A system and method for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine
By designing a supercritical continuous countercurrent extraction system and utilizing valve control and pressure transmission technology, the problems of continuous operation difficulty and extractant loss in existing supercritical fluid extraction technologies have been solved, achieving efficient extraction of vegetable oils and traditional Chinese medicines, and improving the system's stability and ease of maintenance.
Patent Information
- Application Number
- CN202311195668.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-15
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2043-09-15
AI Technical Summary
Existing supercritical fluid extraction technology suffers from problems such as difficulty in continuous operation, high extractant loss during unloading, and high equipment maintenance difficulty, which limit its application prospects.
Design a supercritical continuous countercurrent extraction system, including an extraction tank, a separation tank, a cooler, a pressurizing pump, a preheater, and an extractant storage tank. The system achieves countercurrent extraction and pressure transmission in the extraction tank through valve control, thereby reducing extractant loss and improving system stability and maintainability.
Supercritical continuous countercurrent extraction was achieved, which improved the extraction rate, reduced energy consumption, reduced extractant loss, and made the equipment easy to maintain and automate.
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Figure CN117205600B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the field of chemical separation and high-pressure reaction process and equipment, and particularly relates to a system and method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine. BACKGROUND
[0002] The information disclosed in this BACKGROUND section is only for the purpose of increasing the understanding of the background of the present application and therefore it should not be taken as admitting that such information forms a part of the prior art with respect to the present application.
[0003] Supercritical fluid extraction is a new type of extraction and separation technology, which has the following characteristics: the extraction agent is a gas at normal pressure and room temperature, and is easy to separate from the raffinate phase and the extracted components after extraction; it is operated at a relatively low temperature, and is particularly suitable for the separation of natural substances; the solubility of the supercritical fluid can be adjusted by adjusting the pressure, temperature and introducing a entrainer, and the extracted components can be introduced into the desired product by gradually changing the density, temperature and pressure.
[0004] Great importance has been attached to the research and application development of supercritical fluid extraction technology at home and abroad. At present, there are many patents on supercritical CO2 extraction for separating essential oils, medicines and functional oils at home and abroad. There are more than 120 patents granted in China, mainly involving the process and equipment of supercritical CO2 extraction for oil, which is applied to the extraction of essential oils (vanillin, essential oil components in ginger, sophora flower essential oil, flavonoids, rose essential oil, lavender essential oil, sesame essential oil, tea flower essential oil, etc.), medicines (ginkgo leaves, artemisinin, salvia flower extract, coral ginger essential oil, peony alcohol, medicinal ingredients in ginseng and danshen, chuanxiong, ganoderma spore, lutein, coumarin, diosgenin, polygonum multiflorum extract, etc.), and functional oils (rice bran oil, wheat germ oil, evening primrose oil, tomato seed oil, bopenggua seed oil, ginseng oil, etc.).
[0005] Supercritical CO2 extraction technology can not only quickly and effectively extract and separate the required substances, but also has no solvent residue problem. However, this technology involves a high-pressure reaction system, which requires a large one-time investment in equipment and has a high extraction cost. There are also many problems, such as:
[0006] The patent CN104784963A "Horizontal supercritical fluid extraction kettle and supercritical fluid extraction device" discloses a supercritical fluid extraction device. The horizontal supercritical fluid extraction kettle provided by the invention is provided with a gas distribution device between the gas inlet and the material shelf layer, which can ensure uniform distribution of the supercritical fluid in the extraction kettle. For this horizontal supercritical fluid extraction device, the vertical design of the previous extraction kettle is changed, which solves the problem that the production cost of the vertical extraction kettle increases significantly with the increase of the size of the extraction kettle. Although this device saves cost to some extent, it is difficult to achieve sealing, has low safety and reliability, high energy consumption, and large loss of extraction solvent.
[0007] The application patent CN100427172A "high pressure super high pressure continuous solid material extraction and sterilization device" discloses a high pressure super high pressure continuous solid material extraction and sterilization device, which realizes continuous operation of high pressure super high pressure solid material extraction and sterilization, and has the characteristics of safety, reliability and high efficiency. However, the device is only a unit in the extraction operation, and the complete design and reasonable process flow of the continuous extraction device are not completed, so that the popularization and use of the continuous extraction device are limited.
