A multi-material valuable component efficient leaching device and method based on pressurized dissolved gas cavitation effect

Abstract

The application relates to a multi-material valuable component efficient leaching device and method based on a pressurized dissolved gas cavitation effect, which comprises a cylindrical pressure-resistant container fixed on a support in a horizontal mode, the end port of the pressure-resistant container is provided with a sealing door; a joint pipe A is arranged at the upper part of one end of the pressure-resistant container, a quick opening and closing valve is connected to the joint pipe A, a joint pipe B is arranged at the upper part of the other end of the pressure-resistant container, an air inlet ball valve is connected to the joint pipe B, and a pressure gauge is arranged in the middle part; a joint pipe C is arranged at the lower part of one end of the pressure-resistant container, a liquid discharge ball valve is connected to the joint pipe C, and a liquid inlet pipe is arranged at the upper part of the end; an aeration assembly connected with the air inlet ball valve is arranged in the pressure-resistant container; a pressurized dissolved gas-instantaneous pressure release cavitation mechanism is adopted to form microscale damage force, break through the microscale mass transfer resistance of a solid matrix, efficiently release the wrapped target components, greatly improve the leaching rate and shorten the extraction time; and process parameters can be flexibly adjusted to adapt to various materials from fragile plant tissues to hard mineral ores.

Description

Technical Field

[0001] This invention relates to the field of solid-liquid extraction and separation technology, and in particular to a high-efficiency extraction device and method for valuable components of multiple materials based on pressurized dissolved gas cavitation effect. Background Technology

[0002] Various industrial solid wastes (such as metallurgical slag, fly ash, and waste catalysts), natural minerals (such as lithium ore and rare earth ore), and natural biomass materials (such as Chinese medicinal herbs, tea, fruits and vegetables, and plant roots and stems) contain abundant target components with recycling or deep processing value. The efficient extraction of these components is directly related to the improvement of resource comprehensive utilization rate, efficient development of mineral resources, and product quality and production efficiency in the food and pharmaceutical industries. It is a core and key process in multiple fields such as resource recycling, mining and metallurgy, food processing, and pharmaceutical preparation.

[0003] Currently, traditional extraction technologies generally face numerous bottlenecks in practical applications. These include low mass transfer efficiency, long extraction cycles, high energy consumption, and poor extraction selectivity. Furthermore, for heat-sensitive components such as active ingredients in traditional Chinese medicine and active substances in fruits and vegetables, these technologies easily cause degradation and reduced activity, severely impacting product quality. To improve mass transfer and extraction efficiency, the industry has made various attempts, such as using multi-stage countercurrent extraction towers to optimize the mass transfer path, enhancing material mixing through stirred reactors, and introducing microwave-assisted methods to increase local temperature. However, these existing technologies still struggle to effectively overcome the microscopic mass transfer resistance within the solid matrix and cannot efficiently address the problem of target components being tightly encapsulated by biomass cell walls and mineral lattices, hindering their release. They also have significant shortcomings in extraction efficiency, energy consumption control, applicable material range, and environmental friendliness, failing to meet the urgent needs of various industries for efficient, energy-saving, and universally applicable extraction technologies. Summary of the Invention

[0004] To address the aforementioned problems, this invention proposes a high-efficiency extraction device and method for valuable components from multiple materials based on pressurized dissolved air cavitation effect.

[0005] The technical solution of the present invention is: a high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect, comprising a cylindrical pressure-resistant container fixed horizontally on a support, the port of the pressure-resistant container being provided with a sealing door; a connector pipe A is provided at the upper part of one end of the pressure-resistant container, and a quick-opening and closing valve is connected to the connector pipe A; a connector pipe B is provided at the upper part of the other end, and an inlet ball valve is connected to the connector pipe B; a pressure gauge is provided in the middle; a connector pipe C is provided at the lower part of one end of the pressure-resistant container, and a drain ball valve is connected to the connector pipe C; an inlet pipe is provided at the upper part of this end.

[0006] Preferably, the pressure vessel is equipped with an aeration assembly connected to the inlet valve.

[0007] Preferably, the aeration component is a direct aeration pipe, with a number of nozzles evenly arranged along its length. The direct aeration pipe is located at the bottom of the pressure vessel, and the end of the direct aeration pipe is provided with an elbow pipe connected to the inlet valve.

[0008] Preferably, the aeration component is a spiral aeration pipe fitted into the pressure-resistant container. Several nozzles are evenly arranged on the inner wall of the spiral aeration pipe along its spiral direction. One end of the spiral aeration pipe is provided with an elbow pipe connected to the inlet valve.

