CN109603197B - Supercritical extraction kettle capable of continuously feeding and discharging materials and extraction method - Google Patents
Supercritical extraction kettle capable of continuously feeding and discharging materials and extraction method Download PDFInfo
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- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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Abstract
A supercritical extraction kettle capable of continuously feeding and discharging materials is characterized in that an extraction kettle is arranged on a support, a water bath barrel is arranged outside the extraction kettle, a top cover is arranged at the top of the extraction kettle, at least 2 feeding pipes are arranged on the top cover, feeding valves are arranged on the feeding pipes, feeding end covers provided with the feeding pipes are arranged at the end parts of the feeding pipes, a thrust rod with a lower end provided with a material pushing plate is arranged at the central position of the top cover, a thrust rod gear is arranged on the thrust rod, the thrust rod gear is meshed with a motor gear arranged on an output shaft of a motor, the tail end of the thrust rod is connected with a piston rod of a hydraulic oil cylinder, the hydraulic oil cylinder is connected with a hydraulic pump through an electromagnetic valve, at least 2 slag discharging pipes are arranged at the bottom of the extraction kettle, a slag discharging valve; the invention has simple structure, convenient operation, continuous extraction and manpower and material resource saving, and can be popularized and applied to the field of supercritical extraction.
Description
Technical Field
The invention belongs to the technical field of physical separation devices or equipment, and particularly relates to a supercritical extraction kettle capable of continuously feeding and discharging materials and an extraction method.
Background
Supercritical fluid is a fluid in which a gas is pressurized in a state where the fluid is at or above its critical temperature and critical pressure, and the gas does not liquefy but has a density that increases and has liquid-like properties while retaining gas properties. The supercritical fluid has the advantages of both gas and liquid, has density close to that of liquid, strong dissolving capacity, viscosity close to that of gas, diffusion coefficient far larger than that of common liquid and is beneficial to mass transfer. In addition, the supercritical fluid has zero surface tension and is easily permeated and diffused into micropores of an extracted substance. Therefore, the supercritical fluid has good dissolution and mass transfer characteristics, can quickly reach mass transfer balance with the extract, and realizes effective separation of substances.
The supercritical extraction technology is one of the main directions of grease extraction in the future. From the current literature reports, the oil extraction process has various characteristics of environmental protection, low cost, easy realization and the like, and is even adopted and applied by part of oil production enterprises and used for producing high-end oil. However, this technology has not been widely used to date for decades as it has emerged. Under the traditional supercritical extraction process, the flow direction of an extractant extends along an extraction kettle from bottom to top, an extractant inlet is positioned at the bottom of the extraction kettle, and an extractant outlet is positioned on a cover at the top of the extraction kettle or positioned on the side surface of the upper end of the extraction kettle. Although many literature studies report the influence of the improvement of the supercritical extraction process, including the extraction pressure, extraction temperature, carbon dioxide flow rate, extraction time and other factors on the extraction yield, it is difficult to improve the "chronic" problem of low production efficiency in the supercritical extraction of oil and fat.
The Chinese patent is named as 'a method for extracting grease by rapid supercritical extraction', and patent No. 201410030959X, when an extracting agent flows through an extraction kettle from top to bottom, the method can play the extracting effect of the extracting agent and the squeezing effect of the extracting agent, the extraction efficiency can be greatly improved, but when the extracting agent flows through the extraction kettle from top to bottom, an outlet pipeline is easy to block, the extracting agent is easy to enter and difficult to exit when a material cake filter cake layer is thick, materials at the top are not easy to extract completely, and the extraction efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of complex operations of stopping, relieving pressure, opening a cover, carrying out secondary charging, pressurizing again and the like when material slag is taken out in the extraction process of the conventional supercritical extraction device, and provides a supercritical extraction kettle which is reasonable in design, simple in structure, high in extraction efficiency and convenient to operate and can continuously feed and discharge materials and an extraction method.
