CN110152350A - A kind of subcritical fluids continuously isobaric extraction separation device system and extraction and separation technology - Google Patents
A kind of subcritical fluids continuously isobaric extraction separation device system and extraction and separation technology Download PDFInfo
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- CN110152350A CN110152350A CN201910575431.3A CN201910575431A CN110152350A CN 110152350 A CN110152350 A CN 110152350A CN 201910575431 A CN201910575431 A CN 201910575431A CN 110152350 A CN110152350 A CN 110152350A
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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
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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
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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Abstract
The present invention relates to chemical separatings and bioengineering mechanical equipment field, more particularly to a kind of subcritical fluids continuously isobaric extraction separation device system and extraction and separation technology, which extracts the identical isolated subsystem of series by subcritical fluids medium source, pressurization subsystem, continuous extraction subsystem, with the boosting step by step of continuous extraction subsystem or step by step and pressurization cycle subsystem is constituted.The extraction and separation technology implemented using present apparatus system, by the technological operation of system, complete subcritical fluids extracted or supercritical fluid in the feed bin of extraction and enter corresponding isolated subsystem to be initially separated, discharge valve is periodically turned on, the separated extract come out of isolated subsystem is drawn off.The inventive technique plant automation degree is high, reliable for operation, apparatus system process flow is reasonable, realizes subcritical fluids continuously equal sub- extraction and separation, energy saving zero-emission, craftsmanship is excellent, separating effect is excellent.
Description
One, technical field
It is continuous etc. the present invention relates to chemical separating and bioengineering mechanical equipment field more particularly to a kind of subcritical fluids
Press extraction separation device system and extraction and separation technology.
Two, technical background
Subcritical fluid extraction isolation technics is the another item green chemical technology after supercritical fluid extraction isolation technics,
It is being applied generally in extraction and separation field.But existing subcritical fluid extraction device is mostly to use to open sealing fastly
The batch-type system of structure, production efficiency is low, and energy consumption is high;Extractor is frequently opened, security reliability is low and causes extraction fluid
Significant losses, seriously constrain the popularization and application of this new technology.
China State Intellectual Property Office Patent Office, authorizing announcement number on May 30th, 2012 is
CN101912696B, the patent of entitled " subcritical fluid extraction device and method of active ingredient of natural product " are public
A kind of subcritical fluid extraction device is opened, the leaching system part of the device is by single extractor, evaporator, condenser, molten
Agent tank, compressor etc. are constituted;The device is a kind of subcritical abstraction device of intermittently operated, every time after extraction, with compression
Residual subcritical fluids in extract in extractor are carried out decompression evaporation by machine, after pressure tank to be extracted drops to 0MPa, then
Negative pressure evaporation is carried out with vacuum pump, until pressure is reduced to -0.09MPa hereinafter, opening extraction tank mouth, residue is taken out.For
The subcritical fluids " continuous extraction apparatus " of more kettle parallel forms, essence is still intermittently operated, although to a certain extent
Improve production efficiency, but still there are low efficiency, security reliability is low, energy consumption and extractant loss are big the disadvantages of.
China State Intellectual Property Office Patent Office, authorizing announcement number on October 22nd, 2008 is
CN100427172C, patent name are the patents of invention of " Apparatus for continuous extracting and sterilizing solid materials under high and ultrahigh pressure ", open
A kind of Apparatus for continuous extracting and sterilizing solid materials under high and ultrahigh pressure, the device are driven by pressure cylinder, feed bin chain, feed bin operation
Motivation structure, heat exchanger, fluid enter pipe group and fluid discharge pipe group is constituted, and feed bin chain is mounted in pressure cylinder, feed bin operation
Driving mechanism is mounted on the inlet and outlet both ends of pressure cylinder, is cooperatively connected with the feed bin chain of disengaging pressure cylinder, pressure-bearing cylinder
Heat exchanger is installed on body and fluid enters pipe group and fluid discharge pipe group.The arrangement achieves the extractions of high-voltage and ultra-high solid material
Continuous operation with when sterilizing, has the characteristics that safe and reliable, high-efficient.But the device is one in extracting operation
Unit, fail complete continuous extraction apparatus at Analysis of Nested Design and reasonable process flow, make the popularization and use of continuous extraction apparatus
Critical constraints.
Three, summary of the invention
The purpose of the present invention is overcoming defect existing for existing subcritical fluid extraction device, a kind of subcritical fluids are provided
Continuous equipressure extraction separation device system and extraction and separation technology.
A kind of technical solution of the continuous isobaric extraction separation device system of subcritical fluids of the invention, is by sub-critical flow
Body medium source, pressurization subsystem, continuous extraction subsystem, with the boosting step by step of continuous extraction subsystem or extract total series N phase
Same isolated subsystem and pressurization cycle subsystem is constituted.
The subcritical fluids medium source is by liquefaction storage tank, cooler, refrigeration machine, outlet valve, filling valve and total reflux
Valve group is constituted;The connection relationship respectively formed are as follows:
Cooler is placed in liquefaction tank inside or outside, cooler are connected with refrigeration unit, forms cooling circuit;Liquid
Change outlet and be equipped with outlet valve, exports valve outlet as the outlet of subcritical fluids medium source;There are two subcritical fluids medium sources
Entrance, one is total reflux valve inlet, another fills valve inlet, and total flow back and fills valve outlet after pipe merges at valve outlet
It is connected to liquefaction reservoir inlet.
The pressurization subsystem is made of cooler, force (forcing) pump, pressure reducing valve and overflow valve;The connection relationship respectively formed
Are as follows:
Cooler entrance is pressurized system entry, is exported through pipe and subcritical fluids medium source, i.e. outlet valve outlet
It is connected, cooler outlet is connected through pipe with pressurization pump intake;Pressurization pump discharge is divided into N number of branch, pressurized with pipe
System maximum pressure grade pipe branch is divided into two branches again, is all the way the maximum pressure grade outlet for the subsystem that pressurizes, another
Road is connected with overflow valve inlet;Remaining N-1 branch is connected through pipe is corresponding with the decompression valve inlet of each pressure stage, respectively subtracts
Pressure valve outlet is the pressurized system outlet of other each pressure stages in addition to maximum pressure grade;Overflow valve outlet is cold through being connected to by pipe
But on the pipe between device outlet and pressurization pump intake;Pressurized system outlet quantity, i.e. pressure reducing valve add the quantity of overflow valve
It is identical as the boosting step by step of continuous extraction subsystem or the total series of extraction.
The continuous extraction subsystem by feed bin, extractor cylinder, binning end barrel end, unload storehouse end barrel end,
Binning end locking device unloads storehouse end locking device, binning hydraulic cylinder, unloads storehouse hydraulic cylinder, rack, insulating layer, emptying switching valve, takes out
Switching valve is returned, shut-off valve, drain pump is drawn back, draws back compressor, sealing ring composition;Wherein:
Feed bin is the cylinder with orlop, is equipped with distribution grid close to orlop, has fluid on the barrel between distribution grid and orlop
Enter hole, is equipped with powder blocking plate close to Hatch Opening, has Fluid-exiting apertures, the orlop of feed bin cylinder outer circle on the barrel between powder blocking plate and Hatch Opening
Side is equipped with and binning end locking device or unloads the locking card slot that the dissection type clip quick-opening structure of storehouse end locking device matches, lock
The barrel outer circle of tight card slot two sides and Hatch Opening is equipped with seal groove;
The extractor cylinder of continuous extraction subsystem is cylindrical structure, and cylinder both ends are respectively equipped with the binning with annular flange
End barrel end and unload storehouse end barrel end, cylinder outer wall is equipped with Heat exchange jacekt, extractor cylinder lumen along be divided axially into emptying section,
Series is no less than 2 boosting step by step or extraction section, series are equal to the step pressure reducing section that boosting or the total series of extraction section subtract 1 step by step,
And draw back Duan Gongsi active section;Continuous extraction subsystem extractor cylinder lumen fills feed bin, and every grade boosts or extracts step by step
It takes and is at least packed into a feed bin in section;Emptying section correspond to be packed into feed bin fluid entry holes position extractor barrel wall on set
There is fluid inlet and outlet, boosting or extraction section correspond to the fluid entry holes position and Fluid-exiting apertures position for each feed bin being packed into step by step
Fluid inlet and fluid outlet are respectively equipped on the extractor barrel wall set, step pressure reducing section corresponds to each material being packed into
It is equipped with fluid balance inlet and outlet on the extractor barrel wall of storehouse fluid entry holes position, draws back section corresponding to be packed into feed bin stream
The extractor barrel wall that body enters hole site is equipped with fluid outlet;Each stream on the extractor barrel wall of boosting or extraction section step by step
Body entrance is the entrance of continuous extraction subsystem, and each fluid outlet is to connect on the extractor barrel wall of boosting or extraction section step by step
The outlet of continuous extraction sub-system;
Binning end locking device and storehouse end locking device is unloaded by dissection type clip and hydraulic or be driven by electricity and constitute;Binning end
The dissection type clip quick-opening structure and binning end barrel end of locking device and the locking card slot of feed bin, unload storehouse end locking device
Dissection type clip quick-opening structure correspond to each other matching with the locking card slot for unloading storehouse end barrel end and feed bin;
The connection relationship that continuous extraction subsystem respectively forms are as follows:
Binning hydraulic cylinder is successively sequentially fixedly mounted along axis, binning end locking device, extractor cylinder, unloads the locking of storehouse end
Device, unload storehouse hydraulic cylinder in rack, make binning hydraulic cylinder, binning end locking device, extractor cylinder, unload storehouse end locking dress
It sets, unload that storehouse hydraulic cylinder is mutually coaxial, and binning end locking device matches with binning barrel end, unload storehouse end locking device and unload storehouse
Barrel end matches;
The fluid outlet on section extractor barrel wall is drawn back by pipe and draws back shut-off valve and draws back suction port of compressor phase
Connection, the fluid inlet and outlet emptied on section extractor barrel wall divide two-way, pass through pipe all the way and draw back switching valve and draw back pressure
The outlet of contracting machine is connected, and another way is connected by pipe and emptying switching valve with emptying pump intake, and emptying pump discharge leads to greatly
Gas;The fluid balance inlet and outlet for closely drawing back the step pressure reducing section of section pass through pipe and the boosting step by step or extraction that closely empty section
The fluid inlet of section is connected, and the secondary fluid balance inlet and outlet for suffering the step pressure reducing section for drawing back section suffer emptying section with secondary by pipe
Boosting or the fluid inlet of extraction section step by step be connected, and so on, the fluid balance of whole step pressure reducing sections is imported and exported
It is connected by the way that pipe is corresponding with the fluid inlet of boosting or extraction section step by step that boosting or the total series of extraction section step by step subtract 1;Extraction
Device cylinder body outer wall is taken to coat insulating layer.
The isolated subsystem is by the isobaric isolated subsystem of a weight or double isobaric isolated subsystem, Huo Zheyi
Weight transformation isolated subsystem perhaps double transformation isolated subsystem or without isolated subsystem constitute, in which:
One weight equipressure isolated subsystem is made of isobaric heat exchanger, a reheating device and a weight separator;The company respectively formed
Connect relationship are as follows:
Isobaric heat exchanger cryogenic media entrance is the isobaric isolated subsystem entrance of a weight, isobaric heat exchanger cryogenic media outlet
It is connected through pipe with a reheating device entrance, reheating device outlet is connected through pipe with a weight separator inlet, a weight
Separator outlet is connected through pipe with isobaric heat exchanger high-temperature medium entrance, isobaric heat exchanger high-temperature medium outlet for one again etc.
Isolated subsystem outlet is pressed, a weight separator is exported equipped with extract, and is furnished with a heavy discharge valve.
Double equipressure isolated subsystem is by isobaric heat exchanger, a reheating device, a heavy separator, double heater and double
Separator is constituted: the connection relationship respectively formed are as follows:
Isobaric heat exchanger cryogenic media entrance is double isobaric isolated subsystem entrance, isobaric heat exchanger cryogenic media outlet
It is connected through pipe with a reheating device entrance, reheating device outlet is connected through pipe with a weight separator inlet, a weight
Separator outlet is connected through pipe with double calorifier inlets, and double heater outlet is through pipe and double separator inlet phase
Connection, double separator outlet are connected through pipe with isobaric heat exchanger high-temperature medium entrance, and isobaric heat exchanger high-temperature medium goes out
Mouth is double isobaric isolated subsystem outlet, and a weight separator and double separator are respectively equipped with extract and export, and match respectively
There are a weight discharge valve and double discharge valve.
One weight transformation isolated subsystem is made of a readjustment pressure valve, a weight heat exchanger and a weight separator;The company respectively formed
Connect relationship are as follows:
One resets pressure valve entrance as a heavy transformation isolated subsystem entrance, and a readjustment pressure valve outlet exchanges heat through pipe with one again
Device entrance is connected, and a weight heat exchanger exit is connected through pipe with a weight separator inlet, and a weight separator outlet is a weight
The outlet of transformation isolated subsystem, a weight separator is exported equipped with extract, and is furnished with a heavy discharge valve.
Double transformation isolated subsystem resets a pressure valve, weight heat exchanger, a heavy separator, double pressure regulator valve, double by one
Heat exchanger and double separator are constituted: the connection relationship respectively formed are as follows:
One resets pressure valve entrance as double transformation isolated subsystem entrance, and a readjustment pressure valve outlet exchanges heat through pipe with one again
Device entrance is connected, and a weight heat exchanger exit is connected through pipe with a weight separator inlet, a heavy transformation extractor outlet warp
Pipe is connected with double pressure regulation valve inlet, and double pressure regulation valve outlet is connected through pipe with double heat exchanger entrance, double to change
Hot device outlet is connected through pipe with double separator inlet, and double separator outlet is the outlet of double transformation isolated subsystem,
One weight separator and double separator are respectively equipped with extract outlet, and equipped with a weight discharge valve and double discharge valve.
No isolated subsystem is made of connecting pipe, and the sub- entrance of connecting pipe is no isolated subsystem entrance, even
Connecing with tube outlet is no isolated subsystem outlet.
