CN110237561B

CN110237561B - Supercritical fluid continuous extraction separation device system and extraction separation process

Info

Publication number: CN110237561B
Application number: CN201910576701.2A
Authority: CN
Inventors: 郭建章; 王烨尘; 王威强; 曲延鹏; 李飞; 李守军
Original assignee: Shandong Shuangchao Biological Equipment Technology Co ltd; Qingdao University of Science and Technology
Current assignee: Shandong Shuangchao Biological Equipment Technology Co ltd; Qingdao University of Science and Technology
Priority date: 2019-06-28
Filing date: 2019-06-28
Publication date: 2021-05-14
Anticipated expiration: 2039-06-28
Also published as: CN110237561A

Abstract

The invention relates to the field of chemical separation and bioengineering mechanical equipment, in particular to a supercritical fluid continuous extraction separation device system and an extraction separation process. The extraction separation process is implemented by applying the continuous extraction separation device system, and through the process operation of the system, the supercritical fluid extracted in the extracted bin enters the corresponding separation subsystem to start separation, the discharge valve is periodically opened, and the extract separated by the separation subsystem is discharged. The device has high automation degree, reliable operation of the device system, reasonable process flow of the device system, energy conservation, zero emission and excellent manufacturability, and realizes the continuous extraction and separation of the supercritical fluid.

Description

Supercritical fluid continuous extraction separation device system and extraction separation process

One, the technical field

The invention relates to the field of chemical separation and bioengineering mechanical equipment, in particular to a supercritical fluid continuous extraction separation device system and an extraction separation process.

Second, technical background

Separation techniques play an important role in modern industry. Supercritical fluid extraction is a new separation technology, and has many advantages compared with the traditional separation technology. With the improvement of living standard of substances, the demands for natural foods, medicines, spices and the like are increasingly vigorous, and the supercritical fluid extraction technology has wide prospects. However, most of the existing supercritical fluid extraction devices adopt intermittent devices with quick-opening sealing structures, so that the production efficiency is low and the energy consumption is high; the extractor is frequently started, the safety and the reliability are low, the great loss of the extraction fluid is caused, and the popularization and the application of the new technology are seriously restricted.

The patent of 'a horizontal supercritical fluid extraction kettle and a supercritical extraction device' entitled as a patent with the publication number of CN104784963B issued by the patent office of the national intellectual property office at 2016, 8, 24 and discloses a supercritical fluid extraction device. The horizontal supercritical fluid extraction device changes the vertical design of the traditional extraction kettle, solves the problem that the production cost of the vertical extraction kettle is obviously improved along with the increase of the size of the extraction kettle, saves the cost to a certain extent, but has the defects of low safety and reliability, high energy consumption, high extraction solvent loss and the like, and the sealing of the device is difficult to realize.

The patent office of the national intellectual property office of China issued a patent with a publication number of CN100427172C at 22.10.2008 discloses a high-pressure and ultrahigh-pressure continuous solid material extraction and sterilization device, which comprises a pressure-bearing cylinder, a bin chain, a bin operation driving mechanism, a heat exchanger, a fluid inlet pipe group and a fluid outlet pipe group, wherein the bin chain is arranged in the pressure-bearing cylinder, the bin operation driving mechanism is arranged at two ends of an inlet and an outlet of the pressure-bearing cylinder and is in matched connection with the bin chain which enters and exits the pressure-bearing cylinder, and the heat exchanger, the fluid inlet pipe group and the fluid outlet pipe group are arranged on the pressure-bearing cylinder. The device realizes continuous operation during high-pressure and ultrahigh-pressure solid material extraction and sterilization, and has the characteristics of safety, reliability and high efficiency. However, the device is only one unit in the extraction operation, and the complete set design and reasonable process flow of the continuous extraction device cannot be completed, so that the popularization and the use of the continuous extraction device are seriously limited.

Third, the invention

The invention aims to overcome the defects of the existing supercritical fluid extraction device and provides a supercritical fluid continuous extraction separation device system and an extraction separation process.

The invention relates to a technical scheme of a supercritical fluid continuous extraction separation device system, which consists of a supercritical fluid medium source, a pressurization subsystem, a continuous extraction subsystem, a separation subsystem and a pressurization circulation subsystem, wherein the separation subsystem and the pressurization circulation subsystem are used for step-by-step pressure boosting or total extraction stage number N of the continuous extraction subsystem.

The supercritical fluid medium source consists of a liquefied storage tank, a cooler, a refrigerating unit, an outlet valve, a filling valve and a main return valve group; the cooler is arranged inside or outside the liquefied storage tank and connected with the refrigerating unit to form a cooling loop; an outlet valve is arranged at the outlet of the liquefied storage tank, and the outlet of the outlet valve is a supercritical fluid medium source outlet; the supercritical fluid medium source has two inlets, one is the inlet of the total reflux valve, the other is the inlet of the filling valve, and the outlet of the total reflux valve and the outlet of the filling valve are combined by pipes and then connected to the inlet of the liquefied storage tank.

The pressurization subsystem consists of a cooler, a pressurization pump, a pressure reducing valve and an overflow valve; the connection relationship of each component is as follows:

the inlet of the cooler is the inlet of the pressurizing subsystem and is connected with the outlet of the supercritical fluid medium source, namely the outlet of the outlet valve, and the outlet of the cooler is connected with the inlet of the pressurizing pump through a pipe; the outlet of the pressurizing pump is divided into N branches by a pipe, the highest pressure level pipe branch of the pressurizing subsystem is divided into two branches, one branch is the highest pressure level outlet of the pressurizing subsystem, and the other branch is connected with the inlet of the overflow valve; the other N-1 branches are correspondingly connected with the inlets of the pressure reducing valves of all pressure levels through pipes, and the outlets of the pressure reducing valves are the outlets of the pressurizing subsystems of all pressure levels except the highest pressure level; the outlet of the overflow valve is connected to the pipe between the outlet of the cooler and the inlet of the pressure pump through the pipe; the number of outlets of the pressurizing subsystem, namely the number of the reducing valves and the overflow valves is the same as the step-by-step pressure boosting or the total extraction steps of the continuous extraction subsystem.

The continuous extraction subsystem consists of a storage bin, an extractor barrel, a loading end barrel end, a unloading end barrel end, a loading end locking device, an unloading end locking device, a loading hydraulic cylinder, an unloading hydraulic cylinder, a rack, a heat insulation layer, an emptying pump, an emptying switching valve, a drawing stop valve, a drawing compressor and a sealing ring; wherein:

the bin is a cylinder with a bin bottom, a distribution plate is arranged close to the bin bottom, a fluid inlet hole is formed in the cylinder wall between the distribution plate and the bin bottom, a powder baffle plate is arranged close to the bin opening, a fluid outlet hole is formed in the cylinder wall between the powder baffle plate and the bin opening, a locking clamping groove matched with a split type clamp quick-opening structure of a bin loading end locking device or a bin unloading end locking device is arranged on the bin bottom side of the outer circle of the bin cylinder, and sealing grooves are formed in the two sides of the locking clamping groove and the outer circle of the cylinder wall of the bin opening;

the extraction device barrel of the continuous extraction subsystem is of a cylindrical structure, and the inner cavity of the extraction device barrel is axially divided into a discharge section, a step-by-step boosting or extraction section with the number of steps not less than 2, a step-by-step pressure reduction section with the number of steps equal to the total number of steps of the step-by-step boosting or extraction section minus 1, and a withdrawal section which are four working sections; the inner cavity of the extraction cylinder of the continuous extraction subsystem is filled with bins, and each stage of step-by-step pressure boosting or extraction section is filled with at least one bin; the extraction device cylinder wall of the emptying section corresponding to the fluid inlet hole position of the loaded storage bin is provided with a fluid inlet and a fluid outlet, the extraction device cylinder wall of the step-by-step pressure increasing or extracting section corresponding to the fluid inlet hole position and the fluid outlet hole position of each loaded storage bin is respectively provided with a fluid inlet and a fluid outlet, the extraction device cylinder wall of the step-by-step pressure decreasing section corresponding to the fluid inlet hole position of each loaded storage bin is provided with a fluid balance inlet and a fluid balance outlet, and the extraction device cylinder wall of the drawing-back section corresponding to the fluid inlet hole position of the loaded storage bin is provided with a fluid outlet; each fluid inlet on the wall of the extractor cylinder body of the step-by-step boosting or extracting section is an inlet of the continuous extracting subsystem, and each fluid outlet on the wall of the extractor cylinder body of the step-by-step boosting or extracting section is an outlet of the continuous extracting subsystem;

the loading end locking device and the unloading end locking device are formed by split type clamps and hydraulic or electric drive; the split type clamp quick-opening structure of the loading end locking device is matched with the end part of the loading end barrel body and the locking clamping groove of the bin correspondingly;

the connection relationship of each component of the continuous extraction subsystem is as follows:

