CN107227201B - Device and method for supercritical extraction of grease - Google Patents
Device and method for supercritical extraction of grease Download PDFInfo
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- CN107227201B CN107227201B CN201710627648.5A CN201710627648A CN107227201B CN 107227201 B CN107227201 B CN 107227201B CN 201710627648 A CN201710627648 A CN 201710627648A CN 107227201 B CN107227201 B CN 107227201B
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- 239000004519 grease Substances 0.000 title claims abstract description 22
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 187
- 238000000926 separation method Methods 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 27
- 210000004907 gland Anatomy 0.000 claims abstract description 25
- 238000007789 sealing Methods 0.000 claims abstract description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 16
- 239000001569 carbon dioxide Substances 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 5
- 239000006004 Quartz sand Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims 3
- 239000003925 fat Substances 0.000 claims 2
- 230000007306 turnover Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A device and a method for supercritical extraction of grease are provided, wherein an extraction kettle outer cylinder is arranged on a supporting platform, a liquid outlet pipe communicated with a four-way valve is arranged at the bottom of the extraction kettle outer cylinder, an extraction kettle inner cylinder is arranged inside the extraction kettle outer cylinder, a sealing ring is arranged between the extraction kettle outer cylinder and the extraction kettle inner cylinder, an air inlet pipe communicated with a first three-way valve is arranged at the upper part of the extraction kettle outer cylinder, the first three-way valve is communicated with the four-way valve, the four-way valve is communicated with a one-way valve, liquid gas enters an extraction kettle through the one-way valve, the four-way valve is communicated with a separation kettle through a second three-way valve arranged on a pipeline, a top cover arranged on the extraction kettle outer cylinder is arranged at the top of the extraction kettle inner cylinder, filter layers are symmetrically arranged at the top and the bottom of the extraction kettle inner cylinder, materials are filled between the filter layers, glands arranged on the extraction kettle inner cylinder vertically and air flow channels are arranged between the glands and the top cover; the invention has simple operation, does not need to turn over the whole extraction kettle and has higher extraction efficiency.
Description
Technical Field
The invention belongs to a device or equipment for physical separation, and particularly relates to a device and a method for extracting grease.
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 top cover of the extraction kettle or positioned on the side surface of the upper end of the extraction kettle. Although there are many literature studies reporting the effect of the improvement of the supercritical extraction process, including the extraction pressure, extraction temperature, carbon dioxide flow, extraction time, etc., 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 rapid supercritical extraction method for grease', and patent number 201410030959X, when an extracting agent flows through an extraction kettle from top to bottom, the extraction effect of the extracting agent and the squeezing effect of the extracting agent can be exerted, 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 single outlet is thick in a material cake filter cake layer, the extraction efficiency is not favorably improved, and the traditional supercritical extraction kettle is a fixed kettle body, so that the kettle body is not turned over, the squeezing effect of the extracting agent is not favorably exerted, and the extraction efficiency is not favorably improved.
Disclosure of Invention
The invention aims to solve the technical problems that a supercritical extraction kettle is generally connected with a gas inlet pipe, a gas outlet pipe, a water inlet pipe, a water outlet pipe, a temperature sensor and other components, the turnover of the extraction kettle is extremely inconvenient, the turnover can be realized only by switching a plurality of valves, the operation difficulty is high, and in order to overcome the defects, the invention provides the device and the method for supercritical extraction of the grease, which have the advantages of reasonable design, simple operation, high extraction efficiency and capability of realizing the combination of upper inlet, lower outlet, lower inlet and upper outlet without turning over the extraction kettle.
