CN110152350B - Subcritical fluid continuous isobaric extraction separation device system and extraction separation process - Google Patents

Subcritical fluid continuous isobaric extraction separation device system and extraction separation process Download PDF

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CN110152350B
CN110152350B CN201910575431.3A CN201910575431A CN110152350B CN 110152350 B CN110152350 B CN 110152350B CN 201910575431 A CN201910575431 A CN 201910575431A CN 110152350 B CN110152350 B CN 110152350B
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subsystem
outlet
inlet
bin
pressure
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CN110152350A (en
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王威强
李飞
曲延鹏
李爱菊
李冠忠
李守军
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Shandong Shuangchao Biological Equipment Technology Co ltd
Shandong University
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Shandong Shuangchao Biological Equipment Technology Co ltd
Shandong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0203—Solvent extraction of solids with a supercritical fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/028—Flow sheets
    • B01D11/0284—Multistage extraction

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  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention relates to the field of chemical separation and bioengineering mechanical equipment, in particular to a subcritical fluid continuous isobaric extraction separation device system and an extraction separation process. The extraction separation process implemented by the device system is characterized in that subcritical fluid or supercritical fluid extracted in a storage bin after extraction enters a corresponding separation subsystem to start separation through process operation of the system, a discharge valve is periodically opened, and extract separated by the separation subsystem is discharged. The technical device has high automation degree, reliable operation and reasonable device system process flow, realizes continuous equal-sub extraction separation of subcritical fluid, saves energy, has zero discharge, and has excellent manufacturability and excellent separation effect.

Description

Subcritical fluid continuous isobaric 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 subcritical fluid continuous isobaric extraction separation device system and an extraction separation process.
Second, technical background
The subcritical fluid extraction separation technology is another green chemical technology following the supercritical fluid extraction separation technology, and is being widely applied to the field of extraction separation. However, most of the existing subcritical 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 'subcritical fluid extraction device and method of natural product effective components' is granted by the patent office of the national intellectual property office in 2012, 5, 30, month and the name of CN101912696B, and discloses a subcritical fluid extraction device, wherein a leaching system part of the device comprises a single extraction tank, an evaporation tank, a condenser, a solvent tank, a compressor and the like; the device is a subcritical extraction device operated intermittently, after extraction is finished each time, residual subcritical fluid in an extracted substance in an extraction tank is subjected to reduced pressure evaporation by a compressor, after the pressure of the extraction tank is reduced to 0MPa, negative pressure evaporation is carried out by a vacuum pump until the pressure is reduced to be below-0.09 MPa, an extraction tank opening is opened, and residues are taken out. For a subcritical fluid continuous extraction device in a multi-kettle parallel connection mode, the subcritical fluid continuous extraction device is essentially intermittent operation, and although the production efficiency is improved to a certain extent, the subcritical fluid continuous extraction device still has the defects of low efficiency, low safety and reliability, high energy consumption, high extraction solvent loss and the like.
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 subcritical fluid extraction device and provides a subcritical fluid continuous isobaric extraction separation device system and an extraction separation process.
The technical scheme of the subcritical fluid continuous isobaric extraction separation device system comprises a subcritical 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 the same as the step-by-step pressure boosting or total extraction stage number N of the continuous extraction subsystem.
The subcritical 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 connection relationship of each component is as follows:
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 an outlet of the liquefaction storage tank, and the outlet of the outlet valve is a subcritical fluid medium source outlet; the subcritical fluid medium source has two inlets, one is a main reflux valve inlet, the other 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 through a pipe.
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 subcritical fluid medium source, namely the outlet valve outlet, through a pipe, 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 all the pressure reducing valves are the outlets of the pressurizing subsystems of all the 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 switching valve, a drawing stop valve, an emptying pump, 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, the two ends of the cylinder are respectively provided with a loading end barrel end part and a unloading end barrel end part with circular flanges, the outer wall of the cylinder is provided with a heat exchange sleeve, the inner cavity of the extraction device barrel is axially divided into a emptying section, a step-by-step boosting or extraction section with the number of steps not less than 2, a step-by-step depressurization 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 drawing-back 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 isobaric pressure separation subsystem, or a double variable pressure separation subsystem, or a non-separation subsystem, wherein:
the heavy isobaric separation subsystem consists of an isobaric heat exchanger, a heavy heater and a heavy separator; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger is a heavy isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger is connected with the inlet of a heavy heater through a pipe, the outlet of the heavy heater is connected with the inlet of a heavy separator through a pipe, the outlet of the heavy separator is connected with the high-temperature medium inlet of the isobaric heat exchanger through a pipe, the high-temperature medium outlet of the isobaric heat exchanger is the outlet of the heavy isobaric separation subsystem, and the heavy separator is provided with an extract outlet and is provided with a heavy discharge valve.
The dual isobaric separation subsystem consists of an isobaric heat exchanger, a reheater, a heavy separator, a dual heater and a dual separator; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger is a double isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger is connected with a heavy heater inlet through a pipe, the heavy heater outlet is connected with a heavy separator inlet through a pipe, the heavy separator outlet is connected with a double heater inlet through a pipe, the double heater outlet is connected with a double separator inlet through a pipe, the double separator outlet is connected with a high-temperature medium inlet of the isobaric heat exchanger through a pipe, the high-temperature medium outlet of the isobaric heat exchanger is a double isobaric separation subsystem outlet, and the heavy separator and the double separator are respectively provided with an extract outlet and are respectively provided with a double discharge valve and a double discharge valve.
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 subcritical supercharging circulation subsystem, a supercritical supercharging circulation subsystem, a pumpless subcritical supercharging circulation subsystem or a pumpless supercritical supercharging circulation subsystem, wherein:
the subcritical pressurizing circulation subsystem consists of a voltage stabilizer, a circulating pump and a circulating condenser; the connection relationship of each component is as follows:
the inlet of the circulating condenser is a main inlet of the subcritical pressurizing circulating subsystem, the outlet of the circulating condenser is connected with the inlet of the circulating pump through a pipe, an auxiliary inlet of the subcritical pressurizing circulating subsystem is arranged between the outlet of the circulating condenser and the inlet of the circulating pump through the pipe, the outlet of the circulating pump is divided into two paths, one path is connected with the inlet and the outlet of the pressure stabilizer through the pipe, and the other path is the outlet of the subcritical pressurizing circulating subsystem.
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 subcritical pressurizing circulation subsystem consists of a voltage stabilizer 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 pump-free subcritical pressurizing circulation subsystem, the outlet of the one-way valve is divided into three paths through a pipe, the first path is connected with the inlet and the outlet of the pressure stabilizer, the second path is an auxiliary inlet of the pump-free subcritical pressurizing circulation subsystem, and the third path is an outlet of the pump-free subcritical pressurizing circulation subsystem.