[0008] The application patent CN110237561A "supercritical fluid continuous extraction and separation device system and extraction and separation process" discloses a supercritical fluid continuous extraction and separation device system, which is applied to implement the extraction and separation process. Through the system process operation, the supercritical fluid after extraction in the extraction bin enters the corresponding separation subsystem to start separation, and the discharge valve is periodically opened to discharge the extract separated by the separation subsystem. However, the device needs to be specially designed and manufactured, and the maintenance difficulty is also large, so that the popularization and use are limited.
[0009] From the above, it can be seen that supercritical fluid extraction involves high pressure technology, and there are problems such as great difficulty in continuous operation, great loss of extractant in the discharge process, and difficulty in maintenance, so it is necessary to continue to deeply research the supercritical fluid extraction technology and continuously expand and improve the engineering technology to solve the above problems and expand the application prospect of the supercritical fluid extraction technology. SUMMARY
[0010] In order to solve the problems of the prior art, the purpose of the present application is to provide a supercritical continuous countercurrent extraction system and method for plant oil and traditional Chinese medicine. The supercritical continuous countercurrent extraction device method has the advantages of simple process, less extractant loss, high system stability, easy maintenance and good practical application value.
[0011] In order to achieve the above purpose, the technical scheme of the present application is as follows:
[0012] In a first aspect of the present application, a supercritical continuous countercurrent extraction system for plant oil and traditional Chinese medicine is provided, which comprises an extraction tank, a separation tank, a cooler, a pressurizing pump, a preheater, and an extractant storage tank.
[0013] The extraction tank, the separation tank, the cooler, the pressurizing pump and the preheater are connected in sequence, and the preheater is connected to the extraction tank to form a closed loop. The outlet of the extractant storage tank is connected to the pipeline between the cooler and the pressurizing pump.
[0014] The extraction tank is divided into a pressurizing group and a countercurrent extraction group; the extraction tank of the countercurrent extraction group is used for supercritical continuous countercurrent extraction; after the extraction is completed, a set number of extraction tanks in the countercurrent extraction group are respectively and individually connected with the extraction tanks of the pressurizing group in sequence, and then pressure transmission is performed.
[0015] In some embodiments of the present application, the number of extraction tanks is 8-30.
[0016] In some embodiments of the present application, each extraction tank is arranged in parallel; a feed valve is arranged on the pipeline connected with the feed inlet at the bottom of each extraction tank; the pipelines between the feed inlets and the feed valves of adjacent extraction tanks are connected through pipelines provided with straight-through valves, forming a closed loop; two series-connected discharge valves, i.e., a first discharge valve and a second discharge valve, are arranged on the pipeline connected with the discharge outlet at the top of each extraction tank; the first discharge valve is closer to the discharge outlet at the top of the extraction tank than the second discharge valve; the pipelines between the two series-connected discharge valves of adjacent extraction tanks are connected through pipelines provided with communication valves, forming a closed loop; an emptying valve is arranged on each extraction tank; the use of the extraction tank is controlled through the opening or closing of the valves.
[0017] In some embodiments of the present application, the set number of extraction tanks are two extraction tanks close to the preheater end when cyclic extraction is performed; the two extraction tanks are individually connected with each extraction tank of the pressurizing group, and are connected in sequence according to the order of pressure from high to low, one extraction tank of the pressurizing group is connected each time, and the extraction tank and the extraction tank of the pressurizing group reach pressure balance through pressure transmission.
[0018] In some embodiments of the present application, a first back pressure valve is arranged on the pipeline between the second discharge valve and the separation tank.
[0019] In some embodiments of the present application, a second back pressure valve is arranged on the pipeline between the separation tank and the cooler.
[0020] In some embodiments of the present application, a discharge valve is arranged on the discharge pipeline at the bottom of the separation tank.
[0021] In some embodiments of the present application, the separation tank is a cyclone separator.
[0022] In some embodiments of the present application, each extraction tank is provided with a water bath temperature control device.
[0023] In some embodiments of the present application, an extractant valve is arranged on the outlet pipeline of the extractant storage tank.
[0024] In some embodiments of the present application, a circulation valve is arranged on the pipeline between the cooler and the pressurizing pump; the circulation valve is arranged upstream of the extractant storage tank pipeline connection point.