The technical scheme for solving the technical problems is as follows: an extraction kettle outer cylinder is arranged on the supporting platform, and a liquid outlet pipe which penetrates through the supporting platform and is communicated with the four-way valve through a pipeline is arranged at the bottom of the extraction kettle outer cylinder; a water circulation layer is wrapped outside the outer barrel and used for controlling the temperature of the extraction kettle, and a water inlet and a water outlet are formed in the bottom of the water circulation layer; an extraction kettle inner barrel is arranged in the extraction kettle outer barrel, a sealing ring is respectively arranged above and below the extraction kettle inner barrel, an air inlet pipe communicated with a first three-way valve through a pipeline is arranged at the upper part of the extraction kettle outer barrel, the first three-way valve is communicated with a four-way valve through a pipeline, the four-way valve is communicated with a one-way valve through a pipeline, and liquid gas passes through the one-way valve, flows through the four-way valve and the three-way valve and then enters the extraction kettle; the four-way valve is communicated with the separation kettle through a second three-way valve arranged on the pipeline; extraction cauldron inner tube top is provided with the top cap of installing on the extraction cauldron urceolus, be provided with the top cap sealing washer between top cap and the extraction cauldron urceolus, be used for forming sealed preventing gas leakage with the laminating of extraction cauldron urceolus inner wall, extraction cauldron inner tube top and bottom symmetry are provided with the filter layer of installing on extraction cauldron inner tube lateral wall lock ring, it has the material to fill between the filter layer, the symmetry is provided with the gland of installing on the extraction cauldron inner tube about the filter layer outside, be provided with airflow channel between gland and the top cap, the supercritical fluid that gets into by first three-way valve gets into extraction cauldron inner tube through airflow channel and extracts the material, it is provided with temperature sensor to set up the outside on the top cap, be used for surveing extraction cauldron temperature, be provided with first manometer on the pipeline between intake pipe and the first three-way valve, be provided with the second manometer on the separation cauldron drain pipe.
The filter layer of the invention is a cylindrical shell and a medium filled in the shell, small holes are processed on the shell, and the medium is absorbent cotton or quartz sand.
The gland of the invention is: two upper and lower concentric rings link as an organic wholely through hollow cylinder, and lower ring circumference surface processing has the external screw thread that suits with the internal thread that the extraction cauldron inner tube set up, evenly distributed has the air vent on the ring down, goes up the ring upper surface and is provided with the gas-liquid passageway, and the external diameter of going up the ring is less than the external diameter of ring down and is greater than hollow cylinder's external diameter, goes up the ring and forms the recess with hollow cylinder for the extraction cauldron inner tube is carried out when packing is overturned to the extraction cauldron inner tube.
The method for extracting the grease by adopting the device for extracting the grease by supercritical extraction comprises the following steps:
s1, raw material treatment: crushing the materials until no particles exist;
s2, charging: filling the crushed material into the inner cylinder of the extraction kettle, compacting the material until the material and the inner cylinder wall have no gap, flattening the material surface, screwing the filter layer and the gland, filling the inner cylinder into the outer cylinder of the extraction kettle, and covering the top cover;
s3, extracting earlier stage: carbon dioxide gas is changed into liquid through cooling, the liquid carbon dioxide gas is conveyed to a heater through a booster pump, the heated carbon dioxide gas enters an extraction kettle from an A port to a B port of a four-way valve through a C port and a B port of a first three-way valve through a one-way valve, the liquid gas in the extraction kettle flows through an inner cylinder from top to bottom and then flows out of the extraction kettle, the gas carrying grease enters a separation kettle from a D port to a C port of the four-way valve through a C port and a B port of a second three-way valve, the grease and the gas are separated by the separation kettle, the grease is stored at the lower part of the separation kettle, the gas flows out from the upper part of the separation kettle and then circulates into the extraction kettle through cooling, pressurizing and heating again, the A ports of the first three-way valve and the second three-way valve are both closed, the internal pressure of the extraction kettle is 7.2 MPa-100 MPa, the temperature is 10-80 ℃, when a large amount of carbon dioxide gas without oil appears at an inlet of the separation kettle, the one-way valve is closed, and gas inlet is stopped. Opening an A port and a B port of a first three-way valve and an A port and a B port of a second three-way valve, guiding residual gas in the extraction kettle to a separation kettle, and closing the A port and the B port of the first three-way valve and the A port and the B port of the second three-way valve when the first pressure gauge and the second pressure gauge have the same numerical value;
s4, extraction middle period: opening the top cover of the extraction kettle, taking out the inner cylinder, turning the inner cylinder upside down, putting the inner cylinder into the extraction kettle again, covering the top cover, closing the port A and the port B of the first three-way valve and the port A and the port B of the second three-way valve, opening the one-way valve, starting pressurization, enabling the extractant to enter the inner cylinder from the upper end of the extraction kettle, flowing through the inner cylinder from top to bottom, flowing out of the extraction kettle from the bottom, passing through the port D and the port C of the four-way valve to the separation kettle, closing the one-way valve when a large amount of carbon dioxide gas without oil appears at the inlet of the separation kettle, and ending the middle stage of extraction.