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 pump-free supercritical pressurizing circulation subsystem, the outlet of the one-way valve is divided into two paths through a pipe, the first path is connected with the inlet of the circulation heat exchanger, the second path is an auxiliary inlet of the pump-free supercritical pressurizing circulation subsystem, and the outlet of the circulation heat exchanger is an outlet of the pump-free supercritical pressurizing circulation subsystem.
The connection relationship among the subsystems is as follows:
the outlet of the subcritical fluid medium source is connected with the inlet of the pressurizing subsystem through a pipe, the outlet of each stage of pressurizing subsystem is connected with the corresponding auxiliary inlet of the pressurizing circulation subsystem through a pipe, the main inlet of each stage of pressurizing circulation subsystem is connected with the outlet of each corresponding 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 subcritical 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 each stage and the subcritical fluid medium source inlet are provided with emptying valves.
The extraction and separation process implemented by applying the subcritical fluid continuous isobaric extraction and separation device system comprises the following steps:
(1) emptying a liquefaction storage tank of a subcritical fluid medium source, filling the subcritical fluid medium according to the specification, starting a refrigerating unit, and liquefying the subcritical 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 subcritical fluid medium source inlet, opening reflux valves of all separation subsystems, closing switching valves of all pressurization circulation subsystems, opening emptying valves, opening outlet valves at subcritical fluid medium source outlets, 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 subcritical fluid or 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) starting a withdrawal stop valve and a withdrawal switching valve, enabling subcritical fluid or supercritical fluid medium of a bin at a withdrawal section of an inner cavity of an extractor cylinder of the continuous extraction subsystem to flow into a bin at an evacuation section of the inner cavity of the extractor cylinder of the continuous extraction subsystem, starting a withdrawal compressor after pressure of the bin at the withdrawal section and the pressure of the bin at the evacuation section are balanced until all subcritical fluid or supercritical fluid medium in the bin at the withdrawal section is withdrawn into the bin at the evacuation section, closing the withdrawal stop valve and the withdrawal switching valve, and closing the withdrawal compressor;
(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 bins after extraction are synchronously unloaded out of the continuous extraction subsystem, and in the process, each bin in the inner cavity of the extractor body 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 drawing-back 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 drawing-back of subcritical fluid medium in the bins is sequentially completed in each working section; and (3) the subcritical fluid or supercritical fluid dissolved with the extract in the extraction completed bin enters a corresponding separation subsystem to start separation, and the discharge valve is periodically opened to discharge the extract separated by the separation subsystem.
The invention has the following beneficial effects: the pressurizing circulation subsystem has a subcritical-state and supercritical-state fluid conveying mode, the separation subsystem has supercritical-state and subcritical-state fluid separation conditions which can be selected, and the process flow is simple, convenient and flexible; 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 subcritical extraction pressure of the continuous extraction subsystem is the same as the separation pressure of the separation subsystem, so that the power consumption that the pressure reduction separation is needed after the extraction and the pressure increase extraction is needed after the separation is eliminated; the subcritical fluid medium is recycled in the extraction and separation operations, the subcritical fluid medium discharged out of the storage bin is recycled, and the consumption of the subcritical fluid medium is effectively reduced; the separated supercritical fluid exchanges heat with the subcritical fluid before separation before circulating pressurization; or, during supercritical fluid extraction, the separated gaseous subcritical fluid medium is cooled before being condensed and the pressurized liquid subcritical fluid medium is cooled, so that the heat and cold consumption of the system is effectively reduced. The device has the advantages of reasonable process flow of the device system, high automation degree of the device, reliable operation of the device system, energy conservation, zero emission and excellent manufacturability.
Description of the drawings
FIG. 1 is a schematic structural diagram of a subcritical fluid continuous isobaric extraction separation device system according to the present invention;
FIG. 2 is a schematic diagram of the subcritical boost cycle subsystem shown at 2-1, …, 2- (N-1), 2-N in FIG. 1;
FIG. 3 is a schematic diagram of the supercritical boost cycle subsystem shown at 2-1, …, 2- (N-1), 2-N in FIG. 1;
FIG. 4 is a schematic diagram of the pumpless subcritical boost cycle subsystem shown at 2-1, …, 2- (N-1), 2-N in FIG. 1;
FIG. 5 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. 6 is a schematic diagram of a heavy isobaric pressure separation subsystem shown at 3-1, …, 3- (N-1), 3-N in FIG. 1;
FIG. 7 is a schematic diagram of the dual isobaric separation subsystem shown at 3-1, …, 3- (N-1), 3-N in FIG. 1;
FIG. 8 is a schematic diagram of a single PSR subsystem shown at 3-1, …, 3- (N-1), 3-N in FIG. 1;
FIG. 9 is a schematic diagram of the double-transformer separation subsystem shown at 3-1, …, 3- (N-1) and 3-N in FIG. 1;
FIG. 10 is a schematic diagram of the non-separation sub-systems shown at 3-1, …, 3- (N-1), and 3-N in FIG. 1;
fig. 11 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. a continuous extraction subsystem 1-1, a storage bin 1-1-1 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-n11 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) -NN-1N-1 stage boosting nthN-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 binN-1), N-stage boosting (N)N-1) stock bins 1-1-A-N-NNN-th step up voltageN1-1-B bin, 1-1-B-0 bin to be discharged and pumping back material1-1-B-1 bin, 1-1-B- (N-1) level decompression bin, 1-2 level extraction barrel, 1-2-A loading end barrel end, 1-2-B level unloading end barrel end, 1-2-1 level fluid inlet and outlet, 1-2-3 level fluid inlet and outlet, 1-2-4 level fluid outlet, 1-2-5 level fluid balance inlet and outlet, 1-3-A level fluid return port, 1-3-B level loading end locking device, 1-4-A level unloading end locking device, 1-4-B level loading hydraulic cylinder, 1-5-1 level unloading hydraulic cylinder, 1-1 level decompression bin, 1-2 level fluid inlet and outlet, 1-2-B level fluid balance inlet and outlet, 1-3-A level fluid return port, 1-3-B level loading end, 1-5-2 parts of evacuation switching valve, 1-5-3 parts of draw-back switching valve, 1-6 parts of draw-back stop valve, 1-7 parts of evacuation pump, 1-8 parts of draw-back 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 2-B part of N-1-stage supercharging circulation subsystem, 2-C part of voltage stabilizer, 2-CV part of circulation condenser, 2-E part of one-way valve, 2-HC part of pressure-changing heat exchanger, 2-P part of circulation heat exchanger, 3-1 part of circulation pump, 1-stage separation subsystem, 3- (N-1), 3-N, N-stage separation subsystem 3-E part of N-1-stage separation subsystem, an isobaric heat exchanger 3-H-1, a heavy heater 3-H-2, a double heater 3-HC-1, a heavy heat exchanger 3-HC-2, a double heat exchanger 3-S-1, a heavy separator 3-S-2, a double separator 3-V-1, a heavy discharge valve 3-V-2, a double discharge valve 3-VC-1, a heavy pressure regulating valve 3-VC-2, a double pressure regulating valve 4, a pressurizing subsystem 4-1, a cooler 4-2, a booster pump 4-3-1, a 1-stage pressure reducing valve 4-3- (N-1), an N-1-stage pressure reducing valve 4-4, an overflow valve 5, a subcritical fluid medium source 5-1, a sub-critical fluid medium source 3-H-2, 5-2 parts of liquefied storage tank, 5-3 parts of cooler, 5-4-1 parts of refrigerating unit, 5-4-2 parts of filling valve, 5-4-3 parts of outlet valve, 6-0 parts of total reflux valve, 6-1-1 parts of emptying valve, 6-1- (N-1) parts of 1-stage switching valve, 6-1-N, N parts of N-1-stage switching valve, 6-2-1 parts of 1-stage reflux valve, 6-2- (N-1) parts of N-1-stage reflux valve, 6-2-N, N parts of N-1-stage reflux 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 subcritical fluid multi-stage continuous isobaric extraction separation device system and a process flow are shown in figures 1, 2, 6, 7 and 11.