the bin loading hydraulic cylinder, the bin loading end locking device, the extractor barrel, the bin unloading end locking device and the bin unloading hydraulic cylinder are fixedly installed on the frame in sequence along the axis, so that the bin loading hydraulic cylinder, the bin loading end locking device, the extractor barrel, the bin unloading end locking device and the bin unloading hydraulic cylinder are coaxial with each other, the bin loading end locking device is matched with the end part of the bin loading barrel, and the bin unloading end locking device is matched with the end part of the bin unloading barrel;

a fluid outlet on the cylinder wall of the extractor at the pumping-back section is connected with an inlet of a pumping-back compressor through a pipe and a pumping-back stop valve, a fluid inlet and a fluid outlet on the cylinder wall of the extractor at the emptying section are divided into two paths, one path is connected with an outlet of the pumping-back compressor through the pipe and a pumping-back switching valve, the other path is connected with an inlet of an emptying pump through the pipe and the emptying switching valve, and an outlet of the emptying pump is communicated with the atmosphere; the fluid balance inlet and outlet of the step-by-step pressure reduction section next to the pumping section is connected with the fluid inlet of the step-by-step pressure increasing or extracting section next to the emptying section through a pipe, and so on, the fluid balance inlet and outlet of all the step-by-step pressure reduction sections are correspondingly connected with the fluid inlet of the step-by-step pressure increasing or extracting section with the step-by-step pressure increasing or extracting section total step number minus;

the outer wall of the extractor barrel body is coated with an insulating layer.

The separation subsystem is composed of a double-transformation separation subsystem, or a non-separation subsystem, wherein:

the heavy pressure and variable pressure separation subsystem consists of a heavy pressure regulating valve, a heavy heat exchanger and a heavy separator; the connection relationship of each component is as follows:

the inlet of a heavy pressure regulating valve is the inlet of a heavy pressure changing separation subsystem, the outlet of the heavy pressure regulating valve is connected with the inlet of a heavy heat exchanger through a pipe, the outlet of the heavy heat exchanger is connected with the inlet of a heavy separator through a pipe, the outlet of the heavy separator is the outlet of the heavy pressure changing separation subsystem, and the heavy separator is provided with an extract outlet and is provided with a heavy discharge valve.

The double pressure-changing separation subsystem consists of a double pressure-regulating valve, a double heat exchanger, a double separator, a double pressure-regulating valve, a double heat exchanger and a double separator; the connection relationship of each component is as follows:

the inlet of a heavy pressure regulating valve is the inlet of a double pressure-variable separation subsystem, the outlet of the heavy pressure regulating valve is connected with the inlet of a heavy heat exchanger through a pipe, the outlet of the heavy heat exchanger is connected with the inlet of a heavy separator through a pipe, the outlet of a heavy pressure-variable extractor is connected with the inlet of a double pressure regulating valve through a pipe, the outlet of the double pressure regulating valve is connected with the inlet of the double heat exchanger through a pipe, the outlet of the double heat exchanger is connected with the inlet of the double separator through a pipe, the outlet of the double separator is the outlet of the double pressure-variable separation subsystem, the heavy separator and the double separator are respectively provided with an extract outlet and are provided with a.

The non-separation subsystem is composed of a connecting pipe, the inlet of the connecting pipe is the inlet of the non-separation subsystem, and the outlet of the connecting pipe is the outlet of the non-separation subsystem.

The supercharging circulation subsystem is composed of a supercritical supercharging circulation subsystem or a pumpless supercritical supercharging circulation subsystem, wherein:

the supercritical pressurizing circulation subsystem consists of a pressure swing heat exchanger, a circulation condenser, a circulation pump and a circulation heat exchanger; the connection relationship of each component is as follows:

the low-pressure medium inlet of the pressure-variable heat exchanger is a main inlet of the supercritical pressurizing circulation subsystem, the low-pressure medium outlet of the pressure-variable heat exchanger is connected with the inlet of the circulation condenser through a pipe, the outlet of the circulation condenser is connected with the inlet of the circulation pump through a pipe, the pipe between the outlet of the circulation condenser and the inlet of the circulation pump is provided with an auxiliary inlet of the supercritical pressurizing circulation subsystem, the outlet of the circulation pump is connected with the high-pressure medium inlet of the pressure-variable heat exchanger through a pipe, the high-pressure medium outlet of the pressure-variable heat exchanger is connected with the inlet.

The pump-free supercritical pressurizing circulation subsystem consists of a circulation heat exchanger and a one-way valve; the connection relationship of each component is as follows:

the inlet of the one-way valve is a main inlet of the pumpless supercritical pressurizing circulation subsystem, the outlet of the one-way valve is respectively connected with the inlet of the circulation heat exchanger and an auxiliary inlet of the pumpless supercritical pressurizing circulation subsystem through pipes, and the outlet of the circulation heat exchanger is an outlet of the pumpless supercritical pressurizing circulation subsystem.

The connection relationship among the subsystems is as follows:

the outlet of each stage of pressurizing subsystem is connected with the corresponding secondary inlet of the pressurizing circulation subsystem through a pipe, the main inlet of each stage of pressurizing circulation subsystem is connected with the corresponding outlet of the separation subsystem through a pipe and a switching valve, the inlet of each stage of separation subsystem is connected with the outlet of each corresponding continuous extraction subsystem through a pipe, the outlet of each stage of pressurizing circulation subsystem is connected with the inlet of each corresponding continuous extraction subsystem through a pipe, the outlets of each stage of separation subsystem are divided into two paths through pipes, one path is connected with the inlet of the same supercritical fluid medium source through a reflux valve, and the other path is connected with the outlet of each corresponding stage of pressurizing circulation subsystem through a switching valve; and the connecting pipelines corresponding to the reflux valves of the separation subsystems of all stages and the supercritical fluid medium source inlet are provided with emptying valves.

The extraction and separation process implemented by applying a supercritical fluid continuous extraction and separation device system comprises the following steps:

(1) emptying a liquefaction storage tank of a supercritical fluid medium source, filling the supercritical fluid medium according to the specification, starting a refrigerating unit, and liquefying the supercritical fluid medium;

(2) installing a sealing ring in a sealing groove of each stock bin; opening a bin loading end locking device, pushing empty bins into an inner cavity of an extractor barrel of the continuous extraction subsystem one by using a bin loading hydraulic cylinder, starting to push the empty bins into bins containing extracted substances one by one after the inner cavity of the extractor barrel is filled with the empty bins, and locking the bin loading end locking device and the bin unloading end locking device of the continuous extraction subsystem after a bin is arranged outside a withdrawing section;

(3) closing a main reflux valve at a medium source inlet of the supercritical fluid, opening reflux valves of all separation subsystems, closing switching valves of all pressurization circulation subsystems, opening an emptying valve, opening an outlet valve at a medium source outlet of the supercritical fluid, and discharging air in the continuous extraction subsystem and all separation subsystems; after the air in the continuous extraction subsystem and all the separation subsystems is exhausted, switching valves of all the pressurization circulation subsystems are opened, the air in all the pressurization circulation subsystems is exhausted until the air is exhausted, then return valves of all the separation subsystems are closed, and exhaust valves are closed;

(4) starting a pressurizing subsystem to enable the pressure in the bins of each step-by-step pressure increasing or extracting section in the continuous extraction subsystem, the bins of the corresponding step-by-step pressure decreasing sections in the continuous extraction subsystem, the matched separation subsystem and the pressurizing circulation subsystem to reach set values;

(5) starting all the pressurizing circulation subsystems, starting the bins of the step-by-step pressurizing or extracting sections in the continuous extracting subsystem to finish corresponding step-by-step pressurizing or extracting, enabling the extracted supercritical fluid in the extracted bins to enter corresponding separating subsystems to start separating, periodically starting discharge valves, and discharging the extract separated by the separating subsystems;

(6) when the time of the extraction process is up, the bin in the step-by-step pressure increasing or extracting section closest to the step-by-step pressure decreasing section is closed, the pumping-back switching valve is opened, the emptying pump is started, and the air of the bin in the emptying section of the inner cavity of the extraction cylinder of the continuous extraction subsystem is emptied; closing the emptying switching valve and closing the emptying pump;

(7) retracting a piston rod of the binning hydraulic cylinder, installing a new bin filled with the extracted substances between the binning hydraulic cylinder and the bin locked by the binning end locking device, extending out of the binning hydraulic cylinder piston rod and tightly pushing the newly installed bin; a piston rod of the bin unloading hydraulic cylinder extends out and tightly pushes the bin locked by the bin unloading end locking device; synchronously opening a bin loading end locking device and a bin unloading end locking device; synchronously and continuously extending out a piston rod of a bin loading hydraulic cylinder and retracting a piston rod of a bin unloading hydraulic cylinder, and loading a newly loaded bin into an inner cavity of an extractor cylinder body of the continuous extraction subsystem; synchronously locking a bin loading end locking device and a bin unloading end locking device; retracting the piston rod of the bin unloading hydraulic cylinder, and unloading the ejected bin;