S5, in the later stage of extraction, rotating the four-way valve to enable the port A to be communicated with the port D, enabling the port B to be communicated with the port C, opening the one-way valve, enabling an extracting agent to flow through the port A and the port D of the four-way valve, entering the inner cylinder from the bottom of the extraction kettle, flowing through the inner cylinder from bottom to top, entering the port B and the port C of the four-way valve through the port B and the port C of the first three-way valve after flowing out of the upper end of the extraction kettle, and entering the separation kettle from the port C and the port B of the second three-way valve, wherein the pressure in the extraction kettle is 20-50 MPa, and the temperature is 32-60 ℃.
Because the four-way valve is adopted for connection, the using amount of the valve is greatly reduced, and the original four-way valve connecting structure can be replaced. Meanwhile, the extraction kettle is divided into an outer cylinder and an inner cylinder, the outer cylinder plays the functions of temperature supply, pressure bearing and gas supply, and the inner cylinder is specially used for loading and unloading materials; in order to realize the turnover use of the inner cylinder, the inner cylinder is designed into a vertically symmetrical structure, so that the phenomenon that the extraction kettle connected with a plurality of pipelines is turned over in the extraction process is avoided, and the effect of accelerating extraction can be achieved by directly turning over the inner cylinder of the extraction kettle. The invention has a filter layer and a gland on both ends of the inner cylinder of the extraction kettle, the filter layer of the invention is a cylindrical shell, the shell is filled with absorbent cotton or quartz sand, can effectively overcome the defect that the material leaks through the filter screen in the existing device, the gland is fastened on the inner cylinder of the extraction kettle through screw thread, not only can prevent the filter layer from falling off due to the increase of the pressure in the extraction kettle, but also can support the inner cylinder of the extraction kettle, and the inner cylinder of the extraction kettle can be quickly lifted for turning over or replacing the filler through processing a groove on the gland.
The method of the invention has the following advantages: the upper port and the lower port of the four-way valve are respectively connected with the upper port and the lower port of the extraction kettle, the other two ports are respectively connected with the supercharger and the separation kettle, the four-way valve only needs to be switched by 90 degrees, the switching of the extracting agent in the extraction kettle from top to bottom and from bottom to top can be realized, the using amount of the valve is reduced, and the convenience of operation is realized; in addition, the extraction kettle is designed into an outer cylinder and an inner cylinder, the outer cylinder plays the functions of temperature supply, pressure bearing and gas supply, and the inner cylinder is used for loading, unloading and overturning materials. Based on the symmetrical structural design of the inner cylinder, the whole extraction kettle connected with a plurality of pipelines is prevented from being overturned in the extraction process, and the same effect can be achieved only by directly overturning the inner cylinder of the extraction kettle. In order to realize portable charging and inner cylinder overturning, the inner cylinder is designed to be of a vertically symmetrical structure, the two ends of the extraction kettle are provided with the filter layer and the gland, the filter layer is a cylindrical shell, absorbent cotton or quartz sand is filled in the shell, the defect that materials leak through a filter screen in the conventional device can be effectively overcome, the gland is fastened on the inner cylinder of the extraction kettle through threads, the filter layer can be prevented from falling off due to the increase of pressure in the extraction kettle, the inner cylinder of the extraction kettle can be supported, the inner cylinder of the extraction kettle can be quickly lifted to overturn or replace the filler through a groove processed on the gland, the extraction kettle is easy and convenient to operate, the whole extraction kettle does not need to be overturned, and the extraction efficiency is higher.
Drawings
FIG. 1 is a flow chart of one embodiment of the present invention.
Fig. 2 is a schematic structural diagram of an embodiment of the present invention.
Fig. 3 is a schematic view of the structure of the gland 9 of the present invention.
In the figure: 1. a one-way valve; 2. a four-way valve; 3. a support platform; 4. a water inlet pipe; 5. a first three-way valve; 6. a first pressure gauge; 7. a top cover; 8. a temperature sensor; 9. a gland; 10. a filter layer; 11. a seal ring; 12. circulating the water layer; 13. a second three-way valve; 14. a separation kettle; 15. a second pressure gauge; 16. an outer barrel of the extraction kettle; 17. an inner barrel of an extraction kettle; 18. and (5) discharging a water pipe.