A subcritical fluid multi-stage continuous isobaric extraction and separation device system is composed of a subcritical fluid medium source 5, a pressurizing subsystem 4, a continuous extraction subsystem 1, a 1-stage separation subsystem 3- (N-1), an N-stage ion system 3-N, a 1-stage pressurizing circulation subsystem 2-1, …, an N-1-stage pressurizing circulation subsystem 2- (N-1) and an N-stage pressurizing circulation subsystem 2-N, wherein N is the step-by-step boosting or the total extraction stage in the system, N is larger than 2, and the step-by-step extraction and the step-by-step boosting of subcritical fluid in the system are coincided.
The subcritical 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 valve 5-4-2 is arranged at an outlet of the liquefaction storage tank 5-1, and an outlet of the outlet valve 5-4-2 is an outlet of the subcritical fluid medium source 5; subcritical fluid medium source 5 has two inlets, one is total reflux valve 5-4-3 inlet, another is filling valve 5-4-1 inlet, and total reflux valve 5-4-3 outlet and filling valve 5-4-1 outlet are combined by means of pipe 7, and connected to inlet of 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 subcritical fluid medium source 5 through a pipe 7, namely the outlet valve 5-4-2, 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 stock 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 pumping switching valve 1-5-2, a pumping stop valve 1-5-3, a pumping pump 1-6, a pumping compressor 1-7 and a sealing ring 1-1-6; 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 inner cavity of the barrel 1-2 of the extractor of the continuous extraction subsystem 1 is filled with a bin 1-1, and each stage of pressure boosting or extraction section is filled with at least one bin 1-1; 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-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, …, NN-1No. 1N-1 grade boosting or extracting bin 1-1-A- (N-1) - (N)N-1-1)、nN-1N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -NN-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, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NN(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 body 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 body 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 adjacent 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 step-by-step pressure increase or extraction section adjacent to the emptying section, namely a fluid inlet 1-2-2 of the 1 st step-by-step pressure increase or extraction 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 step-by-step pressure increase or extraction section of the next evacuation section, namely a fluid inlet 1-2-2 of the 2 nd step-by-step pressure increase or extraction section through a pipe 7, and by analogy, 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 of the step-by-step pressure increase or extraction section is reduced by 1 through;
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 isobaric separation subsystem or a double isobaric separation subsystem, wherein:
the heavy isobaric separation subsystem consists of an isobaric heat exchanger 3-E, a heavy heater 3-H-1 and a heavy separator 3-S-1, and the fluid overflowing materials are stainless steel; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger 3-E is a heavy isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger 3-E is connected with the heavy heater 3-H-1 inlet through a pipe 7, the heavy heater 3-H-1 outlet is connected with the heavy separator 3-S-1 inlet through a pipe 7, the heavy separator 3-S-1 outlet is connected with the high-temperature medium inlet of the isobaric heat exchanger 3-E through a pipe 7, the high-temperature medium outlet of the isobaric heat exchanger 3-E is a heavy isobaric separation subsystem outlet, and 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 isobaric separation subsystem consists of an isobaric heat exchanger 3-E, a reheater 3-H-1, a heavy separator 3-S-1, a double heater 3-H-2 and a double separator 3-S-2, and the fluid overflowing materials are stainless steel; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger 3-E is a double isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger 3-E is connected with the inlet of a heavy heater 3-H-1 through a pipe 7, the outlet of the heavy heater 3-H-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 connected with the inlet of a double heater 3-H-2 through a pipe 7, the outlet of the double heater 3-H-2 is connected with the inlet of a double separator 3-S-2 through a pipe 7, the outlet of the double separator 3-S-2 is connected with the high-temperature medium inlet of the isobaric heat exchanger 3-E through a pipe 7, the high-temperature medium outlet of the isobaric heat exchanger 3-E is the, the first separator 3-S-1 and the second separator 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 subcritical supercharging circulation subsystems, wherein:
the subcritical pressurizing circulation subsystem is composed of a voltage stabilizer 2-B, a circulating pump 2-P and a circulating condenser 2-C, and the fluid overflowing material is stainless steel; the connection relationship of each component is as follows:
the inlet of the circulating condenser 2-C is a main inlet of the subcritical pressurizing circulating subsystem, the outlet of the circulating condenser 2-C is connected with the inlet of the circulating pump 2-P through a pipe 7, the pipe 7 between the outlet of the circulating condenser 2-C and the inlet of the circulating pump 2-P is provided with a secondary inlet of the subcritical pressurizing circulating subsystem, the outlet of the circulating pump 2-P is divided into two paths, one path is connected with the inlet and the outlet of the pressure stabilizer 2-B through the pipe 7, and the other path is an outlet of the subcritical pressurizing circulating subsystem.
