Extraction system and method thereof
The extraction device, which combines pressure regulation and multi-frequency ultrasound, solves the problems of long extraction time and low efficiency of traditional extraction methods, and achieves efficient and environmentally friendly extraction results, making it suitable for the food processing industry.
Patent Information
- Application Number
- CN202210107078.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2021-12-27
- Filing Date
- 2022-01-28
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2042-01-28
AI Technical Summary
Existing extraction methods are time-consuming, inefficient, and costly, and have potential impacts on the environment and human health. Traditional ultrasonic extraction suffers from the problem of standing waves reducing cavitation.
A pressure-regulated ultrasonic-assisted extraction device is adopted, which combines inner and outer cylinder structures and a pressure control module. Through pressurization and depressurization extraction, combined with multi-frequency ultrasonic oscillation, the extraction conditions are optimized.
It improves extraction efficiency, shortens extraction time, reduces solvent usage, preserves the natural structure of bioactive substances, reduces impurities, increases extraction rate and purity, and lowers equipment costs.
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Figure CN116392851B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to an extraction system and method thereof, in particular to an extraction system and method thereof applicable to food processing. BACKGROUND
[0002] Generally speaking, "extraction" refers to a method of transferring a compound from one solvent to another due to the difference in solubility (or distribution coefficient) between two mutually insoluble (or slightly soluble) solvents, and through repeated extraction, most of the compound is extracted.
[0003] With the advancement of technology, the extraction method can also be widely applied to food processing. The current common extraction methods include Soxhlet extraction, hot reflux extraction, stirring extraction, immersion extraction, and solid-liquid extraction, etc., and are combined with alkali extraction, acid hydrolysis or alkaline hydrogen peroxide treatment as the main process of extraction. In addition, sometimes enzyme assisted treatment is also combined. However, the above extraction methods usually have the problems of long operation or reaction time, large sample quantity requirement, use of large amounts of organic solvents during the extraction process, and long time heating causing the reduction of the activity of active ingredients, resulting in low concentration of the extracted sample, low extraction efficiency, etc. In addition, in addition to the high labor cost, it may also affect the environment and human health. Therefore, in recent years, novel extraction methods have been studied at home and abroad. For example, due to the high frequency and short wavelength of ultrasonic waves, it has many characteristics such as fixed propagation direction, large energy, strong penetration ability and cavitation effect, and the method of ultrasonic assisted extraction has been started. Compared with traditional extraction methods, ultrasonic extraction can make the extraction liquid fully mixed and contacted, accelerate the swelling and hydration of the material and the solvent, promote the penetration of the solvent, shorten the dissolution equilibrium time of the target active ingredient, improve the diffusion rate of the active ingredient, and improve the shortcomings of traditional solvent extraction. It can effectively shorten the extraction time; at the same time, it can reduce the amount of solvent used and save costs, and it is an environmentally friendly extraction method. In this extraction operation process, it can be operated at low temperature and normal pressure to avoid the volatilization of low-boiling-point substances, and can maximize the retention of the natural structure of bioactive substances and various nutritional ingredients in the extract, avoiding the thermal effects of high-temperature treatment, causing changes, losses, destruction of effective ingredients, and reduction of physiological activity. Problems such as; at the same time, it improves the extraction rate and quality of active ingredients, increases the extraction effect, reduces the dissolution of impurities, has high purity, and the active ingredients are easy to separate and purify; it is also higher than other extraction methods in safety and operation convenience.
[0004] Compared with traditional microwave, supercritical fluid and molecular distillation extraction methods, high intensity ultrasound has lower cost, repeatability, simple operation and easy implementation, and can effectively replace other extraction methods. In industry, it can be applied to improve the extraction of bioactive substances in food, natural plant materials or Chinese herbal medicine field and then be utilized. By changing the extraction conditions, the ultrasound extraction method can solve the problems of time-consuming, effective substance thermal damage and cost reduction in traditional extraction.
[0005] The ultrasound-assisted extraction method has the above industrial advantages. However, single-frequency ultrasound is prone to generate standing waves, which reduces the occurrence of cavitation. The operation of multiple frequencies enhances mechanical vibration and integrates more gas, which leads to an increase in the number of cavitation nuclei. Through the interaction of the cavitation process, the low-frequency negative pressure reduces the cavitation threshold, the resonance frequency is close, the number of cavitation nuclei and the effect are increased, the sound field is also uniform, and different waveforms such as multiple frequency waves appear to improve the cavitation effect. In addition, through the functional component and frequency resonance response, different functional components can be extracted at the same time, and the mechanical equipment is multifunctional. In recent years, pressure-regulated ultrasound-assisted extraction technology has been developed to further improve the extraction efficiency.
[0006] At present, there are few data on pressure-regulated ultrasound-assisted extraction and continuous process data of pressure extraction followed by instant pressure release for decompression extraction in literature and patent searches. Therefore, it is desirable to develop a pressure-regulated ultrasound-assisted extraction device that integrates an ultrasound source and a pressure cooker extraction tank to optimize extraction quality. SUMMARY
[0007] Therefore, to achieve the above purpose, an embodiment of the present application provides an extraction system, wherein the extraction system comprises a containing tank and a pressure control module. The containing tank comprises an outer cylinder, an inner cylinder and a valve. The inner cylinder is arranged in the outer cylinder and has an internal containing space, and an external containing space is formed between the outer cylinder and the inner cylinder. The valve communicates the external containing space and the internal containing space. The pressure control module respectively communicates the external containing space and the internal containing space, thereby respectively and simultaneously controlling the pressure in the external containing space and the pressure in the internal containing space.