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 fig. 2 and 3, the device for supercritical extraction of grease of the present invention comprises an extraction kettle outer cylinder 16 mounted on a support platform 3, a liquid outlet pipe penetrating the support platform 3 and communicating with a four-way valve 2 through a pipeline is processed at the bottom of the extraction kettle outer cylinder 16, an extraction kettle inner cylinder 17 mounted inside the extraction kettle outer cylinder 16, an upper and a lower sealing rings 11 disposed between the extraction kettle outer cylinder 16 and the extraction kettle inner cylinder 17, wherein the sealing rings 11 can prevent an extractant from being connected in series through gaps between the extraction kettle inner cylinder and the extraction kettle outer cylinder, and provide sufficient pressure for extraction; the outer cylinder 16 of the extraction kettle is wrapped with a circulating water layer 12, water heated by a thermostat enters from a water inlet pipe 4 arranged at the bottom of the circulating water layer 12, and flows out from a water outlet pipe 18, and the extraction kettle is insulated to control the temperature of the extraction kettle; an air inlet pipe communicated with a first three-way valve 5 through a pipeline is processed at the upper part of an outer barrel 16 of the extraction kettle, the first three-way valve 5 is communicated with a four-way valve 2 through a pipeline, the four-way valve 2 is communicated with a one-way valve 1 through a pipeline, liquid gas enters the extraction kettle through the one-way valve 1, and the four-way valve 2 is communicated with a separation kettle 14 through a second three-way valve 13 arranged on the pipeline; the top of the extraction kettle inner cylinder 17 is connected with a top cover 7 arranged on the extraction kettle outer cylinder 16 through a threaded fastening connecting piece, the top cover 7 plays a role of fixing the inner cylinder, and a top cover sealing ring is arranged between the top cover 7 and the extraction kettle outer cylinder 16 and is used for being attached to the inner wall of the extraction kettle outer cylinder to form sealing to prevent gas from leaking; a temperature sensor 8 is arranged on the top cover 7 and used for measuring the temperature of the extraction kettle; the top and the bottom of the inner cylinder 17 of the extraction kettle are symmetrically provided with a filter layer 10 arranged on a support ring on the side wall of the inner cylinder 17 of the extraction kettle, furthermore, the filter layer 10 of the embodiment is a cylindrical shell and a medium filled in the shell, the shell is provided with holes, and the medium is absorbent cotton or quartz sand; the material is filled between two filter layers 10, and filter layer 10 outside longitudinal symmetry is provided with the gland 9 of installing on extraction cauldron inner tube 17, and the gland 9 of this embodiment is: two upper and lower concentric rings are connected into an organic whole through hollow cylinder, the outer surface processing of lower ring circumference has the external screw thread that suits with the internal thread of extraction cauldron inner tube, evenly distributed has the air vent on the ring down, extractant and gas pass through the air vent and get into extraction cauldron inner tube 17, it is provided with the gas-liquid passageway to go up the ring upper surface, gas also can get into inside extraction cauldron inner tube 17 through the gas-liquid passageway that sets up on the gland 9 at extraction cauldron inner tube 17 top, the grease through the extraction gets into the drain pipe through the gas-liquid passageway that sets up on the gland 9 of extraction cauldron inner tube 17 bottom, get into cross valve 2 by the drain pipe, gland 9 passes through the screw fastening and connects on extraction cauldron inner tube 17, the external diameter of the last ring of this embodiment is less than the external diameter of lower ring and is greater than hollow cylinder's external diameter, go up the ring and hollow cylinder and form the recess, be used for extraction cauldron inner tube 17 carries out packing and upset extraction cauldron inner tube 17. A gas flow channel is formed between the gland 9 and the top cover 7, liquid gas enters the material in the inner cylinder 17 of the extraction kettle from the gas flow channel for extraction, and a first pressure gauge 6 is arranged on a pipeline between the gas inlet pipe and the first three-way valve and used for measuring the pressure of the extraction kettle; a second pressure gauge 15 is arranged on the liquid outlet pipe of the separation kettle 14 and used for measuring the pressure of the separation kettle.