The technical scheme for solving the technical problems is that an extraction kettle is arranged on a support, a water bath barrel is arranged outside the extraction kettle, a top cover is arranged at the top of the extraction kettle, at least 2 feeding pipes are arranged on the top cover, feeding valves are arranged on the feeding pipes, feeding end covers are arranged at the end parts of the feeding pipes, an inlet pipe is arranged on each feeding end cover, a thrust rod is arranged at the central position of the top cover and penetrates through the top cover, a material pushing plate is arranged at the lower end of the thrust rod, a thrust rod gear is arranged on the thrust rod, the thrust rod gear is meshed with a motor gear arranged on a motor output shaft, the tail end of the thrust rod is connected with a piston rod of a hydraulic cylinder, the hydraulic cylinder is connected with a hydraulic pump through a solenoid valve, at least 2 slag discharging pipes are arranged at the bottom of the extraction kettle, an outlet pipe is arranged on the slag discharging end cover and is communicated with the mass flowmeter and the separation kettle.
The bottom of the extraction kettle is provided with 5 slag discharging pipes, and the top cover is provided with 5 feeding pipes.
The material pushing plate is provided with air inlet holes.
The filtering layer of the invention is a metal powder sintered filtering disc or a metal woven screen.
The top cover of the invention is provided with a thermometer.
The top cover of the invention is provided with a pressure gauge.
Sealing devices are arranged between the top cover and the extraction kettle, between the inlet pipe and the feeding end cover, and between the slag discharging pipe and the slag discharging end cover.
The slag discharging pipe is of a horn-shaped structure with a small inlet and a large outlet.
The invention relates to an extraction method of a supercritical extraction kettle capable of continuously feeding and discharging materials, which comprises the following steps:
s1, controlling the water bath barrel to perform water bath heat preservation on the extraction kettle, opening the top cover, quickly adding materials into the extraction kettle, connecting the thrust rod with the material pushing plate after penetrating through the top cover, and covering the top cover;
s2, opening an electromagnetic valve, controlling a material pushing plate to descend to the surface layer of the material, closing the electromagnetic valve, opening a motor, driving the material pushing plate to rotate by the motor, smoothing the surface of the material, opening the electromagnetic valve to control the material pushing plate to move downwards, compacting the material, using at least one feeding pipe as an extractant inlet, opening a feeding valve and introducing an extractant, performing extrusion extraction on the whole extraction kettle, using at least one feeding pipe as a material supplementing pipe, closing the feeding valve, opening a feeding end cover, loading the material, closing the feeding end cover, opening the feeding valve, enabling the material to enter the extraction kettle under the push of gravity and the extractant, and rotating the material pushing plate downwards again to complete feeding and material supplementing operation;
s3, enabling an extractant to flow through an outlet pipe and a mass flow meter and then reach a separation kettle, realizing separation of the extractant and the extractant through pressure reduction operation, when the mass flow meter digit is greatly reduced, proving that a slag discharging pipe at the end has basically completed squeezing extraction, closing a slag discharging valve, opening a slag discharging end cover, taking out a horn-shaped filter cake in the slag discharging pipe, after finishing material taking, covering the slag discharging end cover, opening a corresponding slag discharging valve, continuing the squeezing extraction of the slag discharging pipe, wherein at least one slag discharging valve is kept in an open state during the process to ensure the continuity of the squeezing extraction of the whole extraction kettle, and the rest slag discharging valves can be partially or completely closed according to the specific conditions of the indication number of the mass flow meter carried on the outlet pipe, and the method is circularly adopted to sequentially take out the material slag in each slag discharging pipe;
s4, when the material in the extraction kettle 2 is reduced, at least one feeding pipe is reserved as an extracting agent inlet, all or part of the other feeding pipes can close a feeding valve, a feeding end cover 5 with the feeding valve closed is opened, the material is added, after the feeding of the feeding pipes is finished, the corresponding feeding valve is opened, the extracting agent is introduced, the material in the feeding pipes enters the extraction kettle under the double effects of gravity and extracting agent flowing, the material supplementing of the extraction kettle is finished through the leveling and compacting operations of a pushing plate, and the feeding is circularly carried out by adopting the method until the material meets the required requirements.