[0025] In some embodiments of the present application, a flow meter is provided between the pressurizing pump and the preheater. The pressurizing rate of the pressurizing pump can be observed through the flow meter.
[0026] In a second aspect of the present application, a method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine is provided, which uses the supercritical continuous countercurrent extraction system described above, and comprises the following steps:
[0027] (1) loading and vacuumizing: each extraction tank is loaded with solid-phase extraction material, and vacuumized, and all valves are closed;
[0028] (2) pressurizing some extraction tanks: the preheater is opened and heated to 40-50℃; extraction agent is added to some extraction tanks, and the pressure is ≥2MPa;
[0029] (3) pressurizing the remaining extraction tanks and circulating: the temperature of the cooler is set to 0-5℃; the preheater is opened and heated to 40-50℃; the valves of the remaining extraction tanks are controlled to be opened and closed, so that the remaining extraction tanks are connected in series, and the extraction agent enters the remaining extraction tanks in sequence; when the pressure in the extraction tank closest to the first back pressure valve reaches the upper limit of the pressure range of the first back pressure valve, the circulation extraction is performed; after the end, the pressurizing pump and the feeding valve are closed; after the circulation extraction is completed, the product is discharged from the discharge valve at the bottom of the separation tank;
[0030] (4) depressurizing two extraction tanks: the two extraction tanks close to the preheater that perform circulation extraction are depressurized to a pressure higher than that of the extraction tanks that do not perform circulation extraction;
[0031] (5) pressure transfer: the valves are controlled to be opened and closed, so that the one extraction tank after depressurization and the extraction tanks that do not perform circulation extraction are connected in order from high to low pressure; one extraction tank that does not perform circulation extraction is connected each time, and through pressure transfer, the one extraction tank after depressurization and the extraction tanks that do not perform circulation extraction reach pressure balance; then the one extraction tank after depressurization is loaded with solid-phase extraction material and vacuumized; the other extraction tank after depressurization is again connected with the extraction tanks that do not perform circulation extraction in order from high to low pressure; one extraction tank that does not perform circulation extraction is connected each time, and through pressure transfer, the other extraction tank after depressurization and the extraction tanks that do not perform circulation extraction reach pressure balance; then the other extraction tank after depressurization is loaded with solid-phase extraction material and vacuumized.
[0032] In some embodiments of the present application, the method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine further comprises the circulation steps (3), (4) and (5). That is, the steps of “circulation extraction→depressurizing two extraction tanks→pressure transfer of extraction tanks” are repeated.
[0033] In some embodiments of the present application, in step (3), the first back pressure valve pressure range can be set according to experience and adjusted within a certain range, for example, the first back pressure valve pressure range is 12-30 MPa, or other pressure values can also be set.
[0034] In some embodiments of the present application, in step (4), the two extraction tanks near the preheater end for cyclic extraction are depressurized to 12 MPa.
[0035] The beneficial effects of the present application are:
[0036] The supercritical continuous countercurrent extraction system of the present application realizes supercritical continuous countercurrent extraction, improves the extraction rate and reduces energy consumption through the reasonable setting of the extraction tank. Through the control of the valve, the extraction tank after extraction is connected with the extraction tank without extraction to realize pressure transmission, so that the extractant released by the extraction tank after extraction is effectively utilized, and the loss of the extractant in the unloading process is reduced.
[0037] The supercritical continuous countercurrent extraction system of the present application is not only suitable for supercritical extraction, but also can be used for other high-pressure processes, and the device is easy to maintain, flexible to operate and easy to realize automatic operation.
[0038] The method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine of the present application effectively utilizes the extractant released by the extraction tank after extraction, reduces the loss of the extractant in the unloading process, and forms the step-by-step transmission of pressure to the extraction tank with newly added solid-phase extraction materials in the regular pressure relief process of the extraction tank, which can be continuously circulated and transmitted. BRIEF DESCRIPTION OF DRAWINGS
[0039] The drawings accompanying the specification of the present application serve to provide a further understanding of the present application, and the illustrative embodiments of the present application and their descriptions serve to explain the present application, and do not constitute an improper limitation on the present application.
