CN217367249U - Extraction system - Google Patents

Extraction system Download PDF

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CN217367249U
CN217367249U CN202220241259.5U CN202220241259U CN217367249U CN 217367249 U CN217367249 U CN 217367249U CN 202220241259 U CN202220241259 U CN 202220241259U CN 217367249 U CN217367249 U CN 217367249U
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pressure
accommodating space
extraction
ultrasonic
extraction system
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蔡依洁
陈仲仁
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Food Industry Research and Development Institute
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Food Industry Research and Development Institute
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Abstract

The utility model relates to an extraction system, it includes storage tank and pressure control module. The containing groove comprises an outer cylinder, an inner cylinder and a valve. The inner cylinder is arranged in the outer cylinder and is provided with an inner accommodating space, and an outer accommodating space is formed between the outer cylinder and the inner cylinder. The valve is communicated with the external accommodating space and the internal accommodating space. The pressure control module is respectively communicated with the external accommodating space and the internal accommodating space so as to respectively and simultaneously control the pressure in the external accommodating space and the pressure in the internal accommodating space.

Description

Extraction system
Technical Field
The utility model relates to an extraction system especially relates to the extraction system that can be applied to food processing.
Background
Generally, the term "extraction" refers to a method of extracting a major part of a compound by transferring the compound from one solvent to another solvent due to the difference in solubility (or partition coefficient) between two mutually insoluble (or slightly soluble) solvents and repeating the extraction several times.
With the advancement of technology. The extraction method can also be widely applied to food processing. The conventional extraction methods include soxhlet extraction, thermal reflux extraction, stirring extraction, immersion extraction, solid-liquid extraction, etc., and alkali extraction, acid hydrolysis, or alkaline hydrogen peroxide treatment is used as the main extraction process. In addition, enzyme-assisted treatment may be used. However, the above extraction methods usually require long operation or reaction time, require a large amount of sample to be extracted, use a large amount of organic solvent during the extraction process, and cause a decrease in the activity of active ingredients due to long-term heating, resulting in a low concentration of the finally obtained extracted sample and a low extraction efficiency. In addition, high labor costs are required, and environmental and human health may be affected. Therefore, novel extraction methods have been studied at home and abroad in recent years. For example, ultrasonic assisted extraction methods have been developed because of the high frequency and short wavelength of ultrasonic waves, which have the characteristics of fixed propagation direction, high energy, strong penetration ability, and cavitation effect. Compared with the traditional extraction method, the ultrasonic extraction can fully mix and contact the extraction liquid, accelerate the swelling and hydration of substances and solvents, promote the penetration of the solvents, shorten the dissolution balance time of target active ingredients, improve the diffusion rate of the active ingredients, improve the defects of the traditional solvent extraction and effectively shorten the extraction time; meanwhile, the method can reduce the usage amount of the solvent and save the cost, and is an environmentally-friendly extraction method. In the extraction operation process, the extraction can be operated at low temperature and normal pressure, the volatilization of low-boiling-point substances is avoided, the natural structures of bioactive substances and various nutritional ingredients in the extract can be retained to the maximum extent, and the problems of change, loss, damage, reduction of physiological activity and the like of active ingredients caused by the heat effect of high-temperature treatment are avoided; meanwhile, the extraction rate and quality of active ingredients are improved, the extraction effect is improved, the dissolution of impurity ingredients is reduced, the purity is high, and the active ingredients are easy to separate and purify; the safety and the operation convenience are higher than other extraction methods.
Compared with the traditional microwave, supercritical fluid and molecular distillation extraction methods, the high-intensity ultrasonic wave has the advantages of lower cost, repeatability and simple and easy operation, can effectively replace other extraction methods, and can be industrially applied to improve the extraction of bioactive substances in the fields of food, natural plant materials or Chinese herbal medicines for further utilization. By changing the extraction conditions, the ultrasonic extraction method can solve the problems of time consumption, thermal damage of effective substances, reduction of production cost and the like in the conventional extraction.
The ultrasonic-assisted extraction method has the above industrial advantages, however, the single-frequency ultrasonic wave is easy to generate standing waves to reduce the occurrence of cavitation, the multi-frequency operation enhances the mechanical vibration, and more gas is mixed into the ultrasonic wave to increase the cavitation nuclei. Through the interactive influence of the cavitation process, the low-frequency negative pressure reduces the cavitation threshold, the resonance frequency is close, the number and the effect of cavitation nuclei are increased, the sound field is uniform, and different waveforms such as frequency doubling waves and the like are generated to improve the cavitation effect. In addition, different functional components can be extracted simultaneously through the functional components and the frequency resonance response, so that the mechanical equipment has multiple functions. In addition, in recent years, pressure-regulated ultrasonic assisted extraction technology has been developed to further improve the extraction efficiency.
In the literature and patent search, the continuous process data of pressure-regulating assisted ultrasonic assisted extraction and pressure-assisted extraction, which can be used for performing pressure-relief extraction by instant pressure release, is less. Therefore, it is desired in the industry to develop a pressure-regulated ultrasonic assisted extraction device, which integrates an ultrasonic source and a pressure cooker extraction tank to optimize the extraction quality.