The pressurization cycle subsystem is by subcritical pressurization cycle subsystem or overcritical pressurization cycle subsystem
System is perhaps constituted without the subcritical pressurization cycle subsystem of pump or without overcritical pressurization cycle subsystem is pumped, in which:
Subcritical pressurization cycle subsystem is made of voltage-stablizer, circulating pump, cycle condenser;The connection relationship respectively formed
Are as follows:
Cycle condenser entrance is subcritical pressurization cycle subsystem main-inlet, and cycle condenser outlet is through pipe and circulation
Pump intake is connected, and pipe enters equipped with subcritical pressurization cycle subsystem pair between cycle condenser outlet and pump entry
Mouthful, circulating-pump outlet divides two-way, is connected all the way through pipe with voltage-stablizer inlet and outlet, another way is subcritical pressurization cycle subsystem
System outlet.
Overcritical pressurization cycle subsystem is made of transformation heat exchanger, cycle condenser, circulating pump, circulation heat exchanger;Respectively
The connection relationship of composition are as follows:
Transformation heat exchanger low-pressure medium entrance is overcritical pressurization cycle subsystem main-inlet, transformation heat exchanger low-pressure medium
Outlet is connected through pipe with cycle condenser entrance, and cycle condenser outlet is connected through pipe with pump entry, recycles
Pipe is equipped with overcritical pressurization cycle subsystem sub-inlet between condensator outlet and pump entry, and circulating-pump outlet is through pipe
It is connected with transformation heat exchanger high-voltage medium inlet, transformation heat exchanger high-voltage media outlet is through pipe and circulation heat exchanger entrance phase
Connection, circulation heat exchanger outlet are that overcritical pressurization cycle subsystem exports.
It is made of without subcritical pressurization cycle subsystem is pumped voltage-stablizer, check valve;The connection relationship respectively formed are as follows:
One-way valve inlet is without the subcritical pressurization cycle subsystem main-inlet of pump, and one-way valved outlet is divided into three by pipe
Road, the first via are connected with voltage-stablizer inlet and outlet, and the second tunnel is without the subcritical pressurization cycle subsystem sub-inlet of pump, and third road is
It is exported without subcritical pressurization cycle subsystem is pumped.
It is made of without overcritical pressurization cycle subsystem is pumped circulation heat exchanger, check valve;The connection relationship respectively formed are as follows:
One-way valve inlet is without the overcritical pressurization cycle subsystem main-inlet of pump, and one-way valved outlet is divided into two by pipe
Road, the first via are connected with circulation heat exchanger entrance, and the second tunnel is without the overcritical pressurization cycle subsystem sub-inlet of pump, circulating picture-changing
Hot device outlet is without the overcritical pressurization cycle subsystem outlet of pump.
Connection relationship between above each subsystem are as follows:
The outlet of subcritical fluids medium source is connected through pipe with pressurized system entry, the outlet of pressurization subsystems at different levels
It is connected through pipe with corresponding pressurization cycle subsystem sub-inlet, pressurization cycle subsystem main-inlets at different levels are through pipe and switching
Valve is connected with each corresponding isolated subsystem outlet, and isolated subsystem entrances at different levels are through pipe and each corresponding continuous extraction
System outlet is connected, and pressurization cycle subsystem outlets at different levels are connected through pipe with each corresponding continuous extraction subsystem entrance
It connects, while isolated subsystem at different levels outlet is each separated into two-way through pipe, all the way through return valve and the same subcritical fluids matchmaker
Matter source inlet is connected, and another way is connected through switching valve with corresponding pressurization cycle subsystem outlets at different levels;Corresponding at different levels
Exhaust-valve is housed on the return valve of isolated subsystem and the connecting line of subcritical fluids medium source inlet.
Using a kind of subcritical fluids extraction and separation technology that continuously isobaric extraction separation device system is implemented, steps are as follows:
(1) the liquefaction storage tank in subcritical fluids medium source is emptied, and is full of subcritical fluids medium by regulation, and open
Refrigeration machine liquefies subcritical fluids medium;
(2) sealing ring will be installed in the seal groove of each feed bin;Binning end locking device is opened, one by one with binning hydraulic cylinder
By the extractor cylinder lumen of empty feed bin push-in continuous extraction subsystem, after extractor cylinder lumen fills sky feed bin, start
Push-in is equipped with the feed bin of extract one by one, when draw back a feed bin is housed outside section after, lock continuous extraction subsystem binning end
Locking device and unload storehouse end locking device;
(3) the total return valve of subcritical fluids medium source inlet is closed, the return valve for being totally separated subsystem is opened, is closed complete
The switching valve of portion's pressurization cycle subsystem opens exhaust-valve, opens the outlet valve of subcritical fluids medium source outlet, and discharge is continuous
Extraction sub-system and the air being totally separated in subsystem;It continuous extraction subsystem and is totally separated in subsystem air and empties
Afterwards, the air in whole pressurization cycle subsystems is discharged in the switching valve for opening whole pressurization cycle subsystems, until emptying, so
The return valve for being totally separated subsystem is closed afterwards, closes exhaust-valve;
(4) starting pressurization subsystem so that feed bin in each boosting step by step or extraction section in continuous extraction subsystem and
Pressure in the feed bin and matched isolated subsystem and pressurization cycle subsystem of its corresponding step pressure reducing section reaches setting value;
(5) start whole pressurization cycle subsystems, boost step by step in continuous extraction subsystem or the feed bin of extraction section starts
Complete it is corresponding boost or extract step by step, complete subcritical fluids extracted or supercritical fluid in the feed bin of extraction and enter
Corresponding isolated subsystem is initially separated, and periodically turns on discharge valve, is drawn off the separated extraction come out of isolated subsystem and is gone out
Object;
(6) it when the feed bin in the boosting step by step or extraction section near step pressure reducing section reaches the extraction process time, closes
Switching valve is drawn back, emptying switching valve is opened, starts drain pump, emptying is emptied in continuous extraction subsystem extractor cylinder lumen
The air of the feed bin of section;Emptying switching valve is closed, drain pump is closed;
(7) binning hydraulic cylinder piston rod is retracted, is filled between the feed bin that binning hydraulic cylinder and binning end locking device are locked
Enter the new feed bin of extract is housed, stretches out binning hydraulic cylinder piston rod and hold out against the feed bin being newly packed into;Storehouse hydraulic cylinder is unloaded in stretching
Piston rod simultaneously holds out against and unloads the feed bin that storehouse end locking device is locked;It is synchronous to open binning end locking device and unload storehouse end locking dress
It sets;It synchronizes and continues to stretch out binning hydraulic cylinder piston rod and retraction and unload storehouse hydraulic cylinder piston rod, the feed bin being newly packed into is loaded into continuously
Extraction sub-system extractor cylinder lumen;It is synchronous to lock binning end locking device and unload storehouse end locking device;It is hydraulic that storehouse is unloaded in retraction
Cylinder piston rod unloads the feed bin being ejected;
(8) emptying switching valve is opened, drain pump is started, emptying is emptied in continuous extraction subsystem extractor cylinder lumen
The air of the feed bin of section;Emptying switching valve is closed, drain pump is closed;
(9) it opens and draws back shut-off valve and draw back switching valve, draw back section in continuous extraction subsystem extractor cylinder lumen
Feed bin subcritical fluids or supercritical fluid medium flow into everywhere in continuous extraction subsystem extractor cylinder lumen empty
The feed bin of section, after drawing back section feed bin and emptying section pressure of silo balance, compressor is drawn back in unlatching, until drawing back in section feed bin
Subcritical fluids or supercritical fluid medium are all withdrawn into emptying section feed bin, and closing draws back shut-off valve and draws back switching valve,
Compressor is drawn back in closing;
(10) (7) step~the (9) step is repeated, so that the feed bin equipped with the extract not extracted is periodically packed into
Continuous extraction subsystem, the feed bin after having extracted synchronously are drawn off continuous extraction subsystem, in this course, continuous extraction
Each feed bin of subsystem extractor cylinder lumen is successively in emptying section, step by step boosting or extraction section, step pressure reducing section and pumping
Section is returned, the emptying of air in feed bin, extract in the boosting step by step of feed bin or feed bin are sequentially completed in each active section
Extraction step by step, in the step pressure reducing of feed bin, feed bin subcritical fluids medium the continuous operation drawn back;Complete the feed bin of extraction
In dissolved with extract subcritical fluids or supercritical fluid enter corresponding isolated subsystem be initially separated, periodically open
Discharge valve is opened, the separated extract come out of isolated subsystem is drawn off.
It is that the present invention generates the utility model has the advantages that pressurization cycle subsystem has the fluid conveying shape of subcritical state and above-critical state
Formula, isolated subsystem have the fluid separation condition of above-critical state and subcritical state available, and process flow is easy flexibly;Continuously
Each pressure classification of boosting or extraction section feed bin step by step of extraction sub-system was different, it can be achieved that classification continuous extraction, both ensure that
The diversity of extract improves extraction efficiency again;First boost step by step along continuous extraction subsystem feed bin direction of advance pressure again by
Grade decompression, has been effectively ensured the security reliability of dynamic sealing;The subcritical abstraction pressure of continuous extraction subsystem with separate subsystem
The separating pressure of system is identical, needs to be depressured separation after eliminating extraction, and the power consumption extracted of boosting is needed after separating;It is sub-
Critical fluids medium is recycled in extraction, lock out operation, and realizes the subcritical fluids medium recycling benefit of discharge feed bin
With effectively reducing the consumption of subcritical fluids medium;Supercritical fluid after separation it is circularly-supercharged it is preceding with separate before Asia
Critical fluids heat exchange;Alternatively, when supercritical fluid extraction, before the gaseous state subcritical fluids medium condensation after separation with it is pressurized
Liquid subcritical fluids medium change it is cold, effectively reduce system heat, cooling capacity consumption.Apparatus of the present invention system process closes
Reason, plant automation degree is high, and apparatus system is reliable for operation, energy saving zero-emission, craftsmanship are excellent.
Four, Detailed description of the invention
Fig. 1 is the structural schematic diagram of the continuous isobaric extraction separation device system of subcritical fluids of the invention;
Fig. 2 be 2-1 in Fig. 1 ..., the structural schematic diagram of subcritical pressurization cycle subsystem shown in 2- (N-1), 2-N;
Fig. 3 be 2-1 in Fig. 1 ..., the structural schematic diagram of overcritical pressurization cycle subsystem shown in 2- (N-1), 2-N;
Fig. 4 be 2-1 in Fig. 1 ..., shown in 2- (N-1), 2-N without the structural representation for pumping subcritical pressurization cycle subsystem
Figure;
Fig. 5 be 2-1 in Fig. 1 ..., shown in 2- (N-1), 2-N without the structural representation for pumping overcritical pressurization cycle subsystem
Figure;
Fig. 6 be 3-1 in Fig. 1 ..., the structural schematic diagram of the isobaric isolated subsystem of a weight shown in 3- (N-1), 3-N;
Fig. 7 be 3-1 in Fig. 1 ..., the structural schematic diagram of double isobaric isolated subsystem shown in 3- (N-1), 3-N;
Fig. 8 be 3-1 in Fig. 1 ..., the structural schematic diagram of a heavy transformation isolated subsystem shown in 3- (N-1), 3-N;
Fig. 9 be 3-1 in Fig. 1 ..., the structural schematic diagram of double transformation isolated subsystem shown in 3- (N-1), 3-N;
Figure 10 be 3-1 in Fig. 1 ..., the structural schematic diagram without isolated subsystem shown in 3- (N-1), 3-N;
Figure 11 is that the part that dotted line D draws a circle to approve embodiment feed bin and extractor cylinder matching relationship shown in range in Fig. 1 is put
Big figure.
Appended drawing reference:
1, continuous extraction subsystem 1-1, feed bin 1-1-1 fluid entry holes 1-1-2, distribution grid 1-1-3, Fluid-exiting apertures
1-1-4, card slot 1-1-5, powder blocking plate 1-1-6, sealing ring 1-1-A, feed bin 1-1-A-0, emptying feed bin 1-1-A- are housed to
1-1,1 grade of the 1st feed bin 1-1-A-1-2 of boosting, 1 grade of the 2nd feed bin 1-1-A-1- (n of boosting1- 1), 1 grade of boosting (n1- 1) feed bin
1-1-A-1-n1, 1 grade of boosting n-th1Feed bin 1-1-A- (N-1) -1, N-1 grades of boostings the 1st feed bin 1-1-A- (N-1) -2, N-1 grades
Boost the 2nd feed bin 1-1-A- (N-1)-(nN-1- 1), N-1 grades of boosting (nN-1- 1) feed bin 1-1-A- (N-1)-nN-1, N-1 grades
Boosting n-thN-11-1-A-N-2, N grades of the 1st feed bin the 2nd feed bin 1-1-A-N- (n of boosting of 1-1-A-N-1, N grades of feed bin boostingsN-
1), N grades of boosting (nN- 1) feed bin 1-1-A-N-nN, N grades boosting n-thNFeed bin 1-1-B, it discharging bin 1-1-B-0 to be unloaded, takes out
Feed back storehouse 1-1-B-1,1 grade of decompression feed bin 1-1-B- (N-1), N-1 grades of decompression feed bin 1-2, extractor cylinder 1-2-A, dress
Storehouse end barrel end 1-2-B, storehouse end barrel end 1-2-1, stream socket 1-2-2, fluid inlet 1-2-3, fluid are unloaded
Outlet 1-2-4, fluid balance inlet and outlet 1-2-5, fluid reflux mouth 1-3-A, binning end locking device 1-3-B, storehouse end is unloaded
Locking device 1-4-A, binning hydraulic cylinder 1-4-B, it unloads storehouse hydraulic cylinder 1-5-1, emptying switching valve 1-5-2, draw back switching valve
1-5-3, draw back shut-off valve 1-6, drain pump 1-7, draw back compressor 1-8, insulating layer 1-9, rack 2-1,1 grade of pressurization follow
Loop subsystems, 2-N, N grades of pressurization cycle subsystem 2-B of N-1 grades of pressurization cycle subsystems, voltage-stablizer 2-C, follow at 2- (N-1)
Ring condenser 2-CV, check valve 2-E, transformation heat exchanger 2-HC, circulation heat exchanger 2-P, circulating pump 3-1,1 grade of segregant
System, 3- (N-1), 3-N, N grades of isolated subsystem 3-E of N-1 grades of isolated subsystems, isobaric heat exchanger 3-H-1, a reheating
Device 3-H-2, double heater 3-HC-1, a weight heat exchanger 3-HC-2, double heat exchanger 3-S-1, a heavy separator 3-S-
2, double separator 3-V-1, a weight discharge valve 3-V-2, double discharge valve 3-VC-1, one reset pressure valve 3-VC-2, double
Pressure regulator valve 4, pressurization subsystem 4-1, cooler 4-2, force (forcing) pump 4-3-1,1 grade of pressure reducing valve 4-3- (N-1), N-1 grades of decompressions
Valve 4-4, overflow valve 5, subcritical fluids medium source 5-1, liquefaction storage tank 5-2, cooler 5-3, refrigeration unit 5-4-1,
Filling valve 5-4-2, outlet valve 5-4-3, total return valve 6-0, exhaust-valve 6-1-1,1 grade of switching valve 6-1- (N-1), N-1 grades
Switching valve 6-1-N, N grade switching valve 6-2-1,6-2-N, N grades of 1 grade of return valve 6-2- (N-1), N-1 grades of return valves return valves
7- pipe
Five, specific embodiment
Describe specific implementation process of the invention in detail with reference to the accompanying drawing.