[0040] Figure 1 It is a supercritical continuous countercurrent extraction device system schematic diagram of the present application embodiment 1.
[0041] Figure 2 It is a supercritical continuous countercurrent extraction device system schematic diagram of the present application embodiment 2.
[0042] 1 - first back pressure valve; 2 - separation tank; 3 - discharge valve; 4 - second back pressure valve; 5 - cooler; 6 - circulation valve; 7 - extractant storage tank; 8 - extractant valve; 9 - pressurizing pump; 10 - flow meter; 11 - preheater; 12-23 - second discharge valve; 24-35 - first discharge valve; 36-47 - communication valve; 48-59 - emptying valve; 60-71 - extraction tank; 72-83 - feeding valve; 84-95 - straight-through valve. Detailed Implementation
[0043] To enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention will be described in detail below with reference to specific embodiments.
[0044] Example 1
[0045] like Figure 1 As shown, a system for supercritical continuous countercurrent extraction of vegetable oils and traditional Chinese medicine includes: 12 extraction tanks (numbered 60-71), a separation tank 2, a cooler 5, a pressurizing pump 9, a preheater 11, an extractant storage tank 7, a flow meter 10, and multiple valves.
[0046] Each of the 12 extraction tanks (numbered 60-71) is equipped with a water bath temperature control device. Each extraction tank has a first discharge valve (numbered 24-35) and a drain valve (numbered 48-59) on its upper part. A second discharge valve (numbered 12-23) is located after the first discharge valve, meaning the first and second discharge valves on each extraction tank are connected in series. Separation tank 2 is also equipped with a water bath temperature control device.
[0047] Each extraction tank (numbered 60-71), separation tank 2, cooler 5, preheater 11, and extractant storage tank 7 is made of 316L stainless steel and is pressure resistant to 50MPa. The extraction tanks (numbered 60-71) have a volume of 2.0 liters, and the separation tank 2 has a volume of 8.0 liters.
[0048] The pipeline between the first and second discharge valves of each extraction tank is connected to the pipeline between the first and second discharge valves of adjacent extraction tanks and is equipped with connecting valves (numbered 36 to 46 respectively). The pipeline between the first discharge valve 35 and the second discharge valve 23 of extraction tank 71 is connected to the pipeline between the first discharge valve 24 and the second discharge valve 12 of extraction tank 60 and is equipped with connecting valve 47. The pipelines equipped with connecting valves form a closed loop.
[0049] Each extraction tank is equipped with a feed valve (numbered 72 to 83) at the bottom. The pipeline between each extraction tank and its feed valve is connected to the pipeline between the adjacent extraction tank and its feed valve and is equipped with a straight-through valve (numbered 84 to 94). The pipeline between extraction tank 71 and its feed valve 83 is connected to the pipeline between extraction tank 60 and its feed valve 72 and is equipped with a straight-through valve 95. The pipelines equipped with straight-through valves also form a closed loop.
[0050] All the pipelines after the second discharge valves are combined and connected to the back pressure valve 1, and then connected to the middle part of the separation tank 2. The lower part of the separation tank 2 is provided with a discharge valve 3, and the upper part is sequentially connected to a back pressure valve 4, a cooler 5 and a circulation valve 6. The upper part of the extractant storage tank 7 is provided with an extractant valve 8. The pipelines after the circulation valve 6 and the extractant valve 8 are combined and connected to a pressurizing pump 9, and then sequentially connected to a flow meter 10 and a preheater 11. All the pipelines before the feed valves (numbered as 72-83) are combined and connected to the preheater 11.
[0051] Example 2
[0052] The same as example 1, the difference is that:
[0053] The separation tank 2 adopts a cyclone separator structure.