SUMMERY OF THE UTILITY MODEL
To achieve the above objective, an embodiment of the present invention provides an extraction system, wherein the extraction system includes a storage tank and a pressure control module. The containing groove comprises an outer cylinder, an inner cylinder and a valve. The inner cylinder is arranged in the outer cylinder and is provided with an inner accommodating space, and an outer accommodating space is formed between the outer cylinder and the inner cylinder. The valve is communicated with the external accommodating space and the internal accommodating space. The pressure control module is respectively communicated with the external accommodating space and the internal accommodating space so as to respectively and simultaneously control the pressure in the external accommodating space and the pressure in the internal accommodating space.
Preferably, the extraction system further comprises: an ultrasonic module, comprising: the first frequency transmitting assembly is arranged on the outer side surface of the inner cylinder and used for providing ultrasonic oscillation with a first frequency for the inner accommodating space; and a second frequency emitting assembly disposed on an outer side surface of the outer barrel to provide ultrasonic oscillation of a second frequency to the external accommodating space.
Preferably, the extraction system further comprises: and the frequency sweeping module is used for respectively measuring the ultrasonic frequency or the energy density which is provided by the ultrasonic module to the external accommodating space and the internal accommodating space, and is used for measuring the energy density applied to the external accommodating space and the internal accommodating space. Wherein the output of the ultrasonic module is adjusted according to the measured ultrasonic frequency or energy density.
Preferably, the ultrasonic module is configured to provide at least two ultrasonic oscillation frequencies to the inner accommodating space and the outer accommodating space simultaneously.
Preferably, the pressure control module further includes: the first pressure source is connected with the inner accommodating space; the second pressure source is connected with the external accommodating space; a first pressure sensor for measuring a pressure within the interior volume and transmitting a first pressure signal in accordance with the measured pressure; a second pressure sensor for measuring a pressure in the external receiving space and transmitting a second pressure signal according to the measured pressure; and a pressure controller for receiving the first pressure signal and the second pressure signal and controlling the first pressure source and the second pressure source to adjust the pressure in the external accommodating space and the internal accommodating space.
Preferably, the first pressure source is a pressurizing machine providing a pressure of 0-5kgf/cm2 to the inner space; the second pressure source is a vacuum pump and provides 0-500mmHg pressure to the external accommodating space.
Preferably, the extraction system further comprises: and the sealing cover is used for sealing the upper openings of the inner cylinder and the outer cylinder in a detachable mode. The sealing cover is provided with a feed hole which can be opened and closed and is communicated with the outside of the extraction system and the inner accommodating space.
Preferably, the inner and outer barrels are substantially cylindrical and concentric.
Preferably, the extraction system further comprises: and the pressure safety control module is used for detecting whether the pressure in the internal accommodating space and the pressure in the external accommodating space are abnormal or not and controlling the pressure relief valve to relieve the pressure in the internal accommodating space and the pressure in the external accommodating space.
Preferably, the extraction system further comprises: the outlet pipeline is arranged on the outer cylinder and communicated with the external accommodating space in an openable and closable manner; and a temperature control module for respectively controlling the temperature of the inner accommodating space and the temperature of the outer accommodating space.
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 object will become more apparent from the following description, the accompanying drawings, and the claims.
Drawings
For clear understanding of the effects achieved by the present invention and the advantages thereof, the present invention will be described in detail with reference to the accompanying drawings and embodiments.
Fig. 1 is a schematic diagram of an extraction system according to an embodiment of the present invention.
Fig. 2 is a flow chart of an extraction method using an extraction system according to an embodiment of the present invention.
FIG. 3 shows the mucopolysaccharide extraction rate (frequency 28kHz, ratio of liquid to feed: 1:10g/mL, time 30 min) of fresh purslane raw material extracted with the assistance of pressure-regulated ultrasound at different energy densities (W/g).
FIG. 4 shows the effect of complex frequency combined (15 min/15 min) ultrasound-assisted extraction on the extraction rate of mucopolysaccharide from fresh purslane raw material (solution ratio 1:10g/mL, energy density 0.05W/g, run time 30 min).
FIG. 5 shows the effect of complex frequency composite ultrasound assisted extraction on the extraction rate of mucopolysaccharide from fresh purslane raw material (solution ratio 1:10g/mL, energy density 0.05W/g, extraction time 30 min).
Description of the symbols
1 extraction system 2 storage tank
3 pressure control module 4 sealing cover
5: housing 6: ultrasonic module
7: temperature control module 11: first pressure source
12 second pressure source 20 inner cylinder
22: outer cylinder 24: valve
26 outlet line 30 first pressure sensor
32 second pressure sensor 34 pressure controller
36 pressure safety control module 38 safety valve
39 manual pressure relief valve 40 feed inlet
50 instrument panel 52 operation panel
60 ultrasonic controller 62 ultrasonic power source
64 first frequency transmission assembly 66 second frequency transmission assembly
68 sweep frequency module 70 temperature controller
72 temperature sensor 74 heating element
76 cooling module 111,121 pipeline
200 inner space 202 opening
204, side wall 220, external accommodation space 222 and opening
Detailed Description
For the purpose of clearly understanding the features, contents and advantages of the present invention and the efficacy achieved thereby, the present invention will be described in detail below with reference to the accompanying drawings in which embodiments are shown, and the drawings are used for illustration and the accompanying description.