The connection relationship among the subsystems is as follows:
an outlet of a subcritical fluid medium source 5, namely an outlet valve 5-4-2 outlet is connected with an inlet of a pressurizing subsystem 4 through a pipe 7, the pressurizing subsystem 4 is provided with N outlets corresponding to the continuous extraction subsystem, each outlet is respectively connected with a corresponding 1-stage pressurizing circulation subsystem 2-1, …, an N-1-stage pressurizing circulation subsystem 2- (N-1) and an auxiliary inlet of an N-stage pressurizing circulation subsystem 2-N through a pipe 7, the 1-stage pressurizing circulation subsystems 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 a corresponding 1-stage separation subsystem 3-1, a corresponding 1-stage separation subsystem 2-N through a pipe 7, a 1-stage switching valve 6-1, a corresponding …, a corresponding N-stage switching valve 6-1- (N-1), and a corresponding, …, 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 outlets of corresponding pressure stages 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 inlets of 1-stage reflux valves 6-2-1 and …, N-1-stage reflux valve 6-2- (N-1), N-stage reflux valve 6-2-N and the same subcritical 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, and the connecting pipelines corresponding to the outlet of the reflux valve and the inlet of the subcritical fluid medium source of each stage of the separation subsystem are provided with emptying valves 6-0.
The extraction and separation process applying the subcritical fluid multistage continuous isobaric extraction and separation device system comprises the following steps:
(1) emptying a liquefaction storage tank 5-1 of a subcritical fluid medium source 5, filling the subcritical fluid medium according to the specification, starting a refrigerating unit 5-3, and liquefying the subcritical 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 main reflux valve 5-4-3 at an inlet of a subcritical 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), opening 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 circulation subsystem 2-1, an N-1-stage switching valve 6-1- (N-1) of the N-1-stage pressurization circulation subsystem 2- (N-1) and an N-stage switching valve 6-1-N of the N-stage pressurization circulation subsystem 2-N, opening an exhaust valve 6-0, opening an outlet valve 5-4-2 at the outlet of a subcritical fluid medium source 5, and discharging air in the continuous extraction subsystem 1 and the stage-1 separation subsystem 3-1, the stage-1 separation subsystem 3- (N-1) and the stage-N ion system 3-N; 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, …, NN-1No. 1N-1 grade boosting or extracting bin 1-1-A- (N-1) - (N)N-1-1)、nN-1N-1 grade pressure boosting or extracting bin 1-1-A- (N-1) -NN-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, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NNPerforming corresponding subcritical fluid step-by-step extraction, enabling subcritical fluid in each boosting or extraction section bin which completes extraction to enter a corresponding 1-stage separation subsystem 3-1, the right, 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 matched with the 1-stage separation subsystem 3-1, the right, 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-NNWhen the extraction process time is up, 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 extractor cylinder of the continuous extraction subsystem 1 is emptiedThe emptying bin 1-1-A-0 of the emptying section of the inner cavity of the body 1-2 is filled with 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 draw-back stop valve 1-5-3 and a draw-back switching valve 1-5-2, enabling subcritical fluid or supercritical fluid medium of a draw-back bin 1-1-B-0 at an inner cavity draw-back section of an extractor cylinder 1-2 of a continuous extraction subsystem 1 to flow into an emptying bin 1-1-A-0 at an inner cavity emptying section of the extractor cylinder 1-2 of the continuous extraction subsystem 1, after pressure balance between the draw-back bin 1-1-B-0 and the emptying bin 1-1-A-0, opening a draw-back compressor 1-7 until all subcritical fluid medium in the draw-back bin 1-1-B-0 is drawn back to the emptying bin 1-1-A-0, closing the draw-back stop valve 1-5-3 and the draw-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 extractor barrel 1-2 of the continuous extraction subsystem 1 is sequentially positioned in an evacuation section, a step-by-step pressure boosting or extracting section, a step-by-step pressure reducing 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 extraction of subcritical fluid of 1-to-N-stage pressure stages of an extracted substance in the step-by-step pressure boosting or extracting section from 1-to-N stages, the step-by-step pressure reduction of N-1 pressure stages in the step-by-step pressure reducing section and the continuous operation of drawing back the subcritical fluid medium in the drawing-back section; subcritical fluid after extraction in the extraction completed silo 1-1 enters a corresponding 1-stage separation subsystem 3-1, an N-1-stage separation subsystem 3- (N-1) and an N-stage 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 subcritical fluid medium is carbon dioxide, the highest subcritical carbon dioxide continuous isobaric extraction separation pressure is 32MPa, the stage difference of each stage of pressure is 8MPa, the stage number N of a step-by-step boosting or extraction section in the subcritical fluid multistage continuous isobaric extraction separation device system is 4, and each pressure stage is that the extraction temperature of the subcritical fluid of 8MPa, 16MPa, 24MPa and 32MPa is 32 ℃, the one-time separation temperature is 35 ℃ or the one-time separation temperature is 35 ℃ and the two-time separation temperature is 40 ℃; 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; the valves matched with each pressure stage supercharging circulation subsystem and the 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 switching valve 6-1 of the 3-stage supercharging circulation subsystem 2-3-3, 4-stage switching valves 6-1-4 of the 4-stage pressurized circulation subsystem 2-4 and 1-stage reflux valves 6-2-1 of the 1-stage separation subsystem 3-1, 2-stage reflux valves 6-2-2 of the 2-stage ion system 3-2, 3-stage reflux valves 6-2-3 of the 3-stage separation subsystem 3-3, 4-stage reflux valves 6-2-4 of the 4-stage separation system 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 subcritical fluid single-stage continuous isobaric extraction separation device system and a process flow are shown in figure 1, figure 2, figure 4, figure 6, figure 7, figure 10 and figure 11.
A subcritical fluid single-stage continuous isobaric extraction and separation device system is composed of a subcritical fluid medium source 5, a pressurizing 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 pressurizing circulation subsystem 2-1 and …, an N-1-stage pressurizing circulation subsystem 2- (N-1) and an N-stage pressurizing circulation subsystem 2-N, wherein N is the step-by-step pressurizing or total extraction stage number in the system, N is larger than 2, and subcritical fluid extraction in the system is overlapped with the step-by-step pressurizing Nth pressure stage.
The subcritical fluid medium source 5 is constructed as in embodiment one.
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, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NN(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 isobaric separation subsystem or a double isobaric separation subsystem, and the constitution of the N-stage ion system 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 subcritical supercharging circulation subsystem, wherein:
the pump-free subcritical pressurizing circulation subsystem is composed of a voltage stabilizer 2-B and a one-way valve 2-CV, and the fluid overflowing materials are all stainless steel; the connection relationship of each component is as follows:
the inlet of the one-way valve 2-CV is a main inlet of the pumpless subcritical supercharging circulation subsystem, the outlet of the one-way valve 2-CV is divided into three paths through a pipe 7, the first path is connected with the inlet and the outlet of the voltage stabilizer 2-B, the second path is an auxiliary inlet of the pumpless subcritical supercharging circulation subsystem, and the third path is an outlet of the pumpless subcritical supercharging circulation subsystem.