Compared with the prior art, the invention has the following advantages:
1. a hydraulic device is adopted to mechanically pressurize the materials, and an extractant (carbon dioxide) which cooperatively enters an inner cylinder pushes a material layer to move downwards so as to automatically compress the materials in real time; meanwhile, the material pushing plate pushes the whole material to move downwards, supercritical squeezing extraction is carried out on the material, and the extraction efficiency is higher.
2. The invention adopts the motor gear which is arranged on the motor output shaft and is meshed with the thrust rod gear, and the material pushing plate is driven to rotate by the rotation of the motor so as to trowel the material in the extraction kettle.
3. The top cover is provided with at least 2 feed pipes, and the function of feeding one feed pipe and feeding the extracting agent into the other feed pipe can be realized by controlling the opening and closing of the feed valves; extraction cauldron bottom is provided with 2 at least pipes of slagging tap, through opening and shutting of control valve of slagging tap, realizes that a pipe of slagging tap takes out the material sediment, another pipe of slagging tap normally squeezes the extraction to make whole extraction process of squeezing incessant in succession.
4. In order to realize rapid slag tapping and increase the area of the filter layer, the slag tapping pipe is designed into a horn-shaped structure with a large outlet and a small inlet.
The invention has simple structure, convenient operation, continuous extraction and manpower and material resource saving, and can be popularized and applied to the field of supercritical extraction.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
In the figure: 1. a water bath cylinder; 2. an extraction kettle; 3. a feed pipe; 4. a feed valve; 5. a feed end cap; 6. an inlet pipe; 7. a material pushing plate; 8. a thrust rod; 9. a thrust rod gear; 10. a hydraulic cylinder; 11. a motor gear; 12. a motor; 13. an electromagnetic valve; 14. a hydraulic pump; 15. a top cover; 16. a slag valve; 17. a slag pipe; 18. a filter layer; 19. a slag discharging end cover; 20. an outlet pipe; 21. a mass flow meter; 22. a separation kettle; 23. and (4) a bracket.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples, but the present invention is not limited to these examples.
Example 1
In the figure 1, the supercritical extraction kettle capable of continuously feeding and discharging materials is characterized in that an extraction kettle 2 is installed on a support 23, a water bath barrel 1 is arranged outside the extraction kettle 2, the side wall of the water bath barrel 1 is processed into a hollow structure, water is filled in the hollow structure, a water inlet pipe communicated with the side wall of the water bath barrel 1 is installed at the lower end of the side wall of the water bath barrel 1, a water outlet pipe communicated with the side wall of the water bath barrel 1 is installed at the upper end of the side wall of the water bath barrel 1, a top cover 15 is fixedly connected and installed at the top of the extraction kettle 2 through a threaded fastening connecting piece, a sealing device is installed between the top cover 15 and the extraction kettle 2 to prevent the gas in the extraction kettle 2 from leaking out to cause insufficient pressure in the barrel, at least 2 feeding pipes 3 are processed on the top cover 15, feeding valves 4 are installed on the feeding pipes 3, feeding end covers 5, install import pipe 6 on feeding end cover 5, inside the extractant got into extraction cauldron 2 through import pipe 6, during the extraction, 1 at least inlet pipe 3 imported as the extractant, open feed valve 4, let in the extractant and extract the material in extraction cauldron 2, but all the other inlet pipes 3 partial or whole feed valve 4 that close, add the material, reinforced completion back, cover corresponding feeding end cover 5, open and correspond feed valve 4, make the material fall into extraction cauldron 2 inside, preferably, the processing of extraction cauldron 2 bottom of this embodiment has 5 pipes 17 of slagging tap, the processing has 5 inlet pipes 3 on top cap 15.