(8) starting an emptying switching valve, starting an emptying pump, and emptying air in a bin at an emptying section of an inner cavity of an extractor cylinder of the continuous extraction subsystem; closing the emptying switching valve and closing the emptying pump;

(9) opening a draw-back stop valve and a draw-back switching valve, wherein supercritical fluid medium in a storage bin at a draw-back section of an inner cavity of an extractor cylinder body of the continuous extraction subsystem flows into a storage bin at an emptying section of the inner cavity of the extractor cylinder body of the continuous extraction subsystem, when the pressure of the storage bin at the draw-back section and the pressure of the storage bin at the emptying section are balanced, a draw-back compressor is opened until all the supercritical fluid medium in the storage bin at the draw-back section is drawn back to the storage bin at the emptying section, the draw-back stop valve and the draw-back switching valve are closed, and;

(10) repeating the step (7) to the step (9), so that the bins containing the unextracted extract are periodically loaded into the continuous extraction subsystem, the extracted bins are synchronously unloaded out of the continuous extraction subsystem, in the process, each bin in the barrel cavity of the extractor of the continuous extraction subsystem is sequentially positioned in an emptying section, a step-by-step pressure boosting or extracting section, a step-by-step pressure reducing section and a withdrawing section, and the continuous operation of emptying air in the bins, step-by-step pressure boosting of the bins or step-by-step extraction of the extracted matter in the bins, step-by-step pressure reduction of the bins and withdrawing of supercritical fluid medium in the bins is sequentially completed in each working section; the supercritical fluid dissolved with the extract in the extraction completed bin enters a corresponding separation subsystem to start separation, and a discharge valve is periodically opened to discharge the extract separated by the separation subsystem.

The invention has the following beneficial effects: the pressure of each step-by-step boosting or extraction section bin of the continuous extraction subsystem is different in grades, so that the graded continuous extraction can be realized, the diversity of extracts is ensured, and the extraction efficiency is improved; the pressure is increased step by step and then reduced step by step along the advancing direction of the storage bin of the continuous extraction subsystem, so that the safety and reliability of the dynamic seal are effectively ensured; the supercritical fluid medium is recycled in the extraction and separation operations, and the fluid medium discharged out of the storage bin is recycled, so that the consumption of the fluid medium is effectively reduced; during supercritical fluid extraction, the separated supercritical fluid medium exchanges heat with the pressurized supercritical fluid medium, so that the heat and cold consumption of the system is effectively reduced. The device has the advantages of reasonable process flow of the system, high automation degree of the device, reliable operation of the system, energy conservation, zero emission and excellent manufacturability.

Description of the drawings

FIG. 1 is a schematic structural diagram of a supercritical fluid continuous extraction separation apparatus system according to the present invention;

FIG. 2 is a schematic diagram of the supercritical boost cycle subsystem shown at 2-1, …, 2- (N-1), 2-N in FIG. 1;

FIG. 3 is a schematic diagram of the pumpless supercritical boost circulation sub-system shown at 2-1, …, 2- (N-1), 2-N in FIG. 1;

FIG. 4 is a schematic diagram of a single PSR subsystem shown at 3-1, …, 3- (N-1), 3-N in FIG. 1;

FIG. 5 is a schematic diagram of the double pressure swing separation subsystem shown at 3-1, …, 3- (N-1), and 3-N in FIG. 1;

FIG. 6 is a schematic diagram of the non-separation sub-systems shown at 3-1, …, 3- (N-1) and 3-N in FIG. 1;

fig. 7 is a partially enlarged view showing the matching relationship between the silo and the extractor barrel, which is shown in the range encircled by the dotted line D in fig. 1.

Reference numerals:

1. the continuous extraction system comprises a continuous extraction subsystem 1-1, a storage bin 1-1-1, a fluid inlet hole 1-1-2, a distribution plate 1-1-3, a fluid outlet hole 1-1-4, a locking clamping groove 1-1-5, a powder baffle 1-1-6, a sealing ring 1-1-A, a storage bin 1-1-A-0 to be filled, an emptying storage bin 1-1-A-1-1, a 1-level boosting storage bin 1-1-A-1-2 and a 1-level boosting storage bin 2 1-1-A-1- (n)₁-1), 1 step-up (n) th₁-1) stock bin 1-1-A-1-n ₁1 st stage boosting nth₁1-1-A- (N-1) -1, N-1 level boosting 1 st bin 1-1-A- (N-1) -2, N-1 level boosting 2 nd bin 1-1-A- (N-1) - (N)_N-1-1), N-1 stage boosting (N)_N-1-1) stock bin 1-1-A- (N-1) -N_N-1N-1 stage boosting nth_N-11-1-A-N-1 stock bin, 1-1-A-N-2N-level boosting 1 stock bin and 1-1-A-N- (N) N-level boosting 2 stock bin_N-1), N-stage boosting (N)_N-1) stock bins 1-1-A-N-N_NN-th step up voltage_N1-1-B stock bin, 1-1-B-0 stock bin to be discharged, 1-1-B-1 stock bin to be pumped back, 1-1-B- (N-1) grade 1 depressurization stock bin, 1-2 grade N-1 depressurization stock bin and extraction1-2-A of a container barrel, 1-2-B of a barrel end of a loading end, 1-2-1 of a barrel end of a unloading end, 1-2-2 of a fluid inlet and outlet, 1-2-3 of a fluid inlet and outlet, 1-2-4 of a fluid outlet, 1-2-5 of a fluid balance inlet and outlet, 1-3-A of a fluid return port, 1-3-B of a locking device of the loading end, 1-4-A of a locking device of the unloading end, 1-4-B of a hydraulic cylinder of the loading, 1-5-1 of a hydraulic cylinder of the unloading, 1-5-2 of an emptying switching valve, 1-5-3 of a drawing switching valve, 1-6 of a drawing stop valve, 1-7 of an emptying pump, 1-8 of a drawing compressor, 1-9 parts of heat insulation layer, 2-1 parts of frame, 1-stage supercharging circulation subsystem, 2- (N-1), 2-N, N-stage supercharging circulation subsystem of N-1-stage supercharging circulation subsystem, 2-C parts of circulation condenser, 2-CV parts of one-way valve, 2-E parts of pressure swing heat exchanger, 2-P parts of circulation heat exchanger, 3-1 parts of circulation pump, 1-stage separation subsystem, 3- (N-1), 3-N, N-stage separation subsystem of N-1 stage separation subsystem, 3-H-1 parts of primary heater, 3-H-2 parts of dual heater, 3-HC-1 parts of primary heat exchanger, 3-HC-2 parts of dual heat exchanger, 3-S-1 parts of dual heat exchanger, 3-S-2 parts of primary separator, 2 parts of secondary separator, and the like, A double separator 3-V-1, a double discharge valve 3-V-2, a double discharge valve 3-VC-1, a double pressure regulating valve 3-VC-2, a double pressure regulating valve 4, a pressurizing subsystem 4-1, a cooler 4-2, a pressurizing pump 4-3-1, a 1-level pressure reducing valve 4-3- (N-1), an N-1-level pressure reducing valve 4-4, an overflow valve 5, a supercritical fluid medium source 5-1, a liquefied storage tank 5-2, a cooler 5-3, a refrigerating unit 5-4-1, a filling valve 5-4-2, an outlet valve 5-4-3, a total reflux valve 6-0, an exhaust valve 6-1-1, a 1-level switching valve 6-1- (N-1), N-1 stage switching valve 6-1-N, N stage switching valve 6-2-1, 1 stage return valve 6-2- (N-1), N-1 stage return valve 6-2-N, N stage return valve 7-pipe

Fifth, detailed description of the invention

The following describes the embodiments of the present invention in detail with reference to the accompanying drawings.

The first embodiment is as follows: a supercritical fluid multistage continuous pressure swing extraction separation device and extraction separation process flow are shown in figure 1, figure 2, figure 4, figure 5 and figure 7.

A supercritical fluid multistage continuous extraction and separation device system is composed of a supercritical fluid medium source 5, a pressurization subsystem 4, a continuous extraction subsystem 1, a 1-stage separation subsystem 3-1, a right-handed separation subsystem 3- (N-1), an N-stage ion system 3-N, a 1-stage pressurization circulation subsystem 2-1, …, an N-1-stage pressurization circulation subsystem 2- (N-1) and an N-stage pressurization circulation subsystem 2-N, wherein N is the step-by-step pressurization or the total extraction stage in the system, N is larger than 2, and the step-by-step extraction and the step-by-step pressurization of the supercritical fluid in the system are coincided.