[0008] Another embodiment of the present application provides an extraction method, which comprises the following steps. The extraction system as described above is provided. The material to be extracted is placed in the inner cylinder of the containing tank. The material to be extracted contained in the inner cylinder is subjected to a first extraction process. The material to be extracted is introduced into the outer cylinder of the containing tank through the valve. The material to be extracted contained in the outer cylinder is subjected to a second extraction process. The first extraction process comprises applying a first pressure to the material to be extracted, and the second extraction process comprises applying a second pressure to the material to be extracted, and the first pressure is greater than the second pressure.
[0009] The details of one or more embodiments of the subject matter described in this specification are set forth in the accompanying drawings and the description below. Other features, aspects, and advantages of the subject matter will become apparent from the description, the drawings and the claims. BRIEF DESCRIPTION OF DRAWINGS
[0010] In order to clearly understand the present application and the effects achievable by the present application, the technical solutions of the present application will be described in detail below in the form of embodiments combined with the drawings.
[0011] Figure 1 A schematic diagram of an extraction system disclosed by an embodiment of the present application.
[0012] Figure 2 A flowchart of an extraction method disclosed by an embodiment of the present application.
[0013] Figure 3 Extraction rates of mucopolysaccharides from fresh raw materials of Portulaca oleracea L. by ultrasound-assisted extraction with different energy densities (W / g) and pressure adjustment (frequency 28 kHz, solution ratio 1:10 g / mL, time 30 minutes) are shown.
[0014] Figure 4 Effects of ultrasound-assisted extraction with complex frequency combination (15 minutes / 15 minutes) on extraction rates of mucopolysaccharides from fresh raw materials of Portulaca oleracea L. (solution ratio 1:10 g / mL, energy density 0.05 W / g, operation time 30 minutes) are shown.
[0015] Figure 5 Effects of ultrasound-assisted extraction with complex frequency combination on extraction rates of mucopolysaccharides from fresh raw materials of Portulaca oleracea L. (solution ratio 1:10 g / mL, energy density 0.05 W / g, extraction time 30 minutes) are shown.
[0016] Legend of symbols
[0017] 1: extraction system 2: containing tank
[0018] 3: pressure control module 4: sealing cover
[0019] 5: outer shell 6: ultrasound module
[0020] 7: temperature control module 11: first pressure source
[0021] 12: second pressure source 20: inner cylinder
[0022] 22: outer cylinder 24: valve
[0023] 26: outlet pipeline 30: first pressure sensor
[0024] 32: second pressure sensor 34: pressure controller
[0025] 36: pressure safety control module 38: safety valve
[0026] 39: manual pressure relief valve 40: feed inlet
[0027] 50: instrument panel 52: operation panel
[0028] 60: ultrasonic controller 62: ultrasonic power source
[0029] 64: first frequency transmitting component 66: second frequency transmitting component
[0030] 68: sweep module 70: temperature controller
[0031] 72: temperature sensor 74: heating component
[0032] 76: cooling component 111, 121: pipe
[0033] 200: internal accommodation space 202: opening
[0034] 204: side wall 220: external accommodation space 222: opening DETAILED DESCRIPTION
[0035] In order to make the features, content and advantages of the present application clear, the present application is described in detail below with the aid of drawings and in the form of embodiments. The drawings used herein are only schematic and are used to assist in the description of the application.
[0036] The present application mainly provides an extraction system 1 and an extraction method. The extraction system 1 and the extraction method use a high-efficiency method of pressure regulation and ultrasonic assistance to extract a solution of a material to be extracted. Figure 1 A schematic diagram of an extraction system 1 according to an embodiment of the present application is shown in FIG. 1. In this embodiment, the extraction system 1 includes an accommodation tank 2, a pressure control module 3, a sealing cover 4 and a housing 5. The housing 5 is used to accommodate the accommodation tank 2 and the pressure control module 3. The sealing cover 4 is detachably arranged on the accommodation tank 2.
[0037] The housing 2 comprises an inner cylinder 20, an outer cylinder 22, a valve 24 and an outlet pipe 26. The inner cylinder 20 is disposed within the outer cylinder 22 and has an inner housing space 200 for housing the material to be extracted. The outer cylinder 22 and the inner cylinder 20 form an outer housing space 220 therebetween for housing the material to be extracted. The openings 202, 222 at the top of the inner cylinder 20 and the outer cylinder 22 are closed by the sealing cover 4. The inner cylinder 20 and the outer cylinder 22 of the present embodiment are cylindrical in shape and concentric to each other. The height of the inner cylinder 20 and the outer cylinder 22 is substantially the same, while the width of the outer cylinder 22 is greater than that of the inner cylinder 20. The material of the outer cylinder 22 and the inner cylinder 20 is metal, such as stainless steel, and is fixed to the base of the housing 2 by welding. The outlet pipe 26 is disposed on the outer cylinder 22 and is in communication with the outer housing space 220 by means of an openable and closable valve, so as to discharge the extracted liquid from the housing 2 through the outlet pipe 26.
[0038] The sealing cover 4 has an openable and closable inlet 40, which is in communication with the outside of the extraction system 1 and the inner housing space 200 of the inner cylinder 20, so as to place the material to be extracted from the inlet 40 into the inner housing space 200 of the inner cylinder 20.