The utility model mainly provides an extraction system which uses 1 and an extraction method to extract a solution of a substance to be extracted by utilizing a high-efficiency mode of pressure adjustment and ultrasonic wave assistance. Fig. 1 is a schematic diagram of an extraction system 1 according to an embodiment of the present invention. In the present embodiment, the extraction system 1 includes a container 2, a pressure control module 3, a sealing cover 4 and a housing 5. The housing 5 is used for accommodating the accommodating groove 2 and the pressure control module 3. The sealing cover 4 is detachably provided on the accommodating groove 2.
The container 2 includes an inner cylinder 20, an outer cylinder 22, a valve 24, and an outlet line 26. The inner cylinder 20 is arranged in the outer cylinder 22 and is provided with an inner accommodating space 200 for accommodating substances to be extracted; an outer accommodating space 220 is formed between the outer cylinder 22 and the inner cylinder 20 for accommodating the substance to be extracted. The openings 202 and 222 above the inner cylinder 20 and the outer cylinder 22 are closed by the seal cover 4. The inner cylinder 20 and the outer cylinder 22 of the present embodiment are cylindrical and concentric, the heights of the inner cylinder 20 and the outer cylinder 22 are substantially the same, and the width of the outer cylinder 22 is greater than the width of the inner cylinder 20. The outer cylinder 22 and the inner cylinder 20 are made of metal, such as stainless steel, and are fixed to the base of the container 2 by welding. The outlet pipe 26 is disposed on the outer cylinder 22 and is connected to the outer receiving space 220 in an openable and closable manner, so as to discharge the extracted liquid from the receiving tank 2 through the outlet pipe 26.
The sealing cover 4 has an openable and closable feed opening 40 which communicates the outside of the extraction system 1 with the inner receiving space 200 of the inner barrel 20 so that the material to be extracted can be placed in the inner receiving space 200 of the inner barrel 20 from the feed opening 40.
The valve 24 penetrates through the sidewall 204 of the inner cylinder 20 to communicate the outer accommodating space 220 in the outer cylinder 22 with the inner accommodating space 200 in the inner cylinder 20. The valve 24 is an electronically controlled bleed valve. The material to be extracted can move from the inner receiving space 200 of the inner drum 20 to the outer receiving space 220 of the outer drum 22 through the valve 24. For example, the valve 24 can be disposed at the bottom end of the sidewall 204 of the inner barrel 20, and the substance to be extracted can directly flow from the inner barrel 20 to the external accommodating space 220 of the outer barrel 22 by gravity or pressure difference.
In one embodiment of the present invention, a first pressure source 11 is provided and is communicated to the interior volume 200 through a conduit 111 extending through the outer housing 5, the outer cartridge 22 and the inner cartridge 20 to provide a first pressure to the interior volume 200. A second pressure source 12 may be provided to communicate with the external receiving space 220 through a conduit 121 extending through the housing 5 and the outer barrel 22 to provide a second pressure to the external receiving space 220.
The pressure control module 3 controls the pressure in the external accommodating space 220 and the pressure in the internal accommodating space 200 respectively and simultaneously. In the present embodiment, the pressure control module 3 further includes 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 receiving space 200 and transmit a first pressure signal to the pressure controller 34 according to the measured pressure. The second pressure sensor 32 is used for measuring the pressure in the external receiving space 220 and transmitting a second pressure signal to the pressure controller 34 according to the measured pressure. The pressure controller 34 is configured to receive the first pressure signal and the second pressure signal to adjust the pressure of the external accommodating space 220 and the pressure of the internal accommodating space 200.
In the present embodiment, the pressure controller 34 can be electrically connected to the first pressure source 11 and the second pressure source 12 to automatically control the pressures provided by the first pressure source 11 and the second pressure source 12, respectively. In the present embodiment, the first pressure source 11 may comprise a pressurizing component, such as an air compressor, which can apply a pressure of 0 to 7kgf/cm 2 For pressurizing said container cavity. In one embodiment, the applied pressure of the pressing assembly can be 0 to 5kgf/cm 2 In the meantime. In the present embodiment, the second pressure source 12 may include a pressure reduction component, such as a vacuum pump, which may apply a pressure of 0 to 700 mmHg. In one embodiment, the applied pressure of the reduced-pressure assembly can be 0 to 500 mmHg. The pressure controller 34 may have a pressure parameter, and the pressure controller 34 may selectively control the on/off of the first pressure source 11 (pressurizing component) and the second pressure source 12 (depressurizing component) according to the pressure parameter and the pressure sensing signal. When the substance to be extracted is treated under high pressure, the pressurization can improve the amount of dissolved gas, improve the cavitation effect and improve the destruction strength of bubbles. When the substance to be extracted is subjected to pressure reduction treatment, heat-sensitive and easily-oxidizable substances are extracted by utilizing the principle that the extraction at low temperature can reduce the solvent solution amount, viscosity and surface tension and influence the ultrasonic cavitation effect. When the material to be extracted is moved from the high-pressure inner cylinder to the outer cylinder, i.e. using instantaneous pressure difference treatment (instant)and (DIC) in a manner that promotes water evaporation, expansion and voiding in the material to increase contact area and reduce diffusion resistance to improve extraction efficiency.