Embodiment one: a kind of multistage continuous isobaric extraction separation device system of subcritical fluids and process flow, as Fig. 1,
Shown in Fig. 2, Fig. 6, Fig. 7, Figure 11.
A kind of multistage continuously isobaric extraction separation device system of subcritical fluids is by subcritical fluids medium source 5, pressurized
System 4,1,1 grade of isolated subsystem 3-1 of continuous extraction subsystem ..., N-1 grades of isolated subsystem 3- (N-1), N fraction ionization series
Unite 3-N, 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1) and N grades of pressurization cycle subsystem 2-
N is constituted, and N is boosting step by step or the total series of extraction in system, and N is greater than 2, and the subcritical fluids in the embodiment system are step by step
Extraction is overlapped with boosting step by step.
The subcritical fluids medium source 5 is by liquefaction storage tank 5-1, cooler 5-2, refrigeration unit 5-3, filling valve 5-4-
1, outlet valve 5-4-2 and total return valve 5-4-3 is constituted, and fluid material for flow is stainless steel;The connection relationship respectively formed are as follows:
Cooler 5-2 is placed in liquefaction storage tank 5 either internally or externally, and cooler 5-2 is connected with refrigeration unit 5-3, is formed
Cooling circuit;The outlet storage tank 5-1 liquefy equipped with outlet valve 5-4-2, the outlet of outlet valve 5-4-2 is subcritical fluids medium source 5
Outlet;Subcritical fluids medium source 5 is there are two entrance, and one is total return valve 5-4-3 entrance, another filling valve 5-4-1 enters
Mouthful, total outlet return valve 5-4-3 and the outlet filling valve 5-4-1 are connected to liquefaction storage tank 5-1 entrance after the merging of pipe 7.
The pressurization subsystem 4 by cooler 4-1, force (forcing) pump 4-2,1 grade of pressure reducing valve 4-3-1 ..., N-1 grades of pressure reducing valves
The overflow valve 4-4 composition of 4-3- (N-1), N stage pressure grade, fluid material for flow are stainless steel;The connection relationship respectively formed are as follows:
Cooler 4-1 entrance is pressurization 4 entrance of subsystem, exports, that is, exports through pipe 7 and subcritical fluids medium source 5
The outlet valve 5-4-2 is connected, and the outlet cooler 4-1 is connected through pipe 7 with force (forcing) pump 4-2 entrance;The outlet force (forcing) pump 4-2 pipe
Son 7 is divided into N number of branch, and pressurization 4 maximum pressure grade pipe branch of subsystem is divided into two branches again, is all the way the subsystem that pressurizes
4 maximum pressure grade outlet, another way are connected with overflow valve 4-4 entrance;Remaining N-1 branch is through the correspondence of pipe 7 and each pressure
The pressure reducing valve of power grade, i.e. 1 grade of pressure reducing valve 4-3-1 ..., the entrances of N-1 grades of pressure reducing valve 4-3- (N-1) be connected, depressurize valve outlet,
That is 1 grade of pressure reducing valve 4-3-1 ..., the outlet of N-1 grades of pressure reducing valve 4-3- (N-1) in addition to maximum pressure grade other each pressure stages plus
Subsystem 4 is pressed to export;Pipe of the outlet overflow valve 4-4 through being connected to by pipe 7 between the outlet cooler 4-1 and force (forcing) pump 4-2 entrance
On son 7;Pressurize 4 export volume of subsystem, i.e. 1 grade of pressure reducing valve 4-3-1 ..., N-1 grade pressure reducing valve 4-3- (N-1) are plus overflow valve
The quantity of 4-4 is identical as the boosting step by step of continuous extraction subsystem 1 or the total series of extraction.
The continuous extraction subsystem 1 by feed bin 1-1, extractor cylinder 1-2, binning end barrel end 1-2-A, unload storehouse
End barrel end 1-2-B, binning end locking device 1-3-A, it unloads storehouse end locking device 1-3-B, binning hydraulic cylinder 1-4-A, unload storehouse
Hydraulic cylinder 1-4-B, it rack 1-9, insulating layer 1-8, emptying switching valve 1-5-1, draws back switching valve 1-5-2, draw back shut-off valve 1-5-
3, drain pump 1-6, draw back compressor 1-7, sealing ring 1-1-6 composition;Wherein:
Feed bin 1-1 is the cylinder with orlop, and material is stainless steel, is equipped with distribution grid 1-1-2, distribution grid 1-1- close to orlop
There is fluid entry holes 1-1-1 on barrel between 2 and orlop, is equipped with powder blocking plate 1-1-5, powder blocking plate 1-1-5 and Hatch Opening close to Hatch Opening
Between barrel on have a Fluid-exiting apertures 1-1-3, the orlop side of feed bin 1-1 cylinder outer circle is equipped with and binning end locking device 1-3-A
Or unload the two sides locking card slot 1-1-4, card slot 1-1-4 that the dissection type clip quick-opening structure of storehouse end locking device 1-3-B matches
Seal groove is equipped with the barrel outer circle of Hatch Opening;
The extractor cylinder 1-2 of continuous extraction subsystem 1 is cylindrical structure, and fluid material for flow is stainless steel, cylinder two
End is respectively equipped with the binning end barrel end 1-2-A with annular flange and unloads storehouse end barrel end 1-2-B, and cylinder outer wall is equipped with and changes
Hot jacket, the inner cavity extractor cylinder 1-2 are N-1's along boosting or extraction section, the series step by step for being divided axially into emptying section, series is N
Step pressure reducing section, and draw back Duan Gongsi active section;Continuous extraction subsystem fills feed bin in 1 inner cavity extractor cylinder 1-2
1-1, every grade step by step boosting or extraction section in be at least packed into a feed bin 1-1;From the binning end of continuous extraction subsystem 1, it is packed into
The feed bin 1-1 number consecutively of the inner cavity extractor cylinder 1-2 are as follows: be housed to feed bin 1-1-A;Empty the emptying feed bin 1-1-A-0 of section;
Boosting or No. 11 grade of boosting of extraction section or extraction feed bin 1-1-A-1-1, No. 21 grade of boostings or extraction feed bin 1-1-A-1- step by step
2、…、n1- No. 11 grade of boosting or extraction feed bin 1-1-A-1- (n1-1)、n1Number 1 grade boosting or extraction feed bin 1-1-A-1-n1...,
No. 1 N-1 grades feed bin 1-1-A- (N-1) -1, No. 2 N-1 grades feed bin 1-1-A- (N-1) -2 that boost or extract that boost or extract ...,
nN-1- No. 1 N-1 grades of boosting or extraction feed bin 1-1-A- (N-1)-(nN-1-1)、nN-1Numbers N-1 grades boostings or extraction feed bin 1-1-A-
(N-1)-nN-1, No. 1 N grades boosting or extraction feed bin 1-1-A-N-1, No. 2 N grade boosting or extract feed bin 1-1-A-N-2 ..., nN-1
Numbers N grades boostings or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or extraction feed bin 1-1-A-N-nN;Step pressure reducing section
N-1 grades of decompression feed bin 1-1-B- (N-1) ..., 1 grade of decompression feed bin 1-1-B-1;That draws back section draws back feed bin 1-1-B-0;Wait draw off
Feed bin 1-1-B;The extractor cylinder 1-2 barrel that emptying section corresponds to the be packed into position feed bin fluid entry holes 1-1-1 is equipped with
Fluid inlet and outlet 1-2-1, boosting or extraction section correspond to the position fluid entry holes 1-1-1 and the stream for each feed bin being packed into step by step
Body portal the position 1-1-3 extractor cylinder 1-2 barrel on be respectively equipped with fluid inlet 1-2-2 and fluid outlet 1-2-3, by
Grade decompression section is equipped with stream on the extractor cylinder 1-2 barrel corresponding to each position feed bin fluid entry holes 1-1-1 being packed into
Body balance inlet and outlet 1-2-4, draws back extractor cylinder 1-2 that section corresponds to the be packed into position feed bin fluid entry holes 1-1-1
Wall is equipped with fluid reflux mouth 1-2-5;Each fluid inlet 1-2-2 is to connect on the extractor barrel wall of boosting or extraction section step by step
The entrance of continuous extraction sub-system 1, each fluid outlet 1-2-3 is continuous extraction on the extractor barrel wall of boosting or extraction section step by step
Take the outlet of subsystem 1;
Binning end locking device 1-3-A and storehouse end locking device 1-3-B is unloaded by dissection type clip and hydraulic or be driven by electricity
It constitutes;The dissection type clip quick-opening structure and binning end barrel end 1-2-A of binning end locking device 1-3-A and the lock of feed bin
Tight card slot 1-1-4, unloads the dissection type clip quick-opening structure of storehouse end locking device 1-3-B and unloads the circle of storehouse end barrel end 1-2-B
The locking card slot 1-1-4 Corresponding matching of ring flange and feed bin;
The connection relationship that continuous extraction subsystem 1 respectively forms are as follows:
Binning hydraulic cylinder 1-4-A, binning end locking device 1-3-A, extractor cylinder is successively sequentially fixedly mounted along axis
1-2, unload storehouse end locking device 1-3-B, unload storehouse hydraulic cylinder 1-4-B in rack, make binning hydraulic cylinder 1-4-A, binning end lock
Device 1-3-A, extractor cylinder 1-2, storehouse end locking device 1-3-B is unloaded, mutually coaxial, the binning end lock that unloads storehouse hydraulic cylinder 1-4-B
Tight device 1-3-A and binning barrel end 1-2-A matches, and unloads storehouse end locking device 1-3-B and unloads storehouse barrel end 1-2-B phase
Matching;
The fluid reflux mouth 1-2-5 on the extractor cylinder 1-2 barrel of fragment position is drawn back by pipe 7 and draws back shut-off valve
1-5-3 is connected with compressor 1-7 entrance is drawn back, and empties the stream socket 1- on the extractor cylinder 1-2 barrel of fragment position
2-1 divides two-way, all the way by pipe 7 and draw back switching valve 1-5-2 with draw back compressor 1-7 export be connected, another way passes through
Pipe 7 and emptying switching valve 1-5-1 are connected with drain pump 1-6 entrance, and drain pump 1-6 leads to atmosphere in outlet;Closely draw back section
Step pressure reducing section, i.e., the fluid balance inlet and outlet 1-2-4 of the 1st grade step pressure reducing section by pipe 7 with closely empty section by
Grade boosting or extraction section, i.e., the 1st grade boosting or the fluid inlet 1-2-2 of extraction section are connected step by step;Secondary suffer draws back section step by step
It is depressured section, i.e., the fluid balance inlet and outlet 1-2-4 of the 2nd grade step pressure reducing section passes through pipe 7 and the secondary boosting step by step for suffering emptying section
Or extraction section, i.e., the 2nd grade step by step boosting or the fluid inlet 1-2-2 of extraction section be connected, and so on, by whole step pressure reducings
The boosting step by step or extraction section that the fluid balance inlet and outlet 1-2-4 of section boosts by pipe 7 and step by step or the total series of extraction section subtracts 1
Fluid inlet correspondence be connected;
Extractor cylinder 1-2 outer wall coats insulating layer 1-8.
1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), N grades of isolated subsystem 3-N are
It is made of the isobaric isolated subsystem of a weight or double isobaric isolated subsystem, in which:
One weight equipressure isolated subsystem is by isobaric heat exchanger 3-E, the heavy separator 3-S-1 structure of a reheating device 3-H-1 and one
At fluid material for flow is stainless steel;The connection relationship respectively formed are as follows:
Isobaric heat exchanger 3-E cryogenic media entrance is the isobaric isolated subsystem entrance of a weight, and isobaric heat exchanger 3-E low temperature is situated between
Matter outlet is connected through pipe 7 with a reheating device 3-H-1 entrance, and the outlet a reheating device 3-H-1 is separated through pipe 7 with one again
Device 3-S-1 entrance is connected, and the outlet a weight separator 3-S-1 is connected through pipe 7 with isobaric heat exchanger 3-E high-temperature medium entrance
It connects, isobaric heat exchanger 3-E high-temperature medium outlet is the isobaric isolated subsystem outlet of a weight, and a heavy separator 3-S-1, which is equipped with, to be extracted out
Object outlet, and it is furnished with a heavy discharge valve 3-V-1.