The supercritical fluid medium source 5 consists of a liquefied storage tank 5-1, a cooler 5-2, a refrigerating unit 5-3, a filling valve 5-4-1, an outlet valve 5-4-2 and a total reflux valve 5-4-3, and the fluid overflowing material is stainless steel; the connection relationship of each component is as follows:

the cooler 5-2 is arranged inside or outside the liquefied storage tank 5-1, and the cooler 5-2 is connected with the refrigerating unit 5-3 to form a cooling loop; an outlet of the liquefaction storage tank 5-1 is provided with an outlet valve 5-4-2, and an outlet of the outlet valve 5-4-2 is an outlet of a supercritical fluid medium source 5; the supercritical fluid medium source 5 has two inlets, one is an inlet of a total reflux valve 5-4-3, the other is an inlet of a filling valve 5-4-1, and an outlet of the total reflux valve 5-4-3 and an outlet of the filling valve 5-4-1 are combined by a pipe 7 and then connected to an inlet of a liquefied storage tank 5-1.

The pressurization subsystem 4 consists of a cooler 4-1, a pressurization pump 4-2, a 1-level pressure reducing valve 4-3-1, …, an N-1-level pressure reducing valve 4-3- (N-1) and an N-level pressure level overflow valve 4-4, and the fluid overflowing material is stainless steel; the connection relationship of each component is as follows:

the inlet of the cooler 4-1 is the inlet of the pressurizing subsystem 4, and is connected with the outlet of the supercritical fluid medium source 5, namely the outlet valve 5-4-2, through a pipe 7, and the outlet of the cooler 4-1 is connected with the inlet of the pressurizing pump 4-2 through the pipe 7; the outlet of the pressure pump 4-2 is divided into N branches by a pipe 7, the pipe branch of the highest pressure level of the pressure subsystem 4 is divided into two branches, one branch is the outlet of the highest pressure level of the pressure subsystem 4, and the other branch is connected with the inlet of the overflow valve 4-4; the rest N-1 branches are correspondingly connected with inlets of pressure reducing valves of all pressure levels, namely 4-3-1, … of the 1-level pressure reducing valve and 4-3- (N-1) of the N-1-level pressure reducing valve through a pipe 7, and outlets of the pressure reducing valves, namely 4-3-1, … of the 1-level pressure reducing valve and 4-3- (N-1) of the N-1-level pressure reducing valve are outlets of pressurizing subsystems 4 of all pressure levels except the highest pressure level; the outlet of the overflow valve 4-4 is connected to the pipe 7 between the outlet of the cooler 4-1 and the inlet of the pressure pump 4-2 through the pipe 7; the number of outlets of the pressurizing subsystem 4, namely the number of 1-stage pressure reducing valves 4-3-1, …, N-1-stage pressure reducing valves 4-3- (N-1) and overflow valves 4-4 is the same as the number of the step-by-step pressure boosting or total extraction stages of the continuous extraction subsystem 1.

The continuous extraction subsystem 1 consists of a storage bin 1-1, an extractor barrel 1-2, a loading end barrel end 1-2-A, a unloading end barrel end 1-2-B, a loading end locking device 1-3-A, a unloading end locking device 1-3-B, a loading hydraulic cylinder 1-4-A, a unloading hydraulic cylinder 1-4-B, a frame 1-9, a heat insulation layer 1-8, an emptying switching valve 1-5-1, a drawing switching valve 1-5-2, a drawing stop valve 1-5-3, a drawing pump 1-6, a drawing compressor 1-7 and a sealing ring 1-1-6, wherein the fluid overflowing material is stainless steel; wherein:

the bin 1-1 is a cylinder with a bin bottom, the material is stainless steel, a distribution plate 1-1-2 is arranged close to the bin bottom, a fluid inlet hole 1-1-1 is arranged on the cylinder wall between the distribution plate 1-1-2 and the bin bottom, a powder baffle plate 1-1-5 is arranged close to a bin opening, a fluid outlet hole 1-1-3 is arranged on the cylinder wall between the powder baffle plate 1-1-5 and the bin opening, a locking clamping groove 1-1-4 matched with a split type clamp quick-opening structure of a bin loading end locking device 1-3-A or a bin unloading end locking device 1-3-B is arranged on the bin bottom side of the outer circle of the bin 1-1 cylinder, and sealing grooves are arranged on two sides of the locking clamping groove 1-1-4 and the outer circle of the bin opening;

an extractor barrel 1-2 of the continuous extraction subsystem 1 is of a cylindrical structure, a fluid overflowing material is stainless steel, two ends of the cylinder are respectively provided with a bin loading end barrel end part 1-2-A and a bin unloading end barrel end part 1-2-B with annular flanges, the outer wall of the cylinder is provided with a heat exchange sleeve, an inner cavity of the extractor barrel 1-2 is axially divided into four working sections, namely a emptying section, a step-by-step boosting or extracting section with the number of steps of N, a step-by-step boosting section with the number of steps of N-1 and a drawing-back section; the storage bin 1-1 is filled with the inner cavity of the extraction cylinder 1-2 of the continuous extraction subsystem 1, and at least one storage bin is arranged in each stage of step-by-step pressure boosting or extraction section; from the loading end of the continuous extraction subsystem 1, the bins 1-1 loaded into the inner cavity of the extractor barrel 1-2 are numbered sequentially as follows: loading the materials into a storage bin 1-1-A; an emptying bin 1-1-A-0 of the emptying section; no. 1 grade boosting or extracting bin 1-1-A-1-1, No. 2 grade 1 boosting or extracting bin 1-1-A-1-2, …, n of step boosting or extracting section₁No. 1 grade 1 pressure boosting or extracting bin 1-1-A-1- (n)₁-1)、n₁No. 1 grade pressure boosting or extracting bin 1-1-A-1-n₁N-1 upgrade of …, No. 11-1-A- (N-1) -1, No. 2N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -2, …, N_N-1No. 1N-1 grade boosting or extracting bin 1-1-A- (N-1) - (N)_N-1-1)、n_N-1N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -N_N-1No. 1N-grade boosting or extracting stock bin 1-1-A-N-1, No. 2N-grade boosting or extracting stock bin 1-1-A-N-2, …, N_NNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)_N-1)、n_NN-grade boosting or extracting bin 1-1-A-N-N_N(ii) a The N-1-level pressure reduction bin 1-1-B- (N-1) and … of the step-by-step pressure reduction section and the 1-1-B-1 of the 1-level pressure reduction bin are arranged in the step-by-step pressure reduction section; a pumping-back bin 1-1-B-0 of the pumping-back section; discharging the materials out of the stock bin 1-1-B; a fluid inlet and outlet 1-2-1 is arranged on the barrel wall of the extractor barrel 1-2 of the emptying section corresponding to the position of the fluid inlet hole 1-1-1 of the loaded bin, a fluid inlet 1-2-2 and a fluid outlet 1-2-3 are respectively arranged on the barrel wall of the extractor barrel 1-2 of the step-by-step boosting or extracting section corresponding to the position of the fluid inlet hole 1-1-1 and the fluid outlet 1-1-3 of each loaded bin, a fluid balance inlet and outlet 1-2-4 is respectively arranged on the barrel wall of the extractor barrel 1-2 of the step-by-step pressure reducing section corresponding to the position of the fluid inlet hole 1-1-1 of each loaded bin, and a fluid return port 1-2-5 is arranged on the barrel wall of the extractor barrel 1-2 of the drawing section corresponding to the position of the fluid inlet hole 1-1-1-1 of the loaded; each fluid inlet 1-2-2 on the wall of the extractor cylinder 1-2 of the step-by-step boosting or extracting section is an inlet of the continuous extracting subsystem 1, and each fluid outlet 1-2-3 on the wall of the extractor cylinder 1-2 of the step-by-step boosting or extracting section is an outlet of the continuous extracting subsystem 1;

the loading end locking device 1-3-A and the unloading end locking device 1-3-B are composed of split type hoops and hydraulic or electric drive; the split type hoop quick-opening structure of the loading end locking device 1-3-A is correspondingly matched with the end part 1-2-A of the barrel body of the loading end and the locking clamping groove 1-1-4 of the bin, and the split type hoop quick-opening structure of the unloading end locking device 1-3-B is correspondingly matched with the annular flange of the end part 1-2-B of the barrel body of the unloading end and the locking clamping groove 1-1-4 of the bin;

the connection relationship of each component of the continuous extraction subsystem 1 is as follows:

sequentially and fixedly mounting a loading hydraulic cylinder 1-4-A, a loading end locking device 1-3-A, an extractor cylinder 1-2, a discharging end locking device 1-3-B and a discharging hydraulic cylinder 1-4-B on a frame along an axis, so that the loading hydraulic cylinder 1-4-A, the loading end locking device 1-3-A, the extractor cylinder 1-2, the discharging end locking device 1-3-B and the discharging hydraulic cylinder 1-4-B are coaxial with each other, the loading end locking device 1-3-A is matched with the end part 1-2-A of the loading cylinder, and the discharging end locking device 1-3-B is matched with the end part 1-2-B of the discharging cylinder;