In the embodiment, the extraction system 1 further includes a pressure safety control module 36 and a safety valve 38, wherein the safety valve 38 is disposed above the sealing cover 4 and is connected to the container 2 (not shown). The pressure value of the safety valve 38 is 1.2kg/cm 2 . The pressure safety control module 36 is used for controlling the safety valve 38 to be activated when the extraction pressure in the receiving tank 2 is abnormal, so as to automatically release the pressure in the receiving tank 2, thereby ensuring the safety during the extraction process.
The extraction system of the present embodiment further comprises a manual pressure relief valve 39 disposed above the sealing cover 4 and connected to the container 2 (not shown). The pressure adjustment of the manual pressure relief valve 39 is between 1 and 30psi (dead per square inch). The user can actively operate the manual relief valve 39 to reduce the pressure in the tank 2 to a desired value.
In the present embodiment, the extraction system 1 further includes an ultrasonic module 6, which includes an ultrasonic controller 60, at least one ultrasonic power source 62, at least one first frequency emitting element 64, and at least one second frequency emitting element 66. The first frequency emitting assembly 64 is disposed on the outer surface of the sidewall 204 of the inner barrel 20 to provide ultrasonic oscillations of at least a first frequency to the inner receiving space 200. The second frequency emitting assembly 66 is disposed on the outer surface of the outer barrel 22 to provide at least one ultrasonic oscillation of a second frequency to the external accommodating space 220. In this embodiment and some embodiments, the first frequency emitting element 64 and the second frequency emitting element 66 can simultaneously provide ultrasonic vibrations of multiple frequencies to the inner accommodating space 200 and the outer accommodating space 220, respectively. For example, the first frequency and the second frequency are 28, 68, and/or 133 kHz.
In the embodiment, the extraction system 1 further includes a sweep module 68 for measuring the ultrasonic frequencies provided by the ultrasonic module 6 to the inner and outer receiving spaces 200 and 220, respectively. In another embodiment, the extraction system further comprises an energy density measuring device for measuring the energy density applied to the inner and outer receiving spaces 200 and 220. Thus, the output of the ultrasonic module 6 is adjusted according to the measured ultrasonic frequency or energy density, which is transmitted to the ultrasonic controller 60. The structure and operation of the ultrasonic module 6 and the frequency sweep module 68 are well known to those skilled in the art and will not be described in detail. As used herein, "energy density" refers to the power provided by the ultrasound module per unit weight of extract, which is in W/g. In one embodiment, the extraction power may be between 0 and 300W. In the present embodiment, the frequency sweep module 68 may include a voltage phase sensor disposed at the bottom or the sidewall of the accommodating tank 2 for regulating and controlling the phase change of the operating voltage, feeding back the operating point to increase the original frequency and reduce the occurrence of standing waves.
In this embodiment, the extraction system 1 may further include a temperature control module 7 for controlling the temperature of the extraction liquid in the inner cylinder 20 and the outer cylinder 22. The temperature control module 7 may include a temperature controller 70, two temperature sensors 72, a heating element 74, and a cooling element 76. The temperature sensor 72 is connected to the inner cylinder 20 and the outer cylinder 22 respectively, and is used for measuring the temperature of the extraction liquid 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 sensor 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, and is used for heating the substance to be extracted 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, and is used for cooling the solution of the substance to be extracted in the inner cylinder 70 according to the instruction of the temperature controller 70. The temperature control module 7 is selectively used for controlling the heating element 74 and the cooling element 76 to be turned on or off according to the set temperature parameter and the temperature sensing signal. In this embodiment, the heating element 74 and the cooling element 76 are used to achieve an extraction temperature of between 0 and 199 ℃.
In addition, the outer casing 5 may be provided with an instrument panel 50 and an operation panel 52, and the instrument panel 50 may display the temperature, the ultrasonic frequency, the energy density, the operation time, the pressure, and the like of the inner cylinder 20 and the outer cylinder 22. The operation panel 52 can operate the above-mentioned values of temperature, ultrasonic frequency, etc., operation time, pressure, etc.
Fig. 2 is a flow chart of an extraction method using an extraction system according to an embodiment of the present invention. An embodiment of the present invention provides an extraction method, which includes the following steps. In step S110, the extraction system 1 described above is provided.
In step S120, the solution of the substance to be extracted is placed in the inner cylinder of the container. For example, the substance to be extracted may be prepared by: directly adding water into a substance to be extracted in a fresh raw material mode, and placing the substance into a stirrer to be beaten into slurry to serve as a solution to be extracted; or drying with hot air or freeze drying, pulverizing to obtain powder, adding extraction solvent (such as water), and making into solution. In one embodiment, the weight percentage of the feedstock to the extraction solvent is 1:10 to 1:50 g/mL.
In step S130, a first extraction process is performed on the substance to be extracted accommodated in the inner barrel. In this embodiment, the first extraction process further comprises heating the material to be extracted to a first temperature. The first extraction treatment may also include applying a first ultrasonic oscillation to the substance to be extracted. The first extraction process may further include applying a first pressure to the substance to be extracted.
For the heating process of the first extraction process, the material to be extracted in the inner drum can be heated to a certain value (for example, maintained at 80 ℃) within a period of time. In other embodiments, the different heating temperatures at which the substance to be extracted is supplied may be sequentially varied over different periods of time (e.g., the substance to be extracted is heated to 60 ℃ over a first period of 20 minutes and the substance to be extracted is heated to 80 ℃ over a second period of 40 minutes).
