TWI819445B - Extraction system and extraction method using the same - Google Patents

Abstract

The present application relates to an extraction system and a extraction method using the extraction system. The extraction system includes a container and a pressure control module. The container includes an outer bucket, an inner bucket and a valve. The inner bucket is disposed within the outer bucket and has an inner accommodating space, and an outer accommodating space is formed between the outer bucket and the inner bucket. The valve connects the outer accommodating space and the inner accommodating space. The pressure control module connects the outer accommodating space and the inner accommodating space for controlling the pressure of the outer accommodating space and the pressure of the inner accommodating space, respectively.

Description

Extraction systems and methods

This application relates to an extraction system and a method thereof, in particular to an extraction system and a method applicable to food processing.

Generally speaking, "extraction" refers to the use of the difference in solubility (or distribution coefficient) of a compound in two mutually immiscible (or slightly soluble) solvents to transfer a compound from one solvent to another, and After repeated extractions, most of the compounds are extracted.

As technology advances. Extraction methods can also be widely used in food processing. Currently, common extraction methods include Soxhlet extraction, thermal reflux extraction, stirring extraction, immersion extraction and solid-liquid extraction, and are combined with alkali extraction, acid hydrolysis or alkaline hydrogen peroxide treatment as the main extraction process. In addition, enzyme-assisted treatment is sometimes used. However, the above-mentioned extraction methods usually require a long operation or reaction time, a large amount of sample is required for extraction, a large amount of organic solvents are used during the extraction process, and long-term heating causes a reduction in the activity of the active ingredients, resulting in the final The concentration of the extracted sample is low and the extraction efficiency is not high. In addition, in addition to high labor costs, it may also have an impact on 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, they have many characteristics such as fixed propagation direction, high energy, strong penetrating ability, and cavitation effect. Therefore, ultrasonic-assisted extraction methods have begun to be used. Compared with traditional extraction methods, ultrasonic extraction can fully mix and contact the extraction liquid, accelerate the swelling and hydration of substances and solvents, promote the penetration of solvents, shorten the dissolution equilibrium time of target active ingredients, increase the diffusion rate of active ingredients, and improve The shortcomings of traditional solvent extraction can effectively shorten the extraction time; at the same time, it can reduce the amount of solvent used and save costs. It is an environmentally friendly extraction method. During this extraction operation, it can be operated at low temperature and normal pressure to avoid the volatilization of low-boiling point substances. It can retain the natural structure of biologically active substances and various nutrients in the extract to the maximum extent, and avoid the thermal effect of high-temperature treatment, causing effective Problems such as changes, losses, damage and reduction in physiological activity of ingredients; at the same time, improve the extraction rate and quality of active ingredients, increase the extraction effect, reduce the dissolution of impurity ingredients, have high purity, and the active ingredients are easy to separate and purify; in terms of safety and operation It is also more convenient than other extraction methods.

Compared with traditional microwave, supercritical fluid, and molecular distillation extraction methods, high-intensity ultrasound is lower in cost, repeatable, simple to operate, and can effectively replace other extraction methods. It can be used in industry Improve the extraction and utilization of bioactive substances in food, natural plant materials or Chinese herbal medicine. By changing the extraction conditions, the ultrasonic extraction method can solve the advantages of traditional extraction that is time-consuming, thermally destroy effective substances, and reduce production costs.

The ultrasonic-assisted extraction method has the above-mentioned industrial advantages. However, single-frequency ultrasonic waves are prone to generate standing waves and reduce the occurrence of cavitation. Multiple-frequency operation increases mechanical vibration and incorporates more gas, resulting in an increase in cavitation nuclei. Through the interactive influence of the cavitation process, low-frequency negative pressure reduces the cavitation threshold, the resonance frequency is close, and the number and effect of cavitation nuclei are increased, which can make the sound field more uniform. Different waveforms such as frequency doubling waves also appear to improve cavitation. In addition, through the resonance response of functional components and frequency, different functional components can be extracted at the same time, making the mechanical equipment multi-functional. In addition, in recent years, pressure-regulated ultrasonic-assisted extraction technology has been researched and developed to further improve extraction efficiency.

Currently, in the literature and patent searches, there is little information on the continuous process of pressure-adjusted ultrasonic-assisted extraction and pressure-reducing extraction that can instantly release pressure for decompression extraction. Therefore, it is expected by the industry to develop a pressure-regulated ultrasonic auxiliary extraction device that integrates the ultrasonic source and the pressure cooker extraction tank to optimize extraction quality.

Therefore, to achieve the above object, an embodiment of the present application provides an extraction system, wherein the extraction system includes a holding tank and a pressure control module. The accommodation tank includes an outer cylinder, an inner cylinder and a valve. The inner cylinder is arranged inside the outer cylinder and has an internal accommodation space. An external accommodation space is formed between the outer cylinder and the inner cylinder. The valve connects the external accommodation space and the internal accommodation space. The pressure control module is connected to the external accommodation space and the internal accommodation space respectively to separately and simultaneously control the pressure in the external accommodation space and the pressure in the internal accommodation space.

