residue, and can use food-grade safe nontoxic harmless extractant.
Because of the defects of the existing extraction technology, the peanut meal has the conditions of high residual oil content and low extraction rate, and inhibits the extraction and utilization of peanut proteins, and other active substances; meanwhile, the peanut meal contains a large amount of beneficial active substances, but the related efficient extraction technology is lack, so that the resource waste is caused, and the high-value utilization degree of the peanut meal is greatly reduced. Therefore, the research of a peanut meal oil extraction process which has high oil extraction efficiency, no organic solvent residue and rich water-soluble and fat-soluble component substances becomes a technical problem to be solved urgently. Moreover, the application of the low-temperature continuous phase-change extraction technology in the field of natural products is mainly focused on the extraction research of plant volatile oil and pigment, and the research of extracting peanut meal oil by adopting low-temperature continuous phase-change is not reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which has the advantages of high extraction rate, rich water-soluble and fat-soluble component substances, safety, environmental protection and low cost, and is suitable for large-scale industrial production. Compared with the traditional extraction method, the method has the advantages that the process is accurate and stable, the quality of the peanut meal oil is better, the extraction rate is obviously improved, and the high-efficiency extraction of the peanut meal oil can be realized. Not only realizes the integrated extraction, saves the economic cost, but also improves the high-value utilization of peanut byproducts and improves the economic benefit of production enterprises.
The invention aims at realizing the following technical scheme:
a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, drying a peanut meal raw material, controlling the water content to be less than or equal to 6%, and crushing to 20-60 meshes to obtain peanut meal powder;
s2, loading the peanut meal processed in the step S1 into an extraction kettle of a continuous phase change extraction device, and adding ethanol for soaking treatment;
s3, carrying out low-temperature continuous phase-change extraction on the peanut meal powder treated in the step S2 to obtain a peanut meal oil product; the technological conditions of the low-temperature continuous phase-change extraction are as follows: putting peanut meal powder into an extraction kettle, compressing an extractant into liquid at the extraction temperature of 40-65 ℃ and the extraction pressure of 0.3-1.0 Mpa, flowing through the extraction kettle at the flow rate of 60-80L/h, continuously extracting for 30-110 min, and then putting the extracted peanut meal oil into an analysis kettle, wherein the analysis temperature is 50-80 ℃ and the analysis pressure is 0.1-0.4 Mpa; the extractant is changed into gas by heating and decompressing, then is changed into liquid by instant compression, and then flows through an extraction kettle to extract the materials again, and the solvent passing through the extraction kettle enters a resolving tank with oil, and the peanut meal oil product is obtained after resolving.
Preferably, the low-temperature continuous phase-change extraction step S3 is cycled multiple times.
Preferably, the concentration of the ethanol in the step S2 is 50-70%, the ratio of the feed liquid to the v is 1:1-1:3, and the soaking is carried out for 1-3 hours.
Preferably, the extractant described in step S3 is n-butane.
Preferably, the extraction temperature in the step S3 is 50-60 ℃ and the extraction pressure is 0.4-0.7 MPa.
Preferably, the flow rate of the extractant in the step S3 is 80L/h.
Preferably, the analysis temperature in the step S3 is 55-75 ℃, and the analysis pressure is 0.25MPa.
In the whole low-temperature continuous phase-change extraction process, the phase-change process of the extracting agent from liquid state to gas state to liquid state is instant and continuous, the extracting agent n-butane is subjected to continuous phase change and recycled, and the extracted peanut meal oil is stored in an analysis kettle and discharged and collected after extraction.
The whole extraction process is carried out under the conditions of closed anaerobic condition, low temperature and low pressure.
The invention also provides peanut meal oil prepared by the extraction method.
The method adopts alcohol extraction to enrich residual trace beneficial substances in peanut meal, the extraction rate of peanut oil extracted from the peanut meal by using a low-temperature continuous phase change technology can reach 99.03%, and the extracted peanut meal oil is rich in resveratrol, flavone and polyphenol beneficial substances.
The invention has the beneficial effects that:
the invention utilizes low-temperature continuous phase-change extraction and ethanol leaching technology to extract peanut meal oil, which effectively improves the extraction rate of peanut meal oil and ensures the maximization of the content of beneficial substances in peanut meal oil. The low-temperature continuous phase change technology has close influence on the improvement of the extraction rate of peanut meal oil and the oil quality on the factors such as the extraction temperature, the extraction pressure, the extraction time, the moisture content of materials, the analysis temperature and the like. The method is scientifically and comprehensively considered, the targeted process conditions are summarized, the whole process is free from high temperature, trace beneficial substances remained in the peanut meal can be enriched in an alcohol extraction mode, active substances are not lost, harmful substances such as polymers and the like can not be generated, and the method is convenient to operate, safe and environment-friendly, and is very suitable for large-scale industrial production.