a fluid backflow port 1-2-5 on the wall of the extractor cylinder body 1-2 at the position of the pumping-back section is connected with an inlet of a pumping-back compressor 1-7 through a pipe 7 and a pumping-back stop valve 1-5-3, a fluid inlet and a fluid outlet 1-2-1 on the wall of the extractor cylinder body 1-2 at the position of the evacuation section are divided into two paths, one path is connected with an outlet of the pumping-back compressor 1-7 through the pipe 7 and a pumping-back switching valve 1-5-2, the other path is connected with an inlet of an evacuation pump 1-6 through the pipe 7 and an evacuation switching valve 1-5-1, and an outlet of the evacuation pump 1-6 is communicated with the atmosphere; a step-by-step pressure reduction section next to the drawing-back section, namely a fluid balance inlet and outlet 1-2-4 of the 1 st step-by-step pressure reduction section is connected with a fluid inlet 1-2-2 of the step-by-step pressure increase or extraction section next to the emptying section through a pipe 7; a step-by-step pressure reduction section of the next drawing-back section, namely a fluid balance inlet and outlet 1-2-4 of the 2 nd step-by-step pressure reduction section is connected with a fluid inlet 1-2-2 of the step-by-step pressure increase or extraction section of the next evacuation section through a pipe 7, and in the same way, fluid balance inlet and outlet 1-2-4 of all step-by-step pressure reduction sections are correspondingly connected with a fluid inlet of the step-by-step pressure increase or extraction section of which the total step number is reduced by 1 through the pipe 7;

the outer wall of the extractor barrel 1-2 is coated with an insulating layer 1-8.

The 1-stage separation subsystem 3-1, the N-1-stage separation subsystem 3- (N-1) and the N-stage ion system 3-N are composed of a double-pressure swing separation subsystem or a double-pressure swing separation subsystem, wherein:

the heavy pressure and variable pressure separation subsystem consists of a heavy pressure regulating valve 3-VC-1, a heavy heat exchanger 3-HC-1 and a heavy separator 3-S-1, and the fluid overflowing materials are all stainless steel; the connection relationship of each component is as follows:

the inlet of a heavy pressure regulating valve 3-VC-1 is the inlet of a heavy pressure changing separation subsystem, the outlet of the heavy pressure regulating valve 3-VC-1 is connected with the inlet of a heavy heat exchanger 3-HC-1 through a pipe 7, the outlet of the heavy heat exchanger 3-HC-1 is connected with the inlet of a heavy separator 3-S-1 through a pipe 7, the outlet of the heavy separator 3-S-1 is the outlet of the heavy pressure changing separation subsystem, the heavy separator 3-S-1 is provided with an extract outlet and is provided with a heavy discharge valve 3-V-1;

the double pressure-changing separation subsystem is composed of a heavy pressure-regulating valve 3-VC-1, a heavy heat exchanger 3-HC-1, a heavy separator 3-S-1, a double pressure-regulating valve 3-VC-2, a double heat exchanger 3-HC-2 and a double separator 3-S-2, wherein the fluid overflowing materials are stainless steel; the connection relationship of each component is as follows:

the inlet of a pressure regulating valve 3-VC-1 is the inlet of a double-pressure transformation separation subsystem, the outlet of the pressure regulating valve 3-VC-1 is connected with the inlet of a double heat exchanger 3-HC-1 through a pipe 7, the outlet of the double heat exchanger 3-HC-1 is connected with the inlet of a double separator 3-S-1 through a pipe 7, the outlet of the double separator 3-S-1 is connected with the inlet of a double pressure regulating valve 3-VC-2 through a pipe 7, the outlet of the double pressure regulating valve 3-VC-2 is connected with the inlet of a double heat exchanger 3-HC-2 through a pipe 7, the outlet of the double heat exchanger 3-HC-2 is connected with the inlet of the double separator 3-S-2 through a pipe 7, the outlet of the double separator 3-S-2 is the outlet of the double-pressure transformation separation, the first separator 3-S-1 and the second separator 3-S-2 are respectively provided with an extract outlet and are respectively provided with a second discharge valve 3-V-1 and a second discharge valve 3-V-2.

The 1-stage supercharging circulation subsystems 2-1 and …, the N-1-stage supercharging circulation subsystem 2- (N-1) and the N-stage supercharging circulation subsystem 2-N are composed of supercritical supercharging circulation subsystems, wherein:

the supercritical pressurizing circulation subsystem is composed of a variable pressure heat exchanger 2-E, a circulation condenser 2-C, a circulation pump 2-P and a circulation heat exchanger 2-HC, and fluid overflowing materials are all stainless steel; the connection relationship of each component is as follows:

the low-pressure medium inlet of the pressure-variable heat exchanger 2-E is a main inlet of a supercritical pressurizing circulation subsystem, the low-pressure medium outlet of the pressure-variable heat exchanger 2-E is connected with the inlet of the circulation condenser 2-C through a pipe 7, the outlet of the circulation condenser 2-C is connected with the inlet of the circulation pump 2-P through the pipe 7, the pipe 7 between the outlet of the circulation condenser 2-C and the inlet of the circulation pump 2-P is provided with an auxiliary inlet of the supercritical pressurizing circulation subsystem, the outlet of the circulation pump 2-P is connected with the high-pressure medium inlet of the pressure-variable heat exchanger 2-E through the pipe 7, the high-pressure medium outlet of the pressure-variable heat exchanger 2-E is connected with the inlet of the circulation heat exchanger 2.

The connection relationship among the subsystems is as follows:

the outlet of the supercritical fluid medium source 5, namely the outlet valve 5-4-2 is connected with the inlet of the pressurizing subsystem 4 through the pipe 7, the pressurizing subsystem 4 is provided with N outlets corresponding to the continuous extraction subsystem, each outlet is respectively connected with the corresponding 1-stage pressurizing circulation subsystem 2-1, …, the N-1-stage pressurizing circulation subsystem 2- (N-1) and the auxiliary inlet of the N-stage pressurizing circulation subsystem 2-N through the pipe 7, the 1-stage pressurizing circulation subsystem 2-1, …, the N-1-stage pressurizing circulation subsystem 2- (N-1), the N-stage pressurizing circulation subsystem 2-N main inlet is respectively connected with the corresponding 1-stage separation subsystem 3-1 through the pipe 7 and the 1-stage switching valve 6-1, …, the N-1-stage switching valve 6-1- (N-1), the N-stage switching valve 6-1-N and the corresponding 1-stage separation subsystem 3-1, …, an N-1 stage separation subsystem 3- (N-1) and an N-fraction ion system 3-N outlet are respectively connected, inlets of a 1 stage separation subsystem 3-1, a …, an N-1 stage separation subsystem 3- (N-1) and an N-fraction ion system 3-N are connected with corresponding outlets of the continuous extraction subsystem 1 through pipes 7, outlets of a 1 stage pressurization circulation subsystem 2-1, a …, an N-1 stage pressurization circulation subsystem 2- (N-1) and an N stage pressurization circulation subsystem 2-N are connected with inlets of corresponding pressure stages of the continuous extraction subsystem 1 through pipes 7, outlets of the 1 stage separation subsystem 3-1, the …, the N-1 stage separation subsystem 3- (N-1) and the N-fraction ion system 3-N are respectively divided into two paths through N pipes 7, one path passes through the inlets of the 1-stage reflux valves 6-2-1 and …, the N-1-stage reflux valve 6-2- (N-1), the N-stage reflux valve 6-2-N and the same supercritical fluid medium source 5, namely, the inlet of the total reflux valve 5-4-3 is connected, the other path is connected with the outlets of the 1-stage pressurizing circulation subsystems 2-1, …, the N-1-stage pressurizing circulation subsystem 2- (N-1) and the N-stage pressurizing circulation subsystem 2-N through the 1-stage switching valves 6-1-1, …, the N-1-stage switching valve 6-1- (N-1) and the N-stage switching valve 6-1-N, an exhaust valve 6-0 is arranged on a connecting pipeline corresponding to the outlet of the reflux valve of each stage of the separation subsystem and the inlet of the supercritical fluid medium source 5.

