Preparation method of sea cucumber active oil

Through the combination of intelligent extraction controller and subcritical fluid extraction method, the temperature, pressure and solvent injection amount are dynamically adjusted, and the problems of low solvent extraction efficiency, insufficient oil purity and safety hazards in the existing sea cucumber oil extraction process are solved, and efficient and environmentally friendly sea cucumber oil extraction is achieved, improving the bioactivity and market competitiveness of the oil.

CN120059844APending Publication Date: 2025-05-30QINGDAO MOON BAY BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510251072.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-04
Publication Date
2025-05-30

AI Technical Summary

Technical Problem

In the existing sea cucumber oil extraction process, the ethanol extraction process is complex, the extraction rate is low, and the solvent residue problem is serious. The carbon dioxide supercritical extraction method equipment is expensive, the operation requirements are high, and there are hidden dangers in production safety. The high temperature and high pressure environment leads to low solvent extraction efficiency, insufficient oil purity, degradation of heat-sensitive components, odor generation, and low solvent recovery efficiency.

Method used

By introducing an intelligent extraction controller, combined with the fine regulation of subcritical fluid extraction method, the temperature, pressure and solvent injection amount are dynamically adjusted in real time to ensure the balance of solubility, extraction efficiency and flavor, carbon dioxide is used as a solvent, and the solvent recovery process is finely regulated to improve the solvent recovery efficiency.

Benefits of technology

It realizes efficient and environmentally friendly sea cucumber oil extraction, maximizes the preservation of key nutrients and flavors, improves the bioactivity, flavor and taste stability of the oil, reduces production costs and energy waste, and avoids safety hazards and high costs of high-pressure equipment.

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Abstract

The invention relates to the technical field of sea cucumber oil, and particularly discloses a sea cucumber active oil preparation method, which is used for solving the problems of low solvent extraction efficiency, insufficient oil purity, thermosensitive component degradation, flavor component loss and solvent waste in the traditional sea cucumber oil extraction process, and comprises the steps of raw material pretreatment, subcritical fluid extraction, solvent recovery and desolvation, and refining. The temperature, the pressure and the solvent injection amount are monitored and adjusted in real time through the intelligent extraction controller in combination with solubility feedback and flavor correction factors; by accurately controlling the temperature, the pressure and the solvent injection amount and dynamically adjusting the extraction time and the flavor correction factor, efficient and environment-friendly oil extraction is achieved, and meanwhile key nutritional ingredients and flavor are reserved to the maximum extent.
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Description

Technical Field

[0001] The present invention relates to the technical field of sea cucumber oil production, and more specifically, to a method for preparing active sea cucumber oil. Background Art

[0002] The existing sea cucumber oil extraction processes mainly adopt the ethanol extraction method and the carbon dioxide supercritical extraction method. Among them, the ethanol extraction method has a complex process, a low extraction rate, and relatively serious solvent residue problems. The carbon dioxide supercritical extraction method has expensive equipment, high operation requirements, and potential production safety hazards. In the Chinese invention patent "An Extraction Process of Deep-Sea Sea Cucumber Oil" with the publication number 201610927071, an extraction process of deep-sea sea cucumber oil for extracting oil components is disclosed. Special equipment is used to liquefy carbon dioxide into a liquid under an ultra-high pressure of 7 to 30 MPa / ㎡. There are safety problems in the control of the production process, which requires very high requirements for operators. Moreover, the carbon dioxide supercritical extraction device is expensive, restricting its large-scale production, and also restricting the development and utilization of sea cucumber oil. More importantly, it is difficult to precisely control the pressure during the ultra-high pressure extraction process, resulting in low solvent extraction efficiency, insufficient oil purity, and the destruction of thermosensitive components in a high-temperature and high-pressure environment (unsaturated fatty acids and collagen are prone to oxidation reactions or thermal degradation under high-temperature conditions, resulting in a reduction in their biological activities. The oxidation reaction of unsaturated fatty acids produces free radicals and peroxides at high temperatures, which not only reduces the biological activities but also causes the finished oil to have an odor and reduce its flavor). The inaccurate control of pressure and time will lead to uneven extraction effects of the solvent. Excessive pressure causes over-extraction of the oil, dissolving non-target components, while too low pressure results in incomplete oil extraction, unable to meet the high-efficiency and high-quality requirements of sea cucumber oil extraction, and insufficient solvent recovery efficiency, leading to energy waste and solvent loss. Summary of the Invention

[0003] In order to overcome the above-mentioned defects of the prior art, the present invention provides a method for preparing active sea cucumber oil, which realizes efficient and environmentally friendly oil extraction by precisely controlling the temperature, pressure, solvent injection amount, and dynamically adjusting the extraction time and flavor correction factor, while maximizing the retention of key nutrients and flavors.