[0039] The valve 24 penetrates the side wall 204 of the inner cylinder 20, so as to be in communication with the outer housing space 220 of the outer cylinder 22 and the inner housing space 200 of the inner cylinder 20. The valve 24 is an electronically controlled release valve. The material to be extracted can be moved from the inner housing space 200 of the inner cylinder 20 to the outer housing space 220 of the outer cylinder 22 through the valve 24. For example, the valve 24 can be disposed at the bottom end of the side wall 204 of the inner cylinder 20, so as to directly flow the material to be extracted from the inner cylinder 20 to the outer housing space 220 of the outer cylinder 22 by gravity or pressure difference.
[0040] In one embodiment of the present application, a first pressure source 11 is provided, which is in communication with the inner housing space 200 through a pipe 111 penetrating the outer shell 5, the outer cylinder 22 and the inner cylinder 20, so as to provide a first pressure to the inner housing space 200. A second pressure source 12 can also be provided, which is in communication with the outer housing space 220 through a pipe 121 penetrating the outer shell 5 and the outer cylinder 22, so as to provide a second pressure to the outer housing space 220.
[0041] The pressure control module 3 controls the pressure in the outer containment space 220 and the inner containment space 200 respectively and simultaneously. In this embodiment, the pressure control module 3 further comprises a first pressure sensor 30, a second pressure sensor 32 and a pressure controller 34. The first pressure sensor 30 is used to measure the pressure in the inner containment space 200 and transmits a first pressure signal to the pressure controller 34 according to the measured pressure. The second pressure sensor 32 is used to measure the pressure in the outer containment space 220 and transmits a second pressure signal to the pressure controller 34 according to the measured pressure. The pressure controller 34 is used to receive the first pressure signal and the second pressure signal to adjust the pressure in the outer containment space 220 and the pressure in the inner containment space 200.
[0042] In this embodiment, the pressure controller 34 is electrically connected to the first pressure source 11 and the second pressure source 12 to automatically control the pressure provided by the first pressure source 11 and the second pressure source 12 respectively. In this embodiment, the first pressure source 11 can comprise a pressurizing component, such as an air compressor, which applies a pressure capable of being 0 to 7 kgf / cm 2 In one embodiment, the pressurizing component applies a pressure capable of being 0 to 5 kgf / cm 2 In this embodiment, the second pressure source 12 can comprise a depressurizing component, such as a vacuum pump, which applies a pressure capable of being 0 to 700 mmHg. In one embodiment, the depressurizing component applies a pressure capable of being 0 to 500 mmHg. The pressure controller 34 can have a pressure parameter, and according to the pressure parameter and the pressure sensing signal, the pressure controller 34 can selectively control the opening and closing of the first pressure source 11 (the pressurizing component) and the second pressure source 12 (the depressurizing component). When the material to be extracted is treated under high pressure, pressurization can increase the amount of dissolved gas, improve the cavitation effect, and also increase the bubble destruction intensity. When the material to be extracted is treated under reduced pressure, using extraction at low temperature can reduce the amount of solvent dissolved gas, viscosity and surface tension, affecting the principle of ultrasonic cavitation effect, to extract heat-sensitive and easily oxidized substances. When the material to be extracted moves from the inner cylinder under high pressure to the outer cylinder, it is an instantaneous controlled pressure drop process (DIC), and this pressure adjustment method promotes the evaporation, expansion and cavitation of water in the material to increase the contact area and reduce the diffusion resistance to improve the extraction efficiency.
[0043] In this embodiment, the extraction system 1 further comprises a pressure safety control module 36 and a safety valve 38, which is arranged above the sealing cover 4 and is connected to the containment groove 2 (not shown). The pressure value of the safety valve 38 is 1.2 kg / cm 2The pressure safety control module 36 is used to control the safety valve 38 to automatically release the pressure in the tank 2 when the extraction pressure in the tank 2 is abnormal, so as to ensure the safety of the extraction process.
[0044] The extraction system of the present embodiment further comprises a manual pressure release valve 39 disposed above the sealing cover 4 and connected to the tank 2 (not shown). The pressure adjustment value of the manual pressure release valve 39 is between 1 and 30 PSI (pound per square inch). The user can actively operate the manual pressure release valve 39 to reduce the pressure in the tank 2 to the desired value.
[0045] In the present embodiment, the extraction system 1 further comprises an ultrasonic module 6, which includes an ultrasonic controller 60, at least one ultrasonic power source 62, at least one first frequency emitting component 64, and at least one second frequency emitting component 66. The first frequency emitting component 64 is disposed on the outer side surface of the side wall 204 of the inner cylinder 20, so as to provide at least one first frequency ultrasonic oscillation to the inner accommodating space 200. The second frequency emitting component 66 is disposed on the outer side surface of the outer cylinder 22, so as to provide at least one second frequency ultrasonic oscillation to the outer accommodating space 220. In the present embodiment and some embodiments, the first frequency emitting component 64 and the second frequency emitting component 66 can respectively provide multiple frequencies of ultrasonic oscillation to the inner accommodating space 200 and the outer accommodating space 220 simultaneously. For example, the first frequency and the second frequency are 28, 68 and / or 133 kHz.