[0009] Preferably, the inlet pipe is inclined to the pressure vessel, with the inclination direction consistent with the length direction of the pressure vessel, or the inlet pipe is tangentially connected to the pressure vessel, and there is an angle between the inlet pipe and the generatrix of the pressure vessel.

[0010] Preferably, the sealing door is connected to the pressure vessel via a locking mechanism. The locking mechanism consists of several ear plates evenly distributed on the outer side of the port of the pressure vessel, a screw rod hinged on the ear plates, and a manual nut connected to the outer end of the screw rod. The outer side of the sealing door is provided with a sleeve seat corresponding to the ear plates. The screw rod slides into the sleeve seat, and the manual nut is supported on the outer end face of the sleeve seat. A spring is sleeved on the screw rod between the sleeve seat and the ear plates.

[0011] Preferably, the port of connector pipe B is equipped with a flange. The inlet valve is connected to the flange via clamps.

[0012] An extraction method for a high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect, comprising the following steps: Step 1: Loading and wetting: Load the solid material into the pressure-resistant container, and inject the leachate through the inlet pipe until the material is submerged. The special connection structure of the inlet pipe causes the leachate to generate a jet effect, which causes the leachate to generate spiral turbulence, and performs preliminary wetting and mass transfer on the solid material. Step 2: Pressurized dissolved gas permeation: Close the quick-opening valve, start the gas source, and introduce high-pressure gas into the pressure-resistant container through the inlet balloon valve to the preset pressure. Maintain the pressure for a period of time to allow the gas to fully dissolve in the extract and permeate into the micropores and fissures of the material under pressure. Step 3: Instantaneous pressure relief cavitation: The rapid opening and closing valve is opened instantly, and the pressure inside the pressure vessel drops to atmospheric pressure in a very short time. The dissolved gas quickly becomes supersaturated and precipitates out, triggering a large-scale cavitation effect, which powerfully releases the target components inside into the extract. Step 4: Separation and Collection: Repeat steps 2 and 3 several times. After extraction is complete, open the drain ball valve to discharge the extract rich in the target components.

[0013] The beneficial technical effects of this invention are: (1) The present invention adopts the "pressurized gas dissolution-instantaneous pressure release" cavitation mechanism to form microscale destructive force, break through the microscopic mass transfer resistance of solid matrix, efficiently release the encapsulated target components, greatly improve the leaching rate and shorten the extraction time; the process parameters can be flexibly adjusted to adapt to various materials from fragile plant tissues to hard mineral ores, and the versatility is extremely strong.

[0014] (2) The core energy consumption of this invention is only the power consumption of the pump and the gas source, which is far lower than that of supercritical extraction and large ultrasonic equipment. The use of air or industrial waste gas can further reduce costs, making it economical to operate. The entire process can be operated at room temperature or low temperature, avoiding the damage of heat-sensitive components by high temperature, and effectively ensuring the activity of the extract and the quality of the product.

[0015] (3) This invention integrates multiple enhancement methods such as atmospheric pressure turbulence, micropore aeration, and pressurized cavitation, and can customize an exclusive extraction process according to the material characteristics, with high operational flexibility; the device is based on standard pressure vessel design, without complex precision parts, and the scale-up design route is clear, making it easy to achieve large-scale continuous or batch production. Attached Figure Description

[0016] Figure 1 This is a three-dimensional structural schematic diagram of the present invention; Figure 2 yes Figure 1 A magnified view of a portion of the image; Figure 3 This is a schematic diagram of the main structure of the present invention (showing the internal direct aeration pipe); Figure 4 This is a schematic diagram of the main structure of the present invention (showing the internal spiral aeration pipe); Figure 5 This is a three-dimensional structural diagram of a direct aeration pipe; Figure 6 This is a schematic diagram of the structure of the extraction device of the present invention with a pusher at the end; Figure 7 This is a physical image of the present invention.