The center of the top cover 15 penetrates through the top cover 15 to be provided with a thrust rod 8, the lower end of the thrust rod 8 is provided with a material pushing plate 7, a thrust rod gear 9 is arranged on the thrust rod 7, the thrust rod gear 9 is meshed with a motor gear 11 arranged on an output shaft of a motor 12, the motor 12 drives the thrust rod 8 to rotate when rotating so as to drive the material pushing plate 7 to rotate and flatten added materials, the tail end of the thrust rod 8 is connected with a piston rod of a hydraulic oil cylinder 10, the hydraulic oil cylinder 10 is connected with a hydraulic pump 14 through an electromagnetic valve 13, the hydraulic pump 14 provides power for the invention, the piston rod of the hydraulic oil cylinder 10 is controlled to move up and down through the electromagnetic valve 13 so as to drive the thrust rod 8 to move up and down, the material pushing plate 7 moves up and down, the material is compacted, then an extracting agent is introduced, the material pushing plate 7 is provided with fine air inlets, so that the extractant can smoothly enter the material and the material cannot move upwards to pass through the material pushing plate 7.
At least 2 slag discharging pipes 17 are processed at the bottom of the extraction kettle 2, the slag discharging pipe 17 of the embodiment is of a horn-shaped structure with small inlet and large outlet, a slag discharging valve 16 is installed at the thin end of the slag discharging pipe 17, a slag discharging end cover 19 is installed at the thick end of the slag discharging pipe 17, a sealing device is installed between the slag discharging pipe 17 and the slag discharging end cover 19 to prevent insufficient pressure in a cylinder caused by external leakage of gas in the extraction kettle 2, a filter layer 18 is installed between the slag discharging pipe 17 and the slag discharging end cover 19, an outlet pipe 20 is installed on the slag discharging end cover 19 and used for discharging and collecting the extracting agent and the extract, a mass flow meter 21 is arranged on the outlet pipe 20 and used for monitoring the extraction condition of the slag discharging pipe 17, the outlet pipe 20 is communicated with a separation kettle 22, and the separation kettle 22. Preferably, the filtering layer 18 of the present invention is a metal powder sintered filter disc or a metal woven screen, so as to prevent the material from blocking the outlet pipe 20, during extraction, at least one slag discharge valve 16 is kept in an open state, extract is collected, the rest of the slag discharge valves 16 can be partially or completely closed, a slag discharge end cover 19 is opened, a material cake filter cake in each slag discharge pipe 17 is taken out in a spiral stirring manner, after the material taking is completed, the slag discharge end cover 19 is covered, the corresponding slag discharge valve 16 is opened, the squeezing extraction is continued, and the material cake filter cake in the slag discharge pipe 17 is sequentially taken out by circularly adopting the method; the invention can ensure that the extraction kettle does not need to be shut down and decompressed when feeding or taking out material cake filter cakes in the extraction process, thereby saving a large amount of time, improving the interception area of the outlet of the whole extraction kettle and the extraction efficiency by the design of the horn-shaped slag outlet, and further, a thermometer and a pressure gauge are arranged on the top cover 15.