For the ultrasonic oscillation of the first extraction process, in the first extraction process of step S130 of an embodiment, the low frequency may be started first to effectively destroy the cell walls of the material in a first time period (e.g., the first 15 minutes, 30 minutes, 60 minutes) so as to increase the diameter of the micropores, shorten the mass transfer distance of the diffusions, and improve the mass transfer efficiency of the internal diffusions; then, the high frequency ultrasonic wave is started in the second time period (for example, the next 15, 30 and 60 minutes), so that the vibration effect is improved, the solute can be rapidly diffused into the solvent, and the extraction efficiency is improved.
In the first extraction process of step S130 of another embodiment, the low-frequency and high-frequency ultrasonic waves can be simultaneously activated to enhance the mechanical vibration at a time period (e.g., 15, 30, 45, 60 minutes), so that more gas is incorporated to increase the number of cavity nuclei, thereby making the sound field uniform, and even generating different waveforms such as frequency doubling waves to enhance the cavity effect, thereby increasing the extraction efficiency.
The pressure application for the first extraction process, similar to the heating process described above, can provide the same pressure for only one period of time, or different pressures for different periods of time.
In the step S130, the modes of ultrasonic oscillation, energy density, pressure application, temperature control, etc. in the first extraction process can be adjusted according to the characteristics of the substance to be extracted, so as to maintain constant values, or provide different ultrasonic frequencies, energy densities, pressures and/or temperatures in different time periods. In some embodiments, only one of the ultrasonic frequency, pressure and temperature adjustments may be used in the first extraction process.
Next, after the first extraction process is completed, in step S140, the material to be extracted is introduced into the outer cylinder 22 of the container 2 through the valve 24. In one embodiment, when the first extraction process reaches a predetermined operation time, the valve 24 can be opened automatically or manually, and the substance to be extracted in the inner barrel 20 falls into the second accommodating space 220 of the outer barrel 22 through the valve 24.
In step S150, a second extraction process is performed on the material to be extracted contained in the outer tub 22. Wherein the second extraction process comprises 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 this embodiment, the second extraction process further comprises heating the material to be extracted to a second temperature. The second extraction treatment further comprises applying a second ultrasonic oscillation to the substance to be extracted.
In one embodiment, similar to the first extraction process, in the second extraction process, the modes of ultrasonic oscillation, pressure application, temperature control, etc. in the second extraction process can be adjusted according to the characteristics of the substance to be extracted, so as to maintain the above-mentioned operation values at constant values, or to provide different ultrasonic frequencies, energy densities, pressures and/or temperatures in different time periods. In some embodiments, only one of the ultrasonic frequency, pressure and temperature adjustments may be used in the second extraction process.
In this embodiment, the first pressure and the second pressure range from 0 to 5kgf/cm absolute pressure 2 (ii) a The first temperature and the second temperature range are between 0 and 199 ℃; and the frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation range from 28 to 133 kHz.
In this embodiment, the method further includes measuring the frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation respectively, or measuring the energy density applied to the outer receiving space and the inner receiving space respectively in steps S130 and S150. Therefore, 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 measured frequency or energy density of the second ultrasonic oscillation, so as to achieve a better ultrasonic oscillation effect.
In addition, the pressure application for the first and second extraction processes may be performed by only pressurizing one of the inner cylinder 20 and the outer cylinder 22 or only depressurizing the one in one embodiment. That is, the pressure may be increased only in the first extraction process or reduced only in the second extraction process, depending on the actual requirements.
In the embodiment of the present invention, the concentric double-cylinder structure design of the inner cylinder 20 and the outer cylinder 22 is used to perform the pressure difference operation, so that after the inner cylinder 20 is pressurized, the pressure can be quickly transferred to the outer cylinder 22 to perform the pressure reduction operation. That is, the material to be extracted can be first extracted under pressure in the inner cylinder 20 of the container 2 and then moved into the outer cylinder 22 through the valve 24. In the process that the substance to be extracted enters the decompression outer cylinder 22 from the pressurized inner cylinder 20, the pressure is rapidly reduced to cause instant pressure difference, the pressure in the substance to be extracted is released outwards, the raw material structure is further rapidly destroyed, and the release effect of the internal extraction substance is increased; in addition, when the outer cylinder 22 is depressurized, the inner cylinder 20 can also perform pressurized extraction of the next batch of material to be extracted at the same time, and semi-continuous operation can be performed, thereby achieving the effects of effectively shortening the extraction time and improving the extraction efficiency.
The utility model discloses in, extraction system 1 can be directed against the biomaterial of different characteristics, and application processing procedure combination and structural design improve extraction efficiency. In one embodiment, a plurality of frequency combination extraction modes are utilized, namely, the cell walls of substances to be extracted can be effectively damaged by starting low frequency firstly, so that the diameter of micropores is increased, the diffusion mass transfer distance is shortened, and the internal diffusion mass transfer efficiency is improved; then, the high-frequency ultrasonic wave is started to improve the vibration effect, so that the solute can be rapidly diffused into the solvent, and the extraction efficiency is improved.
In another embodiment, the low frequency and high frequency ultrasonic enhanced mechanical vibration (such as simultaneously turning on the frequency of 28kHz, 68kHz or 133 kHz) can be turned on simultaneously, more gas is merged to increase the number of cavity nuclei, the sound field can be made uniform, even frequency doubling waves and other different waveforms can be generated to improve the cavity effect, and the extraction efficiency can be further increased.