The invention develops a method for extracting peanut meal oil from peanut meal by utilizing a low-temperature continuous phase-change extraction technology, which does not need to transfer materials, so that the materials are always kept in a low-temperature and low-pressure state, oxidation generated during material transfer is reduced, the industrial production flow is simplified, and the method is favorable for industrial mass production.
The invention takes peanut meal as a raw material, not only realizes the integrated extraction of high extraction rate and enrichment of beneficial substances and saves the economic cost, but also improves the high-value utilization of peanut byproducts and the economic benefit of production enterprises.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The preparation was carried out under conventional conditions or conditions recommended by the manufacturer, where no specific conditions were noted in the examples. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, drying a hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:1) for 1h;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, flowing through the extraction kettle at a certain flow rate to extract peanut meal oil, then entering the analysis kettle, changing the n-butane into gas through heating and decompression, and then changing the n-butane into liquid through compression to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle, and the extracted peanut meal oil is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 45 ℃ and the extraction pressure of 0.5Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 60L/h, is continuously extracted for 45min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 65 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is yellow transparent viscous liquid, the peanut oil has stronger flavor and better sensory quality, and various indexes meet the GB/T1534-2017 standard.
Example 2: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, drying a hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:2) for 2 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, allowing the liquid to flow through the extraction kettle at a certain flow rate to extract peanut meal oil, allowing the peanut meal oil to enter the analysis kettle 1, converting the n-butane into gas through heating and decompression, converting the n-butane into liquid through compression, and allowing the liquid to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle 1, and is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 55 ℃ and the extraction pressure of 0.55Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 80L/h, is continuously extracted for 60min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 65 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is yellow transparent viscous liquid, the peanut oil has stronger flavor and better sensory quality, and various indexes meet the GB/T1534-2017 standard.
Example 3: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, drying a hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:3) for 3 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, allowing the liquid to flow through the extraction kettle at a certain flow rate to extract peanut meal oil, allowing the peanut meal oil to enter the analysis kettle 1, converting the n-butane into gas through heating and decompression, converting the n-butane into liquid through compression, and allowing the liquid to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle 1, and is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of 50 ℃ of extraction temperature and 0.45Mpa of extraction pressure, the peanut meal oil flows through an extraction kettle at a flow rate of 70L/h, is continuously extracted for 55min, flows into a desorption kettle after extracting the peanut meal oil, and has a desorption temperature of 65 ℃ and a desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is yellow transparent viscous liquid, the peanut oil has stronger flavor and better sensory quality, and various indexes meet the GB/T1534-2017 standard.
Example 4: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, squeezing 60% of high-quality peanuts with impurities removed by selection by a hydraulic press, drying at 60 ℃, controlling the water content to be less than or equal to 6%, removing peanut red skin, and crushing to 60 meshes to obtain cold-pressed peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:1) for 1h;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, flowing through the extraction kettle at a certain flow rate to extract peanut meal oil, then entering the analysis kettle, changing the n-butane into gas through heating and decompression, and then changing the n-butane into liquid through compression to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle, and the extracted peanut meal oil is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of 50 ℃ of extraction temperature and 0.55Mpa of extraction pressure, the peanut meal oil flows through an extraction kettle at a flow rate of 60L/h, is continuously extracted for 55min, flows into a desorption kettle after extracting the peanut meal oil, and has a desorption temperature of 65 ℃ and a desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is light yellow transparent viscous liquid, the peanut oil has more faint scent, the faint scent of the peanut oil is similar to that of cold pressed peanut oil, the sensory quality is good, and various indexes meet the GB/T1534-2017 standard.
Example 5: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, squeezing 60% of high-quality peanuts with impurities removed by selection by a hydraulic press, drying at 60 ℃, controlling the water content to be less than or equal to 6%, removing peanut red skin, and crushing to 60 meshes to obtain cold-pressed peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:2) for 2 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, flowing through the extraction kettle at a certain flow rate to extract peanut meal oil, then entering the analysis kettle, changing the n-butane into gas through heating and decompression, and then changing the n-butane into liquid through compression to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle, and the extracted peanut meal oil is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 45 ℃ and the extraction pressure of 0.50Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 60L/h, is continuously extracted for 45min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 65 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is light yellow transparent viscous liquid, the peanut oil has more faint scent, the faint scent of the peanut oil is similar to that of cold pressed peanut oil, the sensory quality is good, and various indexes meet the GB/T1534-2017 standard.