Double equipressure isolated subsystem is by isobaric heat exchanger 3-E, a reheating device 3-H-1, a weight separator 3-S-1, two
Reheating device 3-H-2 and double separator 3-S-2 is constituted, and fluid material for flow is stainless steel;The connection relationship respectively formed are as follows:
Isobaric heat exchanger 3-E cryogenic media entrance is double isobaric isolated subsystem entrance, and isobaric heat exchanger 3-E low temperature is situated between
Matter outlet is connected through pipe 7 with a reheating device 3-H-1 entrance, and reheating device outlet 3-H-1 is separated through pipe 7 with one again
Device 3-S-1 entrance is connected, and the outlet a weight separator 3-S-1 is connected through pipe 7 with double heater 3-H-2 entrance, double
The outlet heater 3-H-2 is connected through pipe 7 with double separator 3-S-2 entrance, and the double outlet separator 3-S-2 is through pipe 7
It is connected with isobaric heat exchanger 3-E high-temperature medium entrance, isobaric heat exchanger 3-E high-temperature medium outlet is double isobaric separation subsystem
System outlet, a heavy separator 3-S-1 and double separator are respectively equipped with extract outlet, and are respectively provided with a heavy discharge valve 3-V-
1, double discharge valve 3-V-2.
1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1), N grades of pressurization cycles
Subsystem 2-N is made of subcritical pressurization cycle subsystem, in which:
Subcritical pressurization cycle subsystem is made of voltage-stablizer 2-B, circulating pump 2-P, cycle condenser 2-C, fluid overcurrent
Material is stainless steel;The connection relationship respectively formed are as follows:
Cycle condenser 2-C entrance is subcritical pressurization cycle subsystem main-inlet, and cycle condenser 2-C is exported through pipe
7 are connected with circulating pump 2-P entrance, and pipe 7 is equipped with subcritical increasing between the outlet cycle condenser 2-C and circulating pump 2-P entrance
Cycle subsystem sub-inlet is pressed, circulating pump 2-P divides two-way in outlet, is connected all the way through pipe 7 with voltage-stablizer 2-B inlet and outlet, separately
It is exported all the way for subcritical pressurization cycle subsystem.
Connection relationship between above each subsystem are as follows:
Subcritical fluids medium source 5 exports, i.e. the outlet outlet valve 5-4-2 is connected through pipe 7 with pressurization 4 entrance of subsystem
It connects, pressurization subsystem 4, which corresponds to continuous extraction subsystem, N number of outlet, and each outlet is through pipe 7 and corresponding 1 grade of pressurization cycle
Subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1), N grades of pressurization cycle subsystem 2-N sub-inlet be respectively connected with
Connect, 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1), N grades of pressurization cycle subsystem 2-N masters
Entrance through pipe 7 and 1 grade switching valve 6-1-1 ..., N-1 grades of switching valve 6-1- (N-1), N grades of switching valve 6-1-N with corresponding 1 grade
Isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), the outlet N grades of isolated subsystem 3-N be respectively connected with, 1 fraction
Ion system 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), N grades of isolated subsystem 3-N entrance through pipe 7 and continuous extraction
The outlet of the corresponding pressure grade of subsystem 1 is connected, 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2-
(N-1), the N grades of outlets pressurization cycle subsystem 2-N are connected through pipe 7 with the entrance of the corresponding pressure grade of continuous extraction subsystem 1
Connect, at the same 1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), N grades of isolated subsystem 3-N outlet difference
Be each separated into two-way through N pipe 7, all the way through 1 grade of return valve 6-2-1 ..., N-1 grades of return valve 6-2- (N-1), N grades of return valves
The entrance of the entrance of 6-2-N and same subcritical fluids medium source 5, i.e., total return valve 5-4-3 is connected, and another way is through 1 grade
Switching valve 6-1-1 ..., N-1 grades of switching valve 6-1- (N-1), N grades of switching valve 6-1-N and 1 grade of pressurization cycle subsystem 2-1 ...,
The outlet of N-1 grades of pressurization cycle subsystem 2- (N-1), N grades of pressurization cycle subsystem 2-N is connected, and corresponds to segregants at different levels
Exhaust-valve 6-0 is housed on the reflux valve outlet of system and the connecting line of subcritical fluids medium source inlet.
Using the extraction and separation technology of the multistage continuous isobaric extraction separation device system of subcritical fluids a kind of, steps are as follows:
(1) the liquefaction storage tank 5-1 in subcritical fluids medium source 5 is emptied, is full of subcritical fluids medium by regulation, and open
Refrigeration machine 5-3 is opened, subcritical fluids medium is liquefied;
(2) sealing ring 1-1-6 will be installed in the seal groove of each feed bin 1-1;Binning end locking device 1-3-A is opened, is used
Binning hydraulic cylinder 1-4-A by the inner cavity extractor cylinder 1-2 of empty feed bin 1-1 push-in continuous extraction subsystem 1, works as extractor one by one
After cylinder 1-2 fills inner cavity sky feed bin 1-1, starts the feed bin 1-1 that push-in one by one is equipped with extract, need when drawing back a section exterior
After unloading discharging bin 1-1-B, locks 1 binning end locking device 1-3-A of continuous extraction subsystem and unload storehouse end locking device 1-3-B;
(3) the total return valve 5-4-3 of 5 entrance of subcritical fluids medium source is closed, 1 grade for opening 1 grade of isolated subsystem 3-1 returns
Flow valve 6-2-1 ..., the N-1 grade return valve 6-2- (N-1) of N-1 grades of isolated subsystem 3- (N-1), N grades of isolated subsystem 3-N
N grades of return valve 6-2-N, close 1 grade of pressurization cycle subsystem 2-1 1 grade of switching valve 6-1-1 ..., N-1 grades of pressurization cycle subsystems
The N grade switching valve 6-1-N of the N-1 grade switching valve 6-1- (N-1) and N grades of pressurization cycle subsystem 2-N of system 2- (N-1), the row of unlatching
Empty valve 6-0 opens the outlet valve 5-4-2 that subcritical fluids medium source 5 exports, and continuous extraction subsystem 1 and 1 grade of segregant is discharged
System 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), the air in N grades of isolated subsystem 3-N;Continuous extraction subsystem 1 and
1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1), after air empties in N grades of isolated subsystem 3-N, open
1 grade of switching valve 6-1-1 of 1 grade of pressurization cycle subsystem 2-1 ..., the N-1 grade switchings of N-1 grades of pressurization cycle subsystem 2- (N-1)
The N grade switching valve 6-1-N of valve 6-1- (N-1) and N grades of pressurization cycle subsystem 2-N, are discharged 1 grade of pressurization cycle subsystem 2-
1 ..., the air in N-1 grades of pressurization cycle subsystem 2- (N-1) and N grades of pressurization cycle subsystem 2-N, until emptying, is then closed
Close 1 grade of isolated subsystem 3-1 1 grade of return valve 6-2-1 ..., the N-1 grade return valve 6- of N-1 grades of isolated subsystem 3- (N-1)
The N grade return valve 6-2-N of 2- (N-1), N grades of isolated subsystem 3-N close exhaust-valve 6-0;
(4) starting pressurization subsystem 4, so that in each feed bin of boosting or extraction section step by step in continuous extraction subsystem 1
1-1 and its feed bin 1-1 and matched 1 grade of isolated subsystem 3-1 of corresponding step pressure reducing section ..., N-1 grades of isolated subsystems
3- (N-1), N grades of isolated subsystem 3-N and 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1)
Reach setting value with the pressure in N grades of pressurization cycle subsystem 2-N;
(5) start 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1) and N grades of pressurizations follow
Loop subsystems 2-N, in continuous extraction subsystem 1 step by step boosting or No. 11 grade of boosting of extraction section or extraction feed bin 1-1-A-1-1,
No. 21 grade boosting or extraction feed bin 1-1-A-1-2 ..., n1- No. 11 grade of boosting or extraction feed bin 1-1-A-1- (n1-1)、n1Number 1 grade
Boosting or extraction feed bin 1-1-A-1-n1..., -1, No. 2 N-1 grades of boosting of No. 1 N-1 grades of boostings or extraction feed bin 1-1-A- (N-1)
Or extraction feed bin 1-1-A- (N-1) -2 ..., nN-1- No. 1 N-1 grades of boosting or extraction feed bin 1-1-A- (N-1)-(nN-1-1)、nN-1
Numbers N-1 grades boostings or extraction feed bin 1-1-A- (N-1)-nN-1, No. 1 N grades feed bin 1-1-A-N-1 that boost or extract, No. 2 N grades of boostings
Or extraction feed bin 1-1-A-N-2 ..., nN- No. 1 N grades of boosting or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or extraction
Feed bin 1-1-A-N-nNIt carries out corresponding subcritical fluids to extract step by step, complete in each boostings at different levels or extraction section feed bin of extraction
Subcritical fluids enter corresponding 1 grade of isolated subsystem 3-1 ..., N-1 grade isolated subsystem 3- (N-1) and N grades separate
Subsystem 3-N is separated, periodically turn on 1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1) and N
The grade isolated subsystem 3-N matched heavy discharge valve 3-V-1 and double discharge valve 3-V-2 of weight discharge valve 3-V-1 or one of institute, is unloaded
Out 1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N institutes are individually separated comes out
Extract;
(6) feed bin in the boosting step by step or extraction section near step pressure reducing section, i.e. extraction feed bin 1-1-A-N-nNIt reaches
When to the extraction process time, switching valve 1-5-2 is drawn back in closing, opens emptying switching valve 1-5-1, starts drain pump 1-6, at emptying
In the air of the emptying feed bin 1-1-A-0 of 1 extractor cylinder 1-2 internal vent section of continuous extraction subsystem;Close emptying switching
Valve 1-5-1 closes drain pump 1-6;
(7) binning hydraulic cylinder 1-4-A piston rod is retracted, in binning hydraulic cylinder 1-4-A and binning end locking device 1-3-A institute
It is packed between the emptying feed bin 1-1-A-0 of locking and is housed to feed bin 1-1-A equipped with extract, stretch out binning hydraulic cylinder 1-4-A
What piston rod and holding out against newly was packed into is housed to feed bin 1-1-A;Stretching, which is unloaded storehouse hydraulic cylinder 1-4-B piston rod and held out against, unloads the locking of storehouse end
The discharging bin 1-1-B to be unloaded that device 1-3-B is locked;It is synchronous to open binning end locking device 1-3-A and unload storehouse end locking device
1-3-B;Synchronize and continue to stretch out binning hydraulic cylinder 1-4-A piston rod and retraction and unload storehouse hydraulic cylinder 1-4-B piston rod, be newly packed into
It is packed into feed bin 1-1-A and is loaded into the 1 extractor inner cavity cylinder 1-2 of continuous extraction subsystem as new emptying feed bin 1-1-A-0, original
No. 11 grade of boosting or extraction feed bin 1-1-A-1-1 that feed bin 1-1-A-0 becomes new are emptied, and so on, until former draw back section
Draw back the discharging bin 1-1-B to be unloaded that feed bin 1-1-B-0 becomes new;Synchronous locking binning end locking device 1-3-A is locked with storehouse end is unloaded
Tight device 1-3-B;Storehouse hydraulic cylinder 1-4-A piston rod is unloaded in retraction, unloads the original discharging bin 1-1-B to be unloaded being ejected;
(8) emptying switching valve 1-5-1 is opened, drain pump 1-6 is started, emptying is in 1 extractor cylinder of continuous extraction subsystem
The air of the emptying feed bin 1-1-A-0 of body 1-2 internal vent section;Emptying switching valve 1-5-1 is closed, drain pump 1-6 is closed;
(9) it opens and draws back shut-off valve 1-5-3 and draw back switching valve 1-5-2, be in 1 extractor cylinder of continuous extraction subsystem
1-2 draws back inner cavity the subcritical fluids for drawing back feed bin 1-1-B-0 of section or supercritical fluid medium flows into everywhere in continuous extraction
The emptying feed bin 1-1-A-0 of 1 extractor cylinder 1-2 internal vent section of subsystem, when draw back feed bin 1-1-B-0 and emptying feed bin 1-
After 1-A-0 pressure balance, compressor 1-7 is drawn back in unlatching, until drawing back the subcritical fluids medium whole quilt in feed bin 1-1-B-0
It is withdrawn into emptying feed bin 1-1-A-0, closing draws back shut-off valve 1-5-3 and draws back switching valve 1-5-2, and compressor 1-7 is drawn back in closing;
(10) (7) step~the (9) step is repeated, so that being housed to feed bin 1-1-A quilt equipped with the extract not extracted
It is periodically packed into continuous extraction subsystem 1, the discharging bin 1-1-B to be unloaded after having extracted synchronously is drawn off continuous extraction subsystem
System 1, in this course, each feed bin 1-1 of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem be successively in emptying section,
Boosting or extraction section, step pressure reducing section and section is drawn back step by step, the feed bin 1-1 continuously pushed successively completes air evacuating in section
Emptying, 1 grade to N grades step by step boosting or extraction section in complete extract 1 grade of subcritical fluids to N stage pressure grade by
Grade extraction, is drawing back completion subcritical fluids medium in section at the step pressure reducing that N-1 pressure stage is completed in step pressure reducing section
The continuous operation drawn back;It completes subcritical fluids extracted in the feed bin 1-1 of extraction and enters corresponding 1 grade of isolated subsystem
3-1 ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N be initially separated, periodically turn on 1 grade of separation
Subsystem 3-1 ..., N-1 grades of isolated subsystem 3- (N-1) and the N grades of matched heavy discharge valve 3-V-1 of isolated subsystem 3-N institute
Or a heavy discharge valve 3-V-1 and double discharge valve 3-V-2, draw off 1 grade of isolated subsystem 3-1 ..., N-1 grades of isolated subsystem 3-
(N-1) and N grades of isolated subsystem 3-N the individually separated extract come out.