That is, the present invention provides an extraction method, which utilizes an ultrasonic module to vibrate a substance to be extracted to perform an ultrasonic assisted extraction process, and can simultaneously or selectively perform a complex frequency combination (different frequencies operate in sequence), a complex operation (different frequencies are simultaneously turned on to perform extraction), a temperature control and pressure adjustment combination (different extraction pressures operate in sequence). The control of the ultrasonic waves, temperature and pressure in the inner and outer cylinders 20, 22 can be adjusted according to the actual requirements, such as the biological characteristics of the material to be extracted.
In step S160, when the second extraction process is finished, the outlet line 26 can be manually or automatically opened to take out the extracted solution.
The results of the embodiment of the present invention applying the pressure-regulating and ultrasonic-assisted extraction system 1 to purslane raw material extraction will be described below. Firstly, when ultrasonic-assisted extraction is carried out, water is used as an extraction solvent, the initial extraction temperature is controlled at 40 ℃, a prepared raw material solution after pretreatment is placed into a containing groove 2 of an extraction system 1, then extraction is carried out by utilizing a pressure control module and an ultrasonic module, extraction parameters can be adjusted, and after an extracted liquid obtains a filtrate, index component content analysis is carried out. The ultrasonic extraction parameters discussed in this section include the feed-to-liquid ratio, frequency, energy density, complex frequency combinations (sequential operation with different frequencies), complex operation (simultaneous activation of different frequencies for extraction), and pressure adjustment combinations (sequential operation with different extraction pressures), etc., and the control group is conventional hot water (95 deg.C) extraction.
First set of experiments
In the experiment of first group, the applicant is right the utility model discloses an extraction system 1 and traditional batch system carry out the experiment comparison to add decompression and adopt the supplementary extraction of ultrasonic wave to treat the influence of the glutinous polysaccharide extraction rate of extraction material (fresh raw materials is given birth to the purslane), pressure, ultrasonic frequency, temperature isoparametric are all the same, and the experimental result is as following table 1:
TABLE 1 extraction rate of polysaccharide from semi-continuous extraction system and conventional batch extraction equipment
Mode of operation Extraction ratio (%) of mucopolysaccharide
The utility model discloses semi-continuous extraction system 59.1
Traditional batch type extraction equipment 55.7
By the upper table show, the utility model discloses a semi-continuous type extraction system 1 compares in traditional batch formula extraction rate effect and though only increases 3.4% extraction rate, nevertheless the utility model discloses a 2 designs of storage tank of concentric binocular are compared in batch formula single cylinder groove mechanism, and two obvious advantages are as follows in addition:
first, if want to reach similar extraction rate under the same operating time, batch formula list barrel groove mechanism need have two sets of list barrel groove test equipment to carry out the series operation, nevertheless the utility model discloses extraction system with two barrel grooves only needs one set just can realize. Under such operation, the system of the present invention can reduce the equipment cost (about RMB 11 ten thousand yuan) by about 35% and the equipment space by 50% compared to the batch type mechanism.
Secondly, aiming at the manufacturing cost and the setting space, a batch type single-cylinder groove mechanism is used for extraction, if the extraction rate close to the extraction system 1 of the utility model is required to be reached, pressure is required to return to the normal pressure in the operation process, and then pressure increasing and reducing equipment is replaced to increase and reduce the pressure, so that the operation time is increased; however, the apparatus of the present invention does not require such a complicated process. Therefore, compared with a batch-type mechanism, the extraction system 1 of the present invention can shorten the process time by about 30% (about 15 minutes).
Second set of experiments
In a second set of experiments, different types of starting materials were used and extracted for 30 minutes.
The first raw material type: purslane powder, 5kgf/cm at normal pressure 2 And 500mmHg, the extraction rate of mucopolysaccharide is respectively improved by 81.3, 143.8 and 123.8% compared with the extraction with traditional hot water under the same experimental conditions of ultrasonic frequency of 28kHz, solution ratio of 1:20g/mL, energy density of 0.05W/g, extraction time of 30 minutes and the like, as shown in the following table 2.
TABLE 2 extraction rate of portulaca oleracea mucopolysaccharide by traditional water extraction and pressure ultrasound assisted extraction
Figure DEST_PATH_GDA0003741597350000101
The second raw material type: fresh herba Portulacae raw material slurry at 5kgf/cm under normal pressure 2 And 500mmHg and the likeUnder different operating pressures, the extraction rates of mucopolysaccharides were respectively increased by 40.9, 150.3 and 84.3% compared with the conventional hot water extraction under the same experimental conditions of ultrasonic frequency of 28kHz, feed-liquid ratio of 1:20g/mL, energy density of 0.05W/g and extraction time of 30 min, as shown in Table 3 below.
TABLE 3 extraction rate of mucopolysaccharide from fresh purslane raw material by conventional water extraction and pressure ultrasonic assisted extraction
Figure DEST_PATH_GDA0003741597350000111
From the second set of experiments, it can be easily known that the extraction rate can be increased regardless of the use of normal pressure, pressurization or depressurization. And the extraction rate by adopting pressurization or depressurization is higher than that of the traditional water extraction and normal pressure.