[0046] In the present embodiment, the extraction system 1 further comprises a frequency sweeping module 68 for measuring the ultrasonic frequency provided by the ultrasonic module 6 to the inner accommodating space 200 and the outer accommodating space 220, respectively. In another embodiment, the extraction system further comprises an energy density measuring device for measuring the energy density applied to the inner accommodating space 200 and the outer accommodating space 220. Thus, the output of the ultrasonic module 6 is adjusted according to the measured ultrasonic frequency or energy density transmitted to the ultrasonic controller 60. The structure and operation of the ultrasonic module 6 and the frequency sweeping module 68 are well known to those skilled in the art, and therefore will not be described in detail in the specification. In the present embodiment, the "energy density" refers to the power provided by the ultrasonic module to the weight of the material to be extracted, and the unit is W / g (watt / gram). In one embodiment, the extraction power can be between 0 and 300 W. In the present embodiment, the frequency sweeping module 68 can include a voltage phase sensor disposed on the bottom or side wall of the tank 2 for regulating the operating voltage phase change, feedback working point to increase the original frequency and reduce the standing wave occurrence.
[0047] In the present embodiment, the extraction system 1 can further comprise a temperature control module 7 for controlling the temperature of the extraction solution in the inner cylinder 20 and the outer cylinder 22. The temperature control module 7 can comprise a temperature controller 70, two temperature sensors 72, a heating assembly 74 and a cooling assembly 76. The temperature sensors 72 are respectively connected to the inner cylinder 20 and the outer cylinder 22 for measuring the temperature of the extraction solution in the inner cylinder 20 and the outer cylinder 22 and generating a temperature sensing signal according to the temperature. The temperature controller 70 is electrically connected to the temperature sensors 72 and receives the temperature sensing signal. The heating assembly 74 is connected to the inner cylinder 20 and the outer cylinder 22 and the temperature controller 70 for heating the extraction solution in the inner cylinder 20 and the outer cylinder 22 according to the instruction of the temperature controller 70. The cooling assembly 76 is connected to the inner cylinder 20 and the outer cylinder 22 and the temperature controller 70 for cooling the extraction solution in the inner cylinder 20 and the outer cylinder 22 according to the instruction of the temperature controller 70. The temperature control module 7 can selectively control the opening and closing of the heating assembly 74 and the cooling assembly 76 according to the set temperature parameter and the temperature sensing signal. In the present embodiment, the extraction temperature can be controlled between 0 to 199°C by using the heating assembly 74 and the cooling assembly 76.
[0048] In addition, the housing 5 can be provided with an instrument panel 50 and an operation panel 52. The instrument panel 50 can display the temperature of the inner cylinder 20 and the outer cylinder 22, the ultrasonic frequency, the energy density, the operation time, the pressure, etc. The operation panel 52 can operate the values of the temperature, the ultrasonic frequency, etc., the operation time, the pressure, etc.
[0049] Figure 2 A flowchart of an extraction method according to an embodiment of the present application. An embodiment of the present application provides an extraction method, which comprises the following steps. In step S110, the extraction system 1 described above is provided.
[0050] In step S120, the extraction solution of the extraction material is placed in the inner cylinder of the accommodation groove. For example, the preparation of the extraction material can include: the extraction material is directly added into a blender with water in the form of fresh raw materials to be beaten into a slurry, thereby serving as the extraction solution; or the extraction material is dried by hot air or freeze-drying method, and then ground into powder to obtain the extraction powder raw material, and then added with an extraction solvent (such as water) to form the extraction solution. In an embodiment, the weight percentage of the raw material and the extraction solvent is 1:10 to 1:50 g / mL.
[0051] In step S130, the extraction material accommodated in the inner cylinder is subjected to a first extraction treatment. In the present embodiment, the first extraction treatment further comprises heating the extraction material to a first temperature. The first extraction treatment can also comprise applying a first ultrasonic oscillation to the extraction material. The first extraction treatment can further comprise applying a first pressure to the extraction material.
[0052] For the heating treatment of the first extraction process, the material to be extracted in the inner cylinder can be heated to a certain value (e.g. maintained at 80°C) within a period of time. In other embodiments, different heating temperatures can be provided to the material to be extracted in different time periods (e.g. the material to be extracted is heated to 60°C in the first 20 minutes and heated to 80°C in the second 40 minutes).
[0053] For the ultrasonic oscillation of the first extraction process, in one embodiment of the first extraction process in step S130, low frequency can be first turned on to effectively destroy the cell walls of the material in the first period (e.g. the first 15, 30, 60 minutes) to increase the diameter of the micropores, shorten the diffusion distance, and improve the efficiency of the internal diffusion. Then, high frequency ultrasonic waves are turned on in the second period (e.g. the next 15, 30, 60 minutes) to improve the vibration effect and enable the solute to rapidly diffuse into the solvent, thereby improving the extraction efficiency.
[0054] In another embodiment of the first extraction process in step S130, low frequency and high frequency ultrasonic waves can be turned on at the same time in a period of time (e.g. 15, 30, 45, 60 minutes) to enhance mechanical vibration, increase the number of cavitation nuclei by incorporating more gas, and make the sound field more uniform, even to the point of generating different waveforms such as multiple frequency waves to improve cavitation effects and thereby increase the extraction efficiency.
[0055] For the pressure application of the first extraction process, similar to the heating treatment described above, the same pressure can be provided in a period of time, or different pressures can be provided in different time periods.