[0004] Sea cucumber oil is rich in unsaturated fatty acids (such as Omega-3 fatty acids), collagen, and trace elements, etc. It is widely used in health products and nutritional supplements, aiming to enhance cardiovascular function, improve immunity, slow down aging, etc. For high-end foods and seasonings, using sea cucumber oil as a natural oil component not only provides flavor but also has edible nutritional value. Therefore, flavor and impact value are also very important. The generation of off-flavors caused by improper control of temperature and pressure damages its taste and flavor and reduces consumers' acceptance. Therefore, the heat-sensitive active ingredients and flavor of sea cucumber oil affect the market competitiveness of products and consumers' acceptance. Therefore, during the extraction process, temperature and pressure need to be precisely controlled to ensure the maximum retention of active ingredients and the stability of flavor and taste.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for preparing sea cucumber active oil, including selection and cleaning, freeze-drying, freeze-dried pulverization, sieving, and supercritical carbon dioxide extraction. The temperature, pressure, and solvent injection amount are monitored and adjusted in real time by an intelligent extraction controller in combination with solubility feedback and a flavor correction factor, including:

[0007] Step 1, raw material pretreatment: Clean the raw material of sea cucumber intestines and eggs, then place the cleaned raw material in a centrifuge for dehydration. After dehydration, spread it flat on a freeze-drying tray. The freeze-drying trays are placed at equal distances for raw material transmission and the raw material transmission pictures are processed based on machine learning classification. Select qualified raw materials and transfer them to a freeze-dryer. Freeze-dry the raw material of sea cucumber intestines and eggs at 60 - 80 °C, and a pulverizer pulverizes the raw material of sea cucumber intestines and eggs into uniform particles of 20 - 30 meshes.

[0008] Step 2, subcritical fluid extraction: Put the particles of the raw material of sea cucumber intestines and eggs and an entrainer into an extraction tank, and perform a pre-vacuum treatment on the extraction tank and a separation tank through a vacuum pump. Use a metering pump to quantitatively inject a solvent to start extraction. During the extraction process, the temperature gradually rises from 40 °C to 50 °C, and the pressure gradually rises from 0.3 MPa to 0.5 MPa. According to the change in solubility, the intelligent extraction controller adjusts the temperature, pressure, and solvent injection amount in real time to ensure the balance between solubility and flavor. Optimize the retention of flavor components through the flavor correction factor formula, and automatically adjust the extraction parameters of the extraction process according to the feedback signal.

[0009] Step 3, solvent recovery and desolvation: The mixture of the solvent and the extract is transferred from the extraction tank to the separation tank at a rate of 0.5 - 1 L / min while maintaining a temperature of 20 - 25°C. The separation tank is heated using a hot water tank and a hot water pump for 30 - 60 minutes, maintaining a temperature of 45 - 55°C. The solvent gas enters the compressor and is pressurized to 5 - 8 MPa. The solvent gas is condensed into a liquid through a condenser, with the condensation temperature between -10 - 0°C and the condensation time of 20 - 30 minutes. The target extract that has completed desolvation in the separation tank is collected as raw material oil into the refining equipment from the separation tank at a rate of 1 - 2 L / min while maintaining a temperature of 30 - 40°C;

[0010] Step 4, refining: The raw material oil is degummed to obtain degummed oil, then alkali-refined to remove acid to obtain alkali-refined oil, and then centrifugally separated to obtain alkali-refined oil. The alkali-refined oil is subjected to decolorization and deodorization treatments, and the supernatant is used as the refined oil.

[0011] As a further solution of the present invention, in Step 2, the intelligent extraction controller dynamically adjusts the extraction pressure based on the current solubility, the initially set extraction pressure, and the extraction time using the extraction pressure dynamic adjustment formula. The extraction pressure dynamic adjustment formula is:

[0012] P opt =P ini +(k 2 ·S oil (P,T)·t ext )

[0013] In the formula: P is the pressure set during the extraction process, T is the temperature set during the extraction process, P opt is the pressure dynamically adjusted according to the solubility and the extraction time, P ini is the initially set extraction pressure, equal to 0.3 MPa, k 1 is the pressure adjustment coefficient, obtained by analyzing the relationship between the solubility and the extraction pressure through experimental data, t ext is the optimal extraction time, dynamically adjusted according to the solubility and the feedback signal, S oil (P,T) is the solubility of the current solvent at the given pressure P and temperature T.

[0014] As a further solution of the present invention, in Step 2, the intelligent extraction controller analyzes and obtains the solubility of the solvent by considering the dual effects of the extraction temperature and the extraction pressure on the material using the solubility analysis formula. The solubility analysis formula is:

[0015]

[0016] In the formula: S oil,0 is the standard solubility, determined according to the solvent type, k 2 is the pressure influence coefficient, obtained through experimental analysis, E αIt is the activation energy required for the dissolution process, which is obtained by experimentally measuring the energy demand of solvents to dissolve oils and fats. R is the gas constant, which is equal to 8.314 J / (mol*K).

[0017] As a further solution of the present invention, in step 2, the intelligent extraction controller uses a dynamic adjustment formula for the solvent injection amount based on the product of the current solubility, the target oil volume, and the optimal extraction time, multiplied by the linear adjustment amount of the current extraction time, and the ratio of the initial solvent volume to dynamically adjust the solvent injection amount during the extraction process. The solvent injection amount formula is:

[0018]

[0019] Where: t is the current time, V sol (t) is the injection volume of the solvent at the current moment, V oil is the target grease volume, k 3 is the solvent injection adjustment coefficient, V sol,ini It is the volume of solvent initially injected during the extraction process, which is calculated based on experimental data according to the solvent's ability to dissolve oils and fats and the material properties.

[0020] As a further solution of the present invention, in step 2, in the solvent injection formula of the intelligent extractor, the optimal extraction time is dynamically adjusted according to the change of solubility based on a preset optimal extraction time analysis formula, and the optimal extraction time analysis formula is:

[0021]

[0022] Where: k 4 is the solubility constant adjustment coefficient, which is obtained based on the relationship between the amount of solvent and the extraction time, k 5 is the solubility change rate constant, which is obtained by analyzing the effect of solubility change over time on extraction time.