The extraction and separation process implemented by applying the supercritical fluid multistage continuous extraction and separation device system comprises the following steps:

(1) emptying a liquefaction storage tank 5-1 of a supercritical fluid medium source 5, filling the supercritical fluid medium according to the specification, starting a refrigerating unit 5-3, and liquefying the supercritical fluid medium;

(2) installing a sealing ring 1-1-6 in a sealing groove of each stock bin 1-1; opening a bin loading end locking device 1-3-A, pushing an empty bin 1-1 into an inner cavity of an extractor barrel 1-2 of a continuous extraction subsystem 1 one by using a bin loading hydraulic cylinder 1-4-A, starting to push the empty bin 1-1 filled with an extracted substance one by one after the inner cavity of the extractor barrel 1-2 is filled with the empty bin 1-1, and locking a bin loading end locking device 1-3-A and a bin unloading end locking device 1-3-B of the continuous extraction subsystem 1 after a withdrawal section is externally provided with the bin 1-1-B to be unloaded;

(3) closing a master reflux valve 5-4-3 at an inlet of a supercritical fluid medium source 5, opening a 1-stage reflux valve 6-2-1 of a 1-stage separation subsystem 3-1, opening an N-1-stage reflux valve 6-2- (N-1) of an N-1-stage separation subsystem 3- (N-1), an N-stage reflux valve 6-2-N of an N-stage ion system 3-N, closing 1-stage switching valves 6-1-1 and … of the 1-stage pressurization cycle subsystem 2-1, an N-1-stage switching valve 6-1- (N-1) of the N-1-stage pressurization cycle subsystem 2- (N-1) and an N-stage switching valve 6-1-N of the N-stage pressurization cycle subsystem 2-N, opening an exhaust valve 6-0, opening an outlet valve 5-4-2 at the outlet of a supercritical fluid medium source 5 to discharge air in the continuous extraction subsystem 1 and the separation subsystem 3-1, the separation subsystem 3- (N-1) of the N-1 stage and the ion system 3-N of the N stage; after air in the continuous extraction subsystem 1 and the 1-stage separation subsystem 3-1, the N-1-stage separation subsystem 3- (N-1) and the N-stage ion system 3-N is exhausted, the 1-stage switching valves 6-1, … of the 1-stage supercharging circulation subsystem 2-1, the N-1-stage switching valve 6-1- (N-1) of the N-1-stage supercharging circulation subsystem 2- (N-1) and the N-stage switching valve 6-1-N of the N-stage supercharging circulation subsystem 2-N are opened, air in the 1-stage supercharging circulation subsystem 2-1, …, the N-1-stage supercharging circulation subsystem 2- (N-1) and the N-stage supercharging circulation subsystem 2-N is exhausted until the air is exhausted, and then the 1-stage reflux valve 6-2-1 of the 1-stage separation subsystem 3-1 is closed, .., stage N-1 reflux valve 6-2- (N-1) of stage N-1 separation subsystem 3- (N-1), stage N reflux valve 6-2-N of stage N ion system 3-N, closing evacuation valve 6-0;

(4) starting the pressurizing subsystem 4, so that the pressure in a bin 1-1 of each step-by-step pressure increasing or extracting section in the continuous extracting subsystem 1, a bin 1-1 of a corresponding step-by-step pressure decreasing section and a matched 1-step separating subsystem 3-1, an N-1-step separating subsystem 3- (N-1), an N-step ion system 3-N, 1-step pressurizing circulating subsystems 2-1 and …, an N-1-step pressurizing circulating subsystem 2- (N-1) and an N-step pressurizing circulating subsystem 2-N reaches a set value;

(5) starting 1-stage pressurizing circulation subsystems 2-1 and …, an N-1-stage pressurizing circulation subsystem 2- (N-1) and an N-stage pressurizing circulation subsystem 2-N, and sequentially boosting the pressure or extracting section 1 in the continuous extraction subsystem 1 or 1-1-A-1-1 and 2 or 1-1-A-1-2, … and N of the continuous extraction subsystem 1₁No. 1 grade 1 pressure boosting or extracting bin 1-1-A-1- (n)₁-1)、n₁No. 1 grade pressure boosting or extracting bin 1-1-A-1-n₁…, No. 1N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -1, No. 2N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -2, …, N_N-1No. 1N-1 grade boosting or extracting bin 1-1-A- (N-1) - (N)_N-1-1)、n_N-1N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -N_N-1No. 1N-grade boosting or extracting stock bin 1-1-A-N-1, No. 2N-grade boosting or extracting stock bin 1-1-A-N-2, …, N_NNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)_N-1)、n_NN-grade boosting or extracting bin 1-1-A-N-N_NPerforming corresponding supercritical fluid extraction step by step, allowing the supercritical fluid in each boosting or extracting section bin which finishes extraction to enter a corresponding 1-stage separation subsystem 3-1, the N-1 stage separation subsystem 3- (N-1) and an N-stage ion system 3-N for separation, periodically opening a double discharge valve 3-V-1 or a double discharge valve 3-V-1 and a double discharge valve 3-V-2 which are matched with the 1-stage separation subsystem 3-1, the N-1 stage separation subsystem 3- (N-1) and the N-stage ion system 3-N, discharging the extracts respectively separated by the 1-stage separation subsystem 3-1, the N-1 stage separation subsystem 3- (N-1) and the N-stage ion system 3-N;

(6) the bin closest to the stage-by-stage pressure-increasing or extracting section of the stage-by-stage pressure-reducing section, i.e. the extracting bin 1-1-A-N-N_NWhen the extraction process time is reached, the pumping-back switching valve 1-5-2 is closed, the emptying switching valve 1-5-1 is opened, the emptying pump 1-6 is started, and the emptying bin 1-1-A at the emptying section of the inner cavity of the cylinder 1-2 of the extractor of the continuous extraction subsystem 1 is emptied0 of air; closing the emptying switching valve 1-5-1 and closing the emptying pump 1-6;

(7) retracting a piston rod of the binning hydraulic cylinder 1-4-A, installing the bin to be loaded 1-1-A filled with the extracted substances between the binning hydraulic cylinder 1-4-A and an emptying bin 1-1-A-0 locked by the binning end locking device 1-3-A, extending the piston rod of the binning hydraulic cylinder 1-4-A and jacking the newly installed bin to be loaded 1-1-A; a piston rod of the bin unloading hydraulic cylinder 1-4-B is extended out and tightly props against the bin to be unloaded 1-1-B locked by the bin unloading end locking device 1-3-B; synchronously opening a bin loading end locking device 1-3-A and a bin unloading end locking device 1-3-B; synchronously and continuously extending a piston rod of a bin loading hydraulic cylinder 1-4-A and retracting a piston rod of a bin unloading hydraulic cylinder 1-4-B, loading the newly loaded bin 1-1-A to be loaded into the inner cavity of an extractor cylinder 1-2 of a continuous extraction subsystem 1 to form a new empty bin 1-1-A-0, loading the original empty bin 1-1-A-0 to form a new No. 1 level boosting or extracting bin 1-1-A-1-1, and so on until the original extraction section of the extraction bin 1-1-B-0 becomes a new bin 1-1-B to be unloaded; synchronously locking a bin loading end locking device 1-3-A and a bin unloading end locking device 1-3-B; retracting a piston rod of the bin unloading hydraulic cylinder 1-4-A, and unloading the ejected original bin 1-1-B to be unloaded;

(8) starting an emptying switching valve 1-5-1, starting an emptying pump 1-6, and emptying air in an emptying bin 1-1-A-0 at an inner cavity emptying section of an extractor cylinder 1-2 of a continuous extraction subsystem 1; closing the emptying switching valve 1-5-1 and closing the emptying pump 1-6;

(9) opening a drawing-back stop valve 1-5-3 and a drawing-back switching valve 1-5-2, enabling the supercritical fluid medium of a drawing-back bin 1-1-B-0 at the drawing-back section of an inner cavity of an extractor barrel 1-2 of a continuous extraction subsystem 1 to flow into an emptying bin 1-1-A-0 at the emptying section of the inner cavity of the extractor barrel 1-2 of the continuous extraction subsystem 1, opening a drawing-back compressor 1-7 after the pressure of the drawing-back bin 1-1-B-0 and the pressure of the emptying bin 1-1-A-0 are balanced until all the supercritical fluid medium in the drawing-back bin 1-1-B-0 is drawn back to the emptying bin 1-1-A-0, closing the drawing-back stop valve 1-5-3 and the drawing-back switching valve 1-5-2, closing the extraction compressor 1-7;

(10) repeating the steps (7) to (9) to periodically load the bin 1-1-A to be loaded with the unextracted extract into the continuous extraction subsystem 1, synchronously unloading the extracted bin 1-1-B to be unloaded out of the continuous extraction subsystem 1, in the process, each bin 1-1 of the inner cavity of the barrel 1-2 of the extractor of the continuous extraction subsystem 1 is sequentially positioned in an evacuation section, a step-by-step pressure increasing or extracting section, a step-by-step pressure decreasing section and a drawing-back section, the bin 1-1 which is continuously pushed finishes the evacuation of air in the evacuation section, the step-by-step supercritical fluid extraction of 1-to-N-stage pressure levels of the extracted matter is finished in the step-by-step pressure increasing or extracting section from 1-to N-stage, the step-by-step pressure decreasing of N-1 pressure levels is finished in the step-by-step pressure decreasing section, and the continuous operation of drawing back the supercritical fluid medium is finished in the drawing-back; the supercritical fluid extracted in the extraction completed bin 1-1 enters the corresponding grade 1 separation subsystem 3-1, the grade N-1 separation subsystem 3- (N-1) and the grade N ion system 3-N to start separation, periodically opening a double discharge valve 3-V-1 or a double discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the 1-level separation subsystem 3-1, the N-1-level separation subsystem 3- (N-1) and the N-level ion system 3-N, and discharging the extracts respectively separated by the 1-stage separation subsystem 3-1, the N-1 stage separation subsystem 3- (N-1) and the N-stage ion system 3-N.