[0056] In the step S130 disclosed in the present application, the ultrasonic oscillation, energy density, pressure application, and temperature control modes in the first extraction process can be adjusted according to the characteristics of the material to be extracted. The same value can be maintained, or different ultrasonic frequencies, energy densities, pressures, and / or temperatures can be provided in different time periods. In some embodiments, at least one of the ultrasonic frequency, pressure, and temperature adjustment can be used in the first extraction process.
[0057] Then, after the first extraction process is completed, the material to be extracted is introduced into the outer cylinder 22 of the holding tank 2 through the valve 24 in step S140. In one embodiment, when the first extraction process has reached a predetermined operation time, the valve 24 can be automatically or manually opened, and the material to be extracted in the inner cylinder 20 falls into the second holding space 220 of the outer cylinder 22 through the valve 24.
[0058] In step S150, a second extraction process is performed on the substance to be extracted accommodated in the outer cylinder 22. The second extraction process includes applying a second pressure to the substance to be extracted, and the first pressure applied in the first extraction process is greater than the second pressure applied in the second extraction process. In the present embodiment, the second extraction process further includes heating the substance to be extracted to a second temperature. The second extraction process further includes applying a second ultrasonic oscillation to the substance to be extracted.
[0059] In an embodiment, similar to the first extraction process, in the second extraction process, the modes of ultrasonic oscillation, pressure application, and temperature control can be adjusted according to the characteristics of the substance to be extracted, and the operation values can be maintained at a constant value, or different ultrasonic frequencies, energy densities, pressures, and / or temperatures can be provided in different time periods. In some embodiments, at least one of the ultrasonic frequency, pressure, and temperature can be adjusted in the second extraction process.
[0060] In the present embodiment, the pressure range of the first pressure and the second pressure is 0-5 kgf / cm 2 ; the temperature range of the first temperature and the second temperature is 0-199°C; and the frequency range of the first ultrasonic oscillation and the second ultrasonic oscillation is 28-133 kHz.
[0061] In the present embodiment, the extraction method further includes measuring the frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation, or measuring the energy density applied to the outer accommodation space and the inner accommodation space, respectively, in steps S130 and S150. Thus, the intensity of the first ultrasonic oscillation and the second ultrasonic oscillation is adjusted according to the measured frequency of the first ultrasonic oscillation and the second ultrasonic oscillation or the measured energy density, to achieve a better ultrasonic oscillation effect.
[0062] In addition, for the pressure application of the first and second extraction processes, in an embodiment, the pressure can be applied only to one of the inner cylinder 20 and the outer cylinder 22, or only the decompression operation can be performed. That is, the pressure can be applied only in the first extraction process, or the decompression can be performed only in the second extraction process, according to actual needs.
[0063] In the embodiments of the present application, the differential pressure operation is performed by the concentric double-cylinder structure design of the inner cylinder 20 and the outer cylinder 22 in the present application, so that the differential pressure operation can be quickly switched from the inner cylinder 20 to the outer cylinder 22 after the pressurization of the inner cylinder 20 is completed. That is, the extraction material can be first pressurized in the inner cylinder 20 of the accommodation groove 2, and then moved to the outer cylinder 22 through the valve 24. In the process of moving the extraction material from the pressurized inner cylinder 20 to the decompressed outer cylinder 22, the instantaneous pressure difference caused by the rapid pressure reduction causes the pressure inside the extraction material to be released outward, and the structure of the raw material is further rapidly destroyed, thereby increasing the release effect of the internal extraction material. In addition, when the outer cylinder 22 is decompressed, the inner cylinder 20 can also simultaneously pressurize the next batch of extraction material, which can be operated semi-continuously, thereby effectively shortening the extraction time and improving the extraction efficiency.
[0064] In the present application, the extraction system 1 can use process combination and structural design to improve the extraction efficiency of biological materials with different characteristics. In an embodiment, a plurality of frequency combination extraction methods are used, that is, low-frequency is first turned on to effectively destroy the cell wall of the extraction material, increase the diameter of the micropore, shorten the diffusion distance, and improve the internal diffusion efficiency; then high-frequency ultrasound is turned on to improve the vibration effect, so that the solute can quickly diffuse into the solvent, thereby improving the extraction efficiency.
[0065] In another embodiment, low-frequency and high-frequency ultrasound can be turned on at the same time to enhance mechanical vibration (for example, 28 kHz, 68 kHz or 133 kHz frequencies are turned on at the same time), and the increase in the number of cavitation nuclei caused by the introduction of more gas can make the sound field more uniform, and even different waveforms such as frequency doubling waves appear to improve the cavitation effect, thereby increasing the extraction efficiency.
[0066] That is, the extraction method of the present application uses the ultrasonic module to oscillate the extraction material to perform ultrasonic-assisted extraction process, and can simultaneously or selectively combine multiple frequencies (different frequencies are operated in sequence), composite operation (different frequencies are turned on at the same time for extraction), temperature control and pressure regulation combination (different extraction pressures are operated in sequence). The control of ultrasonic waves, temperature and pressure in the inner cylinder 20 and the outer cylinder 22 can be adjusted according to actual needs, such as the biological characteristics of the extraction material.
[0067] In step S160, when the second extraction process is completed, the outlet pipeline 26 can be manually or automatically opened to take out the extracted solution.