[0023] As a further solution of the present invention, in step 2, the intelligent extraction controller performs real-time monitoring and dynamic adjustment of the extraction process based on a comprehensive control feedback formula combined with solubility feedback and flavor correction factor. The comprehensive control feedback formula is:

[0024]

[0025] Where: F con It is a comprehensive control feedback signal used to dynamically adjust temperature, pressure, solvent injection volume, flavor correction factor, ΔS oil (P,T,t) is the increment of solubility at the current time as a function of extraction time, k 6 is the influence coefficient of changes in temperature, pressure and solvent injection volume on the extraction efficiency and flavor components, obtained through experimental data analysis.

[0026] As a further solution of the present invention, in step two, the flavor correction factor in the comprehensive control feedback formula in the intelligent extractor analyzes and obtains the retention ability of flavor components at the current extraction temperature, its change amount, extraction pressure, and its change amount. The formula for the flavor correction factor is as follows:

[0027] γ fla =f(T,P,S oil (P,T))·(1+k fla ·ΔT·ΔP)

[0028] In the formula: γ fla is the flavor correction factor, f(T,P,S oil (P,T)) is the flavor correction function, which is obtained by analyzing the changes of flavor components under different temperature, pressure, and solubility conditions based on experimental data. k fla is the coefficient of the influence of flavor components by temperature and pressure, which is obtained by analyzing experimental data. ΔT is the temperature change amount, and ΔP is the pressure change amount.

[0029] As a further solution of the present invention, in step three, the solvent used is carbon dioxide.

[0030] As a further solution of the present invention, in step four, the refining process specifically includes:

[0031] Step 41, degumming: Select the crude oil obtained in step three, add a phosphoric acid solution with a mass concentration of 85%, and the mass ratio of the added phosphoric acid solution is set according to the mass of the crude oil. The mass of the crude oil is 0.2% - 0.5% of the mass of the phosphoric acid solution. Stir and mix for 15 - 30 minutes, and the oil treated with phosphoric acid is separated by a centrifuge to obtain degummed oil as the supernatant;

[0032] Step 42, caustic refining to remove acid: Add a sodium hydroxide solution with a Baume degree of 5 - 10°Bé to the degummed oil, heat to 80 - 90°C, keep for 1 - 15 seconds, and stir evenly at the same time to obtain a saponification mixture;

[0033] Step 43, centrifugal separation: Use a centrifuge to separate at a rotational speed of 5000 - 8000 rpm for 5 - 10 minutes, and filter to obtain the supernatant as the caustic - refined oil;

[0034] Step 44, decolorization and deodorization: Use 2% - 3% of the mass of the caustic - refined oil of activated carbon, keep the temperature at 50 - 60°C for 30 minutes for decolorization, then heat to 70 - 80°C, and introduce air at a ventilation rate of 5 - 10 m 3 / h for 30 - 60 minutes to obtain the crude oil;

[0035] Step 45, filtering impurities and precipitation: Filter the mixture obtained in Step 44 using a 10 - 20 μm filter mesh, and use the supernatant as the refined oil.

[0036] Technical effects of the method for preparing sea cucumber active oil proposed by the present invention:

[0037] By introducing an intelligent extraction controller and combining the fine regulation of the subcritical fluid extraction method, the present invention realizes the real-time dynamic adjustment of temperature, pressure, and solvent injection volume to ensure the balance of solubility, extraction efficiency, and flavor, solving the technical problems in the traditional carbon dioxide supercritical extraction method such as low solvent extraction efficiency, insufficient oil purity, degradation of heat-sensitive components, generation of off-flavors, and low solvent recovery efficiency under high temperature and high pressure. At the same time, by avoiding the safety hazards and high costs of high-pressure equipment, the extraction process of sea cucumber oil is optimized, the biological activity, flavor, and taste stability of the oil are improved, the market competitiveness and consumer acceptance are enhanced, the production cost and energy waste are reduced, and the large-scale production of high-efficiency, safe, and environmentally friendly sea cucumber oil is realized. Description of the Drawings

[0038] Figure 1 It is a flow chart of the method for preparing sea cucumber active oil proposed by the present invention;

[0039] Figure 2 It is a flow chart of the refining of the present invention;

[0040] Figure 3 It is a schematic diagram of the equipment connection of the method for preparing sea cucumber active oil of the present invention;

[0041] In the figure: 1 - solvent storage tank, 2 - extraction tank, 3 - separation tank, 4 - refined oil collection bottle, 5 - metering pump, 6 - compressor, 7 - condenser, 8 - hot water tank, 9 - hot water pump, 10 - pressure gauge, 13 - vacuum pump, 14 - intelligent extraction controller. Detailed Embodiments

[0042] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0043] In the present invention, the ultra-high pressure in subcritical ultra-high pressure extraction refers to the extraction process using a pressure between 7 and 30 MPa / ㎡. This high-pressure environment is to make the solvent enter the liquid state and remain in the subcritical state, thereby improving the extraction efficiency of the solvent, enabling the solvent to effectively dissolve and extract the active ingredients in sea cucumber intestine and eggs, ensuring that the extracted oil components have the required purity and biological activity. At the same time, such a high-pressure environment needs to be precisely controlled to avoid damage and dissolution of heat-sensitive components caused by excessive pressure. In sea cucumber oil, the main heat-sensitive components include unsaturated fatty acids, collagen, and other components related to nutrition and biological activity, especially Omega-3 fatty acids such as EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid), which play important roles in aspects such as cardiovascular health, immune system enhancement, and anti-inflammatory effects. Unsaturated fatty acids are prone to oxidation reactions at high temperatures, generating free radicals and peroxides, which in turn damage their biological activity and even affect the flavor and stability of the oil. Sea cucumber oil contains abundant collagen, and these components have the effects of enhancing skin elasticity, anti-aging, and promoting joint health. Collagen is prone to thermal degradation at high temperatures, resulting in the destruction of its structure and the loss of biological activity. Trace elements such as zinc and selenium make important contributions to immune function and antioxidant capacity. Excessive temperature will destroy their stability and reduce their bioavailability.