Another embodiment of the present application provides an extraction method, which includes the following steps. An extraction system as described above is provided. Place a substance to be extracted into the inner cylinder of the holding tank. A first extraction process is performed on the substance to be extracted contained in the inner cylinder. Introduce the material to be extracted into the outer cylinder of the holding tank through the valve. A second extraction process is performed on the substance to be extracted contained 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.

The details of one or more embodiments of the subject matter described in this specification are set forth in the accompanying drawings and the following description. Other features, aspects and advantages of the subject matter will become apparent from the description, diagrams and technical solutions.

In order to have a clearer understanding of the characteristics, content, advantages and effects of the present invention, the present invention is described in detail below in conjunction with the accompanying drawings and in the form of embodiments. The drawings used are only The figures are for illustrative and auxiliary purposes only, and the proportions and configuration relationships of the attached drawings should not be interpreted to limit the patentable scope of the present invention.

This application mainly provides an extraction system 1 and an extraction method, which uses a high-efficiency method of pressure regulation and ultrasonic assistance to extract a solution of a substance to be extracted. Figure 1 is a schematic diagram of an extraction system 1 disclosed in an embodiment of the present application. In this embodiment, the extraction system 1 includes a receiving tank 2 , a pressure control module 3 , a sealing cover 4 and a shell 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 accommodating groove 2 .

The accommodating tank 2 includes 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 internal accommodation space 200 for accommodating the substance to be extracted; an external accommodation space 220 is formed between the outer cylinder 22 and the inner cylinder 20 for accommodating the substance to be extracted. material. The openings 202 and 222 above 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 this 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 may be made of metal, such as stainless steel, and are respectively fixed to the base of the accommodating tank 2 by welding. The outlet pipeline 26 is disposed on the outer cylinder 22 and is openably and closably connected to the external accommodation space 220 so that the extracted liquid can be discharged from the accommodation tank 2 through the outlet pipeline 26 .

The sealing cover 4 has an openable and closable feed port 40, which communicates with the outside of the extraction system 1 and the internal accommodation space 200 of the inner cylinder 20, whereby the substance to be extracted can be placed into the inner cylinder 20 from the feed port 40. Internal storage space 200.

The valve 24 penetrates the side wall 204 of the inner cylinder 20 to communicate with the external accommodating space 220 in the outer cylinder 22 and the internal accommodating space 200 in the inner cylinder 20 . Valve 24 may be an electronically controlled relief valve. The substance to be extracted can move from the inner containing space 200 of the inner barrel 20 to the outer containing space 220 of the outer barrel 22 through the valve 24 . For example, the valve 24 can be disposed at the bottom of the side wall 204 of the inner cylinder 20 to allow the material to be extracted to flow directly from the inner cylinder 20 to the external accommodation space 220 of the outer cylinder 22 by gravity or pressure difference.

In an embodiment of the present application, a first pressure source 11 is provided and connected to the internal accommodation space 200 through a pipe 111 that penetrates the outer shell 5, the outer cylinder 22 and the inner cylinder 20, so as to provide a first pressure to the interior. Accommodation space 200. A second pressure source 12 may also be provided, connected to the external accommodating 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 external accommodating space 220.

The pressure control module 3 controls the pressure in the external accommodation space 220 and the pressure in the internal accommodation space 200 respectively and simultaneously. In this 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 internal accommodation 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 to measure the pressure in the external accommodation space 220 and transmit 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 of the external accommodation space 220 and the pressure in the internal accommodation space 200 .

In this 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 this embodiment, the first pressure source 11 may include a pressurizing element, such as an air compressor, whose applied pressure may be between 0 and 7 kgf/cm ² to pressurize the container cavity. In one embodiment, the applied pressure of the pressurizing element may be between 0 and 5 kgf/cm ² . In this embodiment, the second pressure source 12 may include a pressure reducing element, such as a vacuum pump, whose applied pressure may be 0 to 700 mmHg. In one embodiment, the pressure applied by the pressure reducing element may range from 0 to 500 mmHg. The pressure controller 34 may have a pressure parameter. The pressure controller 34 may selectively control the first pressure source 11 (pressure element) and the second pressure source 12 (pressure reduction element) based on the pressure parameter and the pressure sensing signal. Open and close. When the material to be extracted is treated with high pressure, pressurization can increase the amount of dissolved gas, increase the cavitation effect, and also increase the intensity of bubble destruction. When the substances to be extracted are treated under reduced pressure, the principle that extraction at low temperature can reduce the amount of solvent dissolved gas, viscosity and surface tension, affecting the ultrasonic cavitation effect, is used to extract heat-sensitive and easily oxidizable substances. When the substance to be extracted is moved from the high-pressure inner cylinder to the outer cylinder, the instantaneous controlled pressure drop process (DIC) is used. This pressure adjustment method will promote the evaporation of water in the material, expansion and cavitation, thereby increasing the Contact area and reduced diffusion resistance improve extraction efficiency.