[0068] The following introduces the results of the pressure regulation and ultrasonic-assisted extraction system 1 provided by the present application applied to the extraction of raw materials of Portulaca oleracea. First, when performing ultrasonic-assisted extraction, water is used as the extraction solvent, the extraction starting temperature is controlled at 40°C, the raw material liquid prepared by pretreatment is placed in the accommodating groove 2 of the extraction system 1, then the pressure control module and the ultrasonic module are used for extraction, and the extraction parameters can be adjusted, and after the extraction liquid is filtered, the content of the index component is analyzed. The ultrasonic extraction operating parameters discussed in this part include liquid ratio, frequency, energy density, complex frequency combination (different frequencies are operated in sequence), complex operation (different frequencies are turned on at the same time for extraction), and pressure regulation combination (different extraction pressures are operated in sequence), etc. The control group is the traditional hot water (95°C) extraction.
[0069] First group of experiments
[0070] In the first group of experiments, the applicant compared the extraction system 1 of the present application with the traditional batch system, and studied the effects of pressure increase and decrease and ultrasonic-assisted extraction on the extraction rate of mucopolysaccharides from the material to be extracted (fresh raw materials of Portulaca oleracea), and the parameters such as pressure, ultrasonic frequency and temperature were the same. The experimental results are shown in Table 1 below:
[0071] Table 1: Mucopolysaccharide extraction rate using the semi-continuous extraction system of the present application and the traditional batch extraction equipment
[0072] Mode of operation Glycosaminoglycan extraction yield (%) Semi-continuous extraction system of the application 59.1 Traditional batch extraction equipment 55.7
[0073] As shown in the above table, the semi-continuous extraction system 1 of the present application has an extraction rate effect of only an increase of 3.4% compared with the traditional batch extraction rate, but the concentric double-cylinder accommodating groove 2 design of the present application has two obvious advantages compared with the batch single-cylinder groove mechanism, as follows:
[0074] First, if similar extraction rates are to be achieved under the same operation time, the batch single-cylinder groove mechanism needs to have two sets of single-cylinder groove test equipment for series operation, but the extraction system with double-cylinder groove of the present application only needs one set to achieve it. Under such operation, the system of the present application can reduce about 35% of the equipment cost (about 110,000 yuan) and 50% of the equipment space compared with the batch mechanism.
[0075] Second, for manufacturing cost and space, if a set of batch single-cylinder groove mechanism is used for extraction, and similar extraction rates to the extraction system 1 of the present application are to be achieved, the pressure needs to be returned to normal pressure during the operation process, and then the pressure increase and decrease equipment needs to be replaced for pressure increase and decrease operation, so the operation time is increased; but the equipment of the present application does not need such a complicated process. Therefore, compared with a set of batch mechanism, the extraction system 1 of the present application can shorten the process time by about 30% (about 15 minutes).
[0076] Second group of experiments
[0077] In the second group of experiments, different forms of raw materials were used, and extraction was carried out for 30 minutes.
[0078] The first raw material form: purslane powder, under normal pressure and 5 kgf / cm³. 2 Under different operating pressures such as 500 mmHg, and using the same experimental conditions such as an ultrasonic frequency of 28 kHz, a solution ratio of 1:20 g / mL, an energy density of 0.05 W / g, and an extraction time of 30 minutes, the extraction rate of mucopolysaccharides was increased by 81.3%, 143.8%, and 123.8% respectively compared with traditional hot water extraction, as shown in Table 2 below.
[0079] Table 2. Extraction rates of purslane powder polysaccharides by traditional water extraction and pressure ultrasonic-assisted extraction
[0080]
[0081] The second type of raw material: purslane fresh raw material slurry, produced under normal pressure at 5 kgf / cm³. 2 Under different operating pressures such as 500 mmHg, and using the same experimental conditions including an ultrasonic frequency of 28 kHz, a material-to-liquid ratio of 1:20 g / mL, an energy density of 0.05 W / g, and an extraction time of 30 minutes, the extraction rate of mucopolysaccharides was increased by 40.9%, 150.3%, and 84.3% respectively compared with traditional hot water extraction, as shown in Table 3 below.
[0082] Table 3. Extraction rates of polysaccharides from fresh purslane raw materials by traditional water extraction and pressure ultrasonic-assisted extraction
[0083]
[0084] The second set of experiments above clearly demonstrates that the extraction rate can be improved regardless of whether atmospheric pressure, pressurized pressure, or reduced pressure is used. Furthermore, the extraction rates using pressurized or reduced pressure are higher than those using traditional water extraction and atmospheric pressure.
[0085] Third group of experiments
[0086] In this experiment, a raw purslane slurry with a material-to-liquid ratio of 1:10 g / mL was used, and different energy densities and extraction times were used for measurement.
[0087] The first scenario involves conducting experiments with different energy densities, such as... Figure 3 As shown: Under the conditions of energy density of 0.05 W / g, frequency of 28 kHz, and extraction time of 30 minutes, its performance under atmospheric pressure, reduced pressure (500 mmHg), and increased pressure (5 kgf / cm²) was as follows. 2The extraction rates of polysaccharides from the samples were 31.0%, 35.9%, and 41.6%, respectively, which were 13.3%, 18.2%, and 23.9% higher than those from traditional hot water extraction (17.7%). When assisted extraction was performed using an energy density of 0.1 W / g, the extraction rates after 30 minutes were [data missing - likely related to extraction rates at atmospheric pressure, reduced pressure (500 mmHg), and increased pressure (5 kgf / cm²).] 2 The extraction rates of polysaccharides were 35.6%, 39.1%, and 46.9%, respectively, which were significantly higher than those of traditional hot water extraction by 17.9%, 21.4%, and 29.2%.