[0044] Example 1

[0045] As Figure 1 shown, the preparation method of sea cucumber active oil includes selection and cleaning, freeze-drying, freeze-dried pulverization, sieving, and carbon dioxide supercritical extraction. The temperature, pressure, and solvent injection amount are monitored and adjusted in real time by an intelligent extraction controller in combination with solubility feedback and flavor correction factors, including:

[0046] Step 1, raw material pretreatment: Clean the raw materials of sea cucumber intestine and eggs, then place the cleaned raw materials in a centrifuge for dehydration. After dehydration, spread them evenly on the freeze-drying tray. The freeze-drying trays are placed at equal distances for raw material transmission and the raw material transmission pictures are processed based on machine learning classification. Select qualified raw materials and transfer them to the freeze-dryer. Freeze-dry the raw materials of sea cucumber intestine and eggs at 60-80°C, and the pulverizer pulverizes the raw materials of sea cucumber intestine and eggs into uniform particles of 20-30 mesh.

[0047] Step 2, subcritical fluid extraction: Put the sea cucumber intestine and egg raw material particles and the entrainer into the extraction tank, and perform a pre-vacuum treatment on the extraction tank and the separation tank through a vacuum pump. Use a metering pump to quantitatively inject the solvent to start the extraction. During the extraction process, the temperature gradually rises from 40°C to 50°C, and the pressure gradually rises from 0.3 MPa to 0.5 MPa. According to the change of solubility, the intelligent extraction controller adjusts the temperature, pressure, and solvent injection amount in real time to ensure the balance between solubility and flavor. Optimize the retention of flavor components through the flavor correction factor formula, and automatically adjust the extraction parameters of the extraction process according to the feedback signal;

[0048] Step 3, solvent recovery and desolventization: The mixture of the solvent and the extract is transferred from the extraction tank to the separation tank at a rate of 0.5 - 1 L / min, maintaining a temperature of 20 - 25°C. Use a hot water tank and a hot water pump to heat the separation tank for 30 - 60 minutes, maintaining a temperature of 45 - 55°C. The solvent gas enters the compressor and is pressurized to maintain 5 - 8 MPa. The solvent gas is condensed into a liquid through a condenser, with the condensation temperature between -10°C and 0°C and the condensation time of 20 - 30 minutes. The target extract that has completed desolventization in the separation tank is collected from the separation tank at a rate of 1 - 2 L / min, maintaining a temperature of 30 - 40°C, and the raw material oil is collected into the refining equipment;

[0049] Step 4, refining: The raw material oil is degummed to obtain degummed oil, then alkali-refined to remove acid to obtain alkali-refined oil, and then centrifugally separated to obtain alkali-refined oil. The alkali-refined oil is subjected to decolorization and deodorization treatments, and the supernatant is used as the refined oil.

[0050] It should be noted that in Step 3, the solvent used is carbon dioxide.

[0051] To clearly illustrate the technical effects of the above technical solutions, specific illustrations are made by setting up an experimental group and a control group. The experimental group adopts a method for extracting sea cucumber intestine and egg oil based on subcritical fluid ultra-high pressure fine regulation, which includes the dynamic adjustment of the real-time temperature, pressure, and solvent injection amount of the intelligent extractor and the use of carbon dioxide as the solvent. The control group adopts the traditional carbon dioxide supercritical extraction method, using traditional equipment and conventional extraction parameters, without fine regulation of temperature, pressure, and solvent injection amount, and using carbon dioxide as the solvent. The experimental steps are as follows:

[0052] Step 1, conduct two groups of experiments under the same raw material conditions;

[0053] Step 2, record and compare the changes in temperature, pressure, and solvent injection amount during the extraction process for each group;

[0054] Step 3, after the extraction is completed, collect the oil samples for analysis and record the relevant data. The experimental data are shown in Table 1:

[0055] Table 1 Comparison table of experimental result data

[0056]

[0057]

[0058] It can be seen from the data comparison in Table 1 that by using an intelligent extraction controller to combine solubility feedback and flavor correction factors for real-time monitoring and dynamic adjustment of temperature, pressure, and solvent injection volume, the extraction process can be precisely controlled to ensure the balance between solubility and flavor, thereby improving the extraction efficiency and the purity of the oil. At the same time, it avoids the degradation and oxidation reactions of heat-sensitive components (such as unsaturated fatty acids and collagen) under high-temperature and high-pressure conditions in traditional methods. Using the flavor correction factor formula to optimize the retention of flavor components can prevent the generation of off-flavors or flavor loss caused by improper temperature and pressure control, ensuring the stable flavor and taste of sea cucumber oil, and enhancing the market competitiveness and consumer acceptance of the product. Using carbon dioxide as a solvent instead of traditional ethanol or other organic solvents solves the problem of solvent residues and reduces the safety hazards in the operation of high-pressure equipment. As a non-toxic and recyclable solvent, carbon dioxide not only reduces environmental pollution but also improves the environmental friendliness of extraction. By finely regulating the solvent recovery process and using a compressor and condenser to recover carbon dioxide solvent, efficient solvent recovery is ensured and energy waste is reduced. This not only improves energy utilization efficiency but also reduces production costs. Through the application of subcritical fluid extraction technology, the high equipment costs, operational complexity, and potential risks of the high-temperature and high-pressure environment in traditional ultra-high-pressure carbon dioxide extraction methods are avoided, and an efficient, safe, and environmentally friendly sea cucumber oil extraction process is achieved.