[0017] In the diagram, 1. Pressure vessel, 11. Connector pipe A, 12. Quick-opening and closing valve, 13. Connector pipe B, 14. Inlet ball valve, 15. Pressure gauge, 16. Connector pipe C, 17. Drain ball valve, 18. Inlet pipe, 19. Clamp, 21. Direct aeration pipe, 22. Spiral aeration pipe, 23. Nozzle, 24. Elbow pipe, 25. Ball head, 26. Nut sleeve, 31. Sealing door, 32. Ear plate seat, 33. Screw, 34. Manual nut, 35. Sleeve seat, 36. Spring, 4. Bracket, 51. Pusher, 511. Base. Detailed Implementation

[0018] Example 1, see appendix Figures 1-6A high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect mainly includes a cylindrical pressure vessel 1 horizontally fixed on a support 4. The pressure vessel 1 has a sealing door 31 at its port. A connector pipe A 11 is provided at the upper part of one end of the pressure vessel 1, which is arranged vertically upward. A quick-opening and closing valve 12 is connected to the connector pipe A 11. The quick-opening and closing valve 12 is selected as a solenoid valve or a starting ball valve. A connector pipe B 13 is provided at the upper part of the other end, which is arranged vertically upward. A ball valve 14 is connected to the connector pipe B 13. A pressure gauge 15 is provided in the middle. A connector pipe C 16 is provided at the lower part of one end of the pressure vessel 1, which is arranged vertically downward. A ball valve 17 is connected to the connector pipe C 16. An inlet pipe 18 is provided at the upper part of this end. The port of the inlet pipe is provided with an internal thread. After the extractant is input from the inlet pipe 18, the inlet pipe is firmly sealed by a threaded plug.

[0019] One end of the pressure vessel 1 is provided with a pusher 51, which is an electric push rod or a hydraulic cylinder. The telescopic rod of the pusher 51 is hinged to the bottom surface of the end of the pressure vessel 1. The lower end of the pusher 51 is hinged to a base 511. The pusher 51 lifts one end of the pressure vessel 1, which facilitates the smooth discharge of the material and extract inside the pressure vessel 1.

[0020] The pressure vessel 1 is equipped with an aeration assembly connected to the inlet balloon valve 14. The aeration assembly is a straight aeration pipe 21, on which several nozzles 23 are evenly arranged along its length. The straight aeration pipe 21 is located at the bottom of the pressure vessel 1, so that the gas covers most of the extract from bottom to top for dissolved gas permeation. The end of the straight aeration pipe 21 is equipped with an elbow pipe 24 connected to the inlet balloon valve 14. The gas is cut into microbubbles by microporous aeration through the nozzles 23 on the straight aeration pipe 21. The microbubbles increase the gas-liquid contact area, prolong the residence time, and also make the gas and liquid mix evenly without dead corners, thereby improving the effect and efficiency of pressurized dissolved gas permeation.

[0021] Alternatively, the aeration component can be designed as a spiral aeration pipe 22 that fits into the pressure vessel 1. The side of the spiral aeration pipe is arranged in close contact with the inner wall of the pressure vessel 1. Several nozzles 23 are evenly arranged on the inner wall of the spiral aeration pipe 22 along its spiral direction. All nozzles point to the center line of the spiral aeration pipe. One end of the spiral aeration pipe 22 is provided with an elbow pipe 24 connected to the inlet balloon valve 14. Gas is synchronously aerated from the circumferential side wall of the pressure vessel 1 to the center through the spiral aeration pipe 22, covering the entire extract for dissolved gas permeation, which further improves the effect and efficiency of pressurized dissolved gas permeation.

[0022] The end of the elbow pipe 24 is provided with a ball head 25, and a nut sleeve 26 is fitted on the outside of the ball head 25. The ball head is pressed tightly against the port of the inlet ball valve 14 by the nut sleeve. The ball surface is used to improve the sealing connection effect and better cope with high pressure gas.

[0023] The inlet pipe 18 is inclined to the pressure vessel 1 and connected to the circulation pump of the extract storage tank through a pipe. The inclination direction is consistent with the length direction of the pressure vessel 1, or the inlet pipe 18 is tangentially connected to the pressure vessel 1. An angle is provided between the inlet pipe 18 and the generatrix of the pressure vessel 1, so that the inlet pipe 18 forms a jet pipe. After the circulation pump is started, the liquid generates spiral turbulence by strengthening the flow field through the inlet pipe 18, which is conducive to fully and efficiently wetting and mass transfer of the material.

[0024] The sealing door 31 is connected to the pressure vessel 1 through a locking mechanism. The locking mechanism mainly consists of several ear plate seats 32 evenly distributed on the outer side of the port of the pressure vessel 1, a screw rod 33 hinged on the ear plate seat, and a manual nut 34 connected to the outer end of the screw rod. The handle part of the manual nut 34 is a ring. The ear plate seat 32 is a channel steel plate, which is welded and fixed to the pressure vessel 1 in the radial direction. The outer side of the sealing door 31 is provided with a sleeve seat 35 corresponding to the ear plate seat 32. The screw rod 33 slides into the sleeve seat 35. The manual nut 34 is supported on the outer end face of the sleeve seat 35. A spring 36 is sleeved on the screw rod 33 between the sleeve seat 35 and the ear plate seat 32.