Typical subcritical fluids medium selects carbon dioxide, the continuous isobaric extraction and separation pressure of highest subcritical carbon dioxide
Power is 32MPa, and differential every stage pressure grade is 8MPa, then in the multistage continuous isobaric extraction separation device system of subcritical fluids by
Grade boosting or extraction section series N are 4, each pressure stage, i.e. the subcritical fluid extraction temperature of 8MPa, 16MPa, 24MPa, 32MPa
For 35 DEG C of 32 DEG C, 35 DEG C of a weight separation temperature or a weight separation temperature and 40 DEG C of double separation temperature;Each pressure stage pressurization follows
Loop subsystems and isolated subsystem are then respectively 1 grade of pressurization cycle subsystem 2-1,2 grades of pressurization cycle subsystem 2-2,3 grades of pressurizations
Cycle subsystem 2-3,4 grades of pressurization cycle subsystem 2-4 and 1 grade of isolated subsystem 3-1,2 grades of isolated subsystem 3-2,3 grades of separation
Subsystem 3-3,4 grades of isolated subsystem 3-4;Distinguish with each pressure stage pressurization cycle subsystem and the matched valve of isolated subsystem
For 2 grades of switching valve 6-1-2,3 of 1 grade of switching valve 6-1-1 of 1 grade of pressurization cycle subsystem 2-1,2 grades of pressurization cycle subsystem 2-2
3 grades of switching valve 6-1-3 of grade pressurization cycle subsystem 2-3,4 grades of switching valve 6-1-4 of 4 grades of pressurization cycle subsystem 2-4 and 1 grade
2 grades of return valve 6-2-2, the 3 grades of isolated subsystems of 1 grade of return valve 6-2-1 of isolated subsystem 3-1,2 grades of isolated subsystem 3-2
4 grades of return valve 6-2-4 of 3 grades of return valve 6-2-3 of 3-3,4 grades of separation system 3-4;1 extractor cylinder of continuous extraction subsystem
1 grade of feed bin 1-1 that boosting or extraction section are packed into step by step to 4 stage pressure grades is two, i.e. n in 1-21=n2=n3=n4
=2, remaining each section, that is, emptying section, 1 grade to 3 grades of step pressure reducing section and drawing back the feed bin 1-1 that section is packed into is respectively 1.
Embodiment two: a kind of continuously isobaric extraction separation device system and the process flow of subcritical fluids single-stage, as Fig. 1,
Shown in Fig. 2, Fig. 4, Fig. 6, Fig. 7, Figure 10, Figure 11.
A kind of subcritical fluids single-stage continuously isobaric extraction separation device system by subcritical fluids medium source 5, pressurized
System 4,1,1 grade of isolated subsystem 3-1 of continuous extraction subsystem ..., N-1 grades of isolated subsystem 3- (N-1), N fraction ionization series
Unite 3-N and 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1), N grades of pressurization cycle subsystems
2-N is constituted, and N is boosting step by step or the total series of extraction in system, and N is greater than 2, the subcritical fluid extraction in the embodiment system
It is overlapped with the N pressure stage to boost step by step.
The composition in the subcritical fluids medium source 5 is the same as embodiment one.
The composition of the pressurization subsystem 4 is the same as embodiment one.
The composition of the continuous extraction subsystem 1 is as in the first embodiment, wherein:
From the binning end of continuous extraction subsystem 1, it is packed into the feed bin of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem
1-1 number consecutively are as follows: be housed to feed bin 1-1-A;Empty the emptying feed bin 1-1-A-0 of section;Boosting or No. 11 of extraction section step by step
Grade boosting or extraction feed bin 1-1-A-1-1 ..., No. 1 N-1 grade boosting or extraction feed bin 1-1-A- (N-1) -1, No. 1 N grades boost or
Extract feed bin 1-1-A-N-1, No. 2 N grade boosting or extract feed bin 1-1-A-N-2 ..., nN- No. 1 N grades of boosting or extraction feed bin 1-
1-A-N-(nN-1)、nNNumbers N grades boostings or extraction feed bin 1-1-A-N-nN;The N-1 grade of step pressure reducing section is depressured feed bin 1-1-B-
(N-1) ..., 1 grade of decompression feed bin 1-1-B-1;That draws back section draws back feed bin 1-1-B-0;Discharging bin 1-1-B to be unloaded.
1 grade of described isolated subsystem 3-1 to the N-1 grades of isolated subsystem 3- (N-1) is made of no isolated subsystem,
In:
No isolated subsystem is made of connecting pipe 7, and material is stainless steel, and 7 entrance of pipe is without separation subsystem
System entrance, the outlet of pipe 7 are the outlet of no isolated subsystem.
The N grade isolated subsystem 3-N is by the isobaric isolated subsystem of a weight or double isobaric isolated subsystem structure
At composition is the same as embodiment one.
1 grade of described pressurization cycle subsystem 2-1 to the N-1 grades of pressurization cycle subsystem 2- (N-1) is by subcritical without pumping
Pressurization cycle subsystem is constituted, in which:
It is made of without subcritical pressurization cycle subsystem is pumped voltage-stablizer 2-B, check valve 2-CV, fluid material for flow is not
Become rusty steel;The connection relationship respectively formed are as follows:
Check valve 2-CV entrance is without the subcritical pressurization cycle subsystem main-inlet of pump, and the outlet check valve 2-CV passes through pipe
7 are divided into three tunnels, and the first via is connected with voltage-stablizer 2-B inlet and outlet, and the second tunnel is to enter without the subcritical pressurization cycle subsystem pair of pump
Mouthful, third Lu Weiwu pumps subcritical pressurization cycle subsystem outlet.
The N grade pressurization cycle subsystem 2-N is made of subcritical pressurization cycle subsystem, and same embodiment is constituted
One.
Connection relationship between above each subsystem is the same as embodiment one.
The extraction and separation technology of the present embodiment technical solution are as follows:
(1) with one step of embodiment (1);
(2) with one step of embodiment (2);
(3) with one step of embodiment (3);
(4) with one step of embodiment (4);
(5) 1 grades of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1) it is in operating status, even
Continue 1 grade to N-1 grades in the extraction sub-system 1 No. 11 grade feed bin 1-1-A-1- that boosts or extract of boosting or extraction section step by step
1 ..., No. 1 N-1 grades boosting or extraction feed bin 1-1-A- (N-1) -1 and 1 grade of isolated subsystem 3-1 ..., N-1 fraction ionization series
System 3- (N-1) and 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grade pressurization cycle subsystem 2- (N-1) correspondence be connected to, holding is respectively
The relevant pressure grade of each boosting of grade or extraction feed bin is constant;Start N grades of pressurization cycle subsystem 2-N, in continuous extraction subsystem 1
N grade boost step by step or extraction section No. 1 N grades boosting or extraction feed bin 1-1-A-N-1, No. 2 N grade boosting or extract feed bin 1-1-
A-N-2、…、nN- No. 1 N grades of boosting or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or extraction feed bin 1-1-A-N-nN
Subcritical fluid extraction is carried out, the n of extraction is completedNSubcritical fluids in a N grades of boosting or extraction feed bin enter N grades of segregants
System 3-N is separated, and the N grades of matched dischargings again of weight discharge valve 3-V-1 or one of isolated subsystem 3-N institute are periodically turned on
Valve 3-V-1 and double discharge valve 3-V-2 draws off the separated extract come out of N grades of isolated subsystem 3-N;
(6) with one step of embodiment (6);
(7) with one step of embodiment (7);
(8) with one step of embodiment (8);
(9) with one step of embodiment (9);
(10) (7) step~the (9) step is repeated, so that being housed to feed bin 1-1-A quilt equipped with the extract not extracted
It is periodically packed into continuous extraction subsystem 1, the discharging bin 1-1-B to be unloaded after having extracted synchronously is drawn off continuous extraction subsystem
System 1, in this course, each feed bin 1-1 of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem be successively in emptying section,
Boosting or extraction section, step pressure reducing section and section is drawn back step by step, the feed bin 1-1 continuously pushed successively completes air evacuating in section
Emptying, 1 grade to N-1 grades step by step boosting or extraction section in complete 1 grade to the boosting step by step of N-1 stage pressure grade, at N grades step by step
The subcritical fluid extraction of the N stage pressure grade of extract is completed in boosting or extraction section, N-1 are completed in step pressure reducing section
The step pressure reducing of pressure stage is drawing back the continuous operation drawn back that subcritical fluids medium is completed in section;Complete the feed bin of extraction
Subcritical fluids extracted enter N grades of isolated subsystem 3-N and are initially separated in 1-1, periodically turn on N grades of isolated subsystems
The matched heavy discharge valve 3-V-1 and double discharge valve 3-V-2 of weight discharge valve 3-V-1 or one of 3-N institute, draws off N fraction ionization series
The separated extract come out of the 3-N that unites.
Typical subcritical fluids medium selects carbon dioxide, and continuously isobaric extraction and separation pressure is subcritical carbon dioxide
50MPa, the differential every stage pressure grade boosted step by step is 10MPa, then the continuous isobaric extraction separation device system of subcritical fluids single-stage
The series of boosting step by step N in system is 5,1 grade to N-1 stage pressure grade, the i.e. subcritical fluids of 10MPa, 20MPa, 30MPa, 40MPa
Temperature is 32 DEG C, N stage pressure grade, i.e. the subcritical fluid extraction temperature of 50MPa is 32 DEG C, 35 DEG C of a weight separation temperature or one
35 DEG C of weight separation temperature and 40 DEG C of double separation temperature;Each pressure stage pressurization cycle subsystem and isolated subsystem are then respectively 1
Grade pressurization cycle subsystem 2-1,2 grades of pressurization cycle subsystem 2-2,3 grades of pressurization cycle subsystem 2-3,4 grades of pressurization cycle subsystems
Unite 2-4,5 grades of pressurization cycle subsystem 2-5 and 1 grade of isolated subsystem 3-1,2 grades of isolated subsystem 3-2,3 grades of isolated subsystem 3-
3,4 grades of isolated subsystem 3-4,5 grades of isolated subsystem 3-5;It is matched with each pressure stage pressurization cycle subsystem and isolated subsystem
Valve be respectively 1 grade of switching valve 6-1-1 of 1 grade of pressurization cycle subsystem 2-1,2 grades of 2 grades of pressurization cycle subsystem 2-2 cut
Change 4 grades of switchings of valve 6-1-2,3 grades of switching valve 6-1-3 of 3 grades of pressurization cycle subsystem 2-3,4 grades of pressurization cycle subsystem 2-4
1 grade of return valve 6-2- of the 5 grades of switching valve 6-1-5 and 1 grade of isolated subsystem 3-1 of valve 6-1-4,5 grades of pressurization cycle subsystem 2-5
1,3 grades of return valve 6-2-3, the 4 grades of segregative lines of 2 grades of return valve 6-2-2 of 2 grades of isolated subsystem 3-2,3 grades of isolated subsystem 3-3
Unite 4 grades of return valve 6-2-4 of 3-4,5 grades of return valve 6-2-5 of 5 grades of separation system 3-5;1 extractor cylinder of continuous extraction subsystem
1 grade of feed bin 1-1 that boosting or extraction section are packed into step by step to 4 stage pressure grades is 1, i.e. n in body 1-21=n2=n3=n4
The feed bin 1-1 that boosting or extraction section are packed into step by step of=1,5 stage pressure grades is 4, i.e. n5=4, it remaining each section, that is, empties
Section, 1 grade to 4 grades of step pressure reducing section and to draw back the feed bin 1-1 that section is packed into be respectively 1.
A kind of embodiment three: multistage continuous isobaric extraction separation device system of the subcritical fluids of supercritical fluid pre-extracted
And process flow, as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Figure 11.
A kind of multistage continuously isobaric extraction separation device system of subcritical fluids of supercritical fluid pre-extracted is by subcritical
Fluid media source 5, pressurization subsystem 4,1,1 grade of isolated subsystem 3-1 of continuous extraction subsystem ..., N-1 grades of isolated subsystem 3-
(N-1), N grades of isolated subsystem 3-N and 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-1),
N grades of pressurization cycle subsystem 2-N are constituted, and N is that the boosting step by step or the total series of extraction, N in system are greater than 2, the embodiment system
In supercritical fluid and subcritical fluids extraction step by step with step by step boosting be overlapped.
The composition in the subcritical fluids medium source 5 is the same as embodiment one.
The composition of the pressurization subsystem 4 is the same as embodiment one.
The composition of the continuous extraction subsystem 1 is the same as embodiment one.
1 grade of isolated subsystem 3-1 is by a heavy transformation isolated subsystem or double transformation isolated subsystem structure
At, in which:
One weight transformation isolated subsystem resets pressure valve 3-VC-1, the heavy separator 3-S- of a weight heat exchanger 3-HC-1 and one by one
1 is constituted, and fluid material for flow is stainless steel;The connection relationship respectively formed are as follows:
One resets pressure valve 3-VC-1 entrance as a heavy transformation isolated subsystem entrance, and one resets the outlet pressure valve 3-VC-1 through pipe
Son 7 is connected with a heavy heat exchanger 3-HC-1 entrance, and a weight heat exchanger 3-HC-1 is exported through pipe 7 and a heavy separator 3-S-1
Entrance is connected, and the outlet a weight separator 3-S-1 is a heavy transformation isolated subsystem outlet, and a heavy separator 3-S-1 is equipped with extraction
Object exports out, and is furnished with a heavy discharge valve 3-V-1;
Double transformation isolated subsystem resets pressure valve 3-VC-1, a weight heat exchanger 3-HC-1, a heavy separator 3-S- by one
1, double pressure regulator valve 3-VC-2, double heat exchanger 3-HC-2 and double separator 3-S-2 are constituted, and fluid material for flow is stainless
Steel;The connection relationship respectively formed are as follows:
One resets pressure valve 3-VC-1 entrance as double transformation isolated subsystem entrance, and one resets the outlet pressure valve 3-VC-1 through pipe
Son 7 is connected with a heavy heat exchanger 3-HC-1 entrance, and a weight heat exchanger 3-HC-1 is exported through pipe 7 and a heavy separator 3-S-1
Entrance is connected, and the outlet a weight separator 3-S-1 is connected through pipe 7 with double pressure regulator valve 3-VC-2 entrance, double pressure regulator valve
The outlet 3-VC-2 is connected through pipe 7 with double heat exchanger 3-HC-2 entrance, and the double outlet heat exchanger 3-HC-2 is through pipe 7 and two
Weight separator 3-S-2 entrance is connected, and the double outlet separator 3-S-2 is that double transformation isolated subsystem exports, and one separates again
Device 3-S-1 and double separator 3-S-2 is respectively equipped with extract outlet, and is respectively provided with a heavy discharge valve 3-V-1 and double unloads
Expect valve 3-V-2.
2 grades of described isolated subsystem 3-2 to the N grades of isolated subsystem 3-N are by the isobaric isolated subsystem or two of a weight
Weight equipressure isolated subsystem is constituted, the same embodiment of composition of the isobaric isolated subsystem of a weight or double isobaric isolated subsystem
One.
1 grade of pressurization cycle subsystem 2-1 is made of overcritical pressurization cycle subsystem, in which:
Overcritical pressurization cycle subsystem is by transformation heat exchanger 2-E, cycle condenser 2-C, circulating pump 2-P, cycle heat exchange
Device 2-HC is constituted, and fluid material for flow is stainless steel;The connection relationship respectively formed are as follows:
Transformation heat exchanger 2-E low-pressure medium entrance is overcritical pressurization cycle subsystem main-inlet, and transformation heat exchanger 2-E is low
Pressure media outlet is connected through pipe 7 with cycle condenser 2-C entrance, and cycle condenser 2-C is exported through pipe 7 and circulating pump 2-
P entrance is connected, and pipe 7 is equipped with overcritical pressurization cycle subsystem between the outlet cycle condenser 2-C and circulating pump 2-P entrance
Sub-inlet, the outlet circulating pump 2-P are connected through pipe 7 with transformation heat exchanger 2-E high-pressure medium entrance, transformation heat exchanger 2-E high
Pressure media outlet is connected through pipe 7 with circulation heat exchanger 2-HC entrance, and the outlet circulation heat exchanger 2-HC is that overcritical pressurization follows
Loop subsystems outlet.
2 grades of pressurization cycle subsystems to N grades of pressurization cycle subsystem 2-N be by subcritical pressurization cycle subsystem
It constitutes, the composition of subcritical pressurization cycle subsystem is the same as embodiment one.
Connection relationship between above-mentioned each subsystem is the same as embodiment one.
The extraction and separation technology of the present embodiment technical solution are as follows:
(1) with one step of embodiment (1);
(2) with one step of embodiment (2);
(3) with one step of embodiment (3);
(4) with one step of embodiment (4);
(5) start 1 grade of pressurization cycle subsystem 2-1,1 grade in continuous extraction subsystem 1 step by step boosting or extraction section 1
Number 1 grade boosting or extraction feed bin 1-1-A-1-1, No. 21 grade of boostings or extraction feed bin 1-1-A-1-2 ..., n1- No. 11 grade of boosting
Or extraction feed bin 1-1-A-1- (n1-1)、n1Number 1 grade boosting or extraction feed bin 1-1-A-1-n1With 1 grade of isolated subsystem 3-1 and 1
The corresponding connection of grade pressurization cycle subsystem 2-1, carries out supercritical fluid extraction, completes No. 11 grade of boosting or the extraction feed bin of extraction
1-1-A-1-1, No. 21 grade boosting or extraction feed bin 1-1-A-1-2 ..., n1- No. 11 grade of boosting or extraction feed bin 1-1-A-1-
(n1-1)、n1Number 1 grade boosting or extraction feed bin 1-1-A-1-n1In supercritical fluid enter 1 grade of isolated subsystem 3-1 divided
From periodically turning on the heavy discharge valve 3-V-1 of 1 grade of matched weight discharge valve 3-V-1 or one of isolated subsystem 3-1 institute and double
Discharge valve 3-V-2 draws off the separated extract come out of 1 grade of isolated subsystem 3-1;Start 2 grades of pressurization cycle subsystem 2-
2 ..., N-1 grades of pressurization cycle subsystem 2- (N-1) and N grades of pressurization cycle subsystem 2-N, in continuous extraction subsystem 12 grades to N
Grade is boosted step by step or No. 12 grades of boostings or extraction feed bin 1-1-A-2-1, No. 22 grades of boostings or extraction feed bin 1-1-A- of extraction section
2-2、…、n2- No. 12 grades of boosting or extraction feed bin 1-1-A-2- (n2-1)、n2Numbers 2 grades boostings or extraction feed bin 1-1-A-2-
n2..., -1, No. 2 N-1 grades of boosting of No. 1 N-1 grades of boostings or extraction feed bin 1-1-A- (N-1) or extraction feed bin 1-1-A- (N-1) -
2、…、nN-1- No. 1 N-1 grades of boosting or extraction feed bin 1-1-A- (N-1)-(nN-1-1)、nN-1Numbers N-1 grades boostings or extraction feed bin 1-
1-A-(N-1)-(nN-1), No. 1 N grades of boostings or extraction feed bin 1-1-A-N-1, No. 2 N grades of boostings or extraction feed bin 1-1-A-N-
2、…、nN- No. 12 grades of boosting or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or extraction feed bin 1-1-A-N-nNIt carries out
Corresponding subcritical fluids extract step by step, and each subcritical fluids boosted or extracted in feed bin at different levels for completing to extract enter opposite
2 grades of isolated subsystem 3-2 answering ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N separated, week
Open to phase property 2 grades of isolated subsystem 3-2 ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N are matched
A weight discharge valve 3-V-1 or one heavy discharge valve 3-V-1 and double discharge valve 3-V-2, draw off 2 grades of isolated subsystem 3-
2 ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N the individually separated extract come out;
(6) with one step of embodiment (6);
(7) with one step of embodiment (7);
(8) with one step of embodiment (8);
(9) with one step of embodiment (9);
(10) (7) step~the (9) step is repeated, so that being housed to feed bin 1-1-A quilt equipped with the extract not extracted
It is periodically packed into continuous extraction subsystem 1, the discharging bin 1-1-B to be unloaded after having extracted synchronously is drawn off continuous extraction subsystem
System 1, in this course, each feed bin 1-1 of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem be successively in emptying section,
Boosting or extraction section, step pressure reducing section and section is drawn back step by step, the feed bin 1-1 continuously pushed successively completes air evacuating in section
Emptying, 1 grade step by step boosting or extraction section in complete extract 1 stage pressure grade supercritical fluid extraction, at 2 grades extremely
N grades boosting or the interior 2 grades of subcritical fluids to N stage pressure grade for completing extract of extraction section extract, step by step step by step step by step
The step pressure reducing of N-1 pressure stage is completed in decompression section, is drawing back the continuous behaviour drawn back that subcritical fluids medium is completed in section
Make;The supercritical fluid completed in the feed bin 1-1 of supercritical fluid extraction is separated into 1 grade of isolated subsystem 3-1, the period
Property open 1 grade of isolated subsystem 3-1 matched heavy discharge valve 3-V-1 of weight discharge valve 3-V-1 or one of institute and double discharge valve
3-V-2 draws off the separated extract come out of 1 grade of isolated subsystem 3-1;2 grades of subcritical fluids to N stage pressure grade is completed to extract
Feed bin 1-1 in subcritical fluids it is corresponding enter 2 grades of isolated subsystem 3-2 ..., N-1 grades of isolated subsystem 3- (N-1) and N
Grade isolated subsystem 3-N separated, periodically turn on 2 grades of isolated subsystem 3-2 ..., N-1 grades of isolated subsystem 3- (N-
And the N grades of matched heavy discharge valve 3-V-1 and double discharge valve 3-V- of weight discharge valve 3-V-1 or one of isolated subsystem 3-N institute 1)
2, draw off 2 grades of isolated subsystem 3-2 ..., N-1 grades of isolated subsystem 3- (N-1) and N grades of isolated subsystem 3-N it is separated come out
Extract.
Typical supercritical fluid medium and subcritical fluids medium select carbon dioxide, and highest subcritical carbon dioxide connects
Continuous equipressure extraction and separation pressure is 50MPa, and differential every stage pressure grade is 10MPa, then the sub-critical flow of supercritical fluid pre-extracted
The series of boosting step by step N in the multistage continuous isobaric extraction separation device system of body is 5;The supercritical fluid extraction of 1 stage pressure grade
Pressure 10MPa, temperature be 50 DEG C, a weight separating pressure 8MPa, temperature 60 C or a heavy separating pressure 8MPa, temperature 60 C and
65 DEG C of double separating pressure 6MPa, temperature;2 grades to N stage pressure grade, the i.e. sub-critical flow of 20MPa, 30MPa, 40MPa, 50MPa
Body extraction temperature is 35 DEG C of 32 DEG C, 35 DEG C of a weight separation temperature or a weight separation temperature and 40 DEG C of double separation temperature;Each pressure
Power grade pressurization cycle subsystem and isolated subsystem are then respectively 1 grade of pressurization cycle subsystem 2-1,2 grades of pressurization cycle subsystems
2-2,3 grades of pressurization cycle subsystem 2-3,4 grades of pressurization cycle subsystem 2-4,5 grades of pressurization cycle subsystem 2-5 and 1 grade of segregant
System 3-1,2 grades of isolated subsystem 3-2,3 grades of isolated subsystem 3-3,4 grades of isolated subsystem 3-4,5 grades of isolated subsystem 3-5;
With each pressure stage pressurization cycle subsystem and the matched valve of isolated subsystem are respectively 1 grade of pressurization cycle subsystem 2-1 1 grade
Switching valve 6-1-1,2 grades of switching valve 6-1-2 of 2 grades of pressurization cycle subsystem 2-2,3 grades of 3 grades of pressurization cycle subsystem 2-3 cut
Change 5 grades of switchings of valve 6-1-3,4 grades of switching valve 6-1-4 of 4 grades of pressurization cycle subsystem 2-4,5 grades of pressurization cycle subsystem 2-5
2 grades of return valve 6-2-2,3 of 1 grade of return valve 6-2-1 of valve 6-1-5 and 1 grade of isolated subsystem 3-1,2 grades of isolated subsystem 3-2
4 grades of return valve 6-2-4, the 5 grades of separation system 3-5 of 3 grades of return valve 6-2-3 of grade isolated subsystem 3-3,4 grades of separation system 3-4
5 grades of return valve 6-2-5;1 grade of boosting step by step or extraction to 5 stage pressure grades in 1 extractor cylinder 1-2 of continuous extraction subsystem
The feed bin 1-1 that section is packed into is 2, i.e. n1=n2=n3=n4=n5=2, remaining each section, i.e., emptying section, 1 grade to 4 grades by
It is respectively 1 that grade, which is depressured section and draws back the feed bin 1-1 that section is packed into,.
A kind of example IV: the continuous isobaric extraction separation device system of the subcritical fluids single-stage of supercritical fluid pre-extracted
And process flow, as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Fig. 9, Figure 10, Figure 11.
Continuously isobaric extraction separation device system is faced by Asia for a kind of subcritical fluids single-stage of supercritical fluid pre-extracted
Boundary fluid media source 5, pressurization subsystem 4,1,1 grade of isolated subsystem 3-1 of continuous extraction subsystem ..., N-1 grades of isolated subsystems
3- (N-1), N grades of isolated subsystem 3-N and 1 grade of pressurization cycle subsystem 2-1 ..., N-1 grades of pressurization cycle subsystem 2- (N-
1), the system that N grades of pressurization cycle subsystem 2-N are constituted is completed, and N is that the boosting step by step or the total series of extraction, N in system are greater than 2,
Supercritical fluid extraction in system is overlapped with the boosting step by step of N-2 stage pressure grade, the subcritical fluids in the embodiment system
Extraction is overlapped with the N stage pressure grade boosted step by step.
The composition in the subcritical fluids medium source 5 is the same as embodiment one.
The composition of the pressurization subsystem 4 is the same as embodiment one.
The composition of the continuous extraction subsystem 1 is as in the first embodiment, wherein:
From the binning end of continuous extraction subsystem 1, it is packed into the feed bin of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem
1-1 number consecutively are as follows: be housed to feed bin 1-1-A;Empty the emptying feed bin 1-1-A-0 of section;Boosting or No. 11 of extraction section step by step
Grade boosting or extraction feed bin 1-1-A-1-1 ..., No. 1 N-3 grades of boostings or extraction feed bin 1-1-A- (N-3) -1, No. 1 N-2 grades of boostings
N-2 grade boostings of extraction feed bin 1-1-A- (N-2) No. -1,2 number or extract feed bin 1-1-A- (N-2) -2 ..., nN-2- No. 1 N-2 grades rise
Pressure or extraction feed bin 1-1-A- (N-2)-(nN-2-1)、nN-2Numbers N-2 grades boostings or extraction feed bin 1-1-A- (N-2)-nN-2, No. 1 N-
1 grade of boosting or extraction feed bin 1-1-A- (N-1) -1, No. 1 N grades of boostings or extraction feed bin 1-1-A-N-1, No. 2 N grades of boostings or extraction
Feed bin 1-1-A-N-2 ..., nN- No. 1 N grades of boosting or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or extraction feed bin 1-
1-A-N-nN;Step pressure reducing section N-1 grade decompression feed bin 1-1-B- (N-1) ..., 1 grade of decompression feed bin 1-1-B-1;Draw back section
Draw back feed bin 1-1-B-0;Discharging bin 1-1-B to be unloaded.
1 grade of isolated subsystem 3-1 ..., N-3 grades of isolated subsystem 3- (N-3) and N-1 grades of isolated subsystem 3-
It (N-1) is to be made of no isolated subsystem, the composition of no isolated subsystem is the same as embodiment two;
The N-2 grade isolated subsystem 3- (N-2) is by a heavy transformation isolated subsystem or double transformation segregant
System is constituted, and the composition of a weight transformation isolated subsystem or double transformation isolated subsystem is the same as embodiment three;
The N grade isolated subsystem 3-N is by the isobaric isolated subsystem of a weight or double isobaric isolated subsystem structure
At the composition of a weight equipressure isolated subsystem or double isobaric isolated subsystem is the same as embodiment one.
1 grade of pressurization cycle subsystem 2-1 ..., N-3 grades of pressurization cycle subsystem 3- (N-3) be by facing without pump Asia
Boundary's pressurization cycle subsystem is constituted, and the composition of no subcritical pressurization cycle subsystem of pump is the same as embodiment two.
The N-2 grade pressurization cycle subsystem 2- (N-2) is made of overcritical pressurization cycle subsystem, overcritical increasing
Press the composition of cycle subsystem with embodiment three;
The N-1 grade pressurization cycle subsystem 2- (N-1) be by constituting without pumping overcritical pressurization cycle subsystem,
In:
It is made of without overcritical pressurization cycle subsystem is pumped circulation heat exchanger 2-HC, check valve 2-CV, fluid material for flow
It is stainless steel;The connection relationship respectively formed are as follows:
Check valve 2-CV entrance is without the overcritical pressurization cycle subsystem main-inlet of pump, and the outlet check valve 2-CV passes through pipe
7 points are two-way, and the first via is connected with circulation heat exchanger 2-HC entrance, and the second tunnel is without the overcritical pressurization cycle subsystem pair of pump
Entrance, the outlet circulation heat exchanger 2-HC is without the overcritical pressurization cycle subsystem outlet of pump.
The N grade pressurization cycle subsystem 2-N is made of subcritical pressurization cycle subsystem, subcritical pressurization cycle
The composition of subsystem is the same as embodiment one.
Connection relationship between above each subsystem is the same as embodiment one.
The extraction and separation technology of the technical solution of the present embodiment are as follows:
(1) with one step of embodiment (1);
(2) with one step of embodiment (2);
(3) with one step of embodiment (3);
(4) with one step of embodiment (4);
(5) 1 grades of pressurization cycle subsystem 2-1 ..., N-3 grades of pressurization cycle subsystem 2- (N-3) it is in operating status, even
Continue 1 grade to N-3 grades in extraction sub-system 11 grade of boost or extract feed bin 1-1-A-1-1 ..., N- of boosting or extraction section step by step
3 grades boosting or extraction feed bin 1-1-A- (N-3) -1 and 1 grade of isolated subsystem 3-1 ..., N-3 grades of isolated subsystem 3- (N-3) and
1 grade of pressurization cycle subsystem 2-1 ..., the corresponding connection of N-3 grades of pressurization cycle subsystem 2- (N-3), keep each boostings at different levels or extraction
The relevant pressure grade in feeding storehouse is constant;Start N-2 grades of pressurization cycle subsystem 2- (N-2), N-2 grades in continuous extraction subsystem 1
Boosting or -1, No. 2 N-2 grades of boosting of No. 1 N-2 grades of boostings of extraction section or extraction feed bin 1-1-A- (N-2) or extraction feed bin step by step
1-1-A-(N-2)-2、…、nN-2- No. 1 N-2 grades of boosting or extraction feed bin 1-1-A- (N-2)-(nN-2-1)、nN-2Numbers N-2 grades boostings
Or extraction feed bin 1-1-A- (N-2)-nN-2Supercritical fluid extraction is carried out, the n of extraction is completedN-2A N-2 grades of boosting or extraction material
Supercritical fluid in storehouse enters N-2 grades of isolated subsystem 3- (N-2) and is separated, and periodically turns on N-2 fraction ionization series
Unite the matched heavy discharge valve 3-V-1 and double discharge valve 3-V-2 of weight discharge valve 3-V-1 or one of 3- (N-2) institute, draws off N-2 grades
The separated extract come out of isolated subsystem 3- (N-2);N-1 grades of pressurization cycle subsystem 2- (N-1) are in operating status, even
N-1 grade in continuous extraction sub-system 1 boost step by step or No. 1 N-1 the grade of extraction section boost or extract feed bin 1-1-A- (N-1) -1 and
The corresponding connection of N-1 grades of isolated subsystem 3- (N-1), keeps the pressure stage of the feed bin constant;Start N grades of pressurization cycle subsystem 2-
N boosting or No. 1 N grade boostings of extraction section or extracts feed bin 1-1-A-N-1, No. 2 N grades step by step for N grades in continuous extraction subsystem 1
Boosting or extraction feed bin 1-1-A-N-2 ..., nN- No. 1 N grades of boosting or extraction feed bin 1-1-A-N- (nN-1)、nNNumbers N grades boostings or
Extract feed bin 1-1-A-N-nNSubcritical fluid extraction is carried out, the n of extraction is completedNIt is subcritical in a N grades of boosting or extraction feed bin
Fluid enters corresponding N grades of isolated subsystem 3-N and is separated, and it is matched to periodically turn on N grades of isolated subsystem 3-N institutes
One weight discharge valve 3-V-1 or one heavy discharge valve 3-V-1 and double discharge valve 3-V-2, draw off N grades of isolated subsystem 3-N and divide
Separate out the extract come;
(6) with one step of embodiment (6);
(7) with one step of embodiment (7);
(8) with one step of embodiment (8);
(9) with one step of embodiment (9);
(10) (7) step~the (9) step is repeated, so that being housed to feed bin 1-1-A quilt equipped with the extract not extracted
It is periodically packed into continuous extraction subsystem 1, the discharging bin 1-1-B to be unloaded after having extracted synchronously is drawn off continuous extraction subsystem
System 1, in this course, each feed bin 1-1 of 1 inner cavity extractor cylinder 1-2 of continuous extraction subsystem be successively in emptying section,
Boosting or extraction section, step pressure reducing section and section is drawn back step by step, the feed bin 1-1 continuously pushed successively completes air evacuating in section
Emptying, boost step by step at 1 grade to N-3 or extraction section in complete 1 grade and risen step by step to the boosting step by step of N-3 stage pressure grade, in N-2
Pressure or extraction section in complete extract N-2 stage pressure grade supercritical fluid extraction, N-1 boost step by step or extraction section in
Complete N-1 stage pressure grade boosting, N grade step by step boosting or extraction section in completion extract N stage pressure grade it is subcritical
Fluid extraction, is drawing back completion subcritical fluids medium in section at the step pressure reducing that N-1 pressure stage is completed in step pressure reducing section
The continuous operation drawn back;The supercritical fluid completed in the feed bin 1-1 of supercritical fluid extraction enters N-2 grades of isolated subsystems
3- (N-2) is separated, and the N-2 grades of matched weight discharge valve 3-V-1 or one of isolated subsystem 3- (N-2) institute are periodically turned on
Weight discharge valve 3-V-1 and double discharge valve 3-V-2 draws off the separated extract come out of N-2 grades of isolated subsystem 3- (N-2);
Subcritical fluids in the feed bin 1-1 of completion subcritical fluids N stage pressure grade extraction enter N grades of isolated subsystem 3-N and are divided
From periodically turning on the heavy discharge valve 3-V-1 of the N grades of matched weight discharge valve 3-V-1 or one of isolated subsystems 3-N institute and double
Discharge valve 3-V-2 draws off the separated extract come out of N grades of isolated subsystem 3-N.
Typical supercritical fluid medium and subcritical fluids medium select carbon dioxide, and highest subcritical carbon dioxide connects
Continuous equipressure extraction and separation pressure is 50MPa, and differential every stage pressure grade is 10MPa, then the sub-critical flow of supercritical fluid pre-extracted
Step by step boosting series N of the body single-stage continuously in isobaric extraction separation device system is 5;The subcritical fluids pressure of 1 stage pressure grade
It is 32 DEG C for 10MPa, temperature;The subcritical fluids pressure of 2 stage pressure grades is 20MPa, temperature is 32 DEG C;3 stage pressure grades surpass
Supercritical fluid extraction pressure is 30MPa, temperature is 50 DEG C, a weight separating pressure 8MPa, temperature 60 C or a heavy separating pressure
8MPa, temperature 60 C and double separating pressure 6MPa, 65 DEG C of temperature;The supercritical fluid pressures of 4 stage pressure grades are 40MPa, temperature
Degree is 40 DEG C;The subcritical fluid extraction temperature of 5 stage pressure grade 50MPa is 32 DEG C, 35 DEG C of a weight separation temperature or one is divided again
35 DEG C from temperature and 40 DEG C of double separation temperature;Each pressure stage pressurization cycle subsystem and isolated subsystem are then respectively 1 grade of increasing
Press cycle subsystem 2-1,2 grades of pressurization cycle subsystem 2-2,3 grades of pressurization cycle subsystem 2-3,4 grades of pressurization cycle subsystem 2-
4,5 grades of pressurization cycle subsystem 2-5 and 1 grade of isolated subsystem 3-1,2 grades of isolated subsystem 3-2,3 grades of isolated subsystem 3-3,4
Grade isolated subsystem 3-4,5 grades of isolated subsystem 3-5;With each pressure stage pressurization cycle subsystem and the matched valve of isolated subsystem
Door is respectively 2 grades of switching valves of 1 grade of switching valve 6-1-1 of 1 grade of pressurization cycle subsystem 2-1,2 grades of pressurization cycle subsystem 2-2
4 grades of switching valve 6- of 6-1-2,3 grades of switching valve 6-1-3 of 3 grades of pressurization cycle subsystem 2-3,4 grades of pressurization cycle subsystem 2-4
1 grade of return valve 6-2-1,2 of the 5 grades of switching valve 6-1-5 and 1 grade of isolated subsystem 3-1 of 1-4,5 grades of pressurization cycle subsystem 2-5
2 grades of return valve 6-2-2 of grade isolated subsystem 3-2,3 grades of return valve 6-2-3 of 3 grades of isolated subsystem 3-3,4 grades of separation systems
5 grades of return valve 6-2-5 of 4 grades of return valve 6-2-4 of 3-4,5 grades of separation system 3-5;1 extractor cylinder of continuous extraction subsystem
1 grade in 1-2, the boosting step by step of 2 stage pressure grades or the feed bin 1-1 that is packed into of extraction section be 1, i.e. n1=n2=1,3 stage pressures
The feed bin 1-1 that boosting or extraction section are packed into step by step of grade is 3, i.e. n3The boosting step by step or extraction section of=3,4 stage pressure grades
The feed bin 1-1 being packed into is 1, n4The feed bin 1-1 that boosting or extraction section are packed into step by step of=1,5 stage pressure grades is 3, i.e.,
n5=3;Remaining each section, that is, emptying section, 1 grade to 4 grades of step pressure reducing section and drawing back the feed bin 1-1 that section is packed into is respectively 1
It is a.
The present invention overcomes existing extraction plant system for supercritical fluid or subcritical fluid extraction device system to connect
The shortcomings that continuous production, realizes subcritical fluids and continuously waits sub- extraction and separation, has process flow reasonable, high degree of automation,
It is reliable for operation, energy saving zero-emission, the excellent advantage of craftsmanship.
Claims (2)
1. the continuous isobaric extraction separation device system of a kind of subcritical fluids, it is characterized in that by subcritical fluids medium source, pressurization
Subsystem, continuous extraction subsystem, isolated subsystem identical with the boosting step by step of continuous extraction subsystem or the total series N of extraction
And pressurization cycle subsystem is constituted;
The subcritical fluids medium source is by liquefaction storage tank, cooler, refrigeration machine, outlet valve, filling valve and always flows back valve group
It constitutes;The connection relationship respectively formed are as follows:
Cooler is placed in liquefaction tank inside or outside, cooler are connected with refrigeration unit, forms cooling circuit;Liquefaction storage
Tank outlet is equipped with outlet valve, exports valve outlet as the outlet of subcritical fluids medium source;Subcritical fluids medium source there are two entrance,
One is total reflux valve inlet, another fills valve inlet, and total flow back and fills valve outlet and connect after pipe merges valve outlet
To liquefaction reservoir inlet;
The pressurization subsystem is made of cooler, force (forcing) pump, pressure reducing valve and overflow valve;The connection relationship respectively formed are as follows:
Cooler entrance is pressurized system entry, is exported through pipe and subcritical fluids medium source, i.e. outlet valve outlet is connected
It connects, cooler outlet is connected through pipe with pressurization pump intake;Pressurization pump discharge is divided into N number of branch with pipe, and pressurize subsystem
Maximum pressure grade pipe branch is divided into two branches again, all the way be pressurization subsystem maximum pressure grade outlet, another way with
Overflow valve inlet is connected;Remaining N-1 branch is connected through pipe is corresponding with the decompression valve inlet of each pressure stage, each pressure reducing valve
Outlet is the pressurized system outlet of other each pressure stages in addition to maximum pressure grade;Overflow valve outlet is through being connected to cooler by pipe
On pipe between outlet and pressurization pump intake;The quantity and company of pressurized system outlet quantity, i.e. pressure reducing valve plus overflow valve
The boosting step by step of continuous extraction sub-system or the total series of extraction are identical;
The continuous extraction subsystem by feed bin, extractor cylinder, binning end barrel end, unload storehouse end barrel end, binning
End locking device unloads storehouse end locking device, binning hydraulic cylinder, unloads storehouse hydraulic cylinder, rack, insulating layer, emptying switching valve, draws back and cut
Valve is changed, shut-off valve, drain pump is drawn back, draws back compressor, sealing ring composition;Wherein:
Feed bin is the cylinder with orlop, is equipped with distribution grid close to orlop, has fluid entry holes on the barrel between distribution grid and orlop,
It is equipped with powder blocking plate close to Hatch Opening, there are Fluid-exiting apertures on the barrel between powder blocking plate and Hatch Opening, the orlop side of feed bin cylinder outer circle is set
Have and binning end locking device or unloads the locking card slot that the dissection type clip quick-opening structure of storehouse end locking device matches, locking clamp
The barrel outer circle of slot two sides and Hatch Opening is equipped with seal groove;
The extractor cylinder of continuous extraction subsystem is cylindrical structure, and cylinder both ends are respectively equipped with the cylinder of the binning end with annular flange
Body end portion is equipped with Heat exchange jacekt with storehouse end barrel end, cylinder outer wall is unloaded, and extractor cylinder lumen edge is divided axially into emptying section, series
No less than 2 boosting step by step or extraction section, series are equal to the step pressure reducing section that boosting or the total series of extraction section subtract 1 step by step, and
Draw back Duan Gongsi active section;Continuous extraction subsystem extractor cylinder lumen fills feed bin, every grade of boosting or extraction section step by step
Inside at least it is packed into a feed bin;It empties section and corresponds to the extractor barrel wall of be packed into feed bin fluid entry holes position equipped with stream
Body inlet and outlet, boosting or extraction section correspond to the fluid entry holes position of each feed bin and Fluid-exiting apertures position being packed into step by step
Fluid inlet and fluid outlet are respectively equipped on extractor barrel wall, step pressure reducing section corresponds to each feed bin stream being packed into
Body enters to be equipped with fluid balance inlet and outlet on the extractor barrel wall of hole site, draws back section and enters corresponding to be packed into feed bin fluid
The extractor barrel wall of hole site is equipped with fluid outlet;Each fluid enters on the extractor barrel wall of boosting or extraction section step by step
Mouth is the entrance of continuous extraction subsystem, and each fluid outlet is continuous extracts on the extractor barrel wall of boosting or extraction section step by step
Take the outlet of subsystem;
Binning end locking device and storehouse end locking device is unloaded by dissection type clip and hydraulic or be driven by electricity and constitute;The locking of binning end
The dissection type clip quick-opening structure and binning end barrel end of device and the locking card slot of feed bin, unload cuing open for storehouse end locking device
Fraction clip quick-opening structure corresponds to each other matching with the locking card slot for unloading storehouse end barrel end and feed bin;
The connection relationship that continuous extraction subsystem respectively forms are as follows:
Binning hydraulic cylinder is successively sequentially fixedly mounted along axis, binning end locking device, extractor cylinder, unloads storehouse end locking dress
Set, unload storehouse hydraulic cylinder in rack, make binning hydraulic cylinder, binning end locking device, extractor cylinder, unload storehouse end locking device,
It is mutually coaxial to unload storehouse hydraulic cylinder, binning end locking device matches with binning barrel end, unloads storehouse end locking device and unloads storehouse cylinder
Body end portion matches;
Fluid outlet on section extractor barrel wall is drawn back by pipe and draws back shut-off valve and is connected with suction port of compressor is drawn back,
Fluid inlet and outlet on emptying section extractor barrel wall divides two-way, passes through pipe all the way and draw back switching valve to go out with compressor is drawn back
Mouth is connected, and another way is connected by pipe and emptying switching valve with emptying pump intake, and emptying pump discharge leads to atmosphere;Closely
The fluid balance inlet and outlet for drawing back the step pressure reducing section of section pass through pipe and the stream of boosting or extraction section step by step for closely emptying section
Body entrance is connected, and the secondary fluid balance inlet and outlet for suffering the step pressure reducing section for drawing back section empty section step by step by pipe and secondary suffer
The fluid inlet of boosting or extraction section is connected, and so on, the fluid balance inlet and outlet of whole step pressure reducing sections are passed through into pipe
Son is corresponding with the fluid inlet of boosting or extraction section step by step that boosting or the total series of extraction section step by step subtract 1 to be connected;
Extractor cylinder body outer wall coats insulating layer;
The isolated subsystem perhaps double isobaric isolated subsystem or one is become again by an isobaric isolated subsystem of weight
Press isolated subsystem perhaps double transformation isolated subsystem or without isolated subsystem constitute, in which:
One weight equipressure isolated subsystem is made of isobaric heat exchanger, a reheating device and a weight separator;The connection respectively formed is closed
System are as follows:
Isobaric heat exchanger cryogenic media entrance is the isobaric isolated subsystem entrance of a weight, and isobaric heat exchanger cryogenic media outlet is through pipe
Son is connected with a reheating device entrance, and reheating device outlet is connected through pipe with a weight separator inlet, and one separates again
Device outlet is connected through pipe with isobaric heat exchanger high-temperature medium entrance, and isobaric heat exchanger high-temperature medium outlet is isobaric point of a weight
Ion system outlet, a weight separator is exported equipped with extract, and is furnished with a heavy discharge valve;
Double equipressure isolated subsystem is by isobaric heat exchanger, a reheating device, a heavy separator, double heater and double separation
Device is constituted: the connection relationship respectively formed are as follows:
Isobaric heat exchanger cryogenic media entrance is double isobaric isolated subsystem entrance, and isobaric heat exchanger cryogenic media outlet is through pipe
Son is connected with a reheating device entrance, and reheating device outlet is connected through pipe with a weight separator inlet, and one separates again
Device outlet is connected through pipe with double calorifier inlets, and double heater outlet is connected through pipe with double separator inlet
It connects, double separator outlet is connected through pipe with isobaric heat exchanger high-temperature medium entrance, isobaric heat exchanger high-temperature medium outlet
It is exported for double isobaric isolated subsystem, a weight separator and double separator are respectively equipped with extract outlet, and are respectively provided with
One weight discharge valve and double discharge valve;
One weight transformation isolated subsystem is made of a readjustment pressure valve, a weight heat exchanger and a weight separator;The connection respectively formed is closed
System are as follows:
One resets pressure valve entrance as a heavy transformation isolated subsystem entrance, and a readjustment pressure valve outlet enters through pipe and a weight heat exchanger
Mouth is connected, and a weight heat exchanger exit is connected through pipe with a weight separator inlet, and a weight separator outlet is a heavy transformation
Isolated subsystem outlet, a weight separator is exported equipped with extract, and is furnished with a heavy discharge valve;
Double transformation isolated subsystem resets pressure valve, a weight heat exchanger, a heavy separator, double pressure regulator valve, double heat exchange by one
Device and double separator are constituted: the connection relationship respectively formed are as follows:
One resets pressure valve entrance as double transformation isolated subsystem entrance, and a readjustment pressure valve outlet enters through pipe and a weight heat exchanger
Mouth is connected, and a weight heat exchanger exit is connected through pipe with a weight separator inlet, and a heavy transformation extractor outlet is through pipe
It is connected with double pressure regulation valve inlet, double pressure regulation valve outlet is connected through pipe with double heat exchanger entrance, double heat exchanger
Outlet is connected through pipe with double separator inlet, and double separator outlet is the outlet of double transformation isolated subsystem, a weight
Separator and double separator are respectively equipped with extract outlet, and equipped with a weight discharge valve and double discharge valve;
No isolated subsystem is made of connecting pipe, and the sub- entrance of connecting pipe is no isolated subsystem entrance, and connection is used
Tube outlet exports for no isolated subsystem;
The pressurization cycle subsystem be by subcritical pressurization cycle subsystem or overcritical pressurization cycle subsystem, or
Person is constituted without the subcritical pressurization cycle subsystem of pump, or without overcritical pressurization cycle subsystem is pumped, in which:
Subcritical pressurization cycle subsystem is made of voltage-stablizer, circulating pump, cycle condenser;The connection relationship respectively formed are as follows:
Cycle condenser entrance is subcritical pressurization cycle subsystem main-inlet, and cycle condenser outlet is pumped into through pipe and circulation
Mouth is connected, and pipe is equipped with subcritical pressurization cycle subsystem sub-inlet between cycle condenser outlet and pump entry, follows
Ring pump discharge divides two-way, is connected all the way through pipe with voltage-stablizer inlet and outlet, and another way is that subcritical pressurization cycle subsystem goes out
Mouthful;
Overcritical pressurization cycle subsystem is made of transformation heat exchanger, cycle condenser, circulating pump, circulation heat exchanger;Each composition
Connection relationship are as follows:
Transformation heat exchanger low-pressure medium entrance is overcritical pressurization cycle subsystem main-inlet, the outlet of transformation heat exchanger low-pressure medium
It is connected through pipe with cycle condenser entrance, cycle condenser outlet is connected through pipe with pump entry, circulating condensing
Pipe is equipped with overcritical pressurization cycle subsystem sub-inlet between device outlet and pump entry, and circulating-pump outlet is through pipe and becomes
Pressure heat exchanger high-voltage medium inlet is connected, and transformation heat exchanger high-voltage media outlet is connected through pipe with circulation heat exchanger entrance
It connects, circulation heat exchanger outlet is that overcritical pressurization cycle subsystem exports;
It is made of without subcritical pressurization cycle subsystem is pumped voltage-stablizer, check valve;The connection relationship respectively formed are as follows:
One-way valve inlet is without the subcritical pressurization cycle subsystem main-inlet of pump, and one-way valved outlet is divided into three tunnels by pipe, the
It is connected all the way with voltage-stablizer inlet and outlet, the second tunnel is without the subcritical pressurization cycle subsystem sub-inlet of pump, third Lu Weiwu pump
Subcritical pressurization cycle subsystem outlet;
It is made of without overcritical pressurization cycle subsystem is pumped circulation heat exchanger, check valve;The connection relationship respectively formed are as follows:
One-way valve inlet is without the overcritical pressurization cycle subsystem main-inlet of pump, and one-way valved outlet is divided into two tunnels by pipe, the
It is connected all the way with circulation heat exchanger entrance, the second tunnel is without the overcritical pressurization cycle subsystem sub-inlet of pump, circulation heat exchanger
Outlet is without the overcritical pressurization cycle subsystem outlet of pump;
Connection relationship between above each subsystem are as follows:
The outlet of subcritical fluids medium source is connected through pipe with pressurized system entry, and the outlet of pressurization subsystems at different levels is through pipe
It is sub to be connected with corresponding pressurization cycle subsystem sub-inlet, pressurization cycle subsystem main-inlets at different levels through pipe and switching valve with
Each corresponding isolated subsystem outlet is connected, and isolated subsystem entrances at different levels are through pipe and each corresponding continuous extraction subsystem
Outlet is connected, and pressurization cycle subsystem outlets at different levels are connected through pipe with each corresponding continuous extraction subsystem entrance, together
When isolated subsystem at different levels outlet through pipe be each separated into two-way, enter all the way through return valve and same subcritical fluids medium source
Mouth is connected, and another way is connected through switching valve with corresponding pressurization cycle subsystems outlets at different levels;Corresponding to segregants at different levels
Exhaust-valve is housed on the return valve of system and the connecting line of subcritical fluids medium source inlet.
2. a kind of application subcritical fluids extraction and separation that continuously isobaric extraction separation device system is implemented described in claim 1
Processing step is as follows:
(1) the liquefaction storage tank in subcritical fluids medium source is emptied, and is full of subcritical fluids medium by regulation, and open refrigeration
Machine liquefies subcritical fluids medium;
(2) sealing ring will be installed in the seal groove of each feed bin;Binning end locking device is opened, it one by one will be empty with binning hydraulic cylinder
Feed bin is pushed into the extractor cylinder lumen of continuous extraction subsystem, after extractor cylinder lumen fills sky feed bin, starts one by one
Push-in is equipped with the feed bin of extract, when draw back a feed bin is housed outside section after, the locking of locking continuous extraction subsystem binning end
Device and unload storehouse end locking device;
(3) the total return valve of subcritical fluids medium source inlet is closed, the return valve for being totally separated subsystem is opened, closes and all increases
The switching valve of cycle subsystem is pressed, exhaust-valve is opened, opens the outlet valve of subcritical fluids medium source outlet, continuous extraction is discharged
Subsystem and the air being totally separated in subsystem;It continuous extraction subsystem and is totally separated in subsystem after air empties, opens
The switching valve of whole pressurization cycle subsystems is opened, the air in whole pressurization cycle subsystems is discharged, until emptying, is then shut off
It is totally separated the return valve of subsystem, closes exhaust-valve;
(4) starting pressurization subsystem, so that feed bin in each boosting step by step or extraction section in continuous extraction subsystem and its right
Pressure in the feed bin and matched isolated subsystem and pressurization cycle subsystem of the step pressure reducing section answered reaches setting value;
(5) start whole pressurization cycle subsystems, boost step by step in continuous extraction subsystem or the feed bin of extraction section starts to complete
Boost or extract step by step accordingly, complete subcritical fluids extracted or supercritical fluid in the feed bin of extraction enter it is opposite
The isolated subsystem answered is initially separated, and periodically turns on discharge valve, draws off the separated extract come out of isolated subsystem;
(6) when the feed bin in the boosting step by step or extraction section near step pressure reducing section reaches the extraction process time, closing is drawn back
Switching valve opens emptying switching valve, starts drain pump, emptying is in continuous extraction subsystem extractor cylinder lumen emptying section
The air of feed bin;Emptying switching valve is closed, drain pump is closed;
(7) binning hydraulic cylinder piston rod is retracted, dress is packed between the feed bin that binning hydraulic cylinder and binning end locking device are locked
There is the new feed bin of extract, stretch out binning hydraulic cylinder piston rod and holds out against the feed bin being newly packed into;Storehouse hydraulic cylinder piston is unloaded in stretching
Bar simultaneously holds out against and unloads the feed bin that storehouse end locking device is locked;It is synchronous to open binning end locking device and unload storehouse end locking device;Together
Step continues to stretch out binning hydraulic cylinder piston rod and storehouse hydraulic cylinder piston rod is unloaded in retraction, and the feed bin being newly packed into is loaded into continuous extraction
System extractor cylinder lumen;It is synchronous to lock binning end locking device and unload storehouse end locking device;Storehouse hydraulic cylinder piston is unloaded in retraction
Bar unloads the feed bin being ejected;
(8) emptying switching valve is opened, starts drain pump, emptying is in continuous extraction subsystem extractor cylinder lumen emptying section
The air of feed bin;Emptying switching valve is closed, drain pump is closed;
(9) it opens and draws back shut-off valve and draw back switching valve, the material of section is drawn back in continuous extraction subsystem extractor cylinder lumen
The subcritical fluids or supercritical fluid medium in storehouse flow into everywhere in continuous extraction subsystem extractor cylinder lumen emptying section
Feed bin, after drawing back section feed bin and emptying section pressure of silo balance, compressor is drawn back in unlatching, is faced until drawing back the Asia in section feed bin
Boundary's fluid or supercritical fluid medium are all withdrawn into emptying section feed bin, and closing draws back shut-off valve and draws back switching valve, close
Draw back compressor;
(10) (7) step~the (9) step is repeated, so that the feed bin equipped with the extract not extracted is periodically packed into continuously
Extraction sub-system, the feed bin after having extracted synchronously are drawn off continuous extraction subsystem, in this course, continuous extraction subsystem
Each feed bin of system extractor cylinder lumen is successively in emptying section, step by step boosting or extraction section, step pressure reducing section and draws back section,
Be sequentially completed in each active section the emptying of air in feed bin, feed bin step by step boosting or feed bin in extract step by step
The continuous operation of subcritical fluids medium drawn back in extraction, the step pressure reducing of feed bin, feed bin;Complete extraction feed bin in dissolved with
The subcritical fluids or supercritical fluid of extract enter corresponding isolated subsystem and are initially separated, and periodically turn on discharging
Valve draws off the separated extract come out of isolated subsystem.
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