[0059] As Figure 2 shown, in Step 4, the refining process specifically includes:

[0060] Step 41, degumming: Select the crude oil obtained in Step 3, add a phosphoric acid solution with a mass concentration of 85%, and the mass ratio of the added phosphoric acid solution is set according to the mass of the crude oil, where the mass of the crude oil is 0.2% - 0.5% of the mass of the phosphoric acid solution. Stir and mix for 15 - 30 minutes, and the oil treated with phosphoric acid is separated by a centrifuge to obtain degummed oil as the supernatant;

[0061] Step 42, caustic refining for deacidification: Add a sodium hydroxide solution with a Baume degree of 5 - 10°Bé to the degummed oil, heat to 80 - 90°C, and maintain for 1 - 15 seconds while stirring evenly to obtain a saponification mixture;

[0062] Step 43, centrifugal separation: Use a centrifuge to separate at a rotational speed of 5000 - 8000 rpm for 5 - 10 minutes, and filter to obtain the supernatant as the caustic-refined oil;

[0063] Step 44, decolorization and deodorization: Use activated carbon accounting for 2% - 3% of the refined oil by mass, maintain the temperature at 50 - 60°C for 30 minutes for decolorization, then heat to 70 - 80°C, and introduce air at a ventilation volume of 5 - 10 m 3 / h for 30 - 60 minutes to obtain crude oil;

[0064] Step 45, filter impurities and precipitate: Filter the mixture obtained in Step 44 using a filter screen with a pore size of 10 - 20 μm, and use the supernatant as the refined oil.

[0065] This refining process improves the purity and quality of sea cucumber oil through steps such as degumming, alkali refining for acid removal, centrifugal separation, decolorization, deodorization, and filtration. Impurities are removed through degumming, acidic substances are effectively removed through alkali refining for acid removal, the oil is finely purified through centrifugal separation, pigments and odor components are removed through decolorization and deodorization treatments, and at the same time, the transparency and taste of the oil are further improved by filtering impurities and precipitate. Finally, high-quality refined oil that is pure, odorless, and has a transparent color is obtained, enhancing the market competitiveness of the product and the acceptance of consumers. In addition, these steps also optimize the retention of bioactive components in the oil, ensuring the nutritional value and flavor stability of the product and meeting the requirements of the high-end market for high-quality sea cucumber oil.

[0066] Example 2

[0067] The difference between Example 2 and Example 1 of the present invention is that this example introduces the real-time monitoring and adjustment of temperature, pressure, and solvent injection volume in a method for preparing sea cucumber active oil through an intelligent extraction controller in combination with solubility feedback and flavor correction factors.

[0068] It should be noted that in Step 2, the extraction pressure is dynamically adjusted based on the current solubility, the initially set extraction pressure, and the extraction time using the extraction pressure dynamic adjustment formula. The extraction pressure dynamic adjustment formula is:

[0069] P opt =P ini +(k 2 ·S oil (P,T)·t ext )

[0070] In the formula: P is the pressure set during the extraction process, T is the temperature set during the extraction process, P opt is the pressure dynamically adjusted according to solubility and extraction time, P ini is the initially set extraction pressure, equal to 0.3 MPa, k 1 is the pressure adjustment coefficient, obtained by analyzing the relationship between solubility and extraction pressure through experimental data, t ext is the optimal extraction time, dynamically adjusted according to solubility and feedback signals, S oil(P, T) is the solubility of the current solvent at a given pressure p and temperature T.

[0071] By adjusting the extraction pressure in real time to keep it always in the optimal state, it can be accurately regulated according to the changes in solubility and the dynamic requirements of extraction time, avoiding the low solvent dissolution efficiency or the dissolution of non-target components caused by improper pressure setting during the extraction process. This dynamic adjustment strategy can ensure that the best pressure conditions are always used at different extraction stages, thereby increasing the extraction rate of the target oil, while minimizing unnecessary dissolution losses and reducing energy consumption. Solubility changes with pressure. By adjusting the pressure to optimize the solvent's dissolution ability, it helps to precisely extract the active ingredients in sea cucumber oil, especially improving the selectivity for the target components, avoiding the dissolution of non-target substances, and ensuring the high purity of the oil. Dynamically adjusting the pressure can adjust the operating conditions according to different feedback signals (such as solubility and time changes), ensuring the stability and consistency during the extraction process, thereby improving the quality consistency and controllability of the product.

[0072] It should be noted that in step two, the current solvent solubility is obtained by analyzing the dual effects of extraction temperature and extraction pressure on the material through the solubility analysis formula. The solubility analysis formula is:

[0073]

[0074] In the formula: S oil,0 is the standard solubility, determined according to the solvent type, k 2 is the pressure influence coefficient, obtained through experimental analysis, E α is the activation energy required for the dissolution process, obtained by analyzing the energy requirements for the solvent to dissolve the oil through experimental measurement. R is the gas constant, equal to 8.314 J / (mol*K).