The typical supercritical fluid medium is carbon dioxide, the highest supercritical carbon dioxide continuous extraction pressure is 32MPa, the pressure stage difference of each stage is 8MPa, the stage number N of a step-by-step boosting or extraction section in the supercritical fluid multistage continuous extraction separation device system is 4, and the supercritical fluid extraction temperature of each pressure stage, namely 8MPa, 16MPa, 24MPa and 32MPa, is 35-80 ℃; the primary separation pressure is 4-10 MPa, the separation temperature is 35-80 ℃, or the primary separation pressure is 6-10 MPa, the separation temperature is 35-80 ℃, the secondary separation pressure is 4-7 MPa, and the separation temperature is 35-80 ℃; each pressure stage pressurization circulation subsystem and each separation subsystem are respectively a 1-stage pressurization circulation subsystem 2-1, a 2-stage pressurization circulation subsystem 2-2, a 3-stage pressurization circulation subsystem 2-3, a 4-stage pressurization circulation subsystem 2-4, a 1-stage separation subsystem 3-1, a 2-stage ion system 3-2, a 3-stage separation subsystem 3-3 and a 4-stage separation subsystem 3-4; valves matched with each pressure stage supercharging circulation subsystem and each separation subsystem are respectively a 1-stage switching valve 6-1-1 of the 1-stage supercharging circulation subsystem 2-1, a 2-stage switching valve 6-1-2 of the 2-stage supercharging circulation subsystem 2-2 and a 3-stage supercharging circulation subsystemA 3-stage switching valve 6-1-3 of the system 2-3, a 4-stage switching valve 6-1-4 of the 4-stage pressurizing circulation subsystem 2-4, a 1-stage reflux valve 6-2-1 of the 1-stage separation subsystem 3-1, a 2-stage reflux valve 6-2-2 of the 2-stage ion system 3-2, a 3-stage reflux valve 6-2-3 of the 3-stage separation subsystem 3-3, and a 4-stage reflux valve 6-2-4 of the 4-stage separation subsystem 3-4; two bins 1-1 are respectively filled in the 1-stage to 4-stage pressure step-by-step boosting or extracting sections in the barrel 1-2 of the extractor of the continuous extraction subsystem 1, namely n₁＝n₂＝n₃＝n₄The other sections, namely, the emptying section, the 1-3-stage step-down section and the withdrawal section are respectively loaded into 1 bin 1-1 as 2.

Example two: a single-stage continuous extraction separation device and process flow of supercritical fluid are shown in FIG. 1, FIG. 2, FIG. 3, FIG. 4, FIG. 5, FIG. 6 and FIG. 7.

A supercritical fluid single-stage continuous extraction and separation device system is composed of a supercritical fluid medium source 5, a pressurization subsystem 4, a continuous extraction subsystem 1, a 1-stage separation subsystem 3-1 and …, an N-1-stage separation subsystem 3- (N-1), an N-stage ion system 3-N, a 1-stage pressurization circulation subsystem 2-1, …, an N-1-stage pressurization circulation subsystem 2- (N-1) and an N-stage pressurization circulation subsystem 2-N, wherein N is the total stage of step-by-step pressurization or extraction in the system, N is larger than 2, and supercritical fluid extraction and the Nth stage pressurization in the system are overlapped.

The supercritical fluid medium source 5 is constructed in the same manner as in the first embodiment.

The pressurizing subsystem 4 is constructed in the same way as the first embodiment.

The continuous extraction subsystem 1 is constructed as in the first embodiment, wherein:

from the loading end of the continuous extraction subsystem 1, the bins 1-1 loaded into the inner cavity of the extractor cylinder 1-2 of the continuous extraction subsystem 1 are numbered sequentially as follows: loading the materials into a storage bin 1-1-A; an emptying bin 1-1-A-0 of the emptying section; no. 1 grade boosting or extracting stock bin 1-1-A-1-1, … of step boosting or extracting section, No. 1N-1 grade boosting or extracting stock bin 1-1-A- (N-1) -1, No. 1N grade boosting or extracting stock bin 1-1-A-N-1, No. 2N grade boosting or extracting stock bin 1-1-A-N-2, …, N_NNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)_N-1)、n_NNumber N stage boost ORExtraction bin 1-1-A-N-N_N(ii) a The N-1-level pressure reduction bin 1-1-B- (N-1) and … of the step-by-step pressure reduction section and the 1-1-B-1 of the 1-level pressure reduction bin are arranged in the step-by-step pressure reduction section; a pumping-back bin 1-1-B-0 of the pumping-back section; and the materials are discharged out of the storage bin 1-1-B.

The 1-stage separation subsystem 3-1 to the N-1-stage separation subsystem 3- (N-1) is composed of a non-separation subsystem, wherein:

the non-separation subsystem is composed of a connecting pipe 7 made of stainless steel, the inlet of the pipe 7 is the inlet of the non-separation subsystem, and the outlet of the pipe 7 is the outlet of the non-separation subsystem.

The N-stage ion system 3-N is composed of a double-pressure swing separation subsystem or a double-pressure swing separation subsystem, and the constitution is the same as that of the first embodiment.

The 1-stage supercharging circulation subsystem 2-1 to the N-1-stage supercharging circulation subsystem 2- (N-1) is composed of a pump-free supercritical supercharging circulation subsystem, wherein:

the pump-free supercritical pressurizing circulation subsystem is composed of a circulation heat exchanger 2-HC and a one-way valve 2-CV, and the fluid flow materials are all stainless steel; the connection relationship of each component is as follows:

the inlet of the one-way valve 2-CV is the main inlet of the pump-free supercritical pressurizing circulation subsystem, the outlet of the one-way valve 2-CV is divided into two paths through a pipe 7, one path is connected with the inlet of the circulation heat exchanger 2-HC, the other path is the auxiliary inlet of the pump-free supercritical pressurizing circulation subsystem, and the outlet of the circulation heat exchanger 2-HC is the outlet of the pump-free supercritical pressurizing circulation subsystem.

The N-stage supercharging circulation subsystem 2-N is composed of a supercritical supercharging circulation subsystem, and the constitution of the supercritical supercharging circulation subsystem is the same as that of the first embodiment.

The connection relationship between the subsystems is the same as that in the first embodiment.

The extraction and separation process implemented by applying a supercritical fluid single-stage continuous extraction and separation device system comprises the following steps:

(1) the same as the step (1) of the embodiment;

(2) the same step (2) as the example;

(3) the same step (3) as the example;

(4) the same step (4) as the example;

(5) the 1-stage pressurizing circulation subsystems 2-1 and … and the N-1-stage pressurizing circulation subsystem 2- (N-1) are in an operating state, 1-stage pressurizing or extracting bin 1-1-A-1-1, … and 1-stage N-1 pressurizing or extracting bin 1-1-A- (N-1) -1 of the 1-stage to N-1-stage step-by-step pressurizing or extracting section in the continuous extracting subsystem 1 and the 1-stage separating subsystem 3-1, The N-1 stage separation subsystem 3- (N-1) is correspondingly communicated with the 1 stage pressurization circulation subsystems 2-1 and … and the N-1 stage pressurization circulation subsystem 2- (N-1), and the corresponding pressure stages of the boosting or extraction bins of each stage are kept unchanged; starting the N-stage pressurizing circulation subsystem 2-N, and continuously extracting N-stage step-by-step pressurizing in the subsystem 1 or No. 1N-stage pressurizing of the extraction section or No. 1-1-A-N-1 of the extraction bin 1-1-A-N-2, …, N_NNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)_N-1)、n_NN-grade boosting or extracting bin 1-1-A-N-N_NPerforming supercritical fluid extraction to obtain n_NSupercritical fluid in the N-stage boosting or extracting bins enters an N-stage ion system 3-N for separation, a double discharge valve 3-V-1 or a double discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the N-stage separation subsystem 3-N are periodically opened, and extract separated from the N-stage ion system 3-N is discharged;

(6) the same step (6) as in the example;

(7) the same procedure as in step (7);

(8) the same step (8) as in the example;

(9) the same step (9) as in example;

(10) repeating the step (7) to the step (9) to ensure that the bins 1-1-A to be filled with the unextracted extracted substances are periodically filled into the continuous extraction subsystem 1, the extracted bins 1-1-B to be discharged are synchronously discharged out of the continuous extraction subsystem 1, in the process, each bin 1-1 of the inner cavity of the extractor body 1-2 of the continuous extraction subsystem 1 is sequentially positioned in an emptying section, a step-by-step boosting or extracting section, a step-by-step pressure reduction section and a drawing-back section, the bin 1-1 which is continuously pushed finishes the emptying of air in an evacuating section, the step-by-step boosting of 1-level to N-1-level pressure levels in the step-by-step boosting or extracting section, and the supercritical fluid extraction of N-level pressure levels of the extracted substances in the step-by-step boosting or extracting section of N-level, The continuous operation of gradual decompression of N-1 pressure stages and the continuous operation of pumping back supercritical fluid medium in the gradual decompression section; the supercritical fluid extracted in the bin 1-1 after extraction enters an N-level ion system 3-N to start separation, a double discharge valve 3-V-1 or a double discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the N-level separation system 3-N are periodically opened, and the extract separated from the N-level ion system 3-N is discharged.