Third set of experiments
In the experiment, fresh purslane raw material slurry with the ratio of material to liquid being 1:10g/mL is adopted, and different energy densities and extraction times are changed for measurement.
The first case was the experiment with different energy densities, as shown in fig. 3: when the energy density was 0.05W/g, the frequency was 28kHz, and the extraction was carried out for 30 minutes, the pressure was normal pressure, reduced pressure (500mmHg), and increased pressure (5 kgf/cm) 2 ) The extraction rates of mucopolysaccharides are respectively 31.0, 35.9 and 41.6%, which are 13.3, 18.2 and 23.9% higher than the extraction rate (17.7%) of mucopolysaccharides extracted by hot water; when the auxiliary extraction was carried out at an energy density of 0.1W/g, the extraction was carried out for 30 minutes under normal pressure, reduced pressure (500mmHg) and increased pressure (5 kgf/cm) 2 ) The extraction rates of mucopolysaccharide are 35.6, 39.1, 46.9%, respectively, which is significantly increased by 17.9, 21.4, 29.2% compared with the conventional hot water extraction.
The second case was experiments with different extraction times: extracting with ultrasonic frequency of 28kHz, solution ratio of 1:10g/mL, and energy density of 0.05W/g under normal pressure for 120 min to obtain viscous polysaccharide extraction rate of 42.0%, which is about 5kgf/cm 2 The extraction rate of mucopolysaccharide (41.6%) is increased by 13.8% compared with conventional extraction with hot water for 120 min by matching with energy density of 0.05W/g for 30 min. If extraction is performed at normal pressure with an energy density of 0.1W/g for 120 minutes, the extraction rate of mucopolysaccharide is 45.8%, which is 6.7% and 17.6% higher than that of conventional extraction with an energy density of 0.1W/g and a pressure of 500mmHg for 30 minutes and 120 minutes. The details are given in table 4 below.
TABLE 4. influence of different energy densities (W/g) in combination with ultrasonic assisted extraction on extraction rate of mucopolysaccharide from fresh purslane raw material
Figure DEST_PATH_GDA0003741597350000112
Figure DEST_PATH_GDA0003741597350000121
The third case is a complex frequency combination, where different frequencies are operated in sequence for extraction, as shown in FIG. 4.
Under the same energy density (0.05W/g), different extraction frequencies were combined in sequence, and the results showed that higher mucopolysaccharide content could be obtained by performing the extraction at 28kHz first, and that the mucopolysaccharide extraction rates of group 1 (ultrasonic 28kHz for 15 minutes and 68kHz for 15 minutes) and group 2 (ultrasonic 28kHz for 15 minutes and 133kHz for 15 minutes) were 42.1 and 35.1%, which are the two groups with the highest mucopolysaccharide content in the multi-frequency combination (15 minutes and 15 minutes). The extraction rate of mucopolysaccharides (42.1%) in group 3 (15 min at 28kHz and 15 min at 68 kHz) was 9.9%, 9.7% and 24.4% higher than that in group 4 (15 min at 68kHz and 15 min at 28 kHz), group 5 (15 min at 133kHz and 15 min at 28 kHz) and group 6 (30 min in conventional hot water extraction).
The fourth case is complex frequency recombination, which is to turn on different frequencies simultaneously for extraction.
Under the same energy density (0.05W/g), the composite operation is carried out by utilizing different extraction frequencies simultaneously. The results show that the extraction effect of mucopolysaccharide from fresh purslane raw material is better than that of the traditional hot water extraction by using the multi-frequency compound extraction for 30 minutes, and the extraction rate of mucopolysaccharide extracted from the group treated by opening 28+68+133kHz at the same time is 48.2% at most and is 30.5% higher than that of the traditional hot water extraction; respectively increasing the extraction rate by 3.8, 8.6 and 19.1 percent compared with the extraction rate of simultaneously opening 28+68, 28+133 and 68+133 kHz; and 6.1% higher than the mucopolysaccharide extraction rate (42.1%) of the multifrequency combined (28 kHz for 15 minutes followed by 68kHz for 15 minutes, as shown in FIG. 5).
In summary, the present invention provides an extraction system and an extraction method thereof, which integrates an ultrasonic source, a pressure extraction tank, and two pressure sources (e.g., a vacuum pump and an air compressor system). Through the design of the inner barrel and the outer barrel, the extract can be subjected to different extraction treatments in the inner barrel and the outer barrel, and the extract can be rapidly moved from the inner barrel to the outer barrel so as to be subjected to pressure increasing and reducing treatment, so that the convenience of the pressure adjusting process is improved, and the volume of the device is greatly reduced. Meanwhile, the multi-frequency ultrasonic treatment can be matched, and the extraction process is carried out according to the characteristics of raw materials and the requirements of products, so that the ultrasonic energy can be fully contacted with the extraction materials, the operating efficiency of ultrasonic energy is improved, the quality of the extraction product is improved, the application range can be further expanded, the process time can be further shortened, and the like.
Furthermore, the utility model discloses a pressure, ultrasonic frequency, energy density and temperature parameter all can be adjusted according to the characteristic or the product demand of treating the extraction material to reach the mesh of optimization.