[0075] By combining the dual effects of temperature and pressure on solubility, the solvent's solubility during the extraction process can be more accurately controlled, thereby ensuring that the target oil component is dissolved to the greatest extent. The formula dynamically adjusts the solubility during the extraction process through changes in temperature and pressure, avoiding the negative impact of too high or too low pressure on solubility. By accurately calculating and adjusting the solubility, the solvent's optimal solubility can be maintained throughout the extraction process, thereby significantly improving the extraction efficiency of oils and fats, ensuring that more target components are extracted, and reducing the possibility of dissolving non-target components. The solubility analysis formula provides a scientific basis for solvent selection, enabling it to optimize solubility based on solvent type, activation energy, temperature and pressure changes, ensuring that the solvent's solubility for target components is maximized, improving extraction selectivity and the purity of target components. By adjusting the extraction pressure and temperature to optimize solubility, the waste of solvent and energy caused by excessively high or low pressure or temperature is avoided, thereby reducing solvent loss and energy consumption, and improving the economy and environmental protection of the production process. The solubility analysis formula can provide real-time feedback to the intelligent extraction controller, enabling it to dynamically adjust the extraction parameters according to different temperature and pressure conditions, thereby further improving the refinement and stability of the extraction process and ensuring the quality and flavor stability of the final oil.

[0076] It should be noted that in step 2, the solvent injection amount is dynamically adjusted based on the product of the current solubility, the target oil volume, and the optimal extraction time, multiplied by the linear adjustment amount of the current extraction time, and the ratio of the initial solvent volume. The solvent injection amount formula is:

[0077]

[0078] Where: t is the current time, V Sol (t) is the injection volume of the solvent at the current moment, V oil is the target grease volume, k 3 is the solvent injection adjustment coefficient, V sol,ini It is the volume of solvent initially injected during the extraction process, which is calculated based on experimental data according to the solvent's ability to dissolve oils and fats and the material properties.

[0079] By means of a dynamic adjustment formula for the solvent injection volume, based on the current solubility, the target oil volume, the linear adjustment of the optimal extraction time and the current extraction duration, the solvent injection volume can be precisely adjusted, which can optimize the solvent usage, improve the extraction efficiency, ensure the stability of the extraction process, avoid solvent waste, and at the same time ensure the optimal ratio of the solvent to the oil, reduce the use of too much or too little solvent, thereby increasing the extraction rate and purity of the oil, maximizing the extraction of the target components, avoiding the dissolution of non-target components, reducing energy consumption and production costs, realizing a more environmentally friendly production process, and ultimately enhancing the flavor, quality and retention of bioactive components of sea cucumber oil, ensuring the high purity and stability of the product.

[0080] It should be noted that in step two, the optimal extraction time is dynamically adjusted according to the change in solubility based on a preset optimal extraction time analysis formula. The optimal extraction time analysis formula is:

[0081]

[0082] In the formula: k 4 is the solubility constant adjustment coefficient, obtained by analyzing the relationship between the solvent volume and the extraction time. k 5 is the solubility change rate constant, obtained by analyzing the influence of the change in solubility over time on the extraction time.

[0083] By dynamically adjusting the optimal extraction time through the optimal extraction time analysis formula, based on the change in solubility, the target oil volume, the solvent injection volume and the solubility change rate, it is possible to accurately calculate and adjust the time for each stage in the extraction process to ensure that the dissolution ability of the solvent and the solubility of the target oil are always in the best state, thereby improving the extraction efficiency, maximizing the extraction of the target components, and at the same time avoiding unnecessary dissolution and over-extraction of non-target components. This technology can flexibly adjust the extraction time according to the real-time change in solubility, ensure that the solvent usage in each stage is optimally matched with the oil volume and solubility, prevent incomplete dissolution or over-dissolution caused by too long or too short extraction time, and increase the extraction rate and purity of the oil. Further, the dynamic adjustment of the optimal extraction time can also effectively avoid solvent waste and excessive energy consumption, ensure that the entire extraction process is more efficient and energy-saving, reduce production costs, and improve the quality and stability of the final oil, retaining key components such as unsaturated fatty acids and collagen to the greatest extent.

[0084] It should be noted that in step two, the intelligent extraction controller monitors and dynamically adjusts the extraction process in real time based on the comprehensive control feedback formula in combination with solubility feedback and flavor correction factors. The comprehensive control feedback formula is:

[0085]

[0086] In the formula: F conThe comprehensive control feedback signal is used to dynamically adjust temperature, pressure, solvent injection volume, and flavor correction factor, ΔS oil (P,T,t) is the increment of solubility at the current time with respect to extraction time, k 6 is the influence coefficient of temperature, pressure, and solvent injection volume changes on extraction efficiency and flavor components, obtained through experimental data analysis.

[0087] Through the comprehensive control feedback formula, the intelligent extraction controller monitors and dynamically adjusts the temperature, pressure, solvent injection volume, and flavor correction factor during the extraction process in real time. Based on solubility feedback and flavor correction factor, it can optimize extraction efficiency and the retention of flavor components. By introducing the solubility increment, coefficients of temperature and pressure changes, and flavor correction factor, this technology ensures that the contact between the solvent and the target oil is always in the optimal state, avoiding the dissolution of non-target components, maximizing the retention of key nutrients (such as unsaturated fatty acids and collagen), while optimizing the stability of flavor components, preventing the generation of off-flavors or flavor loss, thereby improving the purity and quality of oil extraction; at the same time, by dynamically adjusting the solvent injection volume and other key parameters, it avoids waste of energy and solvents, reduces production costs, and realizes an efficient, energy-saving, and environmentally friendly production process. Ultimately, this intelligent control system improves the extraction efficiency, purity, flavor, and taste stability of sea cucumber oil.