In this embodiment, the extraction system 1 further includes a pressure safety control module 36 and a safety valve 38. The safety valve 38 is disposed above the sealing cover 4 and connected to the accommodation tank 2 (not shown). The pressure value of the safety valve 38 may be 1.2 kg/cm ² . The pressure safety control module 36 is used to control that when the extraction pressure in the holding tank 2 is abnormal, the safety valve 38 can be activated to automatically relieve the pressure of the holding tank 2 to ensure safety during the extraction process.

The extraction system of this embodiment further includes a manual pressure relief valve 39, which is disposed above the sealing cover 4 and connected to the accommodation tank 2 (not shown). The pressure adjustment value of the manual pressure relief valve 39 can be between 1 and 30 PSI (pound per square inch). The user can actively operate the manual pressure relief valve 39 to reduce the pressure in the accommodation tank 2 to a desired value.

In this 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 transmitting element 64 and at least one second frequency transmitter. Element 66. The first frequency transmitting element 64 is disposed on the outer surface of the side wall 204 of the inner cylinder 20 to provide ultrasonic oscillation of at least a first frequency to the internal accommodation space 200 . The second frequency transmitting element 66 is disposed on the outer surface of the outer cylinder 22 to provide at least a second frequency of ultrasonic oscillation to the external accommodation space 220 . In this embodiment and some embodiments, the first frequency transmitting element 64 and the second frequency transmitting element 66 can simultaneously provide ultrasonic oscillations 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 may be 28, 68 and/or 133 kHz.

In this embodiment, the extraction system 1 further includes a frequency sweep module 68 for measuring the ultrasonic frequencies provided by the ultrasonic module 6 to the internal accommodating space 200 and the external accommodating space 220 respectively. In another embodiment, the extraction system further includes an energy density measuring device for measuring the energy density applied to the inner accommodation space 200 and the outer accommodation space 220 . Thereby, the measured ultrasonic frequency or energy density is transmitted to the ultrasonic controller 60 to adjust the output of the ultrasonic module 6 . The structure and operation of the ultrasonic module 6 and the frequency sweep module 68 are techniques well known to those with ordinary knowledge in the art, and therefore will not be described in detail here. In this article, "energy density" refers to the power provided by the ultrasonic module per unit weight of the substance to be extracted, and its unit can be W/g (Watt/gram). In one embodiment, the extraction power may range from 0 to 300 W. In this embodiment, the frequency sweep module 68 may include a voltage phase sensor, which is disposed on the bottom or side wall of the accommodating tank 2 to regulate the phase change of the operating voltage, feedback the operating point to increase the original frequency and reduce the Standing waves occur.

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 to measure the temperature of the extraction liquid in the inner cylinder 20 and the outer cylinder 22 and generate 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 element 74 is connected to the inner cylinder 20 and the outer cylinder 22 and the temperature controller 70, and is used to heat the substances to be extracted in the inner cylinder 20 and the outer cylinder 22 according to the instructions of the temperature controller 70. The cooling element 76 is connected to the inner cylinder 20 and the outer cylinder 22 and the temperature controller 70 to cool the solution of the substance to be extracted in the inner cylinder 20 and the outer cylinder 22 according to the instructions of the temperature controller 70 . The temperature control module 7 can selectively control the opening and closing of the heating element 74 and the cooling element 76 based on the set temperature parameters and temperature sensing signals. In this embodiment, the heating element 74 and the cooling element 76 can be used to make the extraction temperature range from 0 to 199°C.

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, ultrasonic frequency, energy density, operating time, pressure, etc. of the inner cylinder 20 and the outer cylinder 22. The operation panel 52 can operate the above-mentioned values such as temperature, ultrasonic frequency, operating time, pressure, etc.

Figure 2 is a flow chart of an extraction method according to an embodiment of the present application. One embodiment of the present application provides an extraction method, which includes the following steps. In step S110, the above-mentioned extraction system 1 is provided.

In step S120, a substance solution to be extracted is placed in the inner cylinder of the holding tank. For example, the preparation method of the substance to be extracted may include: directly adding water to the substance to be extracted as fresh raw materials and placing it in a blender to form a slurry as the solution to be extracted; or drying it with hot air or freeze-drying methods. , carry out grinding processing to obtain the powder raw material to be extracted, add an extraction solvent (such as water) and form a solution to be extracted. In one embodiment, the weight percentage of raw material and extraction solvent is 1:10 to 1:50g/mL.

In step S130, a first extraction process is performed on the substance to be extracted contained in the inner cylinder. In this embodiment, the first extraction process further includes heating the substance to be extracted to a first temperature. The first extraction treatment may also include applying a first ultrasonic shock to the substance to be extracted. The first extraction process may further include applying a first pressure to the material to be extracted.

Regarding the heating treatment of the first extraction process, the substance to be extracted in the inner cylinder can be heated to a certain value within a period of time (for example, maintained at 80°C). In other embodiments, different heating temperatures for the material to be extracted can be provided sequentially in different time periods (for example, the material to be extracted is heated to 60°C in the first period of 20 minutes and the material to be extracted is heated to 40 minutes in the second period). to 80 ℃).

Regarding the ultrasonic vibration of the first extraction process, in the first extraction process of step S130 in one embodiment, the low frequency can be turned on to effectively destroy the cell wall of the material in the first period (for example, the first 15, 30, and 60 minutes) , to increase the diameter of the micropores, shorten the diffusion mass transfer distance, and improve the internal diffusion mass transfer efficiency; then turn on high-frequency ultrasonic waves in the second period (such as the next 15, 30, and 60 minutes) to increase the vibration effect so that the solute can Rapidly diffuses into the solvent to improve extraction efficiency.

In the first extraction process of step S130 in another embodiment, low-frequency and high-frequency ultrasonic waves can be turned on simultaneously for a period of time (for example, 15, 30, 45, 60 minutes) to enhance mechanical vibration and incorporate more gas, resulting in an increase in hole nuclei. , can make the sound field more uniform, and even appear different waveforms such as frequency doubling waves to improve cavitation, thereby increasing extraction efficiency.

Regarding the pressure application in the first extraction process, similar to the aforementioned heating process, the same pressure may be provided only in one period of time, or different pressures may be provided in different periods of time.

In step S130 disclosed in this application, the modes of ultrasonic oscillation, energy density, pressure application and temperature control in the first extraction process can be adjusted according to the characteristics of the substance to be extracted. The modes can be maintained at a constant value or at different values. Provide different ultrasonic frequencies, energy densities, pressures and/or temperatures during the time period. In some embodiments, only at least one of ultrasonic frequency, pressure and temperature adjustment may be used in the first extraction process.

Next, after the first extraction process is completed, in step S140, the substance to be extracted is introduced into the outer cylinder 22 of the holding tank 2 through the valve 24. In one embodiment, when the first extraction process has reached a predetermined operating time, the valve 24 can be opened automatically or manually, and the material to be extracted in the inner cylinder 20 falls into the second container of the outer cylinder 22 through the valve 24 Within space 220.

In step S150, a second extraction process is performed on the substance to be extracted contained in the outer cylinder 22. The second extraction process includes applying a second pressure to the material 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 includes heating the substance to be extracted to a second temperature. The second extraction process further includes applying a second ultrasonic vibration to the material to be extracted.

In one embodiment, similar to the first extraction process, in the second extraction process, the ultrasonic vibration, pressure application, temperature control and other modes in the second extraction process can be adjusted according to the characteristics of the substance to be extracted. These operating values maintain a constant value, or provide different ultrasonic frequencies, energy densities, pressures and/or temperatures in different time periods. In some embodiments, only at least one of ultrasonic frequency, pressure and temperature adjustment may be used in the second extraction process.

In this embodiment, the pressure range of the first pressure and the second pressure is between 0-5 kgf/cm ² absolute pressure; the first temperature and the second temperature range are between 0 and 199°C; and the first ultrasonic oscillation The frequency and the frequency of the second ultrasonic oscillation range from 28 to 133 kHz.

In this embodiment, the extraction method further includes measuring the frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation respectively in steps S130 and S150, or measuring the frequencies applied to the external accommodation space and the internal accommodation respectively. Energy density in space. Thereby, according to the measured frequency of the first ultrasonic oscillation and the frequency or energy density of the second ultrasonic oscillation, the intensity of the first ultrasonic oscillation and the second ultrasonic oscillation are adjusted to achieve better ultrasonic oscillation. Shocking effect.

In addition, regarding the pressure application of the first and second extraction processes, in one embodiment, only one of the inner cylinder 20 and the outer cylinder 22 can be pressurized alone, or only one of the outer cylinder 22 can be pressurized alone. That is, according to actual needs, only the first extraction process can be pressurized, or only the second extraction process can be depressurized.

In the embodiment of the present application, the pressure difference operation is performed through the concentric double-cylinder structure design of the inner cylinder 20 and the outer cylinder 22. After the inner cylinder 20 is pressurized, it can be quickly moved to the outer cylinder 22 for decompression operation. . That is to say, the substance to be extracted can first be extracted under pressure in the inner cylinder 20 of the holding tank 2 , and then moved to the outer cylinder 22 through the valve 24 . When the material to be extracted enters the depressurized outer cylinder 22 from the pressurized inner cylinder 20, an instantaneous pressure difference is caused by the rapid decrease in pressure. The pressure inside the material to be extracted is released outward, and the raw material structure is rapidly destroyed, increasing the internal pressure. The extraction material release effect; in addition, when the outer cylinder 22 is performing a depressurization operation, the inner cylinder 20 can also perform pressurized extraction of the next batch of substances to be extracted at the same time, which can be semi-continuously operated to effectively shorten the extraction time and improve The effect of extraction efficiency.

In this application, the extraction system 1 can use process combination and structural design to improve extraction efficiency for biological materials with different characteristics. In one embodiment, multiple frequency combination extraction methods are used to first turn on low frequency to effectively destroy the cell wall of the substance to be extracted, thereby increasing the diameter of the micropores, shortening the diffusion mass transfer distance, and improving the internal diffusion mass transfer efficiency; and then Turn on high-frequency ultrasonic waves to increase the vibration effect, so that solutes can quickly diffuse into the solvent and improve extraction efficiency.