Example 6: a method for extracting peanut meal oil by utilizing low-temperature continuous phase change, which comprises the following steps:
s1, squeezing 60% of high-quality peanuts with impurities removed by selection by a hydraulic press, drying at 60 ℃, controlling the water content to be less than or equal to 6%, removing peanut red skin, and crushing to 60 meshes to obtain cold-pressed peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:3) for 3 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, flowing through the extraction kettle at a certain flow rate to extract peanut meal oil, then entering the analysis kettle, changing the n-butane into gas through heating and decompression, and then changing the n-butane into liquid through compression to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle, and the extracted peanut meal oil is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 55 ℃ and the extraction pressure of 0.60Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 70L/h, is continuously extracted for 60min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 65 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The product is light yellow transparent viscous liquid, the peanut oil has more faint scent, the faint scent of the peanut oil is similar to that of cold pressed peanut oil, the sensory quality is good, and various indexes meet the GB/T1534-2017 standard.
Comparative example 1
The peanut meal oil is prepared by adopting a traditional leaching method. Drying the hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material by a 60-mesh sieve to obtain peanut meal powder. 1.0kg of the treated peanut meal powder is weighed and leached, the leaching condition is that the leaching temperature is 75 ℃, the leaching time is 3 hours, and the leaching solvent is n-hexane. Then spin-evaporating on a rotary evaporator to separate the n-hexane solvent. Vacuum pressure is 0.7MPa, temperature is 45 ℃, and time is 15-20min. Finally obtaining the peanut grease.
Comparative example 2
The peanut oil is prepared by adopting a butane and ethanol two-step extraction method. Drying the hot pressed peanut meal raw material at 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing the hot pressed peanut meal raw material and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
1.0kg of the processed peanut meal powder is weighed and put into a reaction kettle, butane gas is pressurized into butane liquid, the pressurizing temperature is 40-50 ℃, and the pressure is 0.3-0.5MPa. Then mixing with ethanol and peanut meal powder, and performing two-step extraction. Butane liquid, ethanol and peanut meal in a weight ratio of 1.3:0.5:1; the first extraction is carried out at 50-60deg.C for 0.5-1 hr, and the second extraction is carried out at 35-48deg.C for 1-2 hr to obtain solid peanut meal and extract oil. Distilling the obtained extract oil under reduced pressure of 0.1-0.2MPa at 80-90deg.C for 20-40min. And separating butane gas and ethanol to obtain grease.
Comparative example 3
S1, drying a hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:2) for 2 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, allowing the liquid to flow through the extraction kettle at a certain flow rate to extract peanut meal oil, allowing the peanut meal oil to enter the analysis kettle 1, converting the n-butane into gas through heating and decompression, converting the n-butane into liquid through compression, and allowing the liquid to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle 1, and is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 30 ℃ and the extraction pressure of 0.55Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 80L/h, is continuously extracted for 60min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 65 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
Comparative example 4
S1, drying a hot pressed peanut meal raw material at the temperature of 60 ℃ to ensure that the moisture content is less than or equal to 6%, and crushing and sieving the hot pressed peanut meal raw material with a 60-mesh sieve to obtain peanut meal powder;
s2, weighing 1.0kg of the processed peanut meal, loading the peanut meal into an extraction kettle of a continuous phase-change extraction device, and soaking the peanut meal in 1L of ethanol (m: v=1:2) for 2 hours;
s3, introducing n-butane into the extraction kettle in the step S2, compressing the n-butane into liquid under the condition of being always lower than the critical pressure and the critical temperature of the n-butane, allowing the liquid to flow through the extraction kettle at a certain flow rate to extract peanut meal oil, allowing the peanut meal oil to enter the analysis kettle 1, converting the n-butane into gas through heating and decompression, converting the n-butane into liquid through compression, and allowing the liquid to flow through the extraction kettle for recycling. The re-extraction and analysis conditions are the same as the first time, the extracted peanut meal oil is stored in an analysis kettle 1, and is discharged and collected after the extraction is finished. The extraction conditions are as follows: under the conditions of the extraction temperature of 55 ℃ and the extraction pressure of 0.20Mpa, the peanut meal oil flows through an extraction kettle at the flow rate of 20L/h, is continuously extracted for 60min, flows into a desorption kettle after extracting the peanut meal oil, and has the desorption temperature of 45 ℃ and the desorption pressure of 0.35Mpa. And after the extraction is finished, discharging the peanut meal oil in a desorption kettle, and recovering n-butane to obtain the peanut meal oil.
The technical effects of each embodiment and the comparative example in the invention are compared, and the peanut oil extraction rate and the component content detection are calculated.
Test example peanut oil extraction rate calculation: peanut oil extraction rate/% = peanut oil mass (g)/peanut meal oil content (g) ×100%, peanut meal oil content being obtained by measurement of GB 5009.6-2016 "determination of fat in food".
Flavone content analysis method
Accurately weighing 10mg of rutin standard substance, dissolving in 70% ethanol in 50mL volumetric flask, fixing volume to scale, shaking to obtain control solution with concentration of 0.2g/L. Respectively taking standard solutions 0, 1, 2, 3, 4 and 5mL, taking 1mL of control solution, adding 70% ethanol to 5mL in a 10mL volumetric flask, adding 0.3mL of 5% sodium nitrite solution, shaking uniformly, standing for 5min, adding 0.3mL of 10% aluminum nitrate solution, shaking uniformly, standing for 6min, adding 2mL of 1mol/L sodium hydroxide solution, mixing uniformly, fixing the volume of 70% ethanol to 10mL, standing for 30min, and measuring at 500nm to obtain a standard curve graph
Weighing 10g of peanut meal sample, extracting by adopting a thermal reflux method, filtering, taking 2mL of the peanut meal sample, putting the 2mL of the peanut meal sample into a 10mL volumetric flask, adding 70% ethanol to a constant volume of 5mL, adding 0.3mL of 5% sodium nitrite solution, shaking uniformly, standing for 5min, adding 0.3mL of 10% aluminum nitrate solution, shaking uniformly, standing for 6min, adding 2mL of 1mol/L sodium hydroxide solution, mixing uniformly, 70% ethanol to a constant volume of 10mL, standing for 30min, measuring a light absorption value at 500nm, and calculating the flavone content according to a standard curve equation. And measuring the flavone content of the peanut meal before and after the low-temperature continuous phase-change extraction, wherein the difference value is the flavone content in the peanut meal oil.
Method for analyzing polyphenol content spectrophotometry, which is a method for detecting polyphenol in vegetable oil according to LS/T6119-2017 grain oil
1g of the oil sample (accurate to 0.0001 g) was weighed into a 10mL centrifuge tube, 2mL of 80% (v/v) methanol solution and 2mL of n-hexane were added, the mixture was centrifuged with vortexing at 5000r/min for 5min, the lower layer solution was retained, the extraction was repeated 2 times, and the 3 extracts were combined.
And (3) preparation of a standard substance: accurately weighing 20mg of gallic acid, mixing and dissolving with 80% (v/v) methanol solution, and fixing the volume to 100mL to obtain 200 mug/mL mixed standard stock solution, and gradually diluting into 10, 20, 30, 40, 50 and 60 mug/mL mixed standard use solution.
The Folin-Ciocalteau method was used. Respectively sucking 0.5mL of extracting solution and standard solution into a 10mL centrifuge tube, adding 0.5mL of Fu Lin Fen, shaking up and reacting for 3min, adding 2mL of 7.5% (w/v) saturated sodium carbonate solution and 6.5mL of distilled water, shaking up and reacting for 1min, placing in a dark place for 1h, measuring the light absorption value by an ultraviolet spectrophotometer at 765nm, and performing a blank test.
The calculation formula is as follows:
x-the content of polyphenols in vegetable oils in micrograms per gram (. Mu.g/g)
C-the concentration of polyphenols is determined from the standard curve in micrograms per milliliter (μg/mL)
D-dilution multiple after constant volume of sample, undiluted to 1
m-sample mass in grams (g)
Resveratrol content analysis method
1g of an oil sample (accurate to 0.0001 g) is weighed, 2mL of 100% (v/v) methanol solution and 2mL of n-hexane are added, the mixture is subjected to ultrasonic treatment (40 kHz,150 w) for 30min, the mixture is centrifuged at 5000r/min for 5min, the lower layer solution is removed, the mixture is dried by nitrogen, 100 mu L of methanol solution is taken for redissolution, and the mixture is subjected to organic filter membrane of 0.45 mu m and stored in a dark place, and 10 mu L of sample is taken for HPLC analysis. Accurately weighing 1mg of resveratrol and resveratrol glycoside standard, dissolving with pure methanol solution, fixing volume into 100mL volumetric flask to obtain 10ug/mL mixed standard stock solution, gradually diluting to 0.1, 0.2, 0.5, 1.0 and 2.0 μg/mL mixed standard use solution, and storing in dark place.
High performance liquid chromatography measurement conditions: c18 column, acetonitrile: 0.1% phosphoric acid water = 28:72; isocratic elution at 1.0mL/min, the wavelength of an ultraviolet detector is 306nm, the column temperature is 30 ℃, and the sample injection amount is 10uL.
The extraction rate and the component content detection results of the peanut meal oil extracted in the examples and the comparative examples are shown in table 1.
TABLE 1 peanut meal oil extraction and component content
Group of | Extraction yield (%) | Flavone content (mg/g) | Polyphenol content (μg/g) | Resveratrol content (mug/g) |
Example 1 | 98.54 | 1.30 | 28.62 | 16.10 |
Example 2 | 97.25 | 1.38 | 30.42 | 15.78 |
Example 3 | 98.61 | 1.46 | 33.287 | 16.48 |
Example 4 | 99.03 | 1.11 | 33.80 | 3.92 |
Example 5 | 97.65 | 1.23 | 34.65 | 2.84 |
Example 6 | 98.23 | 1.33 | 36.70 | 3.46 |
Comparative example 1 | 69.88 | 0.03 | 14.06 | 4.26 |
Comparative example 2 | 84.72 | 0.66 | 20.42 | 10.27 |
Comparative example 3 | 75.62 | 0.52 | 18.62 | 8.32 |
Comparative example 4 | 52.66 | 0.25 | 10.77 | 3.78 |
The results show that the extraction rate of peanut oil in peanut meal in the embodiment of the invention is higher than 97%, the highest extraction rate can reach 99.03%, and the extraction rate is obviously superior to that of the comparative example. By detecting the components of the extracted peanut meal oil, the content of flavone, polyphenol and resveratrol in the oil extracted by the embodiment of the invention is higher, which indicates that the extraction technology can enrich beneficial components in the extracted oil to a greater extent, does not damage the components, and is richer in nutrient components than the comparative example.
It should be noted that the above embodiments are merely for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and that other various changes and modifications can be made by one skilled in the art based on the above description and the idea, and it is not necessary or exhaustive to all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (5)
1. The application of a method for extracting peanut meal oil by utilizing low-temperature continuous phase change in improving the content of flavone, polyphenol and resveratrol in the peanut meal oil is characterized by comprising the following steps of:
s1, drying a peanut meal raw material, controlling the water content to be less than or equal to 6%, and crushing to 20-60 meshes to obtain peanut meal powder;
s2, loading the peanut meal processed in the step S1 into an extraction kettle of a continuous phase change extraction device, and adding ethanol for soaking treatment;
s3, carrying out low-temperature continuous phase-change extraction on the peanut meal powder treated in the step S2 to obtain a peanut meal oil product; the technological conditions of the low-temperature continuous phase-change extraction are as follows: putting peanut meal powder into an extraction kettle, compressing an extractant into liquid at the extraction temperature of 40-65 ℃ and the extraction pressure of 0.3-1.0 Mpa, flowing through the extraction kettle at the flow rate of 60-80L/h, continuously extracting for 30-110 min, and then putting the extracted peanut meal oil into an analysis kettle, wherein the analysis temperature is 50-80 ℃ and the analysis pressure is 0.1-0.4 Mpa; the extractant is changed into gas by heating and decompressing, then is changed into liquid by instant compression and then flows through an extraction kettle to re-extract the materials, the solvent passing through the extraction kettle carries oil into a resolution tank, and the peanut meal oil product is obtained after resolution;
the concentration of the ethanol in the step S2 is 50-70%, the ratio of the feed liquid to the v is 1:1-1:3, and the soaking is carried out for 1-3h;
the extractant in the step S3 is n-butane.
2. The use according to claim 1, characterized in that the low temperature continuous phase change extraction step S3 is cycled a plurality of times.
3. The use according to claim 1, wherein the extraction temperature in step S3 is 50 ℃ to 60 ℃ and the extraction pressure is 0.4MPa to 0.7MPa.
4. The use according to claim 1, wherein the extractant flow rate in step S3 is 80L/h.
5. The use according to claim 1, wherein the resolving temperature in step S3 is 55 ℃ to 75 ℃ and resolving pressure is 0.35MPa.
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