The invention relates to an extraction method of a supercritical extraction kettle for continuously extracting grease, which comprises the following steps:
s1, controlling the water bath barrel 1 to perform water bath heat preservation on the extraction kettle 2, opening the top cover 15, quickly adding materials into the extraction kettle 2, connecting the thrust rod 8 with the material pushing plate 8 through the top cover 15, and covering the top cover 15;
s2, opening the electromagnetic valve 13, controlling the material pushing plate 7 to descend to the surface layer of the material, closing the electromagnetic valve 13, opening the motor 12, driving the material pushing plate to rotate by the motor 12, smoothing the surface of the material, opening the electromagnetic valve 13 to control the material pushing plate 7 to move downwards, compacting the material, opening the feed valve 4 and introducing the extractant, performing extrusion extraction on the whole extraction kettle, using at least one feed pipe 3 as a material supplementing pipe, closing the feed valve 4, opening the feed end cover 5, loading the material, closing the feed end cover 5, opening the feed valve 3, allowing the material to enter the extraction kettle 2 under the push of gravity and the extractant, rotating the material pushing plate 7 downwards again, and completing the feeding and material supplementing operation;
s3, enabling an extractant to flow through an outlet pipe 20 and a mass flow meter and then reach a separation kettle, realizing separation of the extractant and the extractant through pressure reduction operation, when the number of the mass flow meter 21 is greatly reduced, proving that a slag discharging pipe 17 at the end has basically completed squeezing extraction, closing a slag discharging valve 16, opening a slag discharging end cover 19, taking out a horn-shaped filter cake in the slag discharging pipe 17, covering the slag discharging end cover 19 after finishing material taking, opening a corresponding slag discharging valve 16, continuing the squeezing extraction of the slag discharging pipe 17, keeping at least one slag discharging valve 16 in an open state during the process to ensure the continuity of the squeezing extraction of the whole extraction kettle 2, and selecting partial or complete closing of the rest slag discharging valves 16 according to the specific conditions of the indication number of the mass flow meter 21 carried on the outlet pipe 20, and cyclically adopting the method to sequentially take out the material slag in each slag discharging pipe 17;
s4, when the material in the extraction kettle 2 is reduced, at least one feed pipe 3 is reserved as an extraction agent inlet, all or part of the rest feed pipes 3 can close the feed valves 4, the feed end cover 5 is opened, the material is added, after the feeding of the feed pipes 3 is finished, the corresponding feed valves 4 are opened, the extraction agent is introduced, the material in the feed pipes 3 enters the extraction kettle 2 under the double effects of gravity and the flowing of the extraction agent, the material feeding of the extraction kettle 2 is finished through the leveling and compacting operation of the material pushing plate 7, and the feeding is circularly carried out by adopting the method until the material reaches the required requirement.
Claims (8)
1. The utility model provides a but supercritical fluid extraction cauldron of continuous business turn over material sets up the extraction cauldron on the support, and the extraction cauldron outside is provided with a water bath section of thick bamboo, its characterized in that: extraction cauldron top be provided with the top cap, be provided with 2 at least inlet pipes on the top cap, be provided with the feed valve on the inlet pipe, the import pipe tip is provided with the feeding end cover, be provided with the import pipe on the feeding end cover, top cap central point puts and pierces through the top cap and is provided with the distance rod, the distance rod lower extreme is provided with the scraping wings, it has the inlet port to process on the scraping wings, be provided with the distance rod gear on the distance rod, the distance rod gear meshes with the motor gear of installing on motor output shaft mutually, the distance rod end is connected with hydraulic cylinder's piston rod, hydraulic cylinder is connected with the hydraulic pump through the solenoid valve, extraction cauldron bottom is provided with 2 at least pipes of slagging tap, be provided with the valve on the pipe of slagging tap, the pipe tip is provided with the end cover of slagging tap, it is.
2. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: the extraction cauldron bottom be provided with 5 pipes of slagging tap, be provided with 5 inlet pipes on the top cap.
3. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: the filtering layer is a metal powder sintered filtering disc or a metal woven screen.
4. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: the top cover is provided with a thermometer.
5. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: the top cover is provided with a pressure gauge.
6. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: and sealing devices are arranged between the top cover and the extraction kettle, between the inlet pipe and the feeding end cover, and between the slag discharging pipe and the slag discharging end cover.
7. The supercritical extraction kettle capable of continuously feeding and discharging materials according to claim 1, is characterized in that: the slag discharging pipe is of a horn-shaped structure with a small inlet and a large outlet.