The N-stage supercharging circulation subsystem 2-N is composed of a subcritical supercharging circulation subsystem, and the structure of the subcritical 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 of the technical scheme of the embodiment 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) 1-stage supercharging circulation subsystem 2-1, … and N-1 stage supercharging circulationThe ring subsystem 2- (N-1) is in an operating state, the 1 st-stage boosting or extraction bin 1-1-A-1- … of the 1 st-stage boosting or extraction section from 1 st stage to N-1 st stage in the continuous extraction subsystem 1, the 1 st-stage boosting or extraction bin 1-1-A- (N-1) -1 is correspondingly communicated with the 1 st-stage separation subsystem 3-1, the N-1 st-stage separation subsystem 3- (N-1) and the 1 st-stage boosting circulation subsystem 2-1, … and the N-1 st-stage boosting circulation subsystem 2- (N-1), and the corresponding pressure stages of the boosting or extraction bins in all stages 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, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NNPerforming subcritical fluid extraction to finish n of extractionNSubcritical 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 cylinder 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 reducing 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 a step-by-step boosting or extracting section, and the subcritical fluid extraction of N-level pressure levels of the extracted substances in the step-by-step boosting or extracting section of N-level, The step-by-step pressure reduction of N-1 pressure stages is completed in the step-by-step pressure reduction section, and the continuous operation of the extraction of the subcritical fluid medium is completed in the extraction section; and (3) the subcritical fluid after extraction in the bin 1-1 which finishes 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 subsystem 3-N are periodically opened, and the extract separated from the N-level ion system 3-N is discharged.
The typical subcritical fluid medium is carbon dioxide, the subcritical carbon dioxide continuous isobaric extraction separation pressure is 50MPa, the step-by-step boosting stage number N in the subcritical fluid single-stage continuous isobaric extraction separation device system is 5, the step-by-step boosting stage number N is from 1 to N-1 pressure stages, namely, the subcritical fluid temperature of 10MPa, 20MPa, 30MPa and 40MPa is 32 ℃, the subcritical fluid temperature of N-stage pressure stages, namely 50MPa, is 32 ℃, the primary separation temperature is 35 ℃ or the primary separation temperature is 35 ℃ and the secondary separation temperature is 40 ℃; 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 bin 1-1 filled with 1-stage to 4-stage pressure step-by-step boosting or extraction section in the barrel 1-2 of the extractor of the continuous extraction subsystem 1, namely n1＝n2＝n3＝n4The stock bin 1-1 in which the step-by-step boosting or extracting section with 1, 5 pressure stages is loaded is 4I.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.
Example three: a supercritical fluid pre-extracted subcritical fluid multistage continuous isobaric extraction separation device system and process flow are shown in FIG. 1, FIG. 2, FIG. 3, FIG. 6, FIG. 7, FIG. 8, FIG. 9 and FIG. 11.
A supercritical fluid pre-extraction subcritical fluid multistage continuous isobaric extraction separation device system is composed of a subcritical fluid medium source 5, a pressurizing subsystem 4, a continuous extraction subsystem 1, 1-stage separation subsystems 3-1 and …, an N-1-stage separation subsystem 3- (N-1), an N-stage ion system 3-N, 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, wherein N is a step-by-step boosting or total extraction stage number in the system, N is larger than 2, and step-by-step extraction and step-by-step boosting of supercritical fluid and subcritical fluid in the system are overlapped.
The subcritical fluid medium source 5 is constructed as in embodiment one.
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.
The 1-stage separation subsystem 3-1 is composed of a double-transformation separation subsystem or a double-transformation 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 2-stage separation subsystem 3-2 to the N-stage ion system 3-N is composed of a double isobaric separation subsystem or a double isobaric separation subsystem, and the structure of the double isobaric separation subsystem or the double isobaric separation subsystem is the same as that of the first embodiment.
The 1-stage supercharging circulation subsystem 2-1 is composed of a supercritical supercharging circulation subsystem, 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 2-stage supercharging circulation subsystem to the N-stage supercharging circulation subsystem 2-N are composed of subcritical supercharging circulation subsystems, and the subcritical supercharging circulation subsystems are the same as the first embodiment.
The connection relationship between the subsystems is the same as that in the first embodiment.
The extraction and separation process of the technical scheme of the embodiment 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) starting a 1-stage pressurizing circulation subsystem 2-1, and continuously extracting 1-stage step-by-step pressurizing or No. 1-stage pressurizing or extracting bins 1-1-A-1-1 and No. 2 1-stage pressurizing or extracting bins 1-1-A-1-2, … … and n in the 1-stage pressurizing circulation 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-n1Is correspondingly communicated with a 1-stage separation subsystem 3-1 and a 1-stage pressurization circulation subsystem 2-1 to perform supercritical fluid extraction, and the 1 # 1-stage pressure boosting or extraction stock bins 1-1-A-1-1 and 2 # 1-stage pressure boosting or extraction stock bins 1-1-A-1-2, … … and n for completing extraction1No. 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-n1The supercritical fluid in the system enters a 1-stage separation subsystem 3-1 for separation, a heavy discharge valve 3-V-1 or a heavy discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the 1-stage separation subsystem 3-1 are periodically opened, and the extract separated by the 1-stage separation subsystem 3-1 is discharged; 2-2, …, N-1 stage pressurizing circulation subsystem 2- (N-1) and N stage pressurizing circulation subsystem 2-N are started, 2-to-N stage stepwise pressurizing or No. 2 stage pressurizing of extraction section 1 or No. 2 stage pressurizing or extraction bins 1-1-A-2-1 and No. 2 stage pressurizing or extraction bins 1-1-A-2-2, … and N in the continuous extraction subsystem 12No. 12 stage boosting or extracting bin 1-1-A-2- (n)2-1)、n2No. 2 grade pressure boosting or extracting bin 1-1-A-2-n2…, number 1N-1-level pressure boosting or extraction bin 1-1-A- (N-1) -1, No. 2N-1 level pressure boosting or extraction bin 1-1-A- (N-1) -2, …, NN-1No. 1N-1 grade boosting or extracting bin 1-1-A- (N-1) - (N)N-1-1)、nN-1No. N-1 grade pressure boosting or extracting storage bin 1-1-A- (N-1) - (N)N-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, …, NNNo. 12 stage boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NNPerforming corresponding subcritical fluid step-by-step extraction, enabling subcritical fluid in each pressure boosting or extraction bin which finishes extraction to enter a corresponding 2-stage separation subsystem 3-2, the second, 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 matched with the 2-stage separation subsystem 3-2, the second, N-1-stage separation subsystem 3- (N-1) and the N-stage ion system 3-N, discharging the extracts respectively separated by the 2-stage separation subsystem 3-2, the N-1 stage separation subsystem 3- (N-1) and the N-stage ion system 3-N;
(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 barrel 1-2 of the extractor 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 reducing section and a drawing-back section, the bin 1-1 which is continuously pushed finishes the emptying of air in an evacuating section, finishes the supercritical fluid extraction of 1 pressure level of the extracted substances in a step-by-step boosting or extracting section of 1 level, finishes the subcritical fluid extraction of 2 level to N level pressure levels of the extracted substances in a step-by step boosting or extracting section of 2 level to N level, The step-by-step pressure reduction of N-1 pressure stages is completed in the step-by-step pressure reduction section, and the continuous operation of the extraction of the subcritical fluid medium is completed in the extraction section; the supercritical fluid in the bin 1-1 which finishes the supercritical fluid extraction enters a stage 1 separation subsystem 3-1 for separation, a heavy discharge valve 3-V-1 or a heavy discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the stage 1 separation subsystem 3-1 are periodically opened, and the extract separated by the stage 1 separation subsystem 3-1 is discharged; subcritical fluid in a bin 1-1 for completing subcritical fluid 2-stage to N-stage pressure stage extraction correspondingly enters a 2-stage ion system 3-2 and …, an 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 matched with the 2-stage separation subsystems 3-2 and …, the N-1-stage separation subsystem 3- (N-1) and the N-stage ion system 3-N, discharging the extracts separated by the 2-stage separation subsystems 3-2 and …, the N-1-stage separation subsystem 3- (N-1) and the N-stage ion system 3-N.