In another embodiment, low-frequency and high-frequency ultrasonic waves can be turned on at the same time to enhance mechanical vibration (for example, frequencies of 28 kHz, 68 kHz, or 133 kHz can be turned on at the same time), and more gas can be incorporated to increase the number of hole nuclei, making the sound field more uniform. , and even different waveforms such as frequency doubled waves appear to improve cavitation and thereby increase extraction efficiency.

In other words, the extraction method of this application uses an ultrasonic module to vibrate the substance to be extracted to perform an ultrasonic-assisted extraction process. It can be simultaneously or selectively combined with multiple frequencies (different frequencies are operated sequentially), and compound operations (different frequencies are turned on at the same time). Frequency extraction), temperature control and pressure adjustment 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 substance to be extracted.

In step S160, when the second extraction process is completed, the outlet pipeline 26 can be opened manually or automatically to take out the extracted solution.

The following introduces the results of the application of the pressure-regulated and ultrasonic-assisted extraction system 1 provided in this application to the extraction of purslane raw materials. First, when performing ultrasonic-assisted extraction, water is used as the extraction solvent. The starting temperature of the extraction is controlled at 40°C. The prepared raw material liquid after pretreatment is placed into the holding tank 2 of the extraction system 1, and then the pressure is used. The control module and ultrasonic module perform extraction and can adjust the extraction parameters. After the filtrate is obtained from the extracted liquid, the index component content is analyzed. The ultrasonic extraction operating parameters discussed in this section include solid-liquid ratio, frequency, energy density, multiple frequency combination (different frequencies are operated in sequence), compound operation (different frequencies are turned on at the same time for extraction) and pressure adjustment combination (different extraction pressures are operated in sequence). Operation) treatment, etc., and the control group is traditional hot water (95 ℃) extraction. First set of experiments

In the first set of experiments, the applicant conducted experimental comparisons between the extraction system 1 of the present application and the traditional batch system to extract mucopolysaccharides from the material to be extracted (fresh purslane raw materials) by adding and reducing pressure and using ultrasonic-assisted extraction. The influence of pressure, ultrasonic frequency, temperature and other parameters are the same. The experimental results are as follows in Table 1: Table 1. Mucopolysaccharide extraction rates using the semi-continuous extraction system of this application and traditional batch extraction equipment Operation method Mucopolysaccharide extraction rate (%) The semi-continuous extraction system of this application 59.1 Traditional batch extraction equipment 55.7

As shown in the table above, although the semi-continuous extraction system 1 of this application only increases the extraction rate by 3.4% compared to the traditional batch extraction system, the design of the concentric double-cylinder holding tank 2 of this application is There are two more obvious advantages for the batch-type single-cylinder tank mechanism:

First, if you want to achieve similar extraction rates under the same operating time, the batch single-cylinder tank mechanism requires two sets of single-cylinder tank test equipment for series operation, but the extraction system with double-cylinder tanks in this application only requires one set. Can. Under such operation, the system of this application can reduce equipment costs by approximately 35% (approximately NT$560,000) and equipment space by 50% compared to batch-type mechanisms.

Second, regarding the manufacturing cost and installation space, a batch-type single-cylinder tank mechanism is used for extraction. If you want to achieve an extraction rate similar to the extraction system 1 of this application, the pressure needs to be returned to normal pressure during the operation. , and then replace the pressure adding and reducing equipment to perform the pressure adding and reducing operation, so the operation time will be increased; but the equipment of this application does not require such a complicated process. Therefore, compared with a batch mechanism, the extraction system 1 of the present application can shorten the process time by about 30% (about 15 minutes). Second set of experiments

In the second set of experiments, different types of raw materials were used for extraction for 30 minutes.

The first raw material type: purslane powder, under different operating pressures such as normal pressure, 5 kgf/cm ² and 500 mmHg, using an ultrasonic frequency of 28 kHz, a solution ratio of 1:20 g/mL, and an energy density of 0.05 W /g, extraction time of 30 minutes, etc. under the same experimental conditions, the mucopolysaccharide extraction rates were increased by 81.3, 143.8 and 123.8% respectively compared with traditional hot water extraction, as shown in Table 2 below. Table 2. Extraction rate of mucopolysaccharide from purslane powder by traditional water extraction and pressure ultrasound-assisted extraction. operating pressure Mucopolysaccharide extraction rate (%) Traditional water extraction 0 8.0 normal pressure 0 14.5 pressurize 5 kgf/cm ² 19.5 Decompress 500mmHg 17.9