[0088] The second scenario involved experiments with different extraction times: extraction was performed for 120 minutes at an ultrasonic frequency of 28 kHz, a solution ratio of 1:10 g / mL, and an energy density of 0.05 W / g under normal pressure. The mucopolysaccharide extraction rate was 42.0%, approximately equivalent to an extraction time of 5 kgf / cm². 2 The extraction rate of polysaccharides obtained by extraction with an energy density of 0.05 W / g for 30 minutes was 41.6%, which is 13.8% higher than that obtained by traditional hot water extraction for 120 minutes. If extracted at atmospheric pressure with an energy density of 0.1 W / g for 120 minutes, the extraction rate of polysaccharides was 45.8%, which is 6.7% and 17.6% higher than that obtained by extraction with a pressure of 500 mmHg and an energy density of 0.1 W / g for 30 minutes, and by traditional hot water extraction for 120 minutes, respectively. Detailed data are shown in Table 4 below.
[0089] Table 4. Effects of different energy densities (W / g) combined with different ultrasonic-assisted extraction times on the extraction rate of polysaccharides from fresh purslane.
[0090]
[0091]
[0092] The third scenario is multi-frequency combination, where different frequencies are extracted sequentially, such as... Figure 4 As shown.
[0093] At the same energy density (0.05 W / g), the results show that the first extraction with 28 kHz frequency can obtain higher mucopolysaccharide content. The mucopolysaccharide extraction rates of the first group (ultrasonic wave of 28 kHz for 15 minutes and 68 kHz for 15 minutes) and the second group (28 kHz for 15 minutes and 133 kHz for 15 minutes) are 42.1% and 35.1%, which are the two groups with the highest mucopolysaccharide content in the ultrasonic-assisted extraction of the frequency combination (15 minutes and 15 minutes). The mucopolysaccharide extraction rate of the third group (28 kHz for 15 minutes and 68 kHz for 15 minutes) is 42.1%, which is 9.9%, 9.7% and 24.4% higher than that of the fourth group (68 kHz for 15 minutes and 28 kHz for 15 minutes), the fifth group (133 kHz for 15 minutes and 28 kHz for 15 minutes) and the sixth group (traditional hot water extraction for 30 minutes), respectively.
[0094] The fourth case is frequency combination, which is to start different frequencies at the same time for extraction.
[0095] At the same energy density (0.05 W / g), the results show that the first extraction with 28 kHz frequency can obtain higher mucopolysaccharide content. The mucopolysaccharide extraction rates of the first group (ultrasonic wave of 28 kHz for 15 minutes and 68 kHz for 15 minutes) and the second group (28 kHz for 15 minutes and 133 kHz for 15 minutes) are 42.1% and 35.1%, which are the two groups with the highest mucopolysaccharide content in the ultrasonic-assisted extraction of the frequency combination (15 minutes and 15 minutes). The mucopolysaccharide extraction rate of the third group (28 kHz for 15 minutes and 68 kHz for 15 minutes) is 42.1%, which is 9.9%, 9.7% and 24.4% higher than that of the fourth group (68 kHz for 15 minutes and 28 kHz for 15 minutes), the fifth group (133 kHz for 15 minutes and 28 kHz for 15 minutes) and the sixth group (traditional hot water extraction for 30 minutes), respectively. Figure 5
[0096] In summary, the extraction system and the extraction method provided by the present application integrate an ultrasonic source, a pressure extraction container slot and two pressure sources (such as a vacuum pump and an air compressor system). Through the design of the inner and outer cylinders, the extracted material can be subjected to different extraction processes in the inner and outer cylinders, and can be quickly moved from the inner cylinder to the outer cylinder for pressure increasing and decreasing processing, improving the convenience of pressure adjustment process, and greatly reducing the size of the device. At the same time, it can be combined with multi-frequency ultrasonic processing to perform extraction process according to the characteristics of the raw material and the product demand, so that the ultrasonic energy can fully contact with the extracted material, improve the operation efficiency of the ultrasonic energy, improve the quality of the extracted material, and further expand the application range and shorten the process time.
[0097] In addition, the pressure, ultrasound frequency, energy density and temperature parameters of the present application can be adjusted according to the characteristics of the material to be extracted or the product requirements, so as to achieve the purpose of optimization.
[0098] Although this specification contains many specifics, these should not be construed as limiting the scope of any features or claims in any way. This specification describes features that may, and often are, present in any single implementation, but these need not be present together in any essential way. Particular features described herein that are present in one embodiment can also be implemented in other embodiments as separate features or in any suitable sub-combination or in any suitable combination. Moreover, although features can be described above as acting in particular combinations and / or in conjunction with / and / or in regard to other features, one or more features from a particular combination can in some cases, e.g., based on an intended application or the like, act independently and / or in sub-combinations apart from that or those features making up the particular combination.
[0099] The present application has been described with reference to the embodiments. The particular applications of the features described in this specification can vary as particular applications can make use of those features in different types of systems and / or in different ways. Moreover, it will be appreciated that those skilled in the art will be able to devise numerous implementations that although not explicitly described herein, embody the principles of the application and are thus within its spirit and scope.