8. The extraction method of the supercritical extraction kettle capable of continuously feeding and discharging materials as claimed in any one of the preceding claims 1 to 7, characterized by comprising the following steps:
s1, controlling the water bath barrel to perform water bath heat preservation on the extraction kettle, opening the top cover, quickly adding materials into the extraction kettle, connecting the thrust rod with the material pushing plate after penetrating through the top cover, and covering the top cover;
s2, opening an electromagnetic valve, controlling a material pushing plate to descend to the surface layer of the material, closing the electromagnetic valve, opening a motor, driving the material pushing plate to rotate by the motor, smoothing the surface of the material, opening the electromagnetic valve to control the material pushing plate to move downwards, compacting the material, using at least one feeding pipe as an extractant inlet, opening a feeding valve and introducing an extractant, performing extrusion extraction on the whole extraction kettle, using at least one feeding pipe as a material supplementing pipe, closing the feeding valve, opening a feeding end cover, loading the material, closing the feeding end cover, opening the feeding valve, enabling the material to enter the extraction kettle under the push of gravity and the extractant, and rotating the material pushing plate downwards again to complete feeding and material supplementing operation;
s3, enabling an extractant to flow through an outlet pipe and a mass flow meter and then reach a separation kettle, realizing separation of the extractant and the extractant through pressure reduction operation, when the mass flow meter digit is greatly reduced, proving that a slag discharging pipe at the end has basically completed squeezing extraction, closing a slag discharging valve, opening a slag discharging end cover, taking out a horn-shaped filter cake in the slag discharging pipe, after finishing material taking, covering the slag discharging end cover, opening a corresponding slag discharging valve, continuing the squeezing extraction of the slag discharging pipe, wherein at least one slag discharging valve is kept in an open state during the process to ensure the continuity of the squeezing extraction of the whole extraction kettle, and the rest slag discharging valves can be partially or completely closed according to the specific conditions of the indication number of the mass flow meter carried on the outlet pipe, and the method is circularly adopted to sequentially take out the material slag in each slag discharging pipe;
s4, when the material in the extraction kettle is reduced, at least one feeding pipe is reserved as an extracting agent inlet, all or part of the other feeding pipes can close a feeding valve, a feeding end cover with the closed feeding valve is opened, the material is added, after the feeding of the feeding pipes is completed, the corresponding feeding valve is opened, the extracting agent is introduced, the material in the feeding pipes enters the extraction kettle under the double effects of gravity and extracting agent flowing, the material supplementing of the extraction kettle is completed through the leveling and compacting operations of a material pushing plate, and the feeding is circularly carried out by adopting the method until the material meets the required requirements.
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Families Citing this family (3)
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| CN114405058B (en) * | 2022-01-21 | 2023-08-04 | 南通市华安超临界萃取有限公司 | Supercritical carbon dioxide extraction device capable of improving material replacement efficiency |
| CN114870429B (en) * | 2022-04-25 | 2023-08-04 | 贵州航天乌江机电设备有限责任公司 | Wall thickness variable continuous extraction device cylinder and continuous extraction device |
| CN115445235B (en) * | 2022-09-19 | 2023-12-29 | 烟台中亚至宝药业有限公司 | Supercritical fluid extraction device and method for total flavonoids of semen cuscutae |
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| CN86106852A (en) * | 1985-09-10 | 1988-04-20 | 维他命公司 | The method and apparatus of extraction liquids from solid |
| CN103773597A (en) * | 2014-01-07 | 2014-05-07 | 牛鹏飞 | Rapid supercritical extraction method of oil |
| CN204815780U (en) * | 2015-08-01 | 2015-12-02 | 陕西森弗高科实业有限公司 | It puts to prevent floating canning of drawing of blockking up |
| CN106807112A (en) * | 2015-11-27 | 2017-06-09 | 王竞甜 | Novel fluid shunt cylinder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10053648B2 (en) * | 2013-01-04 | 2018-08-21 | Matthew Ellis | Continuous-flow extraction system and method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86106852A (en) * | 1985-09-10 | 1988-04-20 | 维他命公司 | The method and apparatus of extraction liquids from solid |
| CN103773597A (en) * | 2014-01-07 | 2014-05-07 | 牛鹏飞 | Rapid supercritical extraction method of oil |
| CN204815780U (en) * | 2015-08-01 | 2015-12-02 | 陕西森弗高科实业有限公司 | It puts to prevent floating canning of drawing of blockking up |
| CN106807112A (en) * | 2015-11-27 | 2017-06-09 | 王竞甜 | Novel fluid shunt cylinder |
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