[0054] Example 3
[0055] A method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine, using the supercritical continuous countercurrent extraction system described in example 1 to extract zanthoxylum bungeanum seed oil, the raw material is zanthoxylum bungeanum seed obtained from Jinan Laiwu after crushing and sorting, and the extractant is CO2, comprising the following steps:
[0056] (1) Feeding and vacuumizing: 1.5 liters of zanthoxylum bungeanum seed is loaded into each of the 12 extraction tanks (numbered as 60-71) of the supercritical continuous countercurrent extraction system, the first discharge valves 24-35, the second discharge valves 12-23, the communication valves 36-47, the feed valves 72-83, the straight-through valves 84-95 and the circulation valve 6 are all opened; the discharge valve 3, the extractant valve 8 and the emptying valves 48-58 are closed, the emptying valve 59 is opened and vacuumized from the emptying valve 59 to 5 Pa pressure in the 12 extraction tanks, and then the emptying valve 59 is closed. The first discharge valves 24-35, the second discharge valves 12-23, the communication valves 36-47, the feed valves 72-83, the straight-through valves 84-95 and the circulation valve 6 are all closed.
[0057] (2) Pressurizing the last 4 extraction tanks (i.e. extraction tanks 68-71): open the preheater 11 and heat it to 40℃; open the extractant valve 8 and the pressurizing pump 9 in turn, open the feed valves 80-83 in turn, add extractant into the extraction tanks 68-71 respectively and make the pressure of each extraction tank 68-71 be 2.0 MPa, 4.0 MPa, 6.0 MPa and 8.0 MPa respectively, and then close the feed valves 80-83, the pressurizing pump 9 and the extractant valve 8.
[0058] (3) The first 7 extraction tanks (i.e. extraction tanks 60-66) are pressurized and circulated: set the temperature of cooler 5 to 0°C; open preheater 11 and warm it up to 40°C; open extraction agent valve 8, pressurizing pump 9, feed valve 78, first discharge valve 30, communication valve 41, first discharge valve 29, straight-through valve 88, first discharge valve 28, communication valve 39, first discharge valve 27, straight-through valve 86, first discharge valve 26, communication valve 37, first discharge valve 25, straight-through valve 84, first discharge valve 24, and second discharge valve 12 in sequence.
[0059] Pressurizing pump 9 is fed at a rate of 10 L / h, the pressure of first back pressure valve 1 is adjusted to 30.0 MPa, and the pressure of back pressure valve 4 is adjusted to 12.0 MPa; when the pressure of extraction tank 60 reaches 30.0 MPa, circulation valve 6 is opened, pressurizing pump 9 is fed at a rate of 10 L / h for 4 hours, and the product is discharged from discharge valve 3, after which feed valve 78 and pressurizing pump 9 are closed.
[0060] (4) The pressure of the two extraction tanks is reduced to 12 MPa: straight-through valve 88 is closed, first discharge valve 30, second discharge valve 18, first discharge valve 29, and second discharge valve 17 are opened (at this time, communication valve 41 can be opened or closed), the pressure of back pressure valve 1 is adjusted to 12.0 MPa, and first discharge valve 30, second discharge valve 18, first discharge valve 29, and second discharge valve 17 are closed when the pressure of extraction tank 65 and extraction tank 66 reaches 12.0 MPa.
[0061] (5) The pressure of the last 7 extraction tanks (i.e. extraction tanks 65-71) is transferred: first discharge valve 30, communication valves 42-46, and first discharge valve 35 are opened, communication valve 46 and first discharge valve 35 are closed when the pressure in extraction tank 66 and extraction tank 71 reaches 10.0 MPa, and first discharge valve 34 is opened.
[0062] Communication valve 45 and first discharge valve 34 are closed when the pressure in extraction tank 66 and extraction tank 70 reaches 8.0 MPa, and first discharge valve 33 is opened.
[0063] Communication valve 44 and first discharge valve 33 are closed when the pressure in extraction tank 66 and extraction tank 69 reaches 6.0 MPa, and first discharge valve 32 is opened.
[0064] Communication valve 43 and first discharge valve 32 are closed when the pressure in extraction tank 66 and extraction tank 68 reaches 4.0 MPa, and first discharge valve 31 is opened.
[0065] Communication valve 42, first discharge valve 31, and first discharge valve 30 are closed when the pressure in extraction tank 66 and extraction tank 67 reaches 2.0 MPa.
[0066] Open the extraction tank 66 and load in 1.5 liters of Zanthoxylum bungeanum Maxim. seeds, open the evacuation valve 54 and evacuate from the evacuation valve 54 to the pressure of the extraction tank 66 is 5 Pa, then close the evacuation valve 54.