In fig. 1, the method for extracting grease by using the device for supercritical extraction of grease comprises the following steps:
s1, raw material treatment: crushing the materials until no particles exist;
s2, charging: filling the crushed material into the inner cylinder of the extraction kettle, compacting the material until the material and the inner cylinder wall have no gap, flattening the material surface, screwing the filter layer and the gland, filling the inner cylinder into the outer cylinder of the extraction kettle, and covering the top cover;
s3, extracting in an earlier stage: carbon dioxide gas is changed into liquid after being cooled, the liquid carbon dioxide gas is conveyed to a heater by a booster pump, the liquid carbon dioxide gas enters an extraction kettle from an A port to a B port of a four-way valve through a one-way valve and then passes through a C port and a B port of a first three-way valve, the liquid carbon gas in the extraction kettle flows out of the extraction kettle after flowing through an inner cylinder from top to bottom, the liquid carbon gas enters a separation kettle from a D port to a C port of the four-way valve through a C port and a B port of a second three-way valve 13, the liquid carbon gas flows out of the separation kettle and then enters the extraction kettle after being cooled, pressurized and heated, the liquid carbon gas circulates again, at the moment, the A ports of the first three-way valve and the second three-way valve are closed, the internal pressure of the extraction kettle is 7.2 MPa-100 MPa, the temperature is 10-80 ℃, the one-way valve is closed when a large amount of carbon dioxide gas exists in the separation kettle and oil is not contained, and gas inlet is stopped. Communicating the port A and the port B of the first three-way valve and the port A and the port B of the second three-way valve, releasing residual gas in the extraction kettle to the separation kettle, and closing the port A and the port B of the first three-way valve and the port A and the port B of the second three-way valve when the first pressure gauge and the second pressure gauge have the same numerical value;
s4, extraction middle period: opening the top cover of the extraction kettle, taking out the inner cylinder, turning the inner cylinder upside down, putting the inner cylinder into the extraction kettle again, covering the top cover, closing the port A and the port B of the first three-way valve and the port A and the port B of the second three-way valve, opening the one-way valve, starting pressurization, enabling the extractant to enter the inner cylinder from the upper end of the extraction kettle, flowing through the inner cylinder of the extraction kettle from top to bottom, flowing out of the extraction kettle from the bottom, passing through the port D and the port C of the four-way valve to the separation kettle, and closing the one-way valve when a large amount of carbon dioxide is in the separation kettle and the oil is not contained.
And S5, in the later stage of extraction, rotating the four-way valve to enable the port A to be communicated with the port D, and meanwhile, enabling the port B to be communicated with the port C. Opening the one-way valve 1, enabling an extracting agent to flow through the port A and the port D of the four-way valve, enabling the extracting agent to enter the inner cylinder from the bottom of the extraction kettle, enabling the extracting agent to flow through the inner cylinder from bottom to top, enabling the extracting agent to flow out of the upper end of the extraction kettle, enabling the extracting agent to enter the port B and the port C of the four-way valve through the port B and the port C of the first three-way valve, enabling the extracting agent to enter the separation kettle through the port C and the port B of the second three-way valve, and enabling the pressure in the extraction kettle to be 20-50 MPa and the temperature to be 32-60 ℃ at the stage.
Claims (4)
1. A device for supercritical extraction of grease is characterized in that: an extraction kettle outer cylinder is arranged on the supporting platform, and a liquid outlet pipe which penetrates through the supporting platform and is communicated with the four-way valve through a pipeline is arranged at the bottom of the extraction kettle outer cylinder; the outer barrel is wrapped with a water circulation layer for controlling the temperature of the extraction kettle, and the bottom of the water circulation layer is provided with a water inlet and a water outlet; an extraction kettle inner barrel is arranged in the extraction kettle outer barrel, a sealing ring is respectively arranged above and below the extraction kettle inner barrel, an air inlet pipe communicated with a first three-way valve through a pipeline is arranged at the upper part of the extraction kettle outer barrel, the first three-way valve is communicated with a four-way valve through a pipeline, the four-way valve is communicated with a one-way valve through a pipeline, and liquid gas passes through the one-way valve, flows through the four-way valve and the three-way valve and then enters the extraction kettle; the four-way valve is communicated with the separation kettle through a second three-way valve arranged on the pipeline; extraction cauldron inner tube top is provided with the top cap of installing on the extraction cauldron urceolus, be provided with the top cap sealing washer between top cap and the extraction cauldron urceolus, be used for forming sealed preventing gas leakage with the laminating of extraction cauldron urceolus inner wall, extraction cauldron inner tube top and bottom symmetry are provided with the filter layer of installing on extraction cauldron inner tube lateral wall supporting ring, it has the material to fill between the filter layer, the symmetry is provided with the gland of installing on the extraction cauldron inner tube about the filter layer outside, be provided with airflow channel between gland and the top cap, the supercritical fluid that gets into by first three-way valve gets into extraction cauldron inner tube through airflow channel and extracts the material, it is provided with temperature sensor to set up the outside on the top cap, be used for surveing extraction cauldron temperature, be provided with first manometer on the pipeline between intake pipe and the first three-way valve, be provided with the second manometer on the separation cauldron drain pipe.
2. The apparatus for supercritical extraction of fat according to claim 1, wherein: the filter layer is a cylindrical shell and a medium filled in the shell, small holes are processed in the shell, and the medium is absorbent cotton or quartz sand.
3. The apparatus for supercritical extraction of fats & oils as claimed in claim 1, wherein: the gland is as follows: two upper and lower concentric rings link as an organic wholely through hollow cylinder, and lower ring circumference surface processing has the external screw thread that suits with the internal thread that the extraction cauldron inner tube set up, evenly distributed has the air vent on the ring down, goes up the ring upper surface and is provided with the gas-liquid passageway, and the external diameter of going up the ring is less than the external diameter of ring down and is greater than hollow cylinder's external diameter, goes up the ring and forms the recess with hollow cylinder for the extraction cauldron inner tube is carried out when packing is overturned to the extraction cauldron inner tube.
4. The method for extracting the grease by using the device for supercritical extracting the grease as claimed in any one of the claims 1 to 3 is characterized by comprising the following steps:
s1, raw material treatment: crushing the materials until no particles exist;
s2, charging: filling the crushed material into the inner cylinder of the extraction kettle, compacting the material until the material and the inner cylinder wall have no gap, flattening the material surface, screwing the filter layer and the gland, filling the inner cylinder into the outer cylinder of the extraction kettle, and covering the top cover;
s3, extracting in an earlier stage: carbon dioxide gas is changed into liquid through temperature reduction, the liquid carbon dioxide gas is conveyed to a heater through a booster pump, the liquid carbon dioxide gas enters an extraction kettle from an A port to a B port of a four-way valve through a C port and a B port of a first three-way valve after being heated, the liquid gas in the extraction kettle flows through an inner cylinder from top to bottom and then flows out of the extraction kettle, gas carrying grease enters a separation kettle from a D port to the C port of the four-way valve through a C port and a B port of a second three-way valve, the grease and the gas are separated by the separation kettle, the grease is stored at the lower part of the separation kettle, the gas flows out of the upper part of the separation kettle and circulates into the extraction kettle again through temperature reduction, pressure increase and temperature increase, the A ports of the first three-way valve and the second three-way valve are closed at the moment, the internal pressure of the extraction kettle is 7.2 MPa-100 MPa, the temperature is 10-80 ℃, and when a large amount of carbon dioxide gas without oil appears at an inlet of the separation kettle, the one-way valve is closed, and gas inlet is stopped; opening an A port and a B port of a first three-way valve and an A port and a B port of a second three-way valve, guiding residual gas in the extraction kettle to a separation kettle, and closing the A port and the B port of the first three-way valve and the A port and the B port of the second three-way valve when the first pressure gauge and the second pressure gauge have the same numerical value;
s4, extraction middle period: opening a top cover of the extraction kettle, taking out the inner cylinder, turning the inner cylinder upside down, putting the inner cylinder into the extraction kettle again, covering the top cover, closing the port A and the port B of the first three-way valve and the port A and the port B of the second three-way valve, opening the one-way valve, starting pressurization, enabling an extracting agent to enter the inner cylinder from the upper end of the extraction kettle, flowing through the inner cylinder from top to bottom, flowing out of the extraction kettle from the bottom, passing through the port D and the port C of the four-way valve to the separation kettle, closing the one-way valve when a large amount of carbon dioxide gas without oil appears at the inlet of the separation kettle, and ending the middle stage of extraction;
s5, in the later stage of extraction, rotating the four-way valve to enable the port A to be communicated with the port D, enabling the port B to be communicated with the port C, opening the one-way valve, enabling an extracting agent to flow through the port A and the port D of the four-way valve, enter the inner barrel through the bottom of the extraction kettle, flow through the inner barrel from bottom to top, flow out of the upper end of the extraction kettle, enter the port B and the port C of the four-way valve through the port B and the port C of the first three-way valve, and enter the separation kettle through the port C and the port B of the second three-way valve, wherein the pressure in the extraction kettle is 20-50 MPa, and the temperature is 32-60 ℃.
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| CN109705976B (en) * | 2017-10-26 | 2023-01-03 | 陕西师范大学 | Extraction device for supercritical extraction of grease |
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