The typical supercritical fluid medium and subcritical fluid medium are carbon dioxide, the highest subcritical carbon dioxide continuous isobaric extraction separation pressure is 50MPa, the pressure stage difference of each stage is 10MPa, and the stage number N of step-by-step pressure boosting in the subcritical fluid multistage continuous isobaric extraction separation device system for supercritical fluid pre-extraction is 5; the supercritical fluid extraction pressure of 1-level pressure level is 10MPa, the temperature is 50 ℃, the first-time separation pressure is 8MPa, the temperature is 60 ℃, or the first-time separation pressure is 8MPa, the temperature is 60 ℃, and the second-time separation pressure is 6MPa, and the temperature is 65 ℃; 2-stage to N-stage pressure stages, namely, the subcritical fluid extraction temperature of 20MPa, 30MPa, 40MPa and 50MPa is 32 ℃, the primary separation temperature is 35 ℃ or the primary separation temperature is 35 ℃ and the secondary separation temperature is 40 ℃; 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; the valves matched with each pressure stage supercharging circulation subsystem and the separation subsystem are respectively a 1-stage switching valve 6-1-1 of the 1-stage supercharging circulation subsystem 2-1 and a 2-stage switching valve of the 2-stage supercharging circulation subsystem 2-26-1-2, 3-stage switching valves 6-1-3 of a 3-stage supercharging circulation subsystem 2-3, 4-stage switching valves 6-1-4 of a 4-stage supercharging circulation subsystem 2-4, 5-stage switching valves 6-1-5 of a 5-stage supercharging circulation subsystem 2-5, 1-stage return valves 6-2-1 of a 1-stage separation subsystem 3-1, 2-stage return valves 6-2-2 of a 2-stage ionization system 3-2, 3-stage return valves 6-2-3 of a 3-stage separation subsystem 3-3, 4-stage return valves 6-2-4 of a 4-stage separation system 3-4, and 5-stage return valves 6-2-5 of a 5-stage separation system 3-5; 2 bins 1-1 are respectively filled in 1-1 of the bins in which 1-5 pressure levels are gradually boosted or the extraction sections are filled in the barrel 1-2 of the extractor of the continuous extraction subsystem 1, namely n1＝n2＝n3＝n4＝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 2.
Example four: a supercritical fluid pre-extracted subcritical fluid single-stage continuous isobaric extraction separation device system and a process flow are shown in figure 1, figure 2, figure 3, figure 4, figure 5, figure 6, figure 7, figure 8, figure 9, figure 10 and figure 11.
A subcritical fluid single-stage continuous isobaric extraction separation device system for supercritical fluid pre-extraction is completed by a system consisting of a subcritical fluid medium source 5, a pressurizing subsystem 4, a continuous extraction subsystem 1, a 1-stage separation subsystem 3-1, …, an N-1-stage separation subsystem 3- (N-1), an N-stage ion system 3-N, a 1-stage pressurizing circulation subsystem 2-1, …, an N-1-stage pressurizing circulation subsystem 2- (N-1) and an N-stage pressurizing circulation subsystem 2-N, wherein N is the step-by-step pressure boosting or the total extraction stage number in the system, N is more than 2, supercritical fluid extraction in the system is superposed with the step-by-step pressure boosting of an N-2-stage pressure stage, and subcritical fluid extraction in the system of the embodiment is superposed with the step-by-step N-stage pressure boosting.
The subcritical fluid medium source 5 is constructed as in embodiment one.
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: to be treatedLoading 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-3 grade boosting or extracting stock bin 1-1-A- (N-3) -1, No. 1N-2 grade boosting or extracting stock bin 1-1-A- (N-2) -1, No. 2N-2 grade boosting or extracting stock bin 1-1-A- (N-2) -2, …, NN-2No. 1N-2 stage boosting or extracting bin 1-1-A- (N-2) - (N)N-2-1)、nN-2N-2 grade pressure boosting or extracting bin 1-1-A- (N-2) -NN-2No. 1N-1 level boosting or extracting bin 1-1-A- (N-1) -1, No. 1N level boosting or extracting bin 1-1-A-N-1, No. 2N level boosting or extracting bin 1-1-A-N-2, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NN(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 subsystems 3-1 and …, the N-3-stage separation subsystem 3- (N-3) and the N-1-stage separation subsystem 3- (N-1) are composed of non-separation subsystems, and the non-separation subsystems are the same as the second embodiment;
the N-2 fraction ion system 3- (N-2) is composed of a double-pressure swing separation subsystem or a double-pressure swing separation subsystem, and the structure of the double-pressure swing separation subsystem or the double-pressure swing separation subsystem is the same as that of the third embodiment;
the N-fraction ion system 3-N is composed of a double isobaric separation subsystem or a double isobaric separation subsystem, and the double isobaric separation subsystem or the double isobaric separation subsystem is composed as in the first embodiment.
The 1-stage supercharging circulation subsystems 2-1, … and the N-3-stage supercharging circulation subsystem 3- (N-3) are composed of a pumpless subcritical supercharging circulation subsystem, and the composition of the pumpless subcritical supercharging circulation subsystem is the same as that of the second embodiment.
The N-2 stage supercharging circulation subsystem 2- (N-2) is composed of a supercritical supercharging circulation subsystem, and the supercritical supercharging circulation subsystem is the same as the third embodiment;
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, the first path is connected with the inlet of the circulating heat exchanger 2-HC, the second path is the auxiliary inlet of the pump-free supercritical pressurizing circulation subsystem, and the outlet of the circulating 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 subcritical supercharging circulation subsystem, and the subcritical supercharging circulation subsystem is the same as the first embodiment.