[0100] The term "a" or "an" is used herein to describe one or more components and / or ingredients. This term is used in its conventional sense with "one or more" to indicate that the quantity of the components and / or ingredients is one or more. The singular forms "a," "an," and "the" are intended to include plural referents unless expressly stated to the contrary. Furthermore, the term "or" as used herein is used in its inclusive sense, i.e., "and / or."
[0101] Unless otherwise defined, spatially relative terms such as "above," "below," "up," "left," "right," "down," "top," "bottom," "vertical," "horizontal," "side," "higher," "lower," "upper," "lower," "over," "under," and the like, can be used herein for ease of describing the illustrated examples. It will be understood that the spatially relative terms are intended to encompass different orientations of the described structures in space as well as various modifications thereof, unless otherwise defined. For example, in the description of some embodiments, a component "on" another component can encompass the case where the former is directly on the latter (e.g., in physical contact with the latter) as well as the case where one or more intervening components are present between the former and the latter. The terms "first," "second," "third," etc. can be used herein to describe various components, but such components should not be limited by these terms. Such terms are only used to distinguish one component from another.
[0102] As used herein, the terms "substantially," "generally," and "about" are used to describe and account for small variations. When utilized in conjunction with an event or circumstance, these terms can mean that the event or circumstance explicitly took place, as well as that the event or circumstance closely approximated taking place.
Claims
1. An extraction system, comprising: a housing, comprising: an outer cylinder; an inner cylinder disposed within the outer cylinder and having an inner housing space, the outer cylinder and the inner cylinder forming an outer housing space therebetween; and a valve communicating the outer housing space and the inner housing space; a pressure control module communicating the outer housing space and the inner housing space, respectively, to control pressure in the outer housing space and pressure in the inner housing space, respectively, and simultaneously, such that, in operation, the inner housing space is at positive pressure and the outer housing space is at negative pressure; and an ultrasound module, comprising: a first frequency emitting component disposed on an outer lateral surface of the inner cylinder; and a second frequency emitting component disposed on an outer lateral surface of the outer cylinder, wherein the first frequency emitting component and the second frequency emitting component can provide ultrasound oscillations of multiple frequencies to the inner housing space and the outer housing space, respectively, and simultaneously.
2. The extraction system of claim 1, further comprising: a sweep module to measure ultrasound frequencies provided by the ultrasound module to the outer housing space and the inner housing space, respectively, or an energy density measuring device to measure energy density applied to the outer housing space and the inner housing space; wherein output of the ultrasound module is adjusted according to the measured ultrasound frequencies or energy density.
3. The extraction system of claim 1, wherein the pressure control module further comprises: a first pressure sensor to measure pressure in the inner housing space and transmit a first pressure signal according to the measured pressure; a second pressure sensor to measure pressure in the outer housing space and transmit a second pressure signal according to the measured pressure; and a pressure controller to receive the first pressure signal and the second pressure signal to adjust pressure in the outer housing space and pressure in the inner housing space.
4. The extraction system of claim 1, further comprising: a seal cover detachably sealing an upper opening of the inner cylinder and the outer cylinder; wherein the inner cylinder and the outer cylinder are substantially cylindrical and concentric; and wherein the seal cover has an openable and closable feed hole communicating an outside of the extraction system and the inner housing space.
5. An extraction method, comprising: providing the extraction system of claim 1; placing a material to be extracted in the inner cylinder of the housing; performing a first extraction process on the material to be extracted placed in the inner cylinder; directing the material to be extracted from the inner cylinder to the outer cylinder of the housing through the valve; and performing a second extraction process on the material to be extracted placed in the outer cylinder; wherein the first extraction process includes applying a first pressure to the material to be extracted and the second extraction process includes applying a second pressure to the material to be extracted, and the first pressure is greater than the second pressure. 6. The extraction method of claim 5, wherein the first extraction process further comprises heating the substance to be extracted to a first temperature, and the second extraction process further comprises heating the substance to be extracted to a second temperature.
7. The extraction method of claim 6, wherein the first extraction process further comprises applying a first ultrasonic oscillation to the substance to be extracted, and the second extraction process further comprises applying a second ultrasonic oscillation to the substance to be extracted.
8. The extraction method of claim 7, further comprising: measuring a frequency of the first ultrasonic oscillation and a frequency of the second ultrasonic oscillation or measuring a power density applied to the outer containment space and the inner containment space, respectively; and wherein the intensity of the first ultrasonic oscillation and the second ultrasonic oscillation is adjusted based on the measured frequency of the first ultrasonic oscillation and the second ultrasonic oscillation or the power density.
9. The extraction method of claim 7, further comprising: measuring a temperature of the substance to be extracted in the outer containment space and the inner containment space, respectively; and wherein the intensity of the first ultrasonic oscillation and the second ultrasonic oscillation is adjusted based on the measured temperature of the substance to be extracted in the outer containment space and the inner containment space, respectively.
10. The extraction method of claim 7, further comprising: measuring a pressure of the substance to be extracted in the outer containment space and the inner containment space, respectively; and wherein the intensity of the first ultrasonic oscillation and the second ultrasonic oscillation is adjusted based on the measured pressure of the substance to be extracted in the outer containment space and the inner containment space, respectively.
9. The extraction method of claim 8, wherein the first pressure and the second pressure have a pressure range of 0-5 kgf / cm 2 ; the first temperature and the second temperature have a temperature range of 0-199°C; and the first ultrasonic oscillation and the second ultrasonic oscillation have a frequency range of 28-133 kHz.
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