CN104004586B - A kind of method of subcritical fluid extraction lipid and device thereof - Google Patents

Abstract

The invention relates to a new method and device for lipid extraction. A method for subcritical fluid extraction of lipids, characterized in that it comprises the following steps: 1) preparation of a device for subcritical fluid extraction of lipids; 2) pretreatment of materials to be extracted; 3) subcritical fluid extraction of materials ; 4) concentration of lipid mixture; 5) lipid separation and precipitation; 6) repeated extraction and precipitation of materials. The method and device can significantly improve the solvent recovery rate and extraction rate.

Description

A method and device for subcritical fluid extraction of lipids

technical field

The invention relates to a new method and device for lipid extraction, in particular to a method for extracting lipids using subcritical low-boiling alkanes and derivatives thereof, and a device for realizing the method.

Background technique

The main methods of oil extraction are pressing method and leaching method. Extracting oil by pressing is a method of extracting oil by squeezing the oil out of the oil plant with the help of external mechanical force. In the traditional pressing oil production process, in order to squeeze out the oil as much as possible, the oil is generally flaked first, steamed and fried at about 120°C, and then pressed. The acid value and non-hydratable phospholipid content are high, and the oil oxidation is serious; at the same time, the oil cake protein denaturation is serious and the utilization rate is low, resulting in unreasonable resource utilization. An improved process for the above problems, that is, the cold pressing oil production process, its remarkable feature is that it can reduce the high-temperature treatment of processed materials, obtain high-quality oil and cake protein, increase the value of processed products, and reduce processing energy consumption and costs at the same time . However, compared with the hot pressing process, the low-temperature pressing process of oil plants has a relatively low oil extraction rate. Generally, the residual oil in the cake is 8% to 16%. In order to fully extract the oil, it is necessary to use the leaching method to extract the residual oil. However, at the present stage, the solvent used for oil extraction by leaching is mainly "No. 6 solvent", and its main component is n-hexane. Deterioration of protein quality and loss of heat-sensitive nutrients. Supercritical CO ₂ extraction is a new oil extraction technology, it has: CO ₂ as a solvent is non-toxic, odorless, non-flammable, and the product has no organic solvent residue; the extraction conditions are relatively mild, and the natural active ingredients can be retained to the greatest extent, etc. . However, in order to achieve higher oil extraction efficiency, the supercritical CO ₂ extraction pressure generally needs to be higher than 30MPa, which requires high equipment, and it is difficult to achieve continuous production, which requires large equipment investment and high energy consumption.

Due to the various problems existing in supercritical extraction technology at this stage, it is difficult to apply it to large-scale production. Therefore, exploring new green, low-consumption and high-efficiency oil extraction technology has become a research hotspot in the field of oil extraction in recent years. As a potential alternative to supercritical extraction technology, subcritical extraction technology has made a lot of research progress with the efforts of domestic and foreign researchers. The invention patent with application number 200910034263.3 discloses a "subcritical fluid extraction device and method for natural product active ingredients", which consists of extraction tank, evaporation tank, condenser, solvent tank, ultrasonic generator, compressor and vacuum pump, etc. This method can select different subcritical extraction media (ethane, propane, butane, isobutane and dimethyl ether, etc.) according to different extraction objects, and combine subcritical fluid extraction technology with ultrasonic extraction technology , improve the extraction rate and shorten the extraction time. However, the extraction enhancement method used in this invention is ultrasonic-assisted, which is difficult to achieve industrialization; the solvent recovery is completely combined with a vacuum pump and a compressor, and there is a phase change in the solvent recovery process, which leads to high energy consumption, long time and low efficiency.

Contents of the invention

In view of the deficiencies in the existing subcritical extraction technology, the purpose of the present invention is to provide a method and device for subcritical fluid extraction of lipids, which can significantly improve the solvent recovery rate and extraction rate.

In order to achieve the above object, the technical solution adopted by the present invention is a method for subcritical fluid extraction of lipids, which is characterized in that it comprises the following steps:

1) Preparation of a device for subcritical fluid extraction of lipids: a device for subcritical fluid extraction of lipids, including solvent tank 1, regulating metering tank 2, extraction tank 3, gas storage tank 4, desolvation tank 5, Membrane module 6, buffer tank 7, first compressor 8, vacuum pump 9, second compressor 10, heat exchanger 11, solvent pump 12; the top and bottom of solvent tank 1 are provided with interfaces respectively; the top of metering tank 2 is adjusted , the bottom and the upper part of the left side wall are respectively provided with interfaces, and the right side wall of the regulating metering tank 2 is provided with a liquid level gauge;

The bottom interface of the solvent tank 1 is connected to the top interface of the regulating metering tank 2 through the pipeline and the second solenoid valve 14; The permeate outlet of the wall is connected, and the pipeline between the interface on the left side wall of the adjustment metering tank 2 and the twelfth electromagnetic valve 24 is provided with a pressure transmitter, and the interface at the bottom of the adjustment metering tank 2 passes through the pipeline in turn through the third electromagnetic valve 15 The fourth electromagnetic valve 16 is connected to the lower interface 3-14 of the extraction tank 3; the upper interface 3-4 on the top of the extraction tank 3 passes through the pipeline sequentially through the fifth electromagnetic valve 17, the gas outlet of the first compressor 8, and the first compressor 8 The air inlet and the sixth solenoid valve 18 are connected to the gas storage tank 4, and the pipeline between the upper interface 3-4 on the top of the extraction tank 3 and the fifth solenoid valve 17 is provided with a pressure transmitter and a branch that is connected with the first solenoid valve in turn. Seven solenoid valves 19, the first compressor 8 air inlets, the first compressor 8 gas outlets, the eighth solenoid valve 20 are connected to the gas storage tank 4, and the pipeline between the sixth solenoid valve 18 and the gas storage tank 4 is provided with Pressure transmitter; the pipeline between the third solenoid valve 15 and the fourth solenoid valve 16 is provided with two branches, the first branch is connected with one end of the ninth solenoid valve 21, the second branch is connected with the thirteenth solenoid valve One end of the electromagnetic valve 25 is connected, the other end of the ninth electromagnetic valve 21 is connected with the right interface 5-3 on the top cover 5-1 of the precipitation tank 5 through a pipeline, and the other end of the thirteenth electromagnetic valve 25 is connected with the vacuum pump through a pipeline. 9 is connected to the air inlet; the left interface 5-4 on the top cover 5-1 of the desolventizing tank 5 is connected to the concentrated solution outlet on the top of the membrane module 6 through the pipeline and the eleventh solenoid valve 23;

The solvent inlet at the bottom of the membrane module 6 is connected to the outlet 5-9 at the bottom of the desolvation tank 5 through the pipeline through the solvent pump 12 and the tenth solenoid valve 22 in sequence, and a pipe is connected between the outlet 5-9 and the tenth solenoid valve 22 It is connected to one end of the nineteenth electromagnetic valve 31, and the other end of the valve 31 is connected to the second pipe interface B; the gas outlet of the vacuum pump 9 is connected to the interface on the left side wall of the buffer tank 7 through the pipeline and the fifteenth electromagnetic valve 27, The pipeline between the air outlet of the vacuum pump 9 and the fifteenth solenoid valve 27 is provided with a branch connected to one end of the fourteenth solenoid valve 26, and the other end of the fourteenth solenoid valve 26 is connected to a third pipe interface C;

The interface on the top of the buffer tank 7 is connected to each other through the pipeline (the second branch) between the sixteenth electromagnetic valve 28 and the fourth electromagnetic valve 16 and the thirteenth electromagnetic valve 25, and the interface at the bottom of the buffer tank 7 is connected through the pipeline. The seventeenth electromagnetic valve 29 is connected to the fourth pipe interface D, and the interface on the right side wall of the buffer tank 7 passes through the second compressor 10, the heat exchanger 11, the eighteenth electromagnetic valve 30 and the top of the solvent tank 1 sequentially through the pipeline. The interface is connected; the pipeline between the interface on the top of the solvent tank 1 and the eighteenth solenoid valve 30 is provided with a pressure transmitter and a branch pipe is connected with one end of the first solenoid valve 13, and the other end of the first solenoid valve 13 is connected with the other end of the first solenoid valve 13. The first pipe interface A is connected;

2) Pretreatment of the material to be extracted: After removing impurities from the material to be extracted, it is rolled into flakes, weighed and loaded into the silo for temporary storage; start the vacuum pump 9 to exhaust the air in the extraction tank 3, so that The vacuum degree reaches below -0.09MPa (absolute pressure 0.01MPa), and the material in the feed bin enters the extraction tank 3 through the feeding solenoid valve 3-10;

3) Subcritical fluid extraction of materials: the subcritical fluid stored in the solvent tank 1 is metered by the adjustment metering tank 2 and then injected into the extraction tank 3. The gas is filled into the extraction tank 3, so that the pressure of the extraction tank 3 reaches 1.5-10 MPa to cause the expansion of the subcritical fluid to enhance the extraction effect, so that the temperature in the extraction tank 3 is 10-70 ° C, and the extraction time is 5-60 min/time ; During the extraction process, the lipids in the material are continuously dissolved into the subcritical fluid to form an extraction mixture; after the extraction process is completed, the gas is recycled to the gas storage tank 4 until the pressure of the extraction tank 3 drops to 1.0-3.0 MPa ;

4) Concentration of the lipid mixture: Start the vacuum pump 9 to exhaust the air in the desolvation tank 5 and the membrane module 6, so that the vacuum degree reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixture is filtered through the middle and bottom of the extraction tank 3 After the plate 3-8 is filtered, it enters the desolvation tank 5 through the fourth electromagnetic valve 16 and the ninth electromagnetic valve 21; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the eleventh electromagnetic valve is adjusted. The degree of opening and closing of the valve 23, thereby controlling the liquid pressure at the solvent inlet of the membrane module 6 to be 0.8-2.6 MPa, the solvent in the extraction mixture passes through the membrane and enters the regulating metering tank 2 to be recycled and reused, and the lipid is trapped by the membrane. Circulating and concentrating until the concentration of the extraction mixture in the precipitation tank 5 rises to 60% to 90% (g/g);

5) Lipid separation and precipitation: After the extraction mixture shrinks, the temperature of the precipitation tank 5 is 20-80° C., the magnetic stirring speed is turned on at 50-600 r/min, and the vacuum pump 9 and the second compressor 10 are turned on to remove the lipid. The concentrated extraction mixture in the solvent tank 5 is evaporated under reduced pressure until the pressure of the desolvation tank 5 drops below -0.09MPa (absolute pressure 0.01MPa) and lasts for more than 5min, and the evaporated solvent is compressed in the second compressor 10 Liquefied, after being cooled by the heat exchanger 11, return to the solvent tank 1 for recycling; the lipid extract after precipitation is discharged through the nineteenth electromagnetic valve 31 and the second pipe interface B;

6) Repeated extraction and precipitation of materials: if one extraction is not complete, repeat steps 3), 4), and 5) for 1 to 3 repeated extractions; after multiple extractions, turn on the vacuum pump 9 and the second compressor 10 Evaporate under reduced pressure the residual solvent of the material in the extraction tank 3 until the pressure of the extraction tank 3 drops below -0.09MPa (absolute pressure 0.01MPa) and last for more than 5min, and the evaporated solvent is compressed and liquefied in the second compressor 10 After being cooled by the heat exchanger 11, it returns to the solvent tank 1 for recycling; the precipitated material is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11.

According to the above scheme, the gas used to enhance the extraction effect in the gas storage tank 4 is CO ₂ .

According to the above scheme, the membrane filled in the membrane module 6 is a ceramic membrane with a molecular weight cut-off of 3kDa-12kDa.

According to the above scheme, the vacuum pump 9 is a diaphragm vacuum pump, and the first compressor 8 and the second compressor 10 are diaphragm compressors.

According to the above scheme, the subcritical fluid is C ₂ ~C ₄ low-boiling alkanes and their derivatives: any one or two or two of ethane, propane, butane, isobutane, R134a (tetrafluoroethane) A mixture of the above in any proportion.

According to the above scheme, the material to be extracted is rapeseed, soybean, peanut, sesame, hemp seed, camellia oleifera seed, flax, walnut kernel or pressed cake.

A subcritical fluid extraction lipid device for realizing the above method is characterized in that it includes a solvent tank 1, a regulating metering tank 2, an extraction tank 3, a gas storage tank 4, a precipitation tank 5, a membrane module 6, a buffer tank 7, First compressor 8, vacuum pump 9, second compressor 10, heat exchanger 11, solvent pump 12; The top and bottom of solvent tank 1 are respectively provided with interface; There is an interface, and the right side wall of the adjustment measuring tank 2 is provided with a liquid level gauge;

The bottom interface of the solvent tank 1 is connected to the top interface of the regulating metering tank 2 through the pipeline and the second electromagnetic valve 14; The permeate outlet of the wall is connected, and the pipeline between the interface on the left side wall of the adjustment metering tank 2 and the twelfth electromagnetic valve 24 is provided with a pressure transmitter, and the interface at the bottom of the adjustment metering tank 2 passes through the pipeline in turn through the third electromagnetic valve 15 The fourth electromagnetic valve 16 is connected to the lower interface 3-14 of the extraction tank 3; the upper interface 3-4 on the top of the extraction tank 3 passes through the pipeline sequentially through the fifth electromagnetic valve 17, the gas outlet of the first compressor 8, and the first compressor 8 The air inlet and the sixth solenoid valve 18 are connected to the gas storage tank 4, and the pipeline between the upper interface 3-4 on the top of the extraction tank 3 and the fifth solenoid valve 17 is provided with a pressure transmitter and a branch that is connected with the first solenoid valve in turn. Seven solenoid valves 19, the first compressor 8 air inlets, the first compressor 8 gas outlets, the eighth solenoid valve 20 are connected to the gas storage tank 4, and the pipeline between the sixth solenoid valve 18 and the gas storage tank 4 is provided with Pressure transmitter; the pipeline between the third solenoid valve 15 and the fourth solenoid valve 16 is provided with two branches, the first branch is connected with one end of the ninth solenoid valve 21, the second branch is connected with the thirteenth solenoid valve One end of the electromagnetic valve 25 is connected, the other end of the ninth electromagnetic valve 21 is connected with the right interface 5-3 on the top cover 5-1 of the precipitation tank 5 through a pipeline, and the other end of the thirteenth electromagnetic valve 25 is connected with the vacuum pump through a pipeline. 9 is connected to the air inlet; the left interface 5-4 on the top cover 5-1 of the desolventizing tank 5 is connected to the concentrated solution outlet on the top of the membrane module 6 through the pipeline and the eleventh solenoid valve 23;

The solvent inlet at the bottom of the membrane module 6 is connected to the outlet 5-9 at the bottom of the desolvation tank 5 through the pipeline through the solvent pump 12 and the tenth solenoid valve 22 in sequence, and a pipe is connected between the outlet 5-9 and the tenth solenoid valve 22 It is connected to one end of the nineteenth electromagnetic valve 31, and the other end of the valve 31 is connected to the second pipe interface B; the gas outlet of the vacuum pump 9 is connected to the interface on the left side wall of the buffer tank 7 through the pipeline and the fifteenth electromagnetic valve 27, The pipeline between the air outlet of the vacuum pump 9 and the fifteenth solenoid valve 27 is provided with a branch connected to one end of the fourteenth solenoid valve 26, and the other end of the fourteenth solenoid valve 26 is connected to a third pipe interface C;

The interface on the top of the buffer tank 7 is connected to the pipeline between the sixteenth electromagnetic valve 28 and the fourth electromagnetic valve 16 and the thirteenth electromagnetic valve 25 through the pipeline, and the interface at the bottom of the buffer tank 7 is connected to the seventeenth electromagnetic valve 29 through the pipeline. It is connected with the fourth pipe interface D, and the interface on the right side wall of the buffer tank 7 is connected to the interface on the top of the solvent tank 1 through the pipeline through the second compressor 10, the heat exchanger 11 and the eighteenth solenoid valve 30 in turn; the top of the solvent tank 1 The pipeline between the interface of the valve and the eighteenth solenoid valve 30 is provided with a pressure transmitter and a branch pipe connected to one end of the first solenoid valve 13, and the other end of the first solenoid valve 13 is connected to the first pipe interface A.

According to the above scheme, the extraction tank 3 includes a top cover 3-1, a cylinder body 3-2 and a bottom cover 3-3, and the top outer center of the top cover 3-1 is provided with an upper interface 3-4, and the top cover 3-1 is obtained by the method. The blue is connected to the upper end of the cylinder body 3-2, the inner upper end of the cylinder body 3-2 is provided with an upper filter plate 3-5, and the outer wall of the cylinder body 3-2 near the lower left side of the upper filter plate 3-5 is provided with a feed pipe 3-6, the inner lower end of the cylinder 3-2 is provided with an inclined lower filter plate 3-8, and the cylinder 3-2 near the upper right side of the lower filter plate 3-8 is provided with a discharge pipe 3-9, The outside of the cylinder 3-2 between the material pipe 3-6 and the discharge pipe 3-9 is covered with a water circulation jacket 3-7, and a temperature sensor is provided on the left side of the cylinder 3-2 near the water circulation jacket 3-7 , the feed pipe 3-6 is connected to the feed solenoid valve 3-10 through the flange, the discharge pipe 3-9 is connected to the discharge solenoid valve 3-11 through the flange, and the lower end of the cylinder 3-2 is connected to the flange through the flange. The bottom cover 3-3 is connected to each other, and an interface 3-14 is set outside the center of the bottom of the bottom cover 3-3.

According to the above scheme, the desolvation tank 5 includes a top cover 5-1 and a tank body 5-2, the outer side of the top cover 5-1 is respectively provided with a right interface 5-3 and a left interface 5-4, and the central outer side of the top cover 5-1 A magnetic transmission assembly 5-5 is provided, and a stirring rod 5-6 matched with the magnetic transmission assembly 5-5 is arranged on the inner side of the center of the top cover 5-1, and "U-shaped" stirring blades are arranged at intervals on the stirring rod 5-6 5-7, the top cover 5-1 is connected to the upper opening of the tank body 5-2 through the flange, the outer wall of the tank body 5-2 is covered with a water circulation jacket 5-8, and the bottom outside of the tank body 5-2 is provided with an outlet 5-9, the bottom of the tank body 5-2 is provided with a temperature sensor.

According to the above scheme, the membrane module 6 is composed of an upper head, a lower head, an outer cylinder and an ultrafiltration membrane. Inside the space formed by the head, the lower head and the outer cylinder, the upper head is provided with a concentrated solution outlet, the lower head is provided with a solution inlet, and the lower left side wall of the outer cylinder is provided with a permeate outlet.

According to the above scheme, the buffer tank 7 is composed of an upper head and a tank body, the upper head and the tank body are connected by flanges, the outer center of the upper head is provided with an interface, and the left and right side walls and the center of the bottom of the tank body are respectively provided with interfaces , There is a pressure transmitter on the outside of the upper head.

The beneficial effects of the present invention are:

1) In the present invention, a certain pressure of _CO2 gas (the pressure of _CO2 gas is 1.5-10MPa) is charged in the subcritical fluid extraction process, so that the volume of the subcritical fluid is expanded to form a _CO2 expanded subcritical liquid, and the viscosity and surface tension Reduced, enhanced solubility (high solvent strength), can significantly reduce subcritical fluid (solvent) usage and increase subcritical fluid extraction rate.

2) The diluting effect of _CO2 on the subcritical fluid (solvent) and the anaerobic environment and flame retardancy provided greatly enhance the production efficiency for some flammable subcritical fluids (ethane, propane, butane, etc.) Safe, reducing the flammability hazard of solvents.

3) When the present invention reclaims the solvent in the extraction mixed liquid, the membrane module (ultrafiltration membrane) is used to concentrate the extracted mixed liquid first, so that most of the subcritical fluid (solvent) is recovered without phase change, and then evaporated under reduced pressure to compress the liquefied The remaining part of the solvent is recovered by means of a method, which greatly reduces energy consumption and improves the efficiency of solvent recovery.

Description of drawings

Fig. 1 is a process flow diagram of the present invention.

Fig. 2 is a structural schematic diagram of an extraction tank in a subcritical fluid extraction device of the present invention.

Fig. 3 is a schematic structural diagram of a desolvation tank in a subcritical fluid extraction device of the present invention.

In the figure: A-the first pipe interface, B-the second pipe interface, C-the third pipe interface, D-the fourth pipe interface; 1-solvent tank, 2-adjusting metering tank, 3-extraction tank, 4-gas Storage tank, 5-desolvation tank, 6-membrane module, 7-buffer tank, 8-first compressor, 9-vacuum pump, 10-second compressor, 11-heat exchanger, 12-solvent pump, 13- The first solenoid valve, 14-the second solenoid valve, 15-the third solenoid valve, 16-the fourth solenoid valve, 17-the fifth solenoid valve, 18-the sixth solenoid valve, 19-the seventh solenoid valve, 20-the first solenoid valve Eight solenoid valves, 21-ninth solenoid valve, 22-tenth solenoid valve, 23-eleventh solenoid valve, 24-twelfth solenoid valve, 25-thirteenth solenoid valve, 26-fourteenth solenoid valve, 27-fifteenth solenoid valve, 28-sixteenth solenoid valve, 29-seventeenth solenoid valve, 30-eighteenth solenoid valve, 31-nineteenth solenoid valve;

3-1—top cover, 3-2—cylinder, 3-3—bottom cover, 3-4—upper interface, 3-5—upper filter plate, 3-6—feeding pipe, 3-7—water circulation clamp Set, 3-8—lower filter plate, 3-9—discharge pipe, 3-10—feed solenoid valve, 3-11—discharge solenoid valve, 3-12—first valve cleaning nozzle, 3-13— The second valve cleans the nozzle, 3-14—the lower interface;

5-1—top cover, 5-2—tank body, 5-3—right interface, 5-4—left interface, 5-5—magnetic drive assembly, 5-6—stirring rod, 5-7—stirring blade, 5-8—water circulation jacket, 5-9—exit.

detailed description

The preferred solution of the present invention is described below in conjunction with the accompanying drawings; it is included in the protection scope of the present invention, but does not limit the present invention.

As shown in Figure 1-3, a kind of method for subcritical fluid extraction lipid, comprises the steps:

1) Preparation of a device for subcritical fluid extraction of lipids: a device for subcritical fluid extraction of lipids, including solvent tank 1, regulating metering tank 2, extraction tank 3, gas storage tank 4, desolvation tank 5, Membrane module 6, buffer tank 7, first compressor 8, vacuum pump 9, second compressor 10, heat exchanger 11, solvent pump 12 and central electronic control unit; the top and bottom centers of solvent tank 1 are provided with interfaces respectively; The top, the center of the bottom, and the upper part of the left side wall of the regulating metering tank 2 are respectively provided with interfaces (the left side of Fig. 1 is left), and the right side wall of the regulating metering tank 2 is provided with a liquid level gauge;

The extraction tank 3 includes a top cover 3-1, a cylinder body 3-2 and a bottom cover 3-3. The top outer center of the top cover 3-1 is provided with an upper interface 3-4, and the top cover 3-1 is connected to the cylinder body through a flange. The upper ends of the 3-2 are connected, and the inner upper end of the cylinder 3-2 is provided with an upper filter plate 3-5, and the outer wall of the cylinder 3-2 near the lower left side of the upper filter plate 3-5 is provided with a feed pipe 3-6, The inner lower end of the cylinder 3-2 is provided with a lower filter plate 3-8 inclined (higher on the left side and lower on the right side), and a discharge pipe is provided on the cylinder 3-2 near the upper right side of the lower filter plate 3-8 3-9, the outside of the cylinder 3-2 between the feed pipe 3-6 and the discharge pipe 3-9 is covered with a water circulation jacket 3-7, and the left outside of the cylinder 3-2 is close to the water circulation jacket 3-7 There is a temperature sensor, the feed pipe 3-6 is connected to the feed solenoid valve 3-10 through the flange, the discharge pipe 3-9 is connected to the discharge solenoid valve 3-11 through the flange, and the feed solenoid valve 3- The pipe wall of 10 is provided with upper and lower two valve cleaning nozzles 3-12, and the discharge electromagnetic valve 3-11 pipe wall is provided with upper and lower valve cleaning nozzles 3-13 (for spraying before the valve is closed). The high-pressure air will clear out the material remaining on the sealing surface of the valve to ensure the high-pressure airtightness of the valve), the lower end of the cylinder 3-2 is connected with the bottom cover 3-3 through the flange, and the bottom center of the bottom cover 3-3 Interface 3-14 is set on the outside;

The desolvation tank 5 includes a top cover 5-1 and a tank body 5-2, the outer side of the top cover 5-1 is provided with a right interface 5-3 and a left interface 5-4 respectively, and the central outer side of the top cover 5-1 is provided with a magnetic drive Component 5-5, the central inner side of the top cover 5-1 is provided with a stirring rod 5-6 matched with the magnetic drive component 5-5, and the stirring rod 5-6 is provided with "U-shaped" stirring blades 5-7 at intervals, The top cover 5-1 is connected to the upper opening of the tank body 5-2 through the flange, the outer wall of the tank body 5-2 is covered with a water circulation jacket 5-8, and the bottom central outer side of the tank body 5-2 is provided with an outlet 5-9 , the bottom of the tank body 5-2 is provided with a temperature sensor;

Membrane module 6 is composed of upper head, lower head, outer cylinder and ultrafiltration membrane. The upper head, lower head and the two ends of the outer cylinder are respectively connected by flanges. Inside the space formed by the head and the outer cylinder, the upper head is provided with a concentrated liquid outlet, the lower head is provided with a solution inlet, and the lower left part of the side wall of the outer cylinder is provided with a permeate outlet;

The buffer tank 7 is composed of an upper head and a tank body, the upper head and the tank body are connected by flanges, the outer center of the upper head is provided with an interface, and the left and right side walls (both side walls) and the center of the bottom of the tank body are respectively provided with Interface, the outer side of the upper head is provided with a pressure transmitter;

The bottom port (bottom port) of the solvent tank 1 is connected to the top port (top port) of the regulating metering tank 2 through the pipeline and the second electromagnetic valve 14; The second solenoid valve 24 is connected to the permeate outlet of the side wall of the membrane module 6, and the pipeline between the interface on the left side wall of the adjustment metering tank 2 and the twelfth solenoid valve 24 is provided with a pressure transmitter, and the center of the bottom of the metering tank 2 is adjusted. The interface of the extraction tank 3 is connected to the lower interface (bottom interface) 3-14 on the bottom cover 3-3 of the extraction tank 3 through the third electromagnetic valve 15 and the fourth electromagnetic valve 16 successively through the pipeline; Through the pipeline, the fifth solenoid valve 17, the gas outlet of the first compressor 8, the air inlet of the first compressor 8 and the sixth solenoid valve 18 are connected to the gas storage tank 4 successively, and the upper interface 3-4 on the top of the extraction tank 3 is connected with the gas storage tank 4. The pipeline between the fifth electromagnetic valve 17 is provided with a pressure transmitter and a branch which are connected successively with the seventh electromagnetic valve 19, the air inlet of the first compressor 8, the air outlet of the first compressor 8, the eighth electromagnetic valve 20 and The gas storage tank 4 is connected, and the pipeline between the sixth electromagnetic valve 18 and the gas storage tank 4 is provided with a pressure transmitter; the pipeline between the third electromagnetic valve 15 and the fourth electromagnetic valve 16 is provided with two branches, the first One branch is connected with one end of the ninth solenoid valve 21, the second branch is connected with one end of the thirteenth solenoid valve 25, and the other end of the ninth solenoid valve 21 is connected with the top cover 5-1 of the precipitation tank 5 through the pipeline. The right interface 5-3 on the top is connected, and the other end of the thirteenth solenoid valve 25 is connected to the air inlet of the vacuum pump 9 through a pipeline; the left interface 5-4 on the top cover 5-1 of the precipitation tank 5 is connected to the first 11. Solenoid valve 23 is connected with the concentrated solution outlet at the top of membrane module 6 (on the upper head);

The solvent inlet at the bottom of the membrane module 6 (on the lower head) is connected to the outlet 5-9 at the bottom of the precipitation tank 5 through the pipeline through the solvent pump 12 and the tenth electromagnetic valve 22 in sequence, and the outlet 5-9 is connected to the tenth electromagnetic valve 22 A pipe between the pipes is connected to one end of the nineteenth electromagnetic valve 31, and the other end of the valve 31 is connected to the second pipe interface B; The interface of the side wall is connected, and the pipeline between the air outlet of the vacuum pump 9 and the fifteenth solenoid valve 27 is provided with a branch and connected with one end of the fourteenth solenoid valve 26, and the other end of the fourteenth solenoid valve 26 is connected with a third pipe interface C;

The interface on the top of the buffer tank 7 (on the upper head) is connected to the pipeline (second branch) between the sixteenth electromagnetic valve 28 and the fourth electromagnetic valve 16 and the thirteenth electromagnetic valve 25 through the pipeline, and the buffer tank The interface at the bottom of 7 is connected to the fourth pipe interface D through the pipeline and the seventeenth electromagnetic valve 29, and the interface on the right side wall of the buffer tank 7 passes through the pipeline in turn through the second compressor 10, heat exchanger 11 (for solvent compression) The endothermic process required for decompression and evaporation of the thermal process and the precipitating process is carried out heat exchange through circulating water) and the eighteenth electromagnetic valve 30 is connected with the interface on the top of the solvent tank 1; the interface on the top of the solvent tank 1 is connected with the eighteenth electromagnetic valve 30 The intermediate pipeline is provided with a pressure transmitter and a branch pipe connected to one end of the first solenoid valve 13, and the other end of the first solenoid valve 13 is connected to the first pipe interface A;

The central electronic control unit is composed of an industrial control computer and an equipment control data acquisition system, which can control the valve opening and closing of the entire device, equipment start and stop, material weighing and delivery, pressure, temperature, liquid level, speed and time process parameters. Remote automatic control, so as to realize the automatic operation of the whole extraction process;

2) Pretreatment of the material to be extracted: After removing impurities (removing stone, iron and other impurities), the material to be extracted is made into thin slices, weighed and put into the silo for temporary storage; start the vacuum pump 9 Evacuate the air in the extraction tank 3 to make the vacuum reach below -0.09MPa (absolute pressure 0.01MPa), and the material in the feed bin enters the extraction tank 3 through the feed solenoid valve 3-10 (close the feed solenoid valve 3 Before -10, the material on the sealing surface of the valve is cleaned by the high-pressure air sprayed from the valve cleaning nozzle 3-12, and then the feeding electromagnetic valve 3-10 and other related valves are closed, and the fourth valve connected with the vacuum pump 9 Electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 are opened);

3) Subcritical fluid extraction of materials: the subcritical fluid (liquid solvent) stored in the solvent tank 1 is injected into the extraction tank 3 after being measured by the metering tank 2, and the material-solvent ratio (mass/volume ratio) is set to 1g:2 ~8mL, then the gas in the gas storage tank 4 (through the sixth solenoid valve 18, the inlet of the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is filled into the extraction tank 3 In the process, make the pressure of the extraction tank 3 reach 1.5-10MPa to cause the subcritical fluid to expand to enhance the extraction effect, control the water temperature of the water circulation jacket 3-7 to make the temperature in the extraction tank 3 10-70°C, and the extraction time is 5-60min/ time; during the extraction process, the lipid in the material is continuously dissolved in the subcritical fluid to form an extraction mixed solution; after the extraction process is completed, the gas is reclaimed by the first compressor 8 (through the seventh electromagnetic valve 19, the first compressor 8, the gas outlet of the first compressor 8 and the eighth electromagnetic valve 20) into the gas storage tank 4, until the pressure of the extraction tank 3 drops to 1.0～3.0MPa;

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the solvent inlet of the membrane module 6. The liquid pressure is 0.8-2.6MPa. The solvent (subcritical fluid) in the extraction mixture passes through the membrane and enters the regulating metering tank 2 to be recycled and reused. The macromolecular lipids are trapped by the membrane and concentrated in a cycle until the extraction and mixing in the desolventization tank 5 Liquid concentration increased to 60% ~ 90% [(g/g) × 100%];

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 20-80°C, and the magnetic stirring speed is 50-600r/min (magnetic stirrer , the rotating speed of stirring bar is 50～600r/min), open vacuum pump 9 (close the 14th solenoid valve 26, open the 15th solenoid valve 27) and the second compressor 10 will the concentrated extraction in the precipitation tank 5 mix The liquid is evaporated under reduced pressure until the pressure of the desolvation tank 5 drops below -0.09MPa (absolute pressure 0.01MPa) and lasts for more than 5min. The evaporated solvent (i.e. subcritical fluid) is compressed and liquefied in the second compressor 10. After the heat exchanger 11 is cooled, return to the solvent tank 1 for recycling; the lipid extract after precipitation is discharged through the nineteenth electromagnetic valve 31 and the second pipe interface B;

6) Repeated extraction and precipitation of materials: if one extraction is not complete, repeat steps 3), 4), and 5) for 1 to 3 repeated extractions; after multiple extractions, turn on the vacuum pump 9 (turn off the fourteenth Solenoid valve 26, open the 15th solenoid valve 27) and second compressor 10 carry out decompression evaporation to the residual solvent of material in extraction tank 3 until the pressure of extraction tank 3 drops below-0.09MPa (absolute pressure 0.01MPa) and Continue more than 5min, the evaporated solvent is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, returns to the solvent tank 1 for recycling; the material after the precipitation (i.e. the residue after the lipid is extracted ) is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11.

According to the above scheme, the gas used to enhance the extraction effect in the gas storage tank 4 is CO ₂ .

According to the above scheme, the membrane filled in the membrane module 6 is a ceramic membrane with a molecular weight cut-off of 3kDa-12kDa.

According to the above scheme, the vacuum pump 9 is a diaphragm vacuum pump, and the first compressor 8 and the second compressor 10 are diaphragm compressors.

According to the above scheme, the subcritical fluid (solvent) is C ₂ ~C ₄ low-boiling alkanes and their derivatives: any one or both of ethane, propane, butane, isobutane, R134a (tetrafluoroethane) A mixture of one or more than two kinds in any proportion.

According to the above scheme, the material to be extracted is rapeseed, soybean, peanut, sesame, hemp seed, camellia oleifera seed, flax, walnut kernel or pressed cake.

Example 1: _CO assisted subcritical butane extraction of oil from rapeseed

1) Preparation of a device for subcritical fluid extraction of lipids: same as above;

2) Pretreatment of the material to be extracted: After the rapeseed is removed of impurities (removing stones, iron and other impurities), it is rolled into thin slices (thickness of the embryo sheet is 0.5mm), and 100kg of the embryo after weighing is weighed. Put the rapeseed into the silo for temporary storage; start the vacuum pump 9 to exhaust the air in the extraction tank 3, so that the vacuum degree reaches below -0.09MPa (absolute pressure 0.01MPa); the material in the silo passes through the feeding electromagnetic valve 3- 10 enters the extraction tank 3 (before closing the feed electromagnetic valve 3-10, the high-pressure air ejected from the valve cleaning nozzle 3-12 cleans the material on the valve sealing surface, and then closes the feed electromagnetic valve 3-10 and Other relevant valves, the fourth electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 that are communicated with the vacuum pump 9 are opened).

3) Subcritical fluid extraction of materials: the butane (subcritical fluid) stored in the solvent tank 1 is metered by the metering tank 2 and injected into the extraction tank 3, and the material-solvent ratio (mass/volume ratio) is set to 1g: 3mL , then the CO in the gas storage tank ₄ Gas (through the sixth solenoid valve 18, the inlet of the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is filled into the extraction tank 3 In, make the pressure of extraction tank 3 reach 7MPa and cause the expansion of subcritical fluid to enhance the extraction effect (the pressure of CO ₂ gas is 7MPa,), control the water temperature of water circulation jacket 3-7 so that the temperature of extraction tank 3 is 40 ℃, and the extraction time is 20min/time; during the extraction process, the lipid in the material is continuously dissolved in the subcritical fluid to form an extraction mixed solution; after the extraction process is completed, the gas is recovered by the first compressor 8 (through the seventh electromagnetic valve 19, the first The air inlet of compressor 8, the air outlet of first compressor 8 and the eighth electromagnetic valve 20) are in the gas storage tank 4, until the pressure of extraction tank 3 drops to 1.2MPa.

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the pressure of the solvent inlet liquid of the membrane module 6 as 1.6MPa, the solvent in the extraction mixture permeates the membrane and enters the adjustment metering tank 2 to be recycled and reused, the macromolecular lipids are intercepted by the membrane, and the concentration of the extraction mixture in the desolventization tank 5 rises to 70% (g/g ).

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 60°C, turn on the magnetic stirring speed to 200r/min, turn on the vacuum pump 9 (close the tenth Four electromagnetic valves 26, open the fifteenth electromagnetic valve 27) and the second compressor 10 carry out decompression and evaporation of the concentrated extraction mixed solution in the desolvation tank 5 until the pressure of the desolvation tank 5 drops to -0.09MPa (absolute pressure 0.01 MPa) and continue for more than 5min, the evaporated solvent is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, it returns to the solvent tank 1 for recycling; The solenoid valve 31 and the second pipe port B are discharged.

6) Repeated extraction and precipitation of the material: Repeat steps 3), 4), and 5) to perform repeated extraction twice; after the multiple extraction processes, turn on the vacuum pump 9 (close the fourteenth electromagnetic valve 26, open the fifteenth Solenoid valve 27) and second compressor 10 carry out decompression evaporation to the residual solvent of material in extraction tank 3 until the pressure of extraction tank 3 drops below-0.09MPa (absolute pressure 0.01MPa) and continue more than 5min, the solvent of evaporation is in Compressed and liquefied in the second compressor 10, cooled by the heat exchanger 11, and then returned to the solvent tank 1 for recycling; the precipitated rapeseed meal is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11. After testing, rapeseed oil contains 0.6ppm of residual solvent (illustrating that the method and device can significantly improve the solvent recovery rate), 0.8% of residual oil in rapeseed meal (illustrating that the method and device can significantly improve the extraction rate), and residual Solvent 150ppm (illustrates that this method and device can significantly improve solvent recovery rate).

Example 2: CO ₂ Assisted Subcritical R134a Extraction of Phospholipids from Soybeans

1) Preparation of a device for subcritical fluid extraction of lipids: same as above;

2) Pretreatment of the material to be extracted: After removing impurities from the soybeans (removing stones, removing iron and other impurities), they are made into thin slices by flaking (thickness of the embryo sheet is 0.4mm), and 100kg of soybeans after flaking are weighed. Put it into the silo for temporary storage; start the vacuum pump 9 to exhaust the air in the extraction tank 3, so that the vacuum degree reaches below -0.09MPa (absolute pressure 0.01MPa); the material in the silo enters through the feed solenoid valve 3-10 In the extraction tank 3 (before closing the feed solenoid valve 3-10, the high-pressure air ejected from the valve cleaning nozzle 3-12 is used to clean the material on the valve sealing surface, and then close the feed solenoid valve 3-10 and other related valve, the fourth electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 that are communicated with the vacuum pump 9 are opened).

3) Subcritical fluid extraction of materials: The tetrafluoroethane (R134a) stored in the solvent tank 1 is metered into the extraction tank 3 after adjusting the metering tank 2, and the material-solvent ratio (mass/volume ratio) is set to 1g: 5mL , then the CO in the gas storage tank ₄ Gas (through the sixth solenoid valve 18, the inlet of the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is filled into the extraction tank 3 In the process, make the pressure of the extraction tank 3 reach 6MPa to cause subcritical fluid expansion to enhance the extraction effect, control the water temperature of the water circulation jacket 3-7 so that the temperature of the extraction tank 3 is 30°C, and the extraction time is 30min/time; during the extraction process, in the material Lipids in the subcritical fluid are continuously dissolved into the subcritical fluid to form an extraction mixture; after the extraction process is completed, the gas is recovered by the first compressor 8 (through the seventh electromagnetic valve 19, the air inlet of the first compressor 8, the first The gas outlet of compressor 8 and the eighth electromagnetic valve 20) are in the gas storage tank 4, until the pressure of extraction tank 3 drops to 1.8MPa.

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the pressure of the solvent inlet liquid of the membrane module 6 as 2.0MPa, the solvent in the extraction mixture permeates the membrane and enters the regulating metering tank 2 to be recycled and reused, the macromolecular lipids are intercepted by the membrane, and the concentration of the extraction mixture in the desolventization tank 5 rises to 60% (g/g ).

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 60°C, turn on the magnetic stirring speed to 230r/min, turn on the vacuum pump 9 (close the tenth Four electromagnetic valves 26, open the fifteenth electromagnetic valve 27) and the second compressor 10 carry out decompression and evaporation of the concentrated extraction mixed solution in the desolvation tank 5 until the pressure of the desolvation tank 5 drops to -0.09MPa (absolute pressure 0.01 MPa) and continue for more than 5min, the evaporated solvent is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, returns to the solvent tank 1 for recycling; Valve 31 and the second pipe connection B discharge.

6) Repeated extraction and precipitation of materials: a total of 1 extraction; after the extraction process, turn on the vacuum pump 9 (close the fourteenth solenoid valve 26, open the fifteenth solenoid valve 27) and the second compressor 10 to the extraction tank 3 The residual solvent of the material in the medium is evaporated under reduced pressure until the pressure of the extraction tank 3 drops below -0.09MPa (absolute pressure 0.01MPa) and lasts for more than 5min. The evaporated solvent is compressed and liquefied in the second compressor 10, and passed through the heat exchanger. 11 After cooling, return to the solvent tank 1 for recycling; the desolvated soybean meal is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11. After testing, the extraction rate of soybean lecithin is 90% (illustrating that the method and device can significantly improve the extraction rate), containing 0.7ppm of residual solvent (illustrating that the method and device can significantly improve the solvent recovery rate), and 180ppm of residual solvent in soybean meal (illustrating The method and device can significantly improve the solvent recovery rate).

Example 3: _CO assisted subcritical propane to extract hemp oil from hemp seeds

1) Preparation of a device for subcritical fluid extraction of lipids: same as above;

2) Pretreatment of the material to be extracted: After removing impurities (stone, iron and other impurities) from the hemp seed, it is made into thin slices (the thickness of the embryo sheet is 0.5mm) by flaking, and weighed 100kg after flaking The hemp seed packed into the silo is temporarily stored; Start the vacuum pump 9 to exhaust the air in the extraction tank 3, so that the vacuum degree reaches below -0.09MPa (absolute pressure 0.01MPa); the material in the silo passes through the feed solenoid valve 3-10 into the extraction tank 3 (before closing the feed solenoid valve 3-10, the high-pressure air sprayed from the valve cleaning nozzle 3-12 is used to clean the material on the valve sealing surface, and then the feed solenoid valve 3-10 is closed. 10 and other relevant valves, the fourth electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 that are communicated with the vacuum pump 9 are opened).

3) Subcritical fluid extraction of materials: the propane (subcritical fluid) stored in the solvent tank 1 is metered by the metering tank 2 and injected into the extraction tank 3, and the material-solvent ratio (mass/volume ratio) is set to 1g: 4mL, Then the CO in the gas storage tank ₄ gas (through the inlet of the sixth solenoid valve 18, the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is charged in the extraction tank 3 , make the pressure of extraction tank 3 reach 5MPa and cause the subcritical fluid to expand to enhance the extraction effect, control the water temperature of water circulation jacket 3-7 to make the temperature of extraction tank 3 be 25 ° C, and the extraction time is 25min/time; during the extraction process, the The lipid is continuously dissolved in the subcritical fluid to form an extraction mixture; after the extraction process is completed, the gas is recovered by the first compressor 8 (through the seventh electromagnetic valve 19, the air inlet of the first compressor 8, the first compression The gas outlet of machine 8 and the eighth electromagnetic valve 20) in gas storage tank 4, drop to 1.6MPa until the pressure of extraction tank 3.

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the pressure of the solvent inlet liquid of the membrane module 6 as 2.0MPa, the solvent in the extraction mixture permeates the membrane and enters the adjustment metering tank 2 to be recycled and reused. The macromolecular lipids are intercepted by the membrane, and the concentration of the extraction mixture in the desolventization tank 5 rises to 80% (g/g ).

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 50°C, turn on the magnetic stirring speed to 180r/min, turn on the vacuum pump 9 (close the tenth Four electromagnetic valves 26, open the fifteenth electromagnetic valve 27) and the second compressor 10 carry out decompression and evaporation of the concentrated extraction mixed solution in the desolvation tank 5 until the pressure of the desolvation tank 5 drops to -0.09MPa (absolute pressure 0.01 MPa) and continue for more than 5min, the evaporated solvent is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, returns to the solvent tank 1 for recycling; Nine solenoid valve 31 and the second pipe interface B discharge.

6) Repeated extraction and precipitation of the material: Repeat steps 3), 4), and 5) for a total of 3 repeated extractions; after the extraction process ends, turn on the vacuum pump 9 (close the fourteenth solenoid valve 26, open the fifteenth solenoid valve 27) and the second compressor 10 carry out decompression evaporation to the residual solvent of the material in the extraction tank 3 until the pressure of the extraction tank 3 drops below -0.09MPa (absolute pressure 0.01MPa) and continue for more than 5min, the evaporated solvent is in the second Compressed and liquefied in the compressor 10, cooled by the heat exchanger 11, and then returned to the solvent tank 1 for recycling; the precipitated hemp seed meal is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11. After testing, the hemp seed oil contains 0.3ppm of residual solvent (illustrating that the method and device can significantly improve the solvent recovery rate), 0.3% of residual oil in the hemp seed meal (illustrating that the method and device can significantly improve the extraction rate), and the residual solvent 100ppm (illustrating that the method and device can significantly improve the solvent recovery rate).

Example 4: _CO2 -assisted subcritical isobutane extraction of oil from camellia oleifera seeds

1) Preparation of a device for subcritical fluid extraction of lipids: same as above;

2) Pretreatment of the material to be extracted: remove the impurities of camellia oleifera seeds (remove stones, iron and other impurities), shell them and make thin slices (the thickness of the embryo slices is 0.4mm), and weigh 100kg to squeegee The last camellia seed is loaded into the feed bin for temporary storage; the vacuum pump 9 is started to exhaust the air in the extraction tank 3, so that the vacuum reaches below -0.09MPa (absolute pressure 0.01MPa), and the material in the feed bin passes through the feed electromagnetic valve 3-10 into the extraction tank 3 (before closing the feed solenoid valve 3-10, the high-pressure air sprayed from the valve cleaning nozzle 3-12 is used to clean the material on the valve sealing surface, and then the feed solenoid valve 3-10 is closed. 10 and other relevant valves, the fourth electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 that are communicated with the vacuum pump 9 are opened);

3) Subcritical fluid extraction of materials: the subcritical fluid (isobutane) stored in the solvent tank 1 is injected into the extraction tank 3 after being measured by the metering tank 2, and the material-solvent ratio (mass/volume ratio) is set to 1g: 2mL, then the gas in the gas storage tank 4 (through the sixth solenoid valve 18, the inlet of the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is charged in the extraction tank 3 , making the pressure of the extraction tank 3 reach 1.5MPa to cause subcritical fluid expansion to enhance the extraction effect, control the water temperature of the water circulation jacket 3-7 so that the temperature in the extraction tank 3 is 10°C, and the extraction time is 5min/time; during the extraction process, The lipid in the material is continuously dissolved in the subcritical fluid to form an extraction mixed solution; after the extraction process is completed, the gas is recovered by the first compressor 8 (through the seventh electromagnetic valve 19, the air inlet of the first compressor 8, The gas outlet of the first compressor 8 and the eighth electromagnetic valve 20) in the gas storage tank 4, until the pressure of the extraction tank 3 drops to 1.0MPa;

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the solvent inlet of the membrane module 6. The liquid pressure is 0.8MPa, and the solvent (subcritical fluid) in the extraction mixture passes through the membrane and enters the regulating metering tank 2 to be recycled and reused. The macromolecular lipids are intercepted by the membrane and concentrated in a cycle until the concentration of the extraction mixture in the desolventization tank 5 Rise to 60% [(g/g) × 100%];

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 20 ° C, and the magnetic stirring speed is 50 r/min (magnetic stirrer, stirring rod) Rotating speed is 50r/min), open vacuum pump 9 (close the 14th solenoid valve 26, open the 15th solenoid valve 27) and the second compressor 10 carry out decompression evaporation to the concentrated extraction mixture in the desolvation tank 5 until The pressure of the desolvation tank 5 drops below -0.09MPa (absolute pressure 0.01MPa) and lasts for more than 5 minutes, and the evaporated solvent (subcritical fluid) is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, Get back to solvent tank 1 and recycle; Camellia oleifera seed oil (lipid extract) after the precipitation is discharged through the nineteenth solenoid valve 31 and the second pipe interface B;

6) Repeated extraction and precipitation of materials: Repeat steps 3), 4), and 5) to perform repeated extraction once; after the extraction process is over, turn on the vacuum pump 9 (close the fourteenth solenoid valve 26, open the fifteenth solenoid valve 27 ) and the second compressor 10 decompress and evaporate the residual solvent of the material in the extraction tank 3 until the pressure of the extraction tank 3 drops below -0.09MPa (absolute pressure 0.01MPa) and continue for more than 5min. Compressed and liquefied in the machine 10, cooled by the heat exchanger 11, and then returned to the solvent tank 1 for recycling; the tea seed meal after precipitation is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11. After testing, the Camellia oleifera seed oil contains 0.6ppm of residual solvent (illustrating that the method and device can significantly improve the solvent recovery rate), 8.7% of residual oil in the tea seed meal (illustrating that the method and device can significantly improve the extraction rate), and the residue in the meal Solvent 175ppm (illustrates that this method and device can significantly improve solvent recovery rate).

Example 5: _CO assisted subcritical isobutane extraction of oil from flax seeds

1) Preparation of a device for subcritical fluid extraction of lipids: same as above;

2) Pretreatment of the material to be extracted: After removing impurities (stone, iron and other impurities) from the flax seeds, they are rolled into thin slices (the thickness of the flakes is 0.6mm), and 100kg of flax after weighing is weighed. Flax seeds are loaded into the silo for temporary storage; start the vacuum pump 9 to exhaust the air in the extraction tank 3, so that the vacuum degree reaches below -0.09MPa (absolute pressure 0.01MPa), and the material in the silo passes through the feed solenoid valve 3- 10 enters the extraction tank 3 (before closing the feed electromagnetic valve 3-10, the high-pressure air ejected from the valve cleaning nozzle 3-12 cleans the material on the valve sealing surface, and then closes the feed electromagnetic valve 3-10 and Other relevant valves, the fourth electromagnetic valve 16, the thirteenth electromagnetic valve 25 and the fourteenth electromagnetic valve 26 that are communicated with the vacuum pump 9 are opened);

3) Subcritical fluid extraction of materials: the subcritical fluid (isobutane) stored in the solvent tank 1 is injected into the extraction tank 3 after being measured by the metering tank 2, and the material-solvent ratio (mass/volume ratio) is set to 1g: 8mL, then the gas in the gas storage tank 4 (through the sixth solenoid valve 18, the inlet of the first compressor 8, the gas outlet of the first compressor 8 and the fifth solenoid valve 17) is charged in the extraction tank 3 , making the pressure of the extraction tank 3 reach 10MPa to cause subcritical fluid expansion to enhance the extraction effect, control the water temperature of the water circulation jacket 3-7 to make the temperature in the extraction tank 3 70°C, and the extraction time is 60min/time; during the extraction process, the material Lipids in the liquid continuously dissolve into the subcritical fluid to form an extraction mixture; after the extraction process is completed, the gas is recovered by the first compressor 8 (through the seventh solenoid valve 19, the air inlet of the first compressor 8, the second The gas outlet of a compressor 8 and the eighth electromagnetic valve 20) in the gas storage tank 4, until the pressure of the extraction tank 3 drops to 3.0MPa;

4) Concentration of the lipid mixture: start the vacuum pump 9 (open the ninth solenoid valve 21, the thirteenth solenoid valve 25 and the fourteenth solenoid valve 26) to exhaust the air in the precipitating tank 5 and the membrane module 6 to make the vacuum pressure reaches -0.09MPa (absolute pressure 0.01MPa); the extraction mixed solution (the mixed solution of lipid and subcritical fluid) is filtered through the middle and lower filter plate 3-8 of the extraction tank 3, and then passed through the fourth electromagnetic valve 16, the ninth electromagnetic valve The valve 21 enters the desolvation tank 5; the solvent pump 12 is started to pump the extraction mixture into the membrane module 6 for ultrafiltration, and the degree of opening and closing of the eleventh solenoid valve 23 is adjusted to control the solvent inlet of the membrane module 6. The liquid pressure is 2.6MPa. The solvent (subcritical fluid) in the extraction mixture passes through the membrane and enters the regulating metering tank 2 to be recycled and reused. The macromolecular lipids are trapped by the membrane and concentrated in a cycle until the concentration of the extraction mixture in the desolventization tank 5 Rise to 90% [(g/g) × 100%];

5) Lipid separation and precipitation: After the extraction mixture shrinks, control the water temperature of the water circulation jacket 5-8 so that the temperature of the precipitation tank 5 is 80°C, and the magnetic stirring speed is 600r/min (magnetic stirrer, stirring rod) Rotating speed is 600r/min), open vacuum pump 9 (close the 14th solenoid valve 26, open the 15th solenoid valve 27) and the second compressor 10 carry out decompression evaporation to the concentrated extraction mixture in the desolvation tank 5 until The pressure of the desolvation tank 5 drops below -0.09MPa (absolute pressure 0.01MPa) and lasts for more than 5 minutes, and the evaporated solvent (subcritical fluid) is compressed and liquefied in the second compressor 10, and after being cooled by the heat exchanger 11, Get back to the solvent tank 1 and recycle; the flax oil after the precipitation is discharged through the nineteenth electromagnetic valve 31 and the second pipe interface B;

6) Repeated extraction and precipitation of the material: repeat steps 3), 4), and 5) for 3 repeated extractions; after the multiple extraction process ends, turn on the vacuum pump 9 (close the fourteenth electromagnetic valve 26, turn on the fifteenth electromagnetic Valve 27) and the second compressor 10 decompress and evaporate the residual solvent of the material in the extraction tank 3 until the pressure of the extraction tank 3 drops below -0.09MPa (absolute pressure 0.01MPa) and continue for more than 5min. The second compressor 10 is compressed and liquefied, and after cooling by the heat exchanger 11, returns to the solvent tank 1 for recycling; the flax meal after precipitation is sucked out of the extraction tank 3 through the discharge solenoid valve 3-11. After testing, contain residual solvent 0.4ppm (illustrate that this method and device can significantly improve solvent recovery rate) in the flaxseed oil, residual oil 0.2% (illustrate that this method and device can significantly improve extraction rate) in the flaxseed meal, residual solvent 165ppm in the meal ( It shows that the method and device can significantly improve the solvent recovery rate).

Claims (9)

1. A method for subcritical fluid extraction of lipids, characterized in that it may further comprise the steps: 1) Preparation of a device for subcritical fluid extraction of lipids: a device for subcritical fluid extraction of lipids, including a solvent tank (1), a regulating metering tank (2), an extraction tank (3), a gas storage tank ( 4), precipitation tank (5), membrane module (6), buffer tank (7), first compressor (8), vacuum pump (9), second compressor (10), heat exchanger (11), Solvent pump (12); the top and the bottom of the solvent tank (1) are respectively provided with interfaces; equipped with level gauges; The bottom interface of the solvent tank (1) is connected to the top interface of the regulating metering tank (2) through the pipeline and the second electromagnetic valve (14); The valve (24) is connected to the permeate outlet of the side wall of the membrane module (6), and the pipe between the interface on the left side wall of the regulating metering tank (2) and the twelfth electromagnetic valve (24) is provided with a pressure transmitter. The interface at the bottom of the adjustment metering tank (2) is connected to the lower interface (3-14) of the extraction tank (3) through the pipeline through the third electromagnetic valve (15) and the fourth electromagnetic valve (16); the top of the extraction tank (3) The upper interface (3-4) passes through the pipeline successively through the fifth solenoid valve (17), the gas outlet of the first compressor (8), the air inlet of the first compressor (8) and the sixth solenoid valve (18) and the gas The storage tank (4) is connected, and the pipeline between the upper interface (3-4) on the top of the extraction tank (3) and the fifth electromagnetic valve (17) is provided with a pressure transmitter and a circuit that is connected with the seventh electromagnetic valve ( 19), the air inlet of the first compressor (8), the air outlet of the first compressor (8), the eighth solenoid valve (20) are connected to the gas storage tank (4), and the sixth solenoid valve (18) is connected to the gas storage tank (4). The pipeline between the tanks (4) is provided with a pressure transmitter; the pipeline between the third solenoid valve (15) and the fourth solenoid valve (16) is provided with two branches, the first branch and the ninth solenoid valve One end of (21) is connected, and the second branch is connected with one end of the thirteenth electromagnetic valve (25), and the other end of the ninth electromagnetic valve (21) is through the top cover (5- 1) is connected to the right interface (5-3), and the other end of the thirteenth electromagnetic valve (25) is connected to the air inlet of the vacuum pump (9) through a pipeline; the top cover (5-1) of the precipitation tank (5) ) on the left interface (5-4) is connected with the concentrated solution outlet on the top of the membrane module (6) through the pipeline and the eleventh electromagnetic valve (23); The solvent inlet at the bottom of the membrane module (6) is connected to the outlet (5-9) at the bottom of the desolvation tank (5) through the pipeline through the solvent pump (12) and the tenth solenoid valve (22) sequentially, and the outlet (5-9) Connect a pipe between the tenth electromagnetic valve (22) and one end of the nineteenth electromagnetic valve (31), and the other end of the nineteenth electromagnetic valve (31) is connected with the second pipe interface (B); the vacuum pump ( The gas outlet of 9) is connected to the interface on the left side wall of the buffer tank (7) through the pipeline and the fifteenth solenoid valve (27), and the pipeline between the gas outlet of the vacuum pump (9) and the fifteenth solenoid valve (27) There is a branch connected to one end of the fourteenth solenoid valve (26), and the other end of the fourteenth solenoid valve (26) is connected to a third pipe interface (C); The interface on the top of the buffer tank (7) is connected to the pipeline between the pipeline and the sixteenth electromagnetic valve (28) and the fourth electromagnetic valve (16) and the thirteenth electromagnetic valve (25), and the bottom of the buffer tank (7) The interface is connected to the fourth pipe interface (D) through the pipeline and the seventeenth solenoid valve (29), and the interface on the right side wall of the buffer tank (7) passes through the pipeline in turn through the second compressor (10), heat exchanger (11) and the eighteenth electromagnetic valve (30) are connected to the interface on the top of the solvent tank (1); the pipeline between the interface on the top of the solvent tank (1) and the eighteenth electromagnetic valve (30) is provided with a pressure transmitter and a The pipeline is connected to one end of the first solenoid valve (13), and the other end of the first solenoid valve (13) is connected to the first pipe interface (A); 2) Pretreatment of the material to be extracted: After removing impurities from the material to be extracted, it is rolled into flakes, weighed and put into the silo for temporary storage; start the vacuum pump (9) to remove the air in the extraction tank (3) Pump out to make the vacuum degree below -0.09MPa, and the material in the feed bin enters the extraction tank (3) through the feed solenoid valve (3-10); 3) Subcritical fluid extraction of materials: the subcritical fluid stored in the solvent tank (1) is metered by the adjustment metering tank (2) and injected into the extraction tank (3), and the material-solvent ratio is set to 1g: 2-8mL, and then Fill the gas in the gas storage tank (4) into the extraction tank (3), make the pressure of the extraction tank (3) reach 1.5-10MPa, cause the subcritical fluid to expand to enhance the extraction effect, and make the temperature in the extraction tank (3) The temperature is 10-70°C, and the extraction time is 5-60min/time; during the extraction process, the lipid in the material is continuously dissolved into the subcritical fluid to form an extraction mixture; after the extraction is completed, the gas is recovered to the gas storage tank (4 ), until the pressure in the extraction tank (3) drops to 1.0-3.0MPa; 4) Concentration of the lipid mixture: start the vacuum pump (9) to exhaust the air in the desolvation tank (5) and the membrane module (6), so that the vacuum degree reaches -0.09MPa; the extraction mixture is passed through the extraction tank (3) After filtering through the lower filter plate (3-8), it enters the precipitation tank (5) through the fourth solenoid valve (16) and the ninth solenoid valve (21); the solvent pump (12) is started to pump the extraction mixture into the membrane Ultrafiltration is carried out in the module (6), and the degree of opening and closing of the eleventh solenoid valve (23) is adjusted, thereby controlling the liquid pressure at the solvent inlet of the membrane module (6) to be 0.8-2.6 MPa, and the solvent in the extraction mixture is permeable Pass through the membrane and enter the regulating metering tank (2) to be recycled and reused, the lipid is retained by the membrane, and concentrated in circulation until the concentration of the extraction mixture in the desolventizing tank (5) rises to 60% to 90% g/g; 5) Lipid separation and precipitation: After the extraction mixture shrinks, the temperature of the precipitation tank (5) is 20-80°C, the magnetic stirring speed is turned on at 50-600r/min, the vacuum pump (9) and the second compression are turned on Machine (10) carries out decompression evaporation to the concentrated extraction mixed solution in the desolvation tank (5) until the pressure of the desolventization tank (5) drops below -0.09MPa and lasts more than 5min, and the evaporated solvent is in the second compressor (10) is compressed and liquefied, and after being cooled by the heat exchanger (11), it returns to the solvent tank (1) for recycling; the lipid extract after the precipitating is passed through the nineteenth electromagnetic valve (31) and the second pipe Port (B) discharge; 6) Repeated extraction and precipitation of materials: if one extraction is not complete, repeat steps 3), 4), and 5) for 1 to 3 repeated extractions; after multiple extractions, turn on the vacuum pump (9) and the second Compressor (10) carries out decompression evaporation to the residual solvent of material in extraction tank (3) until the pressure of extraction tank (3) drops below-0.09MPa and lasts more than 5min, the solvent evaporated in the second compressor (10) After being compressed and liquefied in the heat exchanger (11), it is returned to the solvent tank (1) for recycling; the precipitated material is sucked out of the extraction tank (3) through the discharge solenoid valve (3-11). 2 . The method for extracting lipids with a subcritical fluid according to claim 1 , wherein the gas used to enhance the extraction effect in the gas storage tank ( 4 ) is CO ₂ . 3 . The method for extracting lipids with a subcritical fluid according to claim 1 , wherein the membrane packed in the membrane module ( 6 ) is a ceramic membrane with a molecular weight cut-off of 3 kDa˜12 kDa. 4 . 4 . The method for extracting lipids with a subcritical fluid according to claim 1 , wherein the subcritical fluid is C ₂ -C ₄ low-boiling alkanes and derivatives thereof. 5. the method for a kind of subcritical fluid extraction lipid according to claim 1 is characterized in that: described material to be extracted is rapeseed, soybean, peanut, sesame, hemp seed, camellia oleifera seed, flax, walnut kernels or pressed cakes. 6. realize the device of a kind of subcritical fluid extraction lipid of the described method of claim 1, it is characterized in that comprising solvent tank (1), regulating metering tank (2), extraction tank (3), gas storage tank (4) , desolvation tank (5), membrane module (6), buffer tank (7), first compressor (8), vacuum pump (9), second compressor (10), heat exchanger (11), solvent pump (12); the top and the bottom of the solvent tank (1) are provided with interface respectively; level gauge; The bottom interface of the solvent tank (1) is connected to the top interface of the regulating metering tank (2) through the pipeline and the second electromagnetic valve (14); The valve (24) is connected to the permeate outlet of the side wall of the membrane module (6), and the pipe between the interface on the left side wall of the regulating metering tank (2) and the twelfth electromagnetic valve (24) is provided with a pressure transmitter. The interface at the bottom of the adjustment metering tank (2) is connected to the lower interface (3-14) of the extraction tank (3) through the pipeline through the third electromagnetic valve (15) and the fourth electromagnetic valve (16); the top of the extraction tank (3) The upper interface (3-4) passes through the pipeline successively through the fifth solenoid valve (17), the gas outlet of the first compressor (8), the air inlet of the first compressor (8) and the sixth solenoid valve (18) and the gas The storage tank (4) is connected, and the pipeline between the upper interface (3-4) on the top of the extraction tank (3) and the fifth electromagnetic valve (17) is provided with a pressure transmitter and a circuit that is connected with the seventh electromagnetic valve ( 19), the air inlet of the first compressor (8), the air outlet of the first compressor (8), the eighth solenoid valve (20) are connected to the gas storage tank (4), and the sixth solenoid valve (18) is connected to the gas storage tank (4). The pipeline between the tanks (4) is provided with a pressure transmitter; the pipeline between the third solenoid valve (15) and the fourth solenoid valve (16) is provided with two branches, the first branch and the ninth solenoid valve One end of (21) is connected, and the second branch is connected with one end of the thirteenth electromagnetic valve (25), and the other end of the ninth electromagnetic valve (21) is through the top cover (5- 1) is connected to the right interface (5-3), and the other end of the thirteenth electromagnetic valve (25) is connected to the air inlet of the vacuum pump (9) through a pipeline; the top cover (5-1) of the precipitation tank (5) ) on the left interface (5-4) is connected with the concentrated solution outlet on the top of the membrane module (6) through the pipeline and the eleventh solenoid valve (23); The solvent inlet at the bottom of the membrane module (6) is connected to the outlet (5-9) at the bottom of the desolvation tank (5) through the pipeline through the solvent pump (12) and the tenth solenoid valve (22) sequentially, and the outlet (5-9) Connect a pipe between the tenth electromagnetic valve (22) and one end of the nineteenth electromagnetic valve (31), and the other end of the nineteenth electromagnetic valve (31) is connected with the second pipe interface (B); the vacuum pump ( The gas outlet of 9) is connected to the interface on the left side wall of the buffer tank (7) through the pipeline and the fifteenth solenoid valve (27), and the pipeline between the gas outlet of the vacuum pump (9) and the fifteenth solenoid valve (27) There is a branch connected to one end of the fourteenth solenoid valve (26), and the other end of the fourteenth solenoid valve (26) is connected to a third pipe interface (C); The interface on the top of the buffer tank (7) is connected to the pipeline between the pipeline and the sixteenth electromagnetic valve (28) and the fourth electromagnetic valve (16) and the thirteenth electromagnetic valve (25), and the bottom of the buffer tank (7) The interface is connected to the fourth pipe interface (D) through the pipeline and the seventeenth solenoid valve (29), and the interface on the right side wall of the buffer tank (7) passes through the pipeline in turn through the second compressor (10), heat exchanger (11) and the eighteenth electromagnetic valve (30) are connected to the interface on the top of the solvent tank (1); the pipeline between the interface on the top of the solvent tank (1) and the eighteenth electromagnetic valve (30) is provided with a pressure transmitter and a The pipeline is connected to one end of the first solenoid valve (13), and the other end of the first solenoid valve (13) is connected to the first pipe interface (A); The membrane module (6) is composed of an upper head, a lower head, an outer cylinder and an ultrafiltration membrane. The upper head, the lower head and the two ends of the outer cylinder are respectively connected by flanges. Inside the space formed by the lower head and the outer cylinder, the upper head is provided with a concentrate outlet, the lower head is provided with a solution inlet, and the lower left side wall of the outer cylinder is provided with a permeate outlet. 7. the device of a kind of subcritical fluid extraction lipid according to claim 6 is characterized in that: extraction tank (3) comprises top cover (3-1), cylindrical shell (3-2) and bottom cover (3 -3), the top outer center of the top cover (3-1) is provided with an upper interface (3-4), the top cover (3-1) is connected to the upper end of the cylinder (3-2) through the flange, and the cylinder (3-2) -2) The inner upper end is provided with an upper filter plate (3-5), and the outer wall of the cylinder (3-2) on the lower left side of the upper filter plate (3-5) is provided with a feed pipe (3-6), The inner lower end of the cylinder (3-2) is provided with an inclined lower filter plate (3-8), and the cylinder (3-2) on the upper right side of the lower filter plate (3-8) is provided with a discharge pipe ( 3-9), the outside of the cylinder (3-2) between the feed pipe (3-6) and the discharge pipe (3-9) is covered with a water circulation jacket (3-7), the cylinder (3-2 ) is provided with a temperature sensor near the water circulation jacket (3-7), the feed pipe (3-6) is connected to the feed solenoid valve (3-10) through the flange, and the discharge pipe (3-9) It is connected with the discharge solenoid valve (3-11) through the flange, and the lower end of the cylinder (3-2) is connected with the bottom cover (3-3) through the flange, and the bottom center outside of the bottom cover (3-3) is set Interface (3-14). 8. the device of a kind of subcritical fluid extraction lipid according to claim 6, is characterized in that: desolvation tank (5) comprises top cover (5-1) and tank body (5-2), top cover ( The outer side of 5-1) is provided with right interface (5-3) and left interface (5-4) respectively, and the central outer side of top cover (5-1) is provided with magnetic force transmission assembly (5-5), and top cover (5- 1) A stirring rod (5-6) matching the magnetic drive assembly (5-5) is provided on the inner side of the center, and a "U-shaped" stirring blade (5-7) is arranged at intervals on the stirring rod (5-6). The top cover (5-1) is connected to the upper opening of the tank body (5-2) through the flange, the outer wall of the tank body (5-2) is covered with a water circulation jacket (5-8), and the tank body (5-2) An outlet (5-9) is provided outside the bottom of the tank, and a temperature sensor is provided at the bottom of the tank body (5-2). 9. The device for extracting lipids by a subcritical fluid according to claim 6, characterized in that: the buffer tank (7) is made up of an upper head and a tank body, the upper head and the tank body are connected by a flange, and the upper The outer center of the head is provided with an interface, the left and right side walls of the tank body and the center of the bottom are respectively provided with an interface, and the outer side of the upper head is provided with a pressure transmitter.