[0025] The principle of the locking mechanism is as follows: the sealing door 31 is connected to the screw 33 hinged to the ear plate seat 32 through the sleeve seat 35 on its side. When locking the sealing door, the means nut is turned, and the means nut presses against the sleeve seat 35, driving the sealing door 31 to gradually press against the port of the pressure vessel 1. When opening the sealing door 31, the means nut is turned in the opposite direction, and the pressing force on the sleeve seat 35 is gradually released. The elastic force of the spring 36 on the screw 33 drives the sealing door 31 to move outward, automatically opening the sealing door 31.

[0026] The port of connector pipe B13 is equipped with a flange, and the inlet balloon valve 14 is connected to the flange through clamp 19. The inlet balloon valve 14 can be connected to connector pipe B13 without tightening, ensuring that the aeration assembly can be installed smoothly.

[0027] Example 2, see appendix Figures 1-5 An extraction method for a high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect, comprising the following steps: Step 1: Loading and wetting: Solid materials are loaded into a pressure-resistant container 1. The container is equipped with a sieve plate, grid plate or water-permeable mesh bag to process materials of different forms. Extraction liquid is injected from the inlet pipe 18 until the material is submerged. The special connection structure of the inlet pipe 18 causes the extraction liquid to generate a jet effect, which causes the extraction liquid to generate spiral turbulence, and performs preliminary wetting and mass transfer on the solid materials. Step 2: Pressurized dissolved gas permeation: Close the quick-opening valve 12, start the gas source, which consists of an air compressor, a gas cylinder, and a gas pipe. The gas cylinder is filled with CO2, N2, or other inert gases. High-pressure gas is introduced into the pressure-resistant container 1 through the inlet valve 14 to the preset pressure of 0.2-1.0 MPa. The pressure can be adjusted according to the material characteristics and conditions. The pressure is maintained for a period of time to allow the gas to fully dissolve in the leachate and permeate into the micropores and fissures of the material under pressure.

[0028] Step 3: Instantaneous pressure relief cavitation: Instantly open the rapid opening and closing valve 12, with an opening and closing time of 0.1-0.5 seconds, so that the pressure inside the container drops to normal pressure in a very short time. The dissolved gas quickly becomes supersaturated and precipitates out, generating a huge number of bubbles that violently collapse. This triggers a large-scale cavitation effect in the liquid phase. The local extreme high temperature, high pressure and strong micro-jet generated by the collapse of cavitation bubbles can effectively tear apart plant cell walls, break the surface coating of minerals and open the microporous structure of solid waste residue, thereby powerfully releasing the target components inside into the extract.

[0029] Step 4: Separation and Collection: Repeat steps 2 and 3 several times, i.e., multiple pressurization-depressurization cycles. After extraction is completed, open the drain ball valve 17 to discharge the extract rich in the target components for subsequent solid-liquid separation, concentration and purification processes.

[0030] Example 3: Extraction of heat-sensitive active ingredients from traditional Chinese medicinal materials was performed using the extraction apparatus of Example 1, following the process of Example 2. The specific method is as follows: The dried and pulverized ginkgo leaves are placed into a stainless steel or nylon mesh bag and then into a pressure-resistant container 1. A 50% ethanol aqueous solution is injected into the pressure-resistant container 1 through the liquid inlet pipe 18 to wet the material under normal pressure spiral turbulent circulation for 10 minutes. Then, the inlet balloon valve 14 is closed, nitrogen gas is introduced to pressurize to 0.3 MPa, the pressure is maintained for 5 minutes, and then the pressure is instantly released to normal pressure. This "pressurization-depressurization" cycle is repeated 5 times, with a total processing time of about 40 minutes.

[0031] Extraction effect: Compared with the traditional 60℃ hot reflux extraction for 2 hours, the method of the present invention increases the extraction rate of flavonoids by about 25% at room temperature, and takes less time, avoiding component degradation caused by prolonged heating.

[0032] Example 4: Lithium Leaching from Low-Grade Spodumene Ore Extraction was performed using the extraction apparatus of Example 1 and the process of Example 2, as follows: Dilute sulfuric acid solution is injected into pressure vessel 1 through inlet pipe 18. The circulation pump is started to perform atmospheric pressure stirring and leaching for 30 minutes. Then, air is introduced to pressurize to 0.6 MPa. After holding the pressure for 10 minutes, the pressure is released instantly. The pressurization and depressurization cycle is repeated 3 times.