The second raw material type: fresh purslane raw material slurry, using ultrasonic frequency of 28 kHz, material-to-liquid ratio of 1:20 g/mL, and energy at different operating pressures such as normal pressure, 5 kgf/ ^cm2 and 500 mmHg. Under the same experimental conditions with a density of 0.05 W/g and an extraction time of 30 minutes, the mucopolysaccharide extraction rates are 40.9, 150.3 and 84.3% higher than those of traditional hot water extraction, respectively, as shown in Table 3 below. Table 3. Traditional water extraction and pressure ultrasound-assisted extraction of mucopolysaccharides from fresh purslane raw materials. operating pressure Mucopolysaccharide extraction rate (%) Traditional water extraction 0 15.9 normal pressure 0 22.4 pressurize 5 kgf/cm ² 39.8 Decompress 500mmHg 29.3

From the second set of experiments mentioned above, it can be easily known that the extraction rate can be improved regardless of the method of normal pressure, increased pressure or reduced pressure. And the extraction rate using pressure or reduced pressure is higher than traditional water extraction and normal pressure. The third set of experiments

In this set of experiments, fresh purslane raw material slurry with a material-to-liquid ratio of 1:10 g/mL was used, and different energy densities and extraction times were changed for measurement.

The first situation is to conduct experiments with different energy densities: using an energy density of 0.05 W/g, a frequency of 28 kHz, and an extraction time of 30 minutes, the results include normal pressure, reduced pressure (500 mmHg), and pressurized (5 kgf/cm ² ), the mucopolysaccharide extraction rates are 31.0, 35.9, and 41.6% respectively, which are 13.3, 18.2, and 23.9% higher than the mucopolysaccharide extraction rates of traditional hot water extraction (17.7%); if the energy density of 0.1 W/g is used for auxiliary extraction , after 30 minutes of extraction, the mucopolysaccharide extraction rates at normal pressure, reduced pressure (500 mmHg), and pressurized (5 kgf/cm ² ) were 35.6, 39.1, and 46.9% respectively, which were significantly higher than the mucopolysaccharide extraction rates of traditional hot water extraction. Increases of 17.9, 21.4, and 29.2%. Figure 1: Mucopolysaccharide extraction rate of fresh purslane raw materials with different energy densities (W/g) and pressure-regulated ultrasonic assisted extraction (frequency 28 kHz, material-to-liquid ratio 1:10 g/mL, time 30 minutes)

The second case is to conduct experiments with different extraction times: using an ultrasonic frequency of 28 kHz, a solution ratio of 1:10 g/mL, and an energy density of 0.05 W/g for 120 minutes at normal pressure, the mucopolysaccharide extraction rate is 42.0%, which is approximately equivalent to the mucopolysaccharide extraction rate (41.6%) of extracting for 30 minutes at a pressure of 5 kgf/ ^cm2 and an energy density of 0.05 W/g. It is also 13.8% higher than the extraction rate of traditional hot water extraction for 120 minutes. If the extraction is carried out under normal pressure with an energy density of 0.1 W/g for 120 minutes, the mucopolysaccharide extraction rate is 45.8%, which is better than the extraction at a pressure of 500 mmHg with an energy density of 0.1 W/g for 30 minutes and traditional hot water extraction for 120 minutes. The extraction rate of mucopolysaccharides increased by 6.7 and 17.6%. Detailed data are shown in Table 4 below. Table 4. Effects of different energy densities (W/g) and different ultrasonic-assisted extraction times on the extraction rate of mucopolysaccharides from purslane raw materials Extraction method Extraction pressure Extraction time(min) Energy density (W/g) Mucopolysaccharide extraction rate (%) traditional hot water 0 30 - 17.7 0 120 - 28.2 0 360 - 49.5 Ultrasonic energy density 0.05 W/g 0 30 0.05 30.9 0 60 0.05 32.8 0 90 0.05 36.1 0 120 0.05 42.0 500mmHg 30 0.05 35.9 5 kgf/cm ² 30 0.05 41.6 Ultrasonic energy density 0.1 W/g 0 30 0.1 35.6 0 60 0.1 40.3 0 90 0.1 41.7 0 120 0.1 45.8 500mmHg 30 0.1 39.1 5 kgf/cm ² 30 0.1 46.9

The third situation is complex frequency combination, that is, different frequencies are operated sequentially for extraction.

Under the same energy density (0.05 W/g), different extraction frequencies were used in sequential combination operations. The results showed that extraction at 28 kHz frequency could obtain higher mucopolysaccharide content. Group 1 (sequential ultrasonic wave at 28 kHz) The mucopolysaccharide extraction rates of group 2 (executed at 28 kHz for 15 minutes and 133 kHz for 15 minutes) were 42.1 and 35.1%, which are multiple frequency combinations (executed sequentially for 15 minutes). and 15 minutes), the two groups with the highest mucopolysaccharide content in ultrasound-assisted extraction. The mucopolysaccharide extraction rate (42.1%) of Group 3 (sequentially performed at 28 kHz for 15 minutes and 68 kHz for 15 minutes) was higher than that of Group 4 (sequentially performed at 68 kHz for 15 minutes and 28 kHz for 15 minutes) and Group 4, respectively. Group 5 (133 kHz for 15 minutes and 28 kHz for 15 minutes) and Group 6 (traditional hot water extraction for 30 minutes) were 9.9, 9.7 and 24.4% higher. Figure 2. Effect of multiple-frequency combination (15 minutes/15 minutes) ultrasonic-assisted extraction on the extraction rate of mucopolysaccharides from fresh purslane raw materials (solution ratio 1:10 g/mL, energy density 0.05 W/g, operating time 30 minutes)

The fourth situation is multiple frequency compounding, which means turning on different frequencies for extraction at the same time.