While this specification contains many specific implementation details, these should not be construed as limiting the scope of any features or of what may be claimed, but rather as describing features that are specific to particular embodiments. Certain features that are described in this specification in the context of separate embodiments can also be implemented in combination in a single embodiment. Conversely, various features that are described in the context of a single embodiment can also be implemented in multiple embodiments separately or in any suitable subcombination. Moreover, although features may be described above as acting in certain combinations and even initially claimed as such, one or more features from a claimed combination can in some cases be excised from the combination, and the claimed combination may be directed to a subcombination or variation of a subcombination.
The invention has been described with reference to embodiments and with the understanding that particular applications of the features of the invention can be practiced individually and/or in various combinations and/or on various types. Moreover, those skilled in the art will recognize that various modifications may be made to the embodiments in any of their applications without departing from the scope of the present invention. Moreover, alternative embodiments can be made from different component materials, structures, and/or spatial relationships, and still fall within the scope of the invention.
The terms "a" or "an" are used herein to describe elements and components of the invention. This terminology is used for convenience of description only and is for the purpose of giving the invention the general idea. This description should be read to include one or at least one and the singular also includes the plural unless it is obvious that it is meant otherwise. In addition, the term "or" as used herein is intended to mean "and/or".
Unless otherwise specified, spatial descriptions such as "above," "below," "upward," "left," "right," "downward," "top," "bottom," "vertical," "horizontal," "side," "upper," "lower," "upper," "above," "below," and the like are directed to the directions shown in the figures. It is to be understood that the spatial descriptions used herein are for illustrative purposes only and that actual implementations of the structures described herein can be spatially configured in any relative orientation, such limitations not altering the advantages of the various embodiments of the present invention. For example, in the description of some embodiments, a component provided "on" another component may encompass a situation in which the preceding component is directly on (e.g., in physical contact with) the succeeding component, as well as a situation in which one or more intervening components are located between the preceding and succeeding components.
As used herein, the terms "substantially", "generally" and "about" are used to describe and take into account minor variations. When used in conjunction with an event or circumstance, these terms can mean that the event or circumstance occurs specifically, and that the event or circumstance closely approximates that which occurs.

Claims (10)

1. An extraction system, characterized in that the extraction system comprises:
the storage tank includes:
an outer cylinder;
the inner cylinder is arranged in the outer cylinder and is provided with an inner accommodating space, and an outer accommodating space is formed between the outer cylinder and the inner cylinder; and
the valve is communicated with the external accommodating space and the internal accommodating space; and
and the pressure control module is respectively communicated with the external accommodating space and the internal accommodating space so as to respectively and simultaneously control the pressure in the external accommodating space and the pressure in the internal accommodating space.
2. The extraction system of claim 1, further comprising:
an ultrasonic module, comprising:
the first frequency transmitting assembly is arranged on the outer side surface of the inner cylinder and used for providing ultrasonic oscillation with a first frequency for the inner accommodating space; and
the second frequency transmitting component is arranged on the outer side surface of the outer barrel and used for providing ultrasonic vibration of a second frequency for the outer accommodating space.
3. The extraction system of claim 2, further comprising:
a frequency sweep module for measuring the ultrasonic frequency or energy density measurement device provided by the ultrasonic module to the external accommodation space and the internal accommodation space, respectively, and for measuring the energy density applied to the external accommodation space and the internal accommodation space;
wherein the output of the ultrasonic module is adjusted according to the measured ultrasonic frequency or energy density.
4. The extraction system according to claim 2, wherein the ultrasonic module is configured to provide at least two ultrasonic oscillation frequencies to the inner and outer receiving spaces simultaneously.
5. The extraction system of claim 1, wherein the pressure control module further comprises:
the first pressure source is connected with the inner accommodating space;
the second pressure source is connected with the external accommodating space;
the first pressure sensor is used for measuring the pressure in the internal accommodating space and transmitting a first pressure signal according to the measured pressure;
the second pressure sensor is used for measuring the pressure in the external accommodating space and transmitting a second pressure signal according to the measured pressure; and
and the pressure controller is used for receiving the first pressure signal and the second pressure signal and controlling the first pressure source and the second pressure source according to the first pressure signal and the second pressure signal so as to adjust the pressure in the external accommodating space and the pressure in the internal accommodating space.
6. The extraction system of claim 5, wherein:
the first pressure source is a pressurizer which provides a pressure of 0-5kgf/cm2 to the inner containing space;
the second pressure source is a vacuum pump and provides 0-500mmHg pressure to the external accommodating space.
7. The extraction system of claim 1, further comprising:
a seal cover which detachably seals the upper openings of the inner cylinder and the outer cylinder;
the sealing cover is provided with a feed hole which can be opened and closed and is communicated with the outside of the extraction system and the inner accommodating space.
8. The extraction system of claim 1, wherein the inner drum and the outer drum are substantially cylindrical and concentric.
9. The extraction system of claim 1, further comprising:
and the pressure safety control module is used for detecting whether the pressure in the internal accommodating space and the pressure in the external accommodating space are abnormal or not and controlling the pressure relief valve to relieve the pressure in the internal accommodating space and the pressure in the external accommodating space.
10. The extraction system of claim 1, further comprising:
the outlet pipeline is arranged on the outer cylinder and communicated with the external accommodating space in an openable and closable manner; and
and the temperature control module is used for respectively controlling the temperature of the internal accommodating space and the temperature of the external accommodating space.
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