[0088] It should be noted that in step two, the flavor correction factor obtains the retention ability of flavor components at the current temperature, pressure, and solubility by analyzing the current extraction temperature and its change amount, extraction pressure and its change amount. The formula for the flavor correction factor is:

[0089] γ fla = f(T,P,S oil (P,T))·(1 + k fla ·ΔT·ΔP)

[0090] In the formula: γ fla is the flavor correction factor, f(T,P,S oil (P,T)) is the flavor correction function, obtained by analyzing the changes of flavor components under different temperature, pressure, and solubility conditions based on experimental data. k fla is the coefficient of the influence of flavor components on temperature and pressure, obtained through experimental data analysis. ΔT is the temperature change amount, and ΔP is the pressure change amount.

[0091] Through the flavor correction factor formula, by analyzing the current extraction temperature, pressure and their change amounts, the retention ability of flavor components under different temperature, pressure and solubility conditions can be accurately evaluated, and based on this, the temperature, pressure and solvent injection amount during the extraction process can be dynamically adjusted to maximize the retention of flavor components, avoid flavor loss or off-flavor generation caused by improper temperature and pressure, so as to ensure the flavor stability and taste consistency of sea cucumber oil. By introducing a flavor correction function and a flavor correction factor, this technology enables fine control of the temperature and pressure changes during the extraction process, ensures optimal retention of flavor components at each stage, improves the market competitiveness of the oil and the consumer acceptance, and at the same time avoids the destruction of flavor components by excessive temperature and pressure, achieving efficient and high-flavor oil extraction.

[0092] As Figure 3 shown, in order to implement this improved method proposed by the present invention, the technical solution of this application adopts a set of efficient extraction system, and each key device works together to achieve the best sea cucumber oil extraction effect. First, the solvent storage tank 1 stores the required solvent (carbon dioxide), which is accurately injected into the extraction tank 2 by the metering pump 5 for the extraction process when in use. In the extraction tank, the sea cucumber intestine and egg raw materials are mixed with the solvent, and extraction is carried out under the monitoring of the intelligent extraction controller 14 with controlled temperature and pressure. The extracted mixture is sent to the separation tank 3 for separation of the solvent and the extract, and the solvent is recovered through the compressor 6 and the condenser 7 to ensure the reuse of the solvent. During this process, the vacuum pump 13 helps to maintain an ultra-high pressure environment (between 0.1 MPa and 0.3 MPa) to enhance the dissolution efficiency. The hot water tank 8 and the hot water pump 9 provide the necessary heat source to keep the temperature stable during the extraction and separation processes, while the pressure gauge 10 monitors the pressure in the system in real time to ensure precise control of all operating parameters. Finally, the separated sea cucumber oil is stored in the refined oil collection bottle 4 through the refining process. The entire system dynamically adjusts the temperature, pressure, solvent injection amount, etc. through the intelligent extraction controller 14 to ensure the efficiency, stability and safety of the extraction process, thereby optimizing the oil extraction rate and quality.

[0093] The above is only the specific implementation manner of this application, but the protection scope of this application is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed in this application, and all should be covered by the protection scope of this application. Therefore, the protection scope of this application should be subject to the protection scope of the claims.

[0094] Finally: The above is only the preferred embodiment of the present invention and is not used to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing sea cucumber active oil, comprising selecting and cleaning, freeze drying, freeze drying and crushing, screening, and supercritical carbon dioxide extraction, characterized in that: Temperature, pressure, and solvent injection volume are monitored and adjusted in real time by an intelligent extraction controller combined with solubility feedback and flavor correction factors, including: Step 1, raw material pretreatment: clean the sea cucumber intestines and eggs raw materials, then place the cleaned raw materials in a centrifuge for dehydration, and then spread them on freeze-drying trays after dehydration. The freeze-drying trays are placed equidistantly for raw material transmission and the raw material transmission images are processed based on machine learning classification, and qualified raw materials are selected and transmitted to the freeze dryer. The sea cucumber intestines and eggs raw materials are freeze-dried at 60-80°C, and the sea cucumber intestines and eggs raw materials are crushed into 20-30 mesh uniform particles by a grinder; Step 2, subcritical fluid extraction: put the sea cucumber intestine and egg raw material particles and the entrainer into the extraction tank, and pre-vacuum the extraction tank and the separation tank by a vacuum pump, and use a metering pump to quantitatively inject the solvent to start extraction. During the extraction process, the temperature gradually increases from 40°C to 50°C, and the pressure gradually increases from 0.3MPa to 0.5MPa. According to the change of solubility, the intelligent extraction controller adjusts the temperature, pressure and solvent injection amount in real time to ensure the balance between solubility and flavor, optimizes the retention of flavor components through the flavor correction factor formula, and automatically adjusts the extraction parameters of the extraction process according to the feedback signal; Step 3, solvent recovery and desolventization: the mixture of solvent and extract is transferred from the extraction tank to the separation tank at 0.5-1L / min, maintained at 20-25°C, the separation tank is heated for 30-60 minutes using a hot water tank and a hot water pump, maintained at 45-55°C, the solvent gas enters the compressor and is pressurized, maintained at 5-8MPa, the solvent gas is condensed into liquid by a condenser, the condensation temperature is between -10 and 0°C, the condensation time is 20-30 minutes, the target extract that has completed desolventization in the separation tank is collected from the separation tank at 1-2L / min, maintained at 30-40°C, and the crude oil is collected to the refining equipment; Step 4, refining: the crude oil is degummed to obtain degummed oil, then alkali-refined and deacidified to obtain alkali-refined oil, then centrifuged to obtain alkali-refined oil, the alkali-refined oil is decolorized and deodorized, and the supernatant is used as finished oil.