Under the same energy density (0.05 W/g), different extraction frequencies are used for composite operations at the same time. The results show that using multiple frequency compound extraction for 30 minutes, the extraction effect of mucopolysaccharides from purslane fresh raw materials is better than that of traditional hot water extraction, and the extraction rate of mucopolysaccharides is obtained by using 28+68+133 kHz processing at the same time. The maximum extraction rate is 48.2%, which is 30.5% higher than that of traditional hot water extraction. It also increases the extraction rate by 3.8, 8.6 and 19.1% respectively compared to turning on 28+68, 28+133 and 68+133 kHz at the same time. It is also higher than the multiple frequency combined type (in that order). (28 kHz for 15 minutes and 68 kHz for 15 minutes, as shown in Figure 3), the extraction rate of mucopolysaccharides (42.1%) is 6.1% higher. Figure 3. Effect of multiple-frequency composite ultrasonic-assisted extraction on the extraction rate of mucopolysaccharides from purslane fresh raw materials (solution ratio 1:10 g/mL, energy density 0.05 W/g, extraction time 30 minutes)

Based on the above, this application provides an extraction system and an extraction method that integrate an ultrasonic source, a pressure extraction container 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 materials can be subjected to different extraction processes in the inner and outer cylinders, and the extracted materials can be quickly moved from the inner cylinder to the outer cylinder for pressure increase and decrease, which improves the convenience of the pressure adjustment process. properties and significantly reduce the size of the device. At the same time, it can be combined with multi-frequency ultrasonic treatment to carry out the extraction process according to the characteristics of the raw materials and product requirements, so that the ultrasonic waves can fully contact the extraction materials, improve the efficiency of ultrasonic energy operation, improve the quality of the extracted products, and further expand the scope of application. and shorten the process time.

In addition, the pressure, ultrasonic frequency, energy density and temperature parameters of this application can be adjusted according to the characteristics of the substances to be extracted or product requirements to achieve optimization.

Although this specification contains many specific implementation details, these should not be construed as limiting the scope of any feature or content that may be claimed, but rather as describing features that are specific to particular embodiments. Certain features that are described in this specification within the context of separate embodiments can also be implemented combined in a single embodiment. Conversely, various features described herein within a single embodiment can also be implemented in multiple embodiments separately or in any suitable subcombination. Furthermore, although features may be described above as functioning in a particular combination and even initially claimed as such, one or more features from a claimed combination may in some cases be deleted from the combination, and the claimed combination may be related to A subcombination or a variation of a subcombination.

The invention has been described with reference to the embodiments and it is understood that specific applications of the features of the invention may be practiced individually and/or in various combinations and/or on various types. Furthermore, those skilled in the art will recognize that various modifications may be made to the embodiments in any of their uses without departing from the scope of the invention. Furthermore, alternative embodiments may be constructed with different constituent materials, structures, and/or spatial relationships and still fall within the scope of the present invention. In view of the above, the present invention should be limited to the scope of the patent claims disclosed in this application or any related applications.

The term "a" or "an" used herein is used to describe elements and components of the present invention. This terminology is used only for convenience of description and to give the basic idea of the present invention. This recitation should be understood to include one or at least one, and the singular also includes the plural unless it is expressly stated otherwise. When used with the word "comprising" in a patent application, the term "a" can mean one or more than one. In addition, the word "or" used in this article has the same meaning as "and/or".

Unless otherwise specified, terms such as "above", "below", "up", "left", "right", "down", "top", "bottom", "vertical", "horizontal", "side" Spatial descriptions such as "higher", "lower", "upper", "above", and "below" indicate the direction shown in the figure. It should be understood that the spatial descriptions used herein are for illustrative purposes only and that actual implementations of the structures described herein may be spatially configured in any relative orientation without this limitation altering the advantages of the various embodiments of the present invention. For example, in the description of some embodiments, providing that one element is "on" another element may cover situations where the former element is directly on (e.g., in physical contact with) the latter element, as well as when an element is "on" the latter element. Or a situation where multiple intervening components are located between the previous component and the following component.

As used herein, the terms "substantially," "substantially," "substantially," and "approximately" are used to describe and account for minor changes. When used in connection with an event or circumstance, these terms may mean both a definite occurrence of the event or circumstance and a close approximation of the occurrence of the event or circumstance.

The above-described embodiments are only for illustrating the technical ideas and characteristics of the present invention. Their purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be used to limit the patent scope of the present invention. Equivalent changes or modifications made in accordance with the spirit disclosed in the present invention shall still be covered by the patent scope of the present invention.