[0033] Extraction results: Compared with single atmospheric pressure stirring leaching for 2 hours, the combined process increased the lithium leaching rate from 68% to 92%, shortened the leaching time, and reduced acid consumption.

[0034] Example 5: Leaching of lithium from electrolytic aluminum waste Extraction was performed using the extraction apparatus of Example 1 and the process of Example 2, as follows: Water is injected through inlet pipe 18 to submerge the material. The circulating pump and microporous aeration components are started, and the material is leached under normal pressure for 30 minutes. Then, air or CO2 (industrial waste gas can be used) is introduced to pressurize the material to 0.6 MPa. The pressure is maintained for 10 minutes and then released instantly. The pressurization and depressurization cycle is repeated 3 times.

[0035] Extraction results: Compared with single atmospheric pressure stirring leaching for 2 hours, the combined process increased the lithium leaching rate from 32% to 93%, shortened the leaching time, and reduced acid consumption.

Claims

1. A high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect, characterized in that: The pressure vessel includes a cylindrical pressure vessel fixed horizontally on a support, with a sealing door at one end; a connector pipe A is located at the upper part of one end of the pressure vessel, with a quick-opening and closing valve connected to the connector pipe A; a connector pipe B is located at the upper part of the other end, with an inlet ball valve connected to the connector pipe B; and a pressure gauge is located in the middle; a connector pipe C is located at the lower part of one end of the pressure vessel, with a drain ball valve connected to the connector pipe C; and an inlet pipe is located at the upper part of that end.

2. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 1, characterized in that: The pressure-resistant container is equipped with an aeration assembly connected to the inlet valve.

3. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 2, characterized in that: The aeration component is a direct aeration pipe with several nozzles evenly arranged along its length. The direct aeration pipe is located at the bottom of the pressure vessel, and the end of the direct aeration pipe is provided with an elbow pipe connected to the inlet valve.

4. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 2, characterized in that: The aeration component is a spiral aeration pipe that is fitted into a pressure-resistant container. Several nozzles are evenly arranged on the inner wall of the spiral aeration pipe along its spiral direction. One end of the spiral aeration pipe is provided with an elbow pipe that is connected to the inlet valve.

5. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 1, characterized in that: The inlet pipe is inclined to the pressure vessel, with the inclination direction consistent with the length direction of the pressure vessel, or the inlet pipe is tangentially connected to the pressure vessel, and there is an angle between the inlet pipe and the generatrix of the pressure vessel.

6. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 1, characterized in that: The sealing door is connected to the pressure vessel via a locking mechanism. The locking mechanism consists of several ear plates evenly distributed on the outer side of the port of the pressure vessel, a screw rod hinged on the ear plates, and a manual nut connected to the outer end of the screw rod. The outer side of the sealing door is provided with a sleeve seat corresponding to the ear plates. The screw rod slides into the sleeve seat, and the manual nut is supported on the outer end face of the sleeve seat. A spring is sleeved on the screw rod between the sleeve seat and the ear plates.

7. The high-efficiency extraction device for valuable components of multiple materials based on pressurized dissolved gas cavitation effect according to claim 1, characterized in that: The port of connector pipe B is equipped with a flange. The inlet valve is connected to the flange via clamps.

8. An extraction method for a high-efficiency extraction device for multiple valuable components based on pressurized dissolved gas cavitation effect, as described in any one of claims 1-7, characterized in that... Includes the following steps: Step 1: Loading and wetting: Load the solid material into the pressure-resistant container, and inject the leachate through the inlet pipe until the material is submerged. The special connection structure of the inlet pipe causes the leachate to generate a jet effect, which causes the leachate to generate spiral turbulence, and performs preliminary wetting and mass transfer on the solid material. Step 2: Pressurized dissolved gas permeation: Close the quick-opening valve, start the gas source, and introduce high-pressure gas into the pressure-resistant container through the inlet balloon valve to the preset pressure. Maintain the pressure for a period of time to allow the gas to fully dissolve in the extract and permeate into the micropores and fissures of the material under pressure. Step 3: Instantaneous pressure relief cavitation: The rapid opening and closing valve is opened instantly, and the pressure inside the pressure vessel drops to atmospheric pressure in a very short time. The dissolved gas quickly becomes supersaturated and precipitates out, triggering a large-scale cavitation effect, which powerfully releases the target components inside into the extract. Step 4: Separation and Collection: Repeat steps 2 and 3 several times. After extraction is complete, open the drain ball valve to discharge the extract rich in the target components.

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