The connection relationship between the subsystems is the same as that in the first embodiment.
The extraction and separation process of the technical scheme of the embodiment 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 the N-3-stage pressurizing circulation subsystem 2- (N-3) are in an operating state, 1-stage pressurizing or extracting bins 1-1-A-1- … and 1-1-A- (N-3) -1 of 1-stage to N-3-stage step-by-step pressurizing or extracting sections in the continuous extracting subsystem 1 are correspondingly communicated with the 1-stage separating subsystem 3-1, the N-3-stage separating subsystem 3- (N-3) and the 1-stage pressurizing circulation subsystems 2-1, … and 2- (N-3) to keep the corresponding pressure levels of all stages of pressurizing or extracting bins unchanged; starting an N-2-stage pressurizing circulation subsystem 2- (N-2), and boosting the pressure of the N-2 stages in the continuous extraction subsystem 1 step by step or boosting the pressure of the No. 1N-2 stage of the extraction section or boosting the pressure of the No. 1N-2 stage of the extraction stock bin 1-1-A- (N-2) -1, No. 2N-2 stage or boosting the pressure of the extraction stock bin 1-1-A- (N-2) -2, …, NN-2No. 1N-2 stage boosting or extracting bin 1-1-A- (N-2) - (N)N-2-1)、nN-2N-2 grade pressure boosting or extracting bin 1-1-A- (N-2) -NN-2The supercritical fluid extraction is carried out to carry out,n for completion of extractionN-2The supercritical fluid in the N-2 stage boosting or extracting bin enters an N-2 stage ion system 3- (N-2) for separation, a discharge valve 3-V-1 or a discharge valve 3-V-1 and a discharge valve 3-V-2 matched with the N-2 stage ion system 3- (N-2) are opened periodically, and the extract separated from the N-2 stage ion system 3- (N-2) is discharged; the N-1 stage supercharging circulation subsystem 2- (N-1) is in an operating state, the N-1 stage step-by-step boosting in the continuous extraction subsystem 1 or the No. 1N-1 stage boosting in the extraction section or the extraction bin 1-1-A- (N-1) -1 is correspondingly communicated with the N-1 stage separation subsystem 3- (N-1), and the pressure level of the bin is 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, …, NNNo. 1N-grade boosting or extracting bin 1-1-A-N- (N)N-1)、nNN-grade boosting or extracting bin 1-1-A-N-NNPerforming subcritical fluid extraction to finish n of extractionNSubcritical fluid in the N-stage boosting or extracting bins enters the corresponding N-stage ionic systems 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 ionic systems 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 extract 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-3-level pressure levels in a step-by-step boosting or extracting section, and the step-by-step pressure boosting of 1-level to N-3-level pressure levels in an N-2-level pressure level supercritical fluid extraction of the extracted extract in an N-2-level pressure extraction section, Completing the boosting of N-1 pressure stages in an N-1 step-by-step boosting or extracting section, completing the subcritical fluid extraction of N pressure stages of the extracted substance in an N step-by-step boosting or extracting section, completing the step-by-step decompression of N-1 pressure stages in a step-by-step decompressing section, and completing the continuous operation of withdrawing the subcritical fluid medium in a withdrawing section; the supercritical fluid in the bin 1-1 which finishes supercritical fluid extraction enters an N-2 fraction ion system 3- (N-2) for separation, a discharge valve 3-V-1 or a discharge valve 3-V-1 and a double discharge valve 3-V-2 matched with the N-2 fraction ion system 3- (N-2) are periodically opened, and the extract separated from the N-2 fraction ion system 3- (N-2) is discharged; subcritical fluid in a bin 1-1 for completing subcritical fluid N-stage pressure stage extraction enters an N-stage ion system 3-N for separation, a heavy discharge valve 3-V-1 or a heavy discharge valve 3-V-1 and a heavy 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.
The typical supercritical fluid medium and subcritical fluid medium are carbon dioxide, the highest subcritical carbon dioxide continuous isobaric extraction separation pressure is 50MPa, the pressure stage difference of each stage is 10MPa, and the stage number N of step-by-step pressure boosting in the subcritical fluid single-stage continuous isobaric extraction separation device system for supercritical fluid pre-extraction is 5; the subcritical fluid pressure of the 1-stage pressure level is 10MPa, and the temperature is 32 ℃; the subcritical fluid pressure of the 2-stage pressure stage is 20MPa, and the temperature is 32 ℃; the supercritical fluid extraction pressure of 3-stage pressure level is 30MPa, the temperature is 50 ℃, the first-time separation pressure is 8MPa, the temperature is 60 ℃, or the first-time separation pressure is 8MPa, the temperature is 60 ℃, and the second-time separation pressure is 6MPa, and the temperature is 65 ℃; the supercritical fluid pressure of 4-level pressure level is 40MPa, and the temperature is 40 ℃; the subcritical fluid extraction temperature of 5-stage pressure grade 50MPa is 32 ℃, the primary separation temperature is 35 ℃ or the primary separation temperature is 35 ℃ and the secondary separation temperature is 40 ℃; each pressure stage supercharging circulation subsystem and the separation subsystem are respectively a 1-stage supercharging circulation subsystem 2-1, a 2-stage supercharging circulation subsystem 2-2, a 3-stage supercharging circulation subsystem 2-3, a 4-stage supercharging circulation subsystem 2-4 and a 5-stage supercharging circulationA ring subsystem 2-5, a stage-1 separation subsystem 3-1, a stage-2 ion system 3-2, a stage-3 separation subsystem 3-3, a stage-4 separation subsystem 3-4 and a stage-5 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; the number of bins 1-1 in which 1-stage and 2-stage pressure-level step-by-step boosting or extraction sections are arranged in the barrel 1-2 of the extractor of the continuous extraction subsystem 1 is 1, namely n1＝n2The 1-1 bins into which the stepwise pressure boosting or extraction stages of 1, 3 pressure stages are loaded are 3, i.e. n31 bin 1-1 filled with 3, 4 pressure stages for step-by-step pressure boosting or extraction is provided, n4The 1-1 bins into which the stepwise pressure boosting or extraction stages of 1, 5 pressure stages are loaded are 3, i.e. n53; 1 bin 1-1 filled with the rest sections, namely the emptying section, the 1-4-stage step-by-step pressure reduction section and the drawing-back section, is respectively provided.
The invention overcomes the defect that the existing supercritical fluid extraction device system or subcritical fluid extraction device system can not produce continuously, realizes subcritical fluid continuous equal-grade extraction separation, and has the advantages of reasonable process flow, high automation degree, reliable operation, energy conservation, zero emission and excellent manufacturability.