2. The method for preparing sea cucumber active oil according to claim 1, wherein In step 2, the intelligent extraction controller uses the extraction pressure dynamic adjustment formula to dynamically adjust the extraction pressure based on the current solubility, the initial set extraction pressure and the extraction time. The extraction pressure dynamic adjustment formula is: P opt =P ini +(k2·S oil (P,T)·t ext ) Where: P is the pressure set during the extraction process, T is the temperature set during the extraction process, P opt P is the pressure that is dynamically adjusted according to solubility and extraction time. ini is the initial extraction pressure, which is equal to 0.3 MPa, k1 is the pressure adjustment coefficient, which is obtained by analyzing the relationship between solubility and extraction pressure through experimental data, and t ext is the optimal extraction time, which is dynamically adjusted according to the solubility and feedback signal. pol (P,T) is the solubility of the current solvent at a given pressure P and temperature T.

3. The method for preparing sea cucumber active oil according to claim 2, wherein: In step 2, the intelligent extraction controller considers the dual effects of extraction temperature and extraction pressure on the material through the solubility analysis formula to analyze and obtain the solubility of the solvent. The solubility analysis formula is: Where: S oil,0 is the standard solubility, determined according to the solvent type, k2 is the pressure influence coefficient, obtained through experimental analysis, E α It is the activation energy required for the dissolution process, which is obtained by experimentally measuring the energy demand of solvent dissolving oil. R is the gas constant, which is equal to 8.314 J / (mol*K).

4. The method for preparing sea cucumber active oil according to claim 3, wherein: In step 2, the intelligent extraction controller uses the dynamic adjustment formula of solvent injection volume to dynamically adjust the solvent injection volume during the extraction process based on the product of the current solubility, target oil volume, and optimal extraction time, multiplied by the linear adjustment amount of the current extraction time, and the ratio of the initial solvent volume. The solvent injection volume formula is: Where: t is the current time, V sol (t) is the injection volume of the solvent at the current moment, V oil is the target grease volume, k3 is the solvent injection adjustment coefficient, V sol,ini It is the volume of solvent initially injected during the extraction process, which is calculated based on experimental data according to the solvent's ability to dissolve oils and fats and the material properties.

5. The method for preparing sea cucumber active oil according to claim 4, characterized in that: In step 2, in the solvent injection formula of the intelligent extractor, the optimal extraction time is dynamically adjusted according to the change of solubility based on the preset optimal extraction time analysis formula, and the optimal extraction time analysis formula is: Wherein: k4 is the solubility constant adjustment coefficient, which is obtained by analyzing the relationship between the amount of solvent and the extraction time; k5 is the solubility change rate constant, which is obtained by analyzing the effect of the change of solubility over time on the extraction time.

6. The method for preparing sea cucumber active oil according to claim 4, characterized in that: In step 2, the intelligent extraction controller monitors and dynamically adjusts the extraction process in real time based on a comprehensive control feedback formula combined with solubility feedback and flavor correction factors. The comprehensive control feedback formula is: Where: F con It is a comprehensive control feedback signal used to dynamically adjust temperature, pressure, solvent injection volume, flavor correction factor, ΔS oil (P, T, t) is the increment of solubility at the current time as the extraction time changes, and k6 is the influence coefficient of changes in temperature, pressure, and solvent injection volume on the extraction efficiency and flavor components, which is obtained through experimental data analysis.

7. The method for preparing sea cucumber active oil according to claim 6, characterized in that: In step 2, the flavor correction factor in the comprehensive control feedback formula of the intelligent extractor is analyzed by the current extraction temperature and its variation, the extraction pressure and its variation, to obtain the retention capacity of the flavor components under the current temperature, pressure and solubility. The formula of the flavor correction factor is: γ fla =f(T,P,S oil (P,T))·(1+k fla ·ΔT·ΔP) Where: γ fla is the flavor correction factor, f(T,P,S oil (P,T)) is the flavor correction function, which is obtained based on the experimental data reflecting the changes in flavor components under different temperature, pressure and solubility conditions. fla is the coefficient of the influence of temperature and pressure on flavor components, which is obtained through experimental data analysis. ΔT is the temperature change, and ΔP is the pressure change.

8. The method for preparing sea cucumber active oil according to claim 1, characterized in that: In step three, the solvent used is carbon dioxide.

9. The method for preparing sea cucumber active oil according to claim 1, characterized in that: In step 4, the refining process specifically includes: Step 41, degumming: selecting the crude oil obtained in step 3, adding a phosphoric acid solution with a mass concentration of 85%, wherein the mass ratio of the phosphoric acid solution added is set according to the mass of the crude oil, and the mass of the crude oil is 0.2% to 0.5% of the mass of the phosphoric acid solution, stirring and mixing for 15 to 30 minutes, and separating the oil after phosphoric acid treatment by a centrifuge to obtain degummed oil as a supernatant; Step 42, alkali refining and deacidification: adding a sodium hydroxide solution with a Baume degree of 5 to 10°Bé to the degummed oil, heating to 80 to 90°C, maintaining for 1 to 15 seconds, and uniformly stirring to obtain a saponified mixed solution; Step 43, centrifugal separation: using a centrifugal separator at a rotation speed of 5000-8000 rpm for 5-10 minutes, filtering to obtain a supernatant as alkali oil refining; Step 44, decolorization and deodorization: Use activated carbon with 2% to 3% of the quality of alkali oil refining, maintain 50 to 60°C for decolorization for 30 minutes, then heat to 70 to 80°C and heat at 5 to 10m 3 / h ventilation for 30 to 60 minutes to obtain crude oil; Step 45, filtering impurities and precipitates: Filter the mixture obtained in step 44 using a 10-20 μm filter screen, and use the supernatant as finished oil.

Citation Information

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