1: Extraction system 2: Accommodation tank 3: Pressure control module 4: Sealing cover 5: Shell 6: Ultrasonic module 7: Temperature control module 11: The first source of stress 12: Second source of stress 20: Inner cylinder 22: Outer cylinder 24: Valve 26: Outlet pipe 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: Feeding port 50: Dashboard 52: Operation panel 60: Ultrasonic controller 62: Ultrasonic power source 64: First frequency transmitting component 66: Second frequency transmitting component 68: Frequency sweep module 70: Temperature controller 72: Temperature sensor 74: Heating element 76: Cooling element 111, 121: Pipe 200: Internal storage space 202: Open your mouth 204: Side wall 220: External accommodation space 222: Open your mouth

In order to have a clearer understanding of the effects achieved by the present invention and its advantages, the present invention is described in detail below with reference to the accompanying drawings and in the form of embodiments.

Figure 1 is a schematic diagram of an extraction system disclosed in an embodiment of the present application.

Figure 2 is a flow chart of an extraction method disclosed in an embodiment of the present application.

1: Extraction system 2: Accommodation tank 3: Pressure control module 4: Sealing cover 5: Shell 6: Ultrasonic module 7: Temperature control module 11: The first source of stress 12: Second source of stress 20: Inner cylinder 22: Outer cylinder 24: Valve 26: Outlet pipe 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: Feeding port 50: Dashboard 52: Operation panel 60: Ultrasonic controller 62: Ultrasonic power source 64: First frequency transmitting component 66: Second frequency transmitting component 68: Frequency sweep module 70: Temperature controller 72: Temperature sensor 74: Heating element 76: Cooling element 111, 121: Pipe 200: Internal storage space 202: Open your mouth 204: Side wall 220: External accommodation space 222: Open your mouth

Claims (10)

An extraction system includes: a storage tank, including: an outer cylinder; an inner cylinder, which is arranged in the outer cylinder and has an internal storage space, and an external storage space is formed between the outer cylinder and the inner cylinder. space; and a valve that connects the external accommodation space and the internal accommodation space; and a pressure control module that connects the external accommodation space and the internal accommodation space respectively to separately and simultaneously control the external accommodation space. The pressure inside and the pressure inside the internal containing space. The extraction system of claim 1 further includes: an ultrasonic module, which includes: a first frequency transmitting element disposed on the outer surface of the inner cylinder to provide an ultrasonic wave of a first frequency to the internal accommodation space. Oscillation; and a second frequency transmitting element disposed on the outer surface of the outer cylinder to provide a second frequency of ultrasonic oscillation to the external accommodation space. For example, the extraction system of claim 2 further includes: a frequency sweep module for measuring the ultrasonic frequency provided by the ultrasonic module to the external accommodation space and the internal accommodation space or an energy density measuring device respectively. , used to measure the energy density applied to the external accommodation space and the internal accommodation space; thereby, the ultrasonic module is adjusted according to the measured ultrasonic frequency or energy density the output. The extraction system of claim 1, wherein the pressure control module further includes: a first pressure sensor for measuring the pressure in the internal accommodation space, and transmitting a first pressure sensor according to the measured pressure. pressure signal; a second pressure sensor for measuring the pressure in the external accommodation 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 to adjust the pressure of the external accommodation space and the pressure in the internal accommodation space. The extraction system of claim 1 further includes: a sealing cover that detachably seals the upper opening of the inner cylinder and the outer cylinder; wherein the inner cylinder and the outer cylinder are generally cylindrical and concentric; And wherein, the sealing cover has an openable and closable feed hole, which communicates with the outside of the extraction system and the internal accommodation space. An extraction method, including: providing an extraction system as claimed in claim 1; placing a substance to be extracted in the inner cylinder of the holding tank; and performing a first extraction process on the substance to be extracted contained in the inner cylinder. ; Introduce the substance to be extracted into the outer cylinder of the holding tank through the valve; and perform a second extraction process on the substance to be extracted contained in the outer cylinder; wherein the first extraction process includes the The substance to be extracted exerts a first pressure, and the second The extraction process includes applying a second pressure to the substance to be extracted, and the first pressure is greater than the second pressure. The extraction method of claim 6, wherein the first extraction treatment further includes heating the substance to be extracted to a first temperature, and the second extraction treatment further includes heating the substance to be extracted to a second temperature. The extraction method of claim 7, wherein the first extraction process further includes applying a first ultrasonic shock to the substance to be extracted, and the second extraction process further includes applying a second ultrasonic shock to the substance to be extracted. For example, the extraction method of claim 8 further includes: respectively measuring the frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation or separately measuring the frequency applied to the external accommodating space and the internal accommodating space. Energy density; and thereby, adjust the first ultrasonic oscillation and the second ultrasonic oscillation according to the measured frequency or energy density of the first ultrasonic oscillation and the second ultrasonic oscillation. intensity. The extraction method of claim 9, wherein the pressure range of the first pressure and the second pressure is between 0-5kgf/cm ² absolute pressure; the first temperature and the second temperature range are between 0-199°C; and The frequency of the first ultrasonic oscillation and the frequency of the second ultrasonic oscillation range from 28 to 133 kHz.

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