[0067] Open the first discharge valve 29, the communication valve 41~45, the first discharge valve 34, when the pressure in the extraction tank 65 and the extraction tank 70 reaches 10.0 MPa, close the communication valve 45 and the first discharge valve 34, open the first discharge valve 33;
[0068] When the pressure in the extraction tank 65 and the extraction tank 69 reaches 8.0 MPa, close the communication valve 44 and the first discharge valve 33, open the first discharge valve 32;
[0069] When the pressure in the extraction tank 65 and the extraction tank 68 reaches 6.0 MPa, close the communication valve 43 and the first discharge valve 32, open the first discharge valve 31;
[0070] When the pressure in the extraction tank 65 and the extraction tank 67 reaches 4.0 MPa, close the communication valve 42 and the first discharge valve 31, open the first discharge valve 30;
[0071] When the pressure in the extraction tank 65 and the extraction tank 66 reaches 2.0 MPa, close the communication valve 41, the first discharge valve 30 and the first discharge valve 29;
[0072] Open the extraction tank 65 and load in 1.5 liters of Zanthoxylum bungeanum Maxim. seeds, open the evacuation valve 53 and evacuate from the evacuation valve 53 to the pressure of the extraction tank 65 is 5 Pa, then close the evacuation valve 53. Each time of evacuation is for the extraction tank just loaded with solid phase extraction material.
[0073] During the regular pressure relief process of the extraction tank, the pressure is transferred to the extraction tank with newly added solid phase extraction material in stages, and can be continuously circulated down.
[0074] (6) The last 2 front 5 extraction tank (i.e. the extraction tank 60~64 and the extraction tank 70~71) circulation: set the temperature of the cooler 5 to 0℃; open the preheater 11 and heat to 40℃; open the extraction agent valve 8, the pressurizing pump 9, the feeding valve 76, the first discharge valve 28, the communication valve 39, the first discharge valve 27, the straight-through valve 86, the first discharge valve 26, the communication valve 37, the first discharge valve 25, the straight-through valve 84, the first discharge valve 24, the communication valve 47, the first discharge valve 35, the straight-through valve 94, the first discharge valve 34, the second discharge valve 22 in turn.
[0075] The pressurizing pump 9 feeds at a rate of 10 liters / hour, the pressure of the first back pressure valve 1 is adjusted to 30.0 MPa, and the pressure of the second back pressure valve 4 is adjusted to 12.0 MPa; when the pressure of the extraction tank 70 reaches 30.0 MPa, the circulation valve 6 is opened, the pressurizing pump 9 feeds at a rate of 10 liters / hour for 4 hours, and the product is discharged from the discharge valve 3, after which the feed valve 76 and the pressurizing pump 9 are closed.
[0076] Steps (3) to (6) can be repeated, i.e. the "circulation extraction → two-extraction tank pressure reduction → extraction tank pressure transmission" is repeated. There is no requirement for the number of repetitions, which can be two, three, four, etc.
[0077] Using the above process, 90 liters of Zanthoxylum bungeanum Maxim. seed kernels are consumed, and 20.52 liters of Zanthoxylum bungeanum Maxim. seed kernel oil are obtained.
[0078] Example 4
[0079] A method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine, Zanthoxylum bungeanum Maxim. seed kernel oil is extracted using the supercritical continuous countercurrent extraction system described in Example 2, the raw material is Zanthoxylum bungeanum Maxim. seed kernel obtained by crushing and sorting Zanthoxylum bungeanum Maxim. seed produced in Laiwu, Jinan, the implementation steps are the same as in Example 3, 90 liters of Zanthoxylum bungeanum Maxim. seed kernel are consumed, and 23.61 liters of Zanthoxylum bungeanum Maxim. seed kernel oil are obtained.
[0080] Example 5
[0081] A method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine, peanuts, soybeans, sunflower seeds, grape seeds, and peony seeds are used as raw materials, the raw materials are first baked at 95°C for 12 hours and then crushed into fine powder less than 20 mesh, and then peanut oil, soybean oil, sunflower seed oil, grape seed oil, and peony seed oil are extracted using the supercritical continuous countercurrent extraction method described in Example 4, the raw material consumption and plant oil yield are shown in Table 1.