Claims (2)

1. A subcritical fluid continuous isobaric extraction separation device system is characterized by comprising a subcritical fluid medium source, a pressurizing subsystem, a continuous extraction subsystem, a separation subsystem and a pressurizing circulation subsystem, wherein the separation subsystem and the pressurizing circulation subsystem are the same as the step-by-step pressure boosting or total extraction stage number N of the continuous extraction subsystem;
the subcritical 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 connection relationship of each component is as follows:
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 an outlet of the liquefaction storage tank, and the outlet of the outlet valve is a subcritical fluid medium source outlet; the subcritical 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 through a pipe;
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 subcritical fluid medium source, namely the outlet valve outlet, through a pipe, 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 all the pressure reducing valves are the outlets of the pressurizing subsystems of all the 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 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 switching valve, a drawing stop valve, an emptying pump, 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, the two ends of the cylinder are respectively provided with a loading end barrel end part and a unloading end barrel end part with circular flanges, the outer wall of the cylinder is provided with a heat exchange sleeve, the inner cavity of the extraction device barrel is axially divided into a emptying section, a step-by-step boosting or extraction section with the number of steps not less than 2, a step-by-step depressurization 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 drawing-back 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 is coated with an insulating layer;
the separation subsystem is composed of a double isobaric pressure separation subsystem, or a double pressure swing separation subsystem, or a non-separation subsystem, wherein:
the heavy isobaric separation subsystem consists of an isobaric heat exchanger, a heavy heater and a heavy separator; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger is a heavy isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger is connected with the inlet of a heavy heater through a pipe, the outlet of the heavy heater is connected with the inlet of a heavy separator through a pipe, the outlet of the heavy separator is connected with the high-temperature medium inlet of the isobaric heat exchanger through a pipe, the high-temperature medium outlet of the isobaric heat exchanger is the outlet of the heavy isobaric separation subsystem, and the heavy separator is provided with an extract outlet and is provided with a heavy discharge valve;
the dual isobaric separation subsystem consists of an isobaric heat exchanger, a reheater, a heavy separator, a dual heater and a dual separator; the connection relationship of each component is as follows:
the low-temperature medium inlet of the isobaric heat exchanger is a double isobaric separation subsystem inlet, the low-temperature medium outlet of the isobaric heat exchanger is connected with a heavy heater inlet through a pipe, the outlet of a heavy heater is connected with a heavy separator inlet through a pipe, the outlet of a heavy separator is connected with a double heater inlet through a pipe, the outlet of the double heater is connected with a double separator inlet through a pipe, the outlet of the double separator is connected with a high-temperature medium inlet of the isobaric heat exchanger through a pipe, the high-temperature medium outlet of the isobaric heat exchanger is a double isobaric separation subsystem outlet, and the heavy separator and the double separator are respectively provided with an extract outlet and are respectively provided with a double discharge valve and a double discharge valve;
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 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 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 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 supercharging circulation subsystem is composed of a subcritical supercharging circulation subsystem, a supercritical supercharging circulation subsystem, a pumpless subcritical supercharging circulation subsystem or a pumpless supercritical supercharging circulation subsystem, wherein:
the subcritical pressurizing circulation subsystem consists of a voltage stabilizer, a circulating pump and a circulating condenser; the connection relationship of each component is as follows:
the inlet of the circulating condenser is a main inlet of the subcritical pressurizing circulating subsystem, the outlet of the circulating condenser is connected with the inlet of the circulating pump through a pipe, a secondary inlet of the subcritical pressurizing circulating subsystem is arranged between the outlet of the circulating condenser and the inlet of the circulating pump through the pipe, the outlet of the circulating pump is divided into two paths, one path is connected with the inlet and the outlet of the pressure stabilizer through the pipe, and the other path is the outlet of the subcritical pressurizing circulating subsystem;
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 subcritical pressurizing circulation subsystem consists of a voltage stabilizer 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 subcritical pressurizing circulation subsystem, the outlet of the one-way valve is divided into three paths through a pipe, the first path is connected with the inlet and the outlet of the pressure stabilizer, the second path is an auxiliary inlet of the pumpless subcritical pressurizing circulation subsystem, and the third path is an outlet of the pumpless subcritical pressurizing circulation subsystem;
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 supercharging circulation subsystem, the outlet of the one-way valve is divided into two paths through a pipe, the first path is connected with the inlet of the circulation heat exchanger, the second path is an auxiliary inlet of the pumpless supercritical supercharging circulation subsystem, 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:
the outlet of the subcritical fluid medium source is connected with the inlet of the pressurizing subsystem through a pipe, the outlet of each stage of pressurizing subsystem is connected with the corresponding auxiliary inlet of the pressurizing circulation subsystem through a pipe, the main inlet of each stage of pressurizing circulation subsystem is connected with the outlet of each corresponding 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 subcritical 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 each stage and the subcritical fluid medium source inlet are provided with emptying valves.
2. The extraction separation process implemented by using the subcritical fluid continuous isobaric extraction separation device system according to claim 1, comprises the following steps:
(1) emptying a liquefaction storage tank of a subcritical fluid medium source, filling the subcritical fluid medium according to the specification, starting a refrigerating unit, and liquefying the subcritical 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 subcritical fluid medium source inlet, opening reflux valves of all separation subsystems, closing switching valves of all pressurization circulation subsystems, opening emptying valves, opening outlet valves at subcritical fluid medium source outlets, 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 subcritical fluid or 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) starting a withdrawal stop valve and a withdrawal switching valve, enabling subcritical fluid or supercritical fluid medium of a bin at a withdrawal section of an inner cavity of an extractor cylinder of the continuous extraction subsystem to flow into a bin at an evacuation section of the inner cavity of the extractor cylinder of the continuous extraction subsystem, starting a withdrawal compressor after pressure of the bin at the withdrawal section and the pressure of the bin at the evacuation section are balanced until all subcritical fluid or supercritical fluid medium in the bin at the withdrawal section is withdrawn into the bin at the evacuation section, closing the withdrawal stop valve and the withdrawal switching valve, and closing the withdrawal compressor;
(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 bins after extraction are synchronously unloaded out of the continuous extraction subsystem, and in the process, each bin in the inner cavity of the extractor body 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 drawing-back 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 drawing-back of subcritical fluid medium in the bins is sequentially completed in each working section; and (3) the subcritical fluid or supercritical fluid dissolved with the extract in the extraction completed bin enters a corresponding separation subsystem to start separation, and the discharge valve is periodically opened to discharge the extract separated by the separation subsystem.
CN201910575431.3A 2019-06-28 2019-06-28 Subcritical fluid continuous isobaric extraction separation device system and extraction separation process Active CN110152350B (en)

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