The typical supercritical fluid medium is carbon dioxide, the highest supercritical carbon dioxide continuous extraction separation pressure is 50MPa, the pressure stage difference of each stage is 10MPa, and the stage-by-stage boosting stage number N in the supercritical fluid single-stage continuous extraction separation device system is 5; the supercritical fluid pressure of 1-4 pressure levels is 10MPa, 20MPa, 30MPa and 40MPa, and the temperature is 35 ℃; the supercritical fluid extraction pressure of 5-stage pressure level is 50MPa, and the temperature is 35-80 ℃; the primary separation pressure is 4-10 MPa, the separation temperature is 35-80 ℃, or the primary separation pressure is 6-10 MPa, the separation temperature is 35-80 ℃, the secondary separation pressure is 4-7 MPa, and the separation temperature is 35-80 ℃; each pressure stage pressurization circulation subsystem and each separation subsystem are respectively a 1-stage pressurization circulation subsystem 2-1, a 2-stage pressurization circulation subsystem 2-2, a 3-stage pressurization circulation subsystem 2-3, a 4-stage pressurization circulation subsystem 2-4, a 5-stage pressurization circulation subsystem 2-5, a 1-stage separation subsystem 3-1, a 2-stage ion system 3-2, a 3-stage separation subsystem 3-3, a 4-stage separation subsystem 3-4 and a 5-stage separation subsystem 3-5; valves matched with each pressure stage pressurization circulation subsystem and each separation subsystem are respectively a 1-stage switching valve 6-1-1 of the 1-stage pressurization circulation subsystem 2-1, a 2-stage switching valve 6-1-2 of the 2-stage pressurization circulation subsystem 2-2, a 3-stage switching valve 6-1-3 of the 3-stage pressurization circulation subsystem 2-3, a 4-stage switching valve 6-1-4 of the 4-stage pressurization circulation subsystem 2-4, a 5-stage switching valve 6-1-5 of the 5-stage pressurization circulation subsystem 2-5, a 1-stage return valve 6-2-1 of the 1-stage separation subsystem 3-1, a 2-stage return valve 6-2-2 of the 2-stage ion subsystem 3-2, a 3-stage return valve 6-2-3 of the 3-stage separation subsystem 3, 4-stage reflux valves 6-2-4 of the 4-stage separation systems 3-4 and 5-stage reflux valves 6-2-5 of the 5-stage separation systems 3-5; 1-2 stage-by-stage pressure boosting or extraction section of 1-4 stage pressure in the barrel 1-2 of the extractor of the continuous extraction subsystem 1 is arranged in a bin 1-1Are all 1, i.e. n₁＝n₂＝n₃＝n₄The number of bins 1-1 into which the stepwise pressure boosting or extraction stages of 1, 5 pressure stages are loaded is 4, i.e. n₅The other sections, namely, the emptying section, the 1-4-stage step-down section and the withdrawal section are respectively loaded into 1 bin 1-1 as 4.

The invention overcomes the defect that the traditional supercritical fluid extraction device system can not continuously produce, realizes the continuous extraction and separation of the supercritical fluid, and has the advantages of reasonable process flow, high automation degree, reliable operation, energy saving, zero emission and excellent manufacturability.

Claims

1. A supercritical fluid continuous extraction separation device system is characterized by comprising a supercritical fluid medium source, a pressurization subsystem, a continuous extraction subsystem, a separation subsystem and a pressurization circulation subsystem, wherein the separation subsystem and the pressurization circulation subsystem are used for increasing the pressure step by step or are the same as the total extraction stage number N of the continuous extraction subsystem;

the supercritical fluid medium source consists of a liquefied storage tank, a cooler, a refrigerating unit, an outlet valve, a filling valve and a main return valve group; the cooler is arranged inside or outside the liquefied storage tank and connected with the refrigerating unit to form a cooling loop; an outlet valve is arranged at the outlet of the liquefied storage tank, and the outlet of the outlet valve is a supercritical fluid medium source outlet; the supercritical fluid medium source is provided with two inlets, one inlet is a main reflux valve inlet, the other inlet is a filling valve inlet, and a main reflux valve outlet and a filling valve outlet are connected to the inlet of the liquefied storage tank after being combined by a pipe;

the inlet of the cooler is the inlet of the pressurizing subsystem and is connected with the outlet of the supercritical fluid medium source, namely the outlet of the outlet valve, and the outlet of the cooler is connected with the inlet of the pressurizing pump through a pipe; the outlet of the pressurizing pump is divided into N branches by a pipe, the highest pressure level pipe branch of the pressurizing subsystem is divided into two branches, one branch is the highest pressure level outlet of the pressurizing subsystem, and the other branch is connected with the inlet of the overflow valve; the other N-1 branches are correspondingly connected with the inlets of the pressure reducing valves of all pressure levels through pipes, and the outlets of the pressure reducing valves are the outlets of the pressurizing subsystems of all pressure levels except the highest pressure level; the outlet of the overflow valve is connected to the pipe between the outlet of the cooler and the inlet of the pressure pump through the pipe; the number of outlets of the pressurizing subsystem, namely the number of the reducing valves and the overflow valves is the same as the step-by-step pressure increasing or total extraction step number of the continuous extraction subsystem;

the outer wall of the extractor barrel is coated with an insulating layer;

the inlet of a heavy pressure regulating valve is the inlet of a heavy pressure swing separation subsystem, the outlet of the heavy pressure regulating valve is connected with the inlet of a heavy heat exchanger through a pipe, the outlet of the heavy heat exchanger is connected with the inlet of a heavy separator through a pipe, the outlet of the heavy separator is the outlet of the heavy pressure swing separation subsystem, and the heavy separator is provided with an extract outlet and is provided with a heavy discharge valve;

the inlet of a heavy pressure regulating valve is the inlet of a double pressure-variable separation subsystem, the outlet of the heavy pressure regulating valve is connected with the inlet of a heavy heat exchanger through a pipe, the outlet of the heavy heat exchanger is connected with the inlet of a heavy separator through a pipe, the outlet of a heavy pressure-variable extractor is connected with the inlet of a double pressure regulating valve through a pipe, the outlet of the double pressure regulating valve is connected with the inlet of the double heat exchanger through a pipe, the outlet of the double heat exchanger is connected with the inlet of the double separator through a pipe, the outlet of the double separator is the outlet of the double pressure-variable separation subsystem, the heavy separator and the double separator are respectively provided with an extract outlet and are provided with a;

the non-separation subsystem consists of a pipe for connection, the inlet of the pipe for connection is the inlet of the non-separation subsystem, and the outlet of the pipe for connection is the outlet of the non-separation subsystem;

the low-pressure medium inlet of the pressure-variable heat exchanger is a main inlet of the supercritical pressurizing circulation subsystem, the low-pressure medium outlet of the pressure-variable heat exchanger is connected with the inlet of the circulation condenser through a pipe, the outlet of the circulation condenser is connected with the inlet of the circulation pump through a pipe, the pipe between the outlet of the circulation condenser and the inlet of the circulation pump is provided with an auxiliary inlet of the supercritical pressurizing circulation subsystem, the outlet of the circulation pump is connected with the high-pressure medium inlet of the pressure-variable heat exchanger through a pipe, the high-pressure medium outlet of the pressure-variable heat exchanger is connected with the inlet;

the inlet of the one-way valve is a main inlet of the pumpless supercritical supercharging circulation subsystem, the outlet of the one-way valve is respectively connected with the inlet of the circulation heat exchanger and an auxiliary inlet of the pumpless supercritical supercharging circulation subsystem through pipes, and the outlet of the circulation heat exchanger is an outlet of the pumpless supercritical supercharging circulation subsystem;

the connection relationship among the subsystems is as follows:

2. Extraction separation process implemented by using supercritical fluid continuous extraction separation device system according to claim 1， The method comprises the following steps: