CN106457103A - Method and device for separating and recovering supercritical fluid - Google Patents
Method and device for separating and recovering supercritical fluid Download PDFInfo
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- CN106457103A CN106457103A CN201480078877.0A CN201480078877A CN106457103A CN 106457103 A CN106457103 A CN 106457103A CN 201480078877 A CN201480078877 A CN 201480078877A CN 106457103 A CN106457103 A CN 106457103A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/02—Combinations of filters of different kinds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D50/00—Combinations of methods or devices for separating particles from gases or vapours
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
- D06B9/06—Solvent-treatment of textile materials with recovery of the solvent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
Provided is a method for separating and recovering a supercritical fluid, the method making it possible to reduce maintenance frequency while maintaining a high separation and recovery efficiency. A method for separating and recovering a supercritical fluid including a step 1 for readying a supercritical fluid containing an impurity, a step 2 for changing the fluid into a gaseous state, a step 3 for separating the liquid-state impurity from gaseous-state fluid using a non-adsorption filter (205) having a first mesh size, and a step 4 for using an adsorption filter (216) for further separating the liquid-state impurity from gaseous-state fluid after step 3 using an adsorption filter (216).
Description
Technical field
The present invention relates to the separation and recovery method of supercritical fluid and device.Especially, the present invention relates to contaminating in supercritical
The separation and recovery method of supercritical fluid and device used in color device.
Background technology
In the past, in the case of the dyeing carrying out fibre, employ substantial amounts of water as dyeing medium, and be noted
Water resource saves problem with liquid waste processing etc., thus seeking to develop the staining technique lower to environmental pressure.Therefore, in recent years
Come, as the colouring method that the output of waste liquid compared with the past is few, propose to have by with supercritical carbon dioxide as representative
The method that supercritical fluid is used as dyeing medium.And, dyeing process after supercritical fluid by the impurity separation such as dyestuff
Afterwards, it is reused via after predetermined processing.
In No. 3954103 publications of Japanese Patent No. (patent documentation 1), disclose one kind using supercritical fluid to fiber
Dyeing apparatuses and colouring method that product is dyeed.This dyeing apparatus 70 described in patent documentation 1, as shown in figure 5, tool
Have：The dyeing caldron (autoclave) 71 of storage fibre；Store the fluid becoming dyeing medium stores case (catch box)
72；Fluid is supplied to dyeing caldron 71 and the pump 73 by this liquid pressure rise from storing case 72；Configuration is in pump 73 and dyeing caldron 71
Between and convection cell heated and become the heat exchanger 74 of supercriticality；Dyestuff is made to be dissolved in supercriticality
Dissolving tank (saturator) 75 in fluid (supercritical fluid)；The pressure release valve 76 of the pressure in adjustment dyeing caldron 71；Configuration is being put
The downstream of pressure valve 76 and by dyestuff from the detached separating tank of fluid 77；With the condenser making the fluid condensation after separation dyestuff
78.
By controlling the opening and closing of the valve 92,93 in the downstream of dyeing caldron 71 for the configuration, face having passed through the super of dyeing caldron 71
Boundary's fluid is to pressure release valve 76 side and/or the conveying of pump 73 side.In the case of being somebody's turn to do, the supercritical fluid being transported to pressure release valve 76 side passes through
Discharge from pressure release valve 76 and be depressurized and gasify, then, in separating tank 77, to separate from the fluid having gasified by precipitation
And collect dyestuff.And, after the fluid after having separated dyestuff in separating tank 77 liquefies in condenser 78, it is back to and stores case
In 72.
In Japanese Unexamined Patent Publication 2004-249175 publication (patent documentation 2), disclose following recycling carbon dioxide
Impregnation processing method：In impregnation treatment trough, after making impregnation material be impregnated in base material in supercritical carbon dioxide, will be impregnated with
Fluid after process imports to gas fractionation unit via air relief valve from impregnation treatment trough, removes liquid in gas fractionation unit
Or solid constituent, preserve after the carbon dioxide obtaining compression is become liquefied carbon dioxide or supercritical carbon dioxide
In storing case, heated or compressed it to from the liquefied carbon dioxide or supercritical carbon dioxide storing case derivation as needed
Afterwards it is supplied into impregnation treatment trough, so that supercritical carbon dioxide is full of in impregnation treatment trough.
In patent documentation 2, by arranging filter in gas fractionation unit, thus removing in gas fractionation unit
During liquid or solid composition, separation efficiency improves.Describe non-woven fabrics as the material of filter and spin cloth.Also describe for
Raising gas separation efficiency, and the filter deployment preferably will with fold (pleat) becomes cylindric, and make carbon dioxide gass
Body passes through towards inner side outside it.
In No. 4669231 publications of Japanese Patent No. (patent documentation 3), to provide one kind from from using supercritical titanium dioxide
Dud is constantly separated and energy in the carbon dioxide that the cleaning device of carbon or liquid CO 2 and/or drying device are discharged
The carbon dioxide regeneration recovery that the residual component in the carbon dioxide of discharge fluid after enough reclaiming is reduced to specified value fills
It is set to purpose it is proposed that a kind of gas-liquid separation mechanism, it is made up of following part：Controlled in the way of keeping the gas-liquid rate of regulation
Discharge the temperature of fluid and the temperature adjusting mechanism of pressure adjustment and pressure adjustmenting mechanism；With will by this temperature adjusting mechanism and
Pressure adjustmenting mechanism carries out the gas-liquid separation pressure vessel that the discharge fluid after pressure adjustment is separated into gas and liquid.
Mist separating mechanism is directed to by the gasiform carbon dioxide that gas-liquid separation mechanism obtains, by mist
(mist) separate.And, the dud in the carbon dioxide being removed after mist is separated by dud removing mechanism.In mist
It is provided with filter in separating mechanism and dud removing mechanism, catch liquid in mist separating mechanism, remove in dud
Go in mechanism, dud to be fixed on adsorbent.
Prior art literature
Patent documentation
Patent documentation 1：No. 3954103 publications of Japanese Patent No.
Patent documentation 2：Japanese Unexamined Patent Publication 2004-249175 publication
Patent documentation 3：No. 4669231 publications of Japanese Patent No.
Content of the invention
Like this, in the prior art document it can be seen that the description of separation and recovery method about supercritical fluid.But
It is to pass through precipitation in patent documentation 1 and dyestuff separated from the fluid having gasified and collects, but its concrete mechanism indefinite.
Record setting filter in gas fractionation unit in patent documentation 2, if but due to the mechanism described in the document then
Produce and frequently carry out the necessity of filter replacement, therefore practicality insufficient.In addition, only disclosing in patent documentation 2
Based on the gas separating mechanism of filter, if being only the mechanism of filter, then it is difficult to separation, the especially mist of dud
The separation of foam composition.In patent documentation 3, discharge fluid and entered in gas-liquid separation pressure vessel with the gas-liquid rate specifying, because
There is the discharge fluid discharging fluid and gaseous state of liquid condition in this in gas-liquid separation pressure vessel simultaneously.Therefore, difficult
To remove dissolving impurity in a liquid, and to the discharge fluid requiring in gas-liquid separation pressure vessel for keeping liquid condition
High withstand voltage.
The present invention is to research and develop in view of the foregoing, and its problem is to provide one kind to be able to maintain that high separation recovery efficiencies
And separation and recovery method or the separating and reclaiming device of the supercritical fluid safeguarding frequency can be reduced.
The present invention in one aspect, is a kind of separation and recovery method of supercritical fluid, including：
Operation 1, prepares the supercritical fluid containing impurity；
Operation 2, makes above-mentioned change of fluid become gaseous state；
Operation 3, using the non-adsorbed type filter with the first mesh, separates from the above-mentioned fluid being in gaseous state
The impurity being in liquid condition or solid state or being in the admixture of liquid/solid；With
Operation 4, using absorption type filter, being in the above-mentioned fluid of gaseous state further after via operation 3
Separation is in liquid condition or solid state or is in the impurity of the admixture of liquid/solid.
In an embodiment of the separation and recovery method of the supercritical fluid of the present invention, in operation 3, impurity is upper
State fluid move upward in filter, until the period discharged from filter top is by filters trap, filtered
The impurity that device captures moves downwards in filter because of gravity, and is discharged from filter bottom.
In an other embodiment of the separation and recovery method of the supercritical fluid of the present invention, in operation 3 and operation 4
Between, also include operation 3 ', in operation 3 ', using the non-adsorbed type filter with second mesh less than the first mesh,
Being in the above-mentioned fluid of gaseous state after via operation 3 be separately in further liquid condition or solid state or
It is in the impurity of the admixture of liquid/solid.
In an other embodiment of the separation and recovery method of the supercritical fluid of the present invention, in operation 3 ', miscellaneous
Matter above-mentioned fluid in filter in the horizontal direction or be moved upward compared with horizontal direction, until by the side from filter
The period that portion or top are discharged by filters trap, by filters trap to impurity move downwards in filter because of gravity
Dynamic, and be discharged from filter bottom.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, non-adsorbed type filter
For metal system, absorption type filter is chemical fibre system, natural fiber system or synthetic resin multiple aperture plasma membrane system.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, remove in operation 3
90～98% impurity.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, operation 2 exists to operation 4
Under the pressure of one atmospheric pressure～7.38MPa and above-mentioned fluid maintain gaseous state in the state of implement.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, operation 2 by making on
State fluid pressure, produce gasification cold energy and make fluid temperature (F.T.) reduce to carry out.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, supercritical fluid is super
Critical carbon dioxide.
In another other embodiment of the separation and recovery method of the supercritical fluid of the present invention, super containing impurity faces
Boundary's fluid is discharged from supercritical dyeing device, contains dyestuff in impurity.
The present invention on the other hand, is a kind of separating and reclaiming device of supercritical fluid, possesses：
Air relief valve, it is used for making the supercritical fluid containing impurity be changing into gaseous state；
First separating tank, it is arranged on the rear class of above-mentioned air relief valve, has for from the above-mentioned fluid being in gaseous state
The non-adsorbed type filtration that middle separation is in liquid condition or solid state or is in the impurity of the admixture of liquid/solid
Device, and this non-adsorbed type filter has the first mesh；With
Second separating tank, it is arranged at the rear class of non-adsorbed type filter, has for from being in the above-mentioned of gaseous state
The suction being separately in liquid condition or solid state further in fluid or being in the impurity of the admixture of liquid/solid
Attached type filter.
In an embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, non-adsorbed type filter has
Discharge the construction of gas from bottom drain and from sidepiece or top.
In an other embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, the first separating tank 201
In the bottom of above-mentioned filter, there is the volume for temporarily storing the liquid discharged from non-adsorbed type filter 205.
In another other embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, it is also equipped with the 3rd and separates
Groove 202, it is arranged between the first separating tank 201 and the second separating tank 203, has for from by from the first separating tank 201 row
The non-adsorbed type filter 209 being in the impurity being separately in liquid condition in the above-mentioned fluid of gaseous state further going out,
This non-adsorbed type filter 209 has second mesh less than the first mesh.
In another other embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, non-adsorbed type filter
205th, 209,222 is metal system, and absorption type filter 216 is chemical fibre system, natural fiber system or synthetic resin multiple aperture plasma membrane
System.
In another other embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, supercritical fluid is super
Critical carbon dioxide.
In another other embodiment of the separating and reclaiming device of the supercritical fluid of the present invention, super containing impurity faces
Boundary's fluid is discharged from supercritical dyeing device, contains dyestuff in impurity.
Brief description
Fig. 1 is the first reality of the supercritical dyeing system of the separating and reclaiming device representing the supercritical fluid possessing the present invention
Apply the skeleton diagram of mode.
Fig. 2 is the skeleton diagram of the embodiment of three-level formula separating tank representing the present invention.
Fig. 3 is to represent the skeleton diagram of with the separating tank of non-adsorbed type filter that can be applied to the present invention.
Fig. 4 is the second reality of the supercritical dyeing system of the separating and reclaiming device representing the supercritical fluid possessing the present invention
Apply the skeleton diagram of mode.
Fig. 5 is the outline of the supercritical dyeing system described in No. 3954103 publications of Japanese Patent No. (patent documentation 1)
Figure.
Fig. 6 is the state diagram of carbon dioxide.
Specific embodiment
The separation and recovery method ＞ of ＜ 1. supercritical fluid
In an embodiment of the separation and recovery method of the supercritical fluid of the present invention, including：
Operation 1, prepares the supercritical fluid containing impurity；
Operation 2, makes above-mentioned change of fluid become gaseous state；
Operation 3, using the non-adsorbed type filter with the first mesh, separates from the above-mentioned fluid being in gaseous state
The impurity being in liquid condition or solid state or being in the admixture of liquid/solid；With
Operation 4, using absorption type filter, being in the above-mentioned fluid of gaseous state further after via operation 3
Separation is in liquid condition or solid state or is in the impurity of the admixture of liquid/solid.
(operation 1)
Prepare the supercritical fluid containing impurity in operation 1.Often it is useful in as the material forming supercritical fluid
Normal temperature and pressure (example：20 DEG C a, atmospheric pressure) under for gas material, can enumerate for example alkane (especially ethane, propane, penta
Alkane), ammonia, carbon dioxide, carbon monoxide, nitrous oxide etc., but examine in terms of the height from critical temperature and processing safety etc.
Consider and preferably use carbon dioxide.These materials function as medium generally when carrying out first supercritical processing.Containing miscellaneous
The supercritical fluid of matter is generated by various first supercritical processing.The such as cleaning of supercritical dyeing, supercritical, supercritical can be enumerated
Drying, supercritical extraction, using postcritical high molecular forming processing etc..Therefore, along with the impurity also root of supercritical fluid
Various according to the content of first supercritical processing, but, for example, in the case of supercritical dyeing, comprise as impurity to contaminate
Material, the Soft flocks being mixed into from treated object because of supercritical dyeing supercritical fluid, adhesive dust, water, oils and fatss etc., as
The present invention explanation impurity in the main component of liquid condition and enumerate water, oils and fatss.
Additionally, after, for example sometimes above-mentioned " is in liquid condition or solid state or is in liquid/solid
The impurity of admixture " is only recited as " impurity ".
(operation 2)
Supercritical fluid is made to be changing into gaseous state in operation 2.Now, if at least a portion being set to impurity becomes liquid
Temperature and pressure condition as body state, then the impurity of liquid condition will not be dissolved in gas, therefore, it is possible in operation 3 hold
Change places impurity gas-liquid separation from fluid.Method as making supercritical fluid be changing into gaseous state, is not particularly limited, but
The preferred decompression method because easy.Do not need special chiller, it is enough using air relief valve.Due to changing in supercritical fluid
Gasification cold energy can be produced, so the temperature of fluid also can reduce naturally when becoming gaseous state.Because the temperature with fluid reduces,
The saturation capacity of gasiform impurity also reduces and liquid impurity increases, it is possible to obtaining separation efficiency, to rise this excellent
Point.If considering the separation efficiency of supercritical fluid and impurity, preferably set supercritical fluid all become gaseous state that
At the temperature of sample and pressure condition.This is because, if supercritical fluid is changing into liquid condition, operation 3 forms super facing
The organic efficiency of the material of boundary's fluid reduces.
Between operation 1 and operation 2, lead to surpass to prevent produce supercritical fluid temperature with being not intended to from reducing
Critical fluids freeze in pipe arrangement in conveying or block pipe arrangement it is preferred that in order to maintain supercriticality and as needed
Heated.As heating means, it is not particularly limited, suitably select resistive heating device, induction heating apparatus, medium heating
Device, microwave heating equipment, burning heater etc..
(operation 3)
In operation 3, using the non-adsorbed type filter with the first mesh, from the above-mentioned fluid being in gaseous state
Separate the impurity being in liquid condition.Here, non-adsorbed type filter refer to will not surface adsorption captured liquid
The material of impurity filter, if defining in more detail, refer to temporary transient to the collision on filter material surface by impurity
Trapping impurity, but the long-time filter being detained of impurity cannot be made because of its material and smooth-shaped.As will not inhale on surface
The filter of the material of attached impurity, can enumerate rustless steel, ferrum, copper, silver, zinc, nickel, chromium, aluminum, Hastelloy (Hastelloy),
Because of the filter of section's inorganic matters such as metal filter or glass, pottery such as alloy (inconel) like this, preferably will not
Get rusty, tough and there is thermostability, price also suitable rustless steel.As the shape of the filter in operation 3, can enumerate and remove
Foam (demister) type, mesh-type, fold-type, pouch-type, candle (candle) type, cascade type etc., from the big impurity of a large amount of trappings
From the viewpoint of efficiency high, preferably foam removal type.If using non-adsorbed type filter, liquid impurity can be because of gravity
Naturally come off from filter, therefore do not need to change filter, with little need for maintenance.Even if in the case of producing dirt
Performance is just able to maintain that by cleaning.
By only using non-adsorbed type filter it becomes possible to the liquid impurity of separating most.For instance, it is possible to set
The mesh of filter makes it possible to remove 90～98%, is typically 92～96% impurity.Also can be according to treating capacity by filter
Configure in series or in parallel.If the separation efficiency of the impurity in operation 3 is set to too low, the absorption type filter to rear class
Burden, its change frequency uprise.On the other hand, if the separation efficiency of the impurity in operation 3 is set to too high, fill
Put and become to maximize, and separating rate is slack-off, easily produce mesh blocking and change frequency and uprise.Other filter itself
Price also uprises.And there is the limit for separation efficiency.Therefore, it is desirable to be set with the separation efficiency in above-mentioned scope for standard
Determine the mesh of the non-adsorbed type filter in operation 3.
If the mesh of the filter in operation 3 is too small, through deterioration of efficiency thus separating rate is slack-off, if on the other hand
The mesh of filter is excessive, and dud passes through filter with hardly becomeing trapped in, therefore, it is desirable to be suitable in operation 3
0.5 μm～270 μm of the size average out to of mesh, more preferably 1 μm～20 μm of average out to.The size of mesh is defined as, and is being seen with SEM
The minimum diameter of a circle of each sieve aperture can be passed through, by the meansigma methodss of the sieve aperture of arbitrary more than 100 during the sieve aperture examining filter
It is set to the meansigma methodss of the size of mesh.
The separation efficiency improving impurity aspect it is desirable to liquid is discharged from bottom and gas is from sidepiece using having
Or the filter of construction that top is discharged.When using the filter having configuration which, impurity is in above-mentioned fluid in mistake
In filter in the horizontal direction or be moved upward compared with horizontal direction, the phase until being discharged from the sidepiece of filter or top
Between by filters trap, by filters trap to impurity move downwards in filter because of gravity, from filter bottom
Discharge.Because the moving direction of impurity and the moving direction of fluid are different, so both separation can be promoted.
(operation 4)
In operation 4, using absorption type filter, enter the above-mentioned fluid being in gaseous state after via operation 3
One step separation impurity.In the present invention, absorption type filter refers to the liquid impurity absorption capturing in the material on surface
The filter of matter, if defining in more detail, referring to by its material and Porous or fine complicated shape and having strong
Van der Waals for twine network impurity, by impurity capture and attracts and makes it be difficult to the filter coming off.As by impurity absorption
In the filter of the material on surface, chemical fibre system, natural fiber system and synthetic resin multiple aperture plasma membrane system can be enumerated, as change
Learn fiber can enumerate for example by resin-made, especially PET, PP (polypropylene), nylon (Nylon), carbamate, acrylic acid
The plastic chemical fibre such as resin, acetass, staple fibre constitute filter, as natural fiber can enumerate by
The filter that the such as Plant fiber such as cotton, fiber crops, thin,tough silk, Pilus Caprae seu Oviss, paper or animal fiber are constituted, can as synthetic resin multiple aperture plasma membrane
Enumerate PE (polyethylene), PP (polypropylene), PU (polyurethane), EVA (ethylene-vinyl acetate copolymer), PTFE (polytetrafluoroethyl-ne
Alkene) etc. synthetic resin multiple aperture plasma membrane.The non-woven fabrics of PP are preferably used from reasons such as processability, durability, economy
Or spinning cloth.Shape as the filter in operation 4 can enumerate foam removal type, mesh-type, fold-type, pouch-type, candle type, cascade type
Deng, but and the shape of the efficiency high of shape also big impurity a large amount of from trapping and preferred foam removal type.Absorption type filter table
Reveal very excellent separation efficiency, but due to by the liquid adsorption comprising impurity capturing in filter, so when super
Need during the adsorption capacity crossing filter to change filter.Therefore, in the separation and recovery side of the supercritical fluid improving the present invention
The practicality aspect of method, reduces it and changes frequency while the performance preferably adsorbing type filter used in maintaining operation 4.
Also according to treating capacity, filter can be configured in series or in parallel.
As described above, in the present invention, most impurity is divided from fluid by the non-adsorbed type filter in operation 3
From.In operation 4, the only trace impurity of remaining part to be separated, the load therefore, it is possible to make absorption type filter is very little, from
And significantly reduce replacing frequency.Detached impurity only overall a few percent of impurity in operation 4, but, be in order to
Highly purified fluid recovery is recycled and important operation.After operation 4, preferably the impurity in fluid be removed 99% with
On, more preferably it is removed more than 99.5%, be further preferably removed more than 99.9%.
(operation 3 ')
It is also possible between operation 3 and operation 4, make for the purpose of mitigating the load to the absorption type filter in operation 4
With having the non-adsorbed type filter of the mesh less than the first mesh, carry out further being in gas shape after via operation 3
The operation 3 ' of impurity is separated further in the above-mentioned fluid of state.Due to using non-adsorbed type filter, so maintainability is high.Pass through
Carry out operation 3 ', the separation efficiency of impurity can be made to rise 2～6%, be typically 3～5%.Therefore, it is possible to make to transfer to subsequently
The impurity of operation 4 is overall less than 2% of impurity, preferably less than 1%.
Filtered by making the mesh of non-adsorbed type filter used in operation 3 ' be less than non-adsorbed type used in operation 3
The mesh of device, and can remove in operation 3 cannot detached small drop etc..If the mesh mistake of the filter in operation 3 '
Little, then pass through deterioration of efficiency thus separating rate is slack-off, on the other hand, if the mesh of the filter in operation 3 ' is excessive, more
Dud can pass through from filter, it is therefore preferable that size average out to 0.1 μm～10 μ of the mesh being suitable in operation 3 '
M, more preferably 0.1 μm～1 μm of average out to.The size of mesh is as defined above.
Used in operation 3 ', the material of non-adsorbed type filter can be identical with operation 3 with shape, but from intensity, durable
Property, economy set out the reasons why optimal, preferably material be rustless steel, for shape, from the pass of filter volume and filter area
System sets out, the big fold-type of the filter area of preferably per unit volume.In the aspect of separation efficiency improving impurity, with operation
3 similarly have the filtration from the construction that bottom is discharged and gas is discharged for the liquid from sidepiece or top it is desirable to use
Device.
(other)
Fluid via the removing foreign matter after operation 4 also can save as gaseous state, if but being considered as supercritical
Fluid recycles and storage space, then expect to preserve with the state making volume reduce after liquefying.If in addition, considering to face for super
The fluid that boundary is processed is repeatedly circulated, then in order to strongly suppress pressure to rise required energy expenditure, and expect operation 2～4
Implement in the state of maintaining high pressure.Therefore, for operation 2～4, in the container of resistance to pressure, maintain gas shape in fluid
State, impurity maintain and set high pressure in the range of liquid condition, such as when using carbon dioxide as supercritical fluid, in figure
Pressure and temperature is set in the range of as shown in (3) of the carbon dioxide state diagram shown in 6.That is, refer to supercritical pressure with
Down be below 7.38MPa, preferably more than atmospheric pressure and for gaseous state temperature.
The separating and reclaiming device ＞ of ＜ 2. supercritical fluid
It is described with reference to the shooting flow of the separation and recovery method of supercritical fluid for realizing the above-mentioned present invention
The embodiment of the separating and reclaiming device of body.
(first embodiment)
Show in Fig. 1 the supercritical fluid with the present invention separating and reclaiming device 100, using carbon dioxide as dye
The skeleton diagram of the first embodiment of supercritical dyeing system that color medium uses.The supercritical dyeing system tool of present embodiment
Standby cooler 101, supply pump 102, preheater 103, supply open and close valve 104, dyeing caldron 105, circulating pump 107, pressure transducer
111st, air relief valve 115, separating tank 116, carbon dioxide store case 119.
Storing in case 119 in carbon dioxide and stored liquefied carbon dioxide, being boosted until being changing into by supply pump 102
After supercriticality, send to dyeing caldron 105 via supply open and close valve 104.In dyeing caldron 105, although not shown, but maintain
Fibre, the dyestuff being dissolved in supercritical carbon dioxide is supplied to fibre, carries out dyeing process.By supercritical two
In the case that carbonoxide uses to dye to fibre as dyeing medium, as dyestuff, preferably use disperse dyes,
Oil-soluble dyes.
After being initially supplied supercritical carbon dioxide, so that circulating pump 107 is operated, so that supplied supercritical carbon dioxide is existed
In dyeing caldron 105, the direction of the arrow A along in figure circulates.Thus, supercritical carbon dioxide is flowing out from the outlet of dyeing caldron 105
Afterwards, import to the entrance of dyeing caldron 105 again via circulating path.By recycling supercritical carbon dioxide, can be right
Fibre carries out level dyeing, and can suppress the consumption of carbon dioxide, and cost of implementation is cut down.
In addition, the pressure in dyeing caldron 105 is measured by pressure transducer 111, control the operating of supply pump 102.Thus,
Pressure in dyeing caldron 105 is adjusted and remains the setting pressure carrying out dyeing the regulation processing.
After dyeing process terminates, circulating pump 107 stops, and the stream of supercritical carbon dioxide being dissolved with dyestuff is to air relief valve
115.Air relief valve 115 controls the output of carbon dioxide, and makes to have passed through the supercritical carbon dioxide gasification of air relief valve 115.
By the impurity gas-liquid separation such as dyestuff from carbon dioxide in separating tank 116.Fig. 2 shows the one of the construction of separating tank 116
The ideograph of example, bottom depicts the flow graph of the flowing representing carbon dioxide and impurity, and top depicts and separates for representing
The general profile chart of the configuration of filter in each separating tank in groove 116.As shown in Fig. 2 separating tank 116 is to have first point
Third grade structure from groove 201, the second separating tank 203 and the 3rd separating tank 202.The 3rd separating tank 202 can be omitted, but from mitigation
It is desirable to arrange the 3rd separating tank 202 from the viewpoint of burden to the second separating tank 203 and raising maintainability.
First separating tank 201 is arranged on the rear class of air relief valve 115, has for from the carbon dioxide being in gaseous state
Separate the non-adsorbed type filter 205 of impurity 206, this non-adsorbed type filter 205 has the first mesh.From substantially cylinder type
The carbon dioxide that the entrance 204 of the first separating tank 201 flows into, is filtered with cylinder type from the medial wall being located at the first separating tank 201
Space between the lateral wall of device 205 by and downwards move after, reversion and from the opening positioned at bottom for the filter to mistake
Enter in filter.Contain the impurity 206 of small droplet-like in carbon dioxide, extending along vertical in carbon dioxide
The period passed through upward in filter 205, impurity is caught by non-adsorbed type filter 205 and from carbon dioxide separation.
The impurity being captured by non-adsorbed type filter 205 moves downwards in filter 205 because of gravity, soon from
The opening temporary safe-keeping positioned at bottom of filter 205 in the bottom space of the first separating tank 201, finally from liquid outlet 207
Discharge.In the first separating tank 201 detached impurity be liquid-drop diameter, solid particle size than larger impurity, most liquid
Impurity is separated herein.
Pass through from the opening positioned at top for the filter 205 and flow to the 3rd from the carbon dioxide of outlet 208 discharge and separate
Groove 202.3rd separating tank 202 has non-adsorbed type filter 209, for further from the carbon dioxide be in gaseous state
Separate and be in the impurity such as the dyestuff of liquid condition 210.In order to improve separation efficiency, the mesh of the filter in the 3rd separating tank sets
Surely must be less than the mesh of the filter in the first separating tank.
The carbon dioxide flowing into from the entrance 211 of the 3rd separating tank 202 of substantially cylinder type, from the 3rd separating tank 202
Space between the inner tube of medial wall and the concentric circles inside it by and move downwards.From the 3rd separating tank 202
Be located at bottom opening flow out carbon dioxide reversion and the bottom from multiple cylinder type filters 209 and sidepiece entered into
In filter, wherein the plurality of cylinder type filter 209 is along the circumferential direction equably arranged near the central authorities of the 3rd separating tank 202
Row.The more small droplet-like failing to remove in the first separating tank 201 and small solid, shaped is contained in carbon dioxide
Impurity 210, the period passed through upward in filter 209 in carbon dioxide, impurity caught by non-adsorbed type filter 209 and
From carbon dioxide separation.
The impurity being captured by non-adsorbed type filter 209 moves downwards in filter 209 because of gravity, soon from
The opening temporary safe-keeping positioned at bottom of filter 209 in the bottom space of the 3rd separating tank 202, finally from liquid outlet 212
Discharge.In the 3rd separating tank 202, detached impurity is the smaller impurity of liquid-drop diameter, solid particle size, and it is miscellaneous that here reclaims
The amount of matter is considerably less compared with the first separating tank.But, go out from the viewpoint of the filter replacement frequency reducing the second separating tank 203
Send out, the 3rd separating tank 202 plays an important role.
In the present embodiment, in order to other forms of the construction of separating tank are described, and the construction by the 3rd separating tank 202
It is changed to different from the first separating tank 201, but do not need additionally different constructions, Liang Zheke in addition to the mesh of filter
To be same configuration.Also further each separating tank can be set to other constructions.There is shown in Fig. 3 non-adsorbed type filter
Other examples another of separating tank.
The entrance 221 of the separating tank 220 from substantially cylinder type for the carbon dioxide flows into, and the medial wall from separating tank 220 with
Space between the inner tube of the concentric circles inside it by and move downwards.Carbon dioxide is from separating tank 220
After opening located at bottom flows out, the non-adsorbed type of reversion and cylinder type near the central authorities being arranged at separating tank 220 filters
The filter bottom of device 222 and lateral part enter in filter.Carbon dioxide in filter 222 by and from filter
The period that medial part flows out, the small droplet-like comprising in carbon dioxide and the impurity 223 of small solid, shaped are by non-adsorbed
Type filter 222 catches and from carbon dioxide separation.
The impurity 223 being captured by non-adsorbed type filter 222 moves downwards in filter 222 because of gravity, no
Flow out from the bottom of filter 222 long and fall because of gravity, temporary safe-keeping in the bottom of separating tank 220, finally from liquid discharge
Mouth 224 discharge.With regard to the size of the mesh of filter 222, as long as according to being to use as the first separating tank or as second
Separating tank is using suitably setting.
In addition, referring again to the 3rd separating tank 202 of Fig. 2, from the opening positioned at top for the filter 209 pass through and from going out
The carbon dioxide of mouth 213 discharge flow to the second separating tank 203.Second separating tank 203 has for from being in the two of gaseous state
Separately it is in the absorption type filter 216 of the impurity such as the dyestuff of liquid condition 215 further in carbonoxide.From substantially cylinder type
The carbon dioxide that the entrance 214 of the second separating tank 203 flows into, from the medial wall of the second separating tank 203 with same inside it
Space between the inner tube of heart round shape by and move downwards.Flow out from the opening located at bottom for second separating tank 203
Carbon dioxide, inverts and the top from multiple cylinder type filters 216 and sidepiece enters in filter, the plurality of cylinder type mistake
Filter 216 along the circumferential direction equably arranges near the central authorities of the second separating tank 203.It is included in the 3rd point in carbon dioxide
Fail the impurity 215 of the more small droplet-like and small solid, shaped removing in groove 202, in carbon dioxide in filter
The period passed through downwards in 216, impurity be adsorbed type filter 216 catch and from carbon dioxide separation.By filter 216
The carbon dioxide being cleaned afterwards is from outlet 217 discharge.This carbon dioxide can be reused in supercritical dyeing and process.
Although absorption type filter 216 is high to the separation efficiency of impurity, because filter is fixed in impurity 215 absorption
216, so separation efficiency extremely reduces when exceeding the adsorption capacity of filter 216.Accordingly, it would be desirable to periodic replacement filter.
In the present invention, due to most impurity can be separated off in prime, so as a example the effect of the second separating tank 203
As only separated 1% about impurity.Therefore, the situation phase with the separating tank being not provided with prime using non-adsorbed type filter
Than, or even 1/100 about can be reduced to by safeguarding frequency.
(second embodiment)
Figure 4 illustrates the supercritical fluid with the present invention separating and reclaiming device 300, carbon dioxide is used as
The skeleton diagram of the second embodiment of supercritical dyeing system of dyeing medium.The supercritical dyeing system of present embodiment possesses
Supply pump 102, supply open and close valve 104, dyeing caldron 105, circulating pump 107, pressure transducer 111, heater 114, air relief valve
115th, separating tank 116, compressor 117, aftercooler 118, carbon dioxide store case 119.
Storing in case 119 in carbon dioxide and stored liquefied carbon dioxide, being boosted by supply pump 102 until being changing into super
After critical state, send to dyeing caldron 105 via supply open and close valve 104 and preheater 103.By in preheater 103 to super
Critical carbon dioxide is heated, and can stably maintain supercriticality.In dyeing caldron 105, although not shown, but keep
There is fibre, the dyestuff being dissolved in supercritical carbon dioxide is supplied to fibre, carries out dyeing process.
Circulating pump 107 in dyeing process, the action of pressure transducer 111 are identical with illustrate in first embodiment,
Therefore omitted.
After dyeing process terminates, circulating pump 107 stops, and the supercritical carbon dioxide being dissolved with dyestuff is from heater 114
And after air relief valve 115 passes through, flowed into separating tank 116 with gaseous state.Heater 114 plays to be prevented from super facing with being not intended to
The temperature of boundary's fluid reduces and supercritical carbon dioxide frost or the effect blocking pipe arrangement in pipe arrangement in conveying.Dividing
In groove 116, as described above, isolating the impurity such as dyestuff from carbon dioxide.
The gasiform carbon dioxide being cleaned via separating tank 116 is pressurizeed by compressor 117 to recycle,
And cooled in aftercooler 118 further, thus liquefy.Carbon dioxide after liquefaction returns to carbon dioxide and stores case
119, thus complete reusable preparation.
Description of reference numerals
The separating and reclaiming device of 100 supercritical fluids
101 coolers
102 supply pumps
103 preheaters
104 supply open and close valves
105 dyeing caldrons
107 circulating pumps
111 pressure transducers
114 heaters
115 air relief valve
116 separating tanks
117 compressors
118 aftercoolers
119 carbon dioxide store case
201 first separating tanks
202 the 3rd separating tanks
203 second separating tanks
The entrance of 204 first separating tanks
205 non-adsorbed type filters
206 impurity
207 liquid outlets
The outlet of 208 first separating tanks
209 non-adsorbed type filters
210 impurity
The entrance of 211 the 3rd separating tanks
212 liquid outlets
The outlet of 213 the 3rd separating tanks
The entrance of 214 second separating tanks
215 impurity
216 absorption type filters
The outlet of 217 second separating tanks
220 separating tanks
The entrance of 221 separating tanks
222 non-adsorbed type filters
223 impurity
224 liquid outlets
The outlet of 225 separating tanks
The separating and reclaiming device of 300 supercritical fluids
Claims (17)
1. a kind of separation and recovery method of supercritical fluid is it is characterised in that include：
Operation 1, prepares the supercritical fluid containing impurity；
Operation 2, makes described change of fluid become gaseous state；
Operation 3, using the non-adsorbed type filter (205) with the first mesh, divides from the described fluid being in gaseous state
From be in liquid condition or solid state or be in liquid/solid admixture impurity；With
Operation 4, using absorption type filter (216), being in the described fluid of gaseous state further after via operation 3
Separation is in liquid condition or solid state or is in the impurity of the admixture of liquid/solid.
2. supercritical fluid as claimed in claim 1 separation and recovery method it is characterised in that
In operation 3, impurity moves upward in described fluid, until by filter (205) in filter (205)
The period that portion discharges is caught by filter (205), and the impurity being captured by filter (205) is because of gravity in filter (205)
Inside move downwards, and be discharged from filter (205) bottom.
3. supercritical fluid as claimed in claim 1 or 2 separation and recovery method it is characterised in that
Between operation 3 and operation 4, also include operation 3 ', in operation 3 ', using having second mesh less than the first mesh
Non-adsorbed type filter (209), being in the described fluid of gaseous state after via operation 3 be separately in liquid further
Body state or solid state or be in liquid/solid admixture impurity.
4. supercritical fluid as claimed in claim 3 separation and recovery method it is characterised in that
In operation 3 ', impurity described fluid in filter (209) in the horizontal direction or compared with horizontal direction upward
Mobile, until being caught by filter (209) by the period discharged from sidepiece or the top of filter (209), by filter (209)
The impurity capturing moves downwards in filter (209) because of gravity, and is discharged from filter (209) bottom.
5. the supercritical fluid as any one of Claims 1-4 separation and recovery method it is characterised in that
Non-adsorbed type filter (205,209,222) is metal system, and absorption type filter (216) is chemical fibre system, natural fibre
Dimension system or synthetic resin multiple aperture plasma membrane system.
6. the supercritical fluid as any one of claim 1 to 5 separation and recovery method it is characterised in that
90～98% impurity is removed in operation 3.
7. the supercritical fluid as any one of claim 1 to 6 separation and recovery method it is characterised in that
Operation 2 to operation 4 under the pressure of an atmospheric pressure～7.38MPa and described fluid maintain gaseous state state
Lower enforcement.
8. the supercritical fluid as any one of claim 1 to 7 separation and recovery method it is characterised in that
Operation 2 makes fluid temperature (F.T.) reduce carrying out by making described fluid pressure, generation gasify cold energy.
9. the supercritical fluid as any one of claim 1 to 8 separation and recovery method it is characterised in that
Supercritical fluid is supercritical carbon dioxide.
10. supercritical fluid as claimed in any one of claims 1-9 wherein separation and recovery method it is characterised in that
Supercritical fluid containing impurity is discharged from supercritical dyeing device, comprises dyestuff in impurity.
A kind of 11. separating and reclaiming devices of supercritical fluid (100,300) are it is characterised in that possess：
Air relief valve (115), it is used for making the supercritical fluid containing impurity be changing into gaseous state；
First separating tank (201), it is arranged on the rear class of described air relief valve (115), has for from the institute being in gaseous state
State separation in fluid to be in liquid condition or solid state or be in the non-adsorbed of the impurity of admixture of liquid/solid
Type filter (205), and this non-adsorbed type filter (205) has the first mesh；With
Second separating tank (203), it is arranged at the rear class of non-adsorbed type filter (205), has for from being in gaseous state
Described fluid in be separately in liquid condition or solid state further or be in the miscellaneous of the admixture of liquid/solid
The absorption type filter (216) of matter.
The separating and reclaiming device of 12. supercritical fluids as claimed in claim 11 it is characterised in that
Non-adsorbed type filter (205) has the construction discharging gas from bottom drain and from sidepiece or top.
The separating and reclaiming device of 13. supercritical fluids as described in claim 11 or 12 it is characterised in that
First separating tank (201) has the liquid for discharging from non-adsorbed type filter (205) in the bottom of described filter
The volume that body temporarily stores.
The separating and reclaiming device of 14. supercritical fluids as any one of claim 11 to 13 it is characterised in that
It is also equipped with the 3rd separating tank (202), it is arranged between the first separating tank (201) and the second separating tank (203), has use
In being separately in liquid condition further from being in the described fluid of gaseous state of being discharged from the first separating tank (201)
The non-adsorbed type filter (209) of impurity, this non-adsorbed type filter (209) has second mesh less than the first mesh.
The separating and reclaiming device of 15. supercritical fluids as any one of claim 11 to 14 it is characterised in that
Non-adsorbed type filter (205,209,222) is metal system, and absorption type filter (216) is chemical fibre system, natural fibre
Dimension system or synthetic resin multiple aperture plasma membrane system.
The separating and reclaiming device of 16. supercritical fluids as any one of claim 11 to 15 it is characterised in that
Supercritical fluid is supercritical carbon dioxide.
The separating and reclaiming device of 17. supercritical fluids as any one of claim 11 to 16 it is characterised in that
Supercritical fluid containing impurity is discharged from supercritical dyeing device, contains dyestuff in impurity.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2014/062997 WO2015173934A1 (en) | 2014-05-15 | 2014-05-15 | Method and device for separating and recovering supercritical fluid |
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| CN106457103A true CN106457103A (en) | 2017-02-22 |
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| CN201480078877.0A Pending CN106457103A (en) | 2014-05-15 | 2014-05-15 | Method and device for separating and recovering supercritical fluid |
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| Country | Link |
|---|---|
| CN (1) | CN106457103A (en) |
| TW (1) | TWI566833B (en) |
| WO (1) | WO2015173934A1 (en) |
Cited By (3)
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| CN107163618A (en) * | 2017-06-02 | 2017-09-15 | 广州立达尔生物科技股份有限公司 | Supercritical fluid column chromatography prepares the method and device of high-purity capsochrome Capsaicin |
| CN110075657A (en) * | 2019-05-23 | 2019-08-02 | 广东碳染科技有限公司 | Supercritical mixed-flow internal heating type clean separation kettle |
| CN110629570A (en) * | 2018-06-21 | 2019-12-31 | 远东新世纪股份有限公司 | Method for dyeing textile substrates containing residual oligomers |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835561B (en) * | 2016-11-21 | 2019-10-22 | 大连工业大学 | A kind of supercritical CO2Separating still in anhydrous equipment for dyeing and finishing |
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Also Published As
| Publication number | Publication date |
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| TWI566833B (en) | 2017-01-21 |
| WO2015173934A1 (en) | 2015-11-19 |
| TW201603883A (en) | 2016-02-01 |
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