[0082] Table 1 Raw material consumption and plant oil yield of supercritical continuous countercurrent extraction of plant oil
[0083] Raw material Peanut kernel Soybean Sunflower seed Grape seed Peony seed Raw material weight (kg) 40.20 40.25 20.58 20.44 25.12 Vegetable oil yield (kg) 17.97 7.87 8.81 3.60 5.15 Oil yield rate (%) 44.69 19.56 42.82 17.61 20.50
[0084] Example 6
[0085] A method for supercritical continuous countercurrent extraction of plant oil and traditional Chinese medicine, honeysuckle, ginkgo leaves, salvia, peppermint, and cassia seeds are used as raw materials, the raw materials are first baked at 95°C for 12 hours and then crushed into fine powder less than 20 mesh, and then extraction is carried out using the supercritical continuous countercurrent extraction method described in Example 4, the raw material consumption and extract yield are shown in Table 2.
[0086] Table 2 Raw material consumption and extract yield of supercritical continuous countercurrent extraction of traditional Chinese medicine
[0087] Raw material Honeysuckle flower Ginkgo leaf Salvia miltiorrhiza Mint Cassia seed Raw material weight (kg) 20.29 20.15 20.11 20.52 20.17 Extract yield (kg) 0.44 0.48 0.86 0.71 0.49 Extraction rate (%) 2.15 2.40 4.29 3.45 2.41
[0088] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. The present application can be variously changed and modified by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the present application.
Claims
1. A system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine, characterized in that, The system comprises an extraction tank, a separation tank, a cooler, a pressurizing pump, a preheater and an extractant storage tank. The extraction tank, the separation tank, the cooler and the pressurizing pump are connected in sequence, and the preheater is connected to the extraction tank to form a closed loop. The extraction tank is divided into a pressurizing group and a countercurrent extraction group. Each extraction tank is connected to the preheater in parallel.
2. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
3. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
4. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
5. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein the system further comprises a pump for pumping the supercritical fluid into the extraction column. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
6. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein, The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
7. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein the system further comprises a pump for pumping the supercritical fluid into the extraction column. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
8. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein, The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
9. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein, The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
10. The system for supercritical continuous counter-current extraction of plant oil and traditional Chinese medicine according to claim 1, wherein, The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence.
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The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction tank of the pressurizing group in sequence. The two extraction tanks are connected to each extraction (4) Two extraction tanks are depressurized: two extraction tanks close to the preheater end that are to be subjected to the circulation extraction are depressurized to a pressure higher than that of the extraction tanks that are not subjected to the circulation extraction; (5) Pressure transmission: the opening and closing of the valves are controlled so that the one extraction tank that is depressurized and the extraction tanks that are not subjected to the circulation extraction are sequentially connected in the order of pressure from high to low, one extraction tank that is not subjected to the circulation extraction is connected each time, and the one extraction tank that is depressurized and the extraction tanks that are not subjected to the circulation extraction are brought to pressure balance through pressure transmission; then the one extraction tank that is depressurized is filled with solid-phase extraction materials and vacuumized; the other extraction tank that is depressurized is again sequentially connected with the extraction tanks that are not subjected to the circulation extraction in the order of pressure from high to low, one extraction tank that is not subjected to the circulation extraction is connected each time, and the other extraction tank that is depressurized and the extraction tanks that are not subjected to the circulation extraction are brought to pressure balance through pressure transmission; then the other extraction tank that is depressurized is filled with solid-phase extraction materials and vacuumized.
12. The method for supercritical continuous countercurrent extraction of vegetable oils and traditional Chinese medicines as described in claim 11, characterized in that, The circulation step (3), step (4) and step (5) are also included.
13. The method for supercritical continuous countercurrent extraction of vegetable oils and traditional Chinese medicines as described in claim 11, characterized in that, In step (3), the upper limit of the pressure range of the first back pressure valve is 30 MPa.
14. The method for supercritical continuous countercurrent extraction of vegetable oils and traditional Chinese medicines as described in claim 11, characterized in that, In step (4), the two extraction tanks close to the preheater end that are to be subjected to the circulation extraction are depressurized to 12 MPa. In step (4), the two extraction tanks close to the preheater end that are to be subjected to the circulation extraction are depressurized to 12 MPa.
Citation Information
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