CN104812532B - Cooling agent renovation process and cooling agent regenerating unit - Google Patents
Cooling agent renovation process and cooling agent regenerating unit Download PDFInfo
- Publication number
- CN104812532B CN104812532B CN201280077378.0A CN201280077378A CN104812532B CN 104812532 B CN104812532 B CN 104812532B CN 201280077378 A CN201280077378 A CN 201280077378A CN 104812532 B CN104812532 B CN 104812532B
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- Prior art keywords
- cooling agent
- hollow
- fibre membrane
- tramp material
- membrane
- Prior art date
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- 239000002826 coolant Substances 0.000 title claims abstract description 233
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000009418 renovation Methods 0.000 title claims abstract description 31
- 230000001172 regenerating effect Effects 0.000 title claims description 41
- 239000012528 membrane Substances 0.000 claims abstract description 174
- 239000000835 fiber Substances 0.000 claims abstract description 117
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims description 89
- 238000005520 cutting process Methods 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 238000005119 centrifugation Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 19
- 239000012510 hollow fiber Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 30
- 229910052710 silicon Inorganic materials 0.000 description 30
- 239000010703 silicon Substances 0.000 description 30
- 238000001914 filtration Methods 0.000 description 28
- 238000005374 membrane filtration Methods 0.000 description 19
- 230000002093 peripheral effect Effects 0.000 description 19
- 239000007788 liquid Substances 0.000 description 15
- 239000012530 fluid Substances 0.000 description 11
- 230000004907 flux Effects 0.000 description 7
- 230000000903 blocking effect Effects 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 6
- 230000007774 longterm Effects 0.000 description 5
- 239000003507 refrigerant Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
- B24B57/02—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/034—Lumen open in more than two directions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B27/00—Other grinding machines or devices
- B24B27/06—Grinders for cutting-off
- B24B27/0633—Grinders for cutting-off using a cutting wire
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
- B28D5/0076—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material for removing dust, e.g. by spraying liquids; for lubricating, cooling or cleaning tool or work
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2315/00—Details relating to the membrane module operation
- B01D2315/14—Batch-systems
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Grinding-Machine Dressing And Accessory Apparatuses (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The present invention provides a kind of cooling agent renovation process, it is characterized in that, can recycle the cooling agent used when crystal ingot is cut off with scroll saw, to make the cooling agent in the way of laminar condition flows in each hollow bulb of one or more hollow-fibre membranes of hollow form, the cooling agent is supplied respectively in from one end of each hollow-fibre membrane to hollow bulb, the aperture of the film of hollow-fibre membrane is less than 0.05 μm.
Description
Technical field
The present invention relates to a kind of cooling agent renovation process and cooling agent regenerating unit, the product ingots such as silicon are cut off from using scroll saw
When the cooling agent that is used in remove the tramp materials such as cutting swarf so that the cooling agent can be recycled.
Background technology
(section) is cut off to silicon ingot by using scroll saw for the silicon wafer of solar cell etc. and is obtained.Cut-out
The method of silicon ingot has two kinds of bonded-abrasive mode and free abrasive mode.Bonded-abrasive mode is used consolidates the abrasive particles such as carborundum
The scroll saw and cooling agent (coolant) cuts off silicon ingot.In addition, free abrasive mode is using scroll saw and contains abrasive particle
Cooling agent (mud) cut off silicon ingot.
In general, from from the viewpoint of manufacturing cost, the cooling agent used in the cut off operation of silicon ingot (is made
Used cooling agent) recycled.Cutting swarf (below, also referred to as " cutting in the used cooling agent containing silicon
Bits "), the tramp material such as scroll saw clipped wire, abrasive particle (with the situation that free abrasive mode is cut off) in itself.Therefore, if directly
Used cooling agent is recycled, the scuffing of silicon wafer surface, the breakage of silicon wafer, cutting machine is likely to result in
Deterioration etc..Therefore, used cooling agent is reused after the tramp materials such as cutting swarf are removed by filtering, centrifugation etc..
For example, patent document 1 discloses a kind of cooling agent to used in the cut off operation of silicon ingot carries out film mistake
The method (cooling agent renovation process) filtered and can recycle.In the cooling agent renovation process, using filter membrane to using
Cooling agent filtered, accordingly, from the cooling agent remove tramp material.Describe in detail as follows.
The cooling agent renovation process uses ceramic membrane that the aperture (membrane aperture) in the hole of filter membrane is 1~10 μm as mistake
Filter membrane.The filter membrane is hollow tube-shape (drum).And, by so-called cross flow one (cross-flow) mode from making
Used cooling agent removes the tramp materials such as cutting swarf, and the cross flow configuration is in the hollow bulb of the filter membrane of the hollow tube-shape
Or outside allows used cooling agent relative to the mode that the surface (filter membrane surface) of filter membrane is abreast flowed.
In the filtering of the cross flow configuration, generally used cooling agent is increased relative to the flow velocity of filter membrane surface
Greatly.Accordingly, the tramp materials such as the cutting swarf of filter membrane surface to be piled up in are struck off using the flowing of used cooling agent, therefore,
Tramp material is inhibited to the accumulation of filter membrane surface, as a result, the film of filter membrane is blocked being inhibited.
Here, in cooling agent renovation process, if will be risen using ceramic membrane cost, therefore, in recent years using having
Machine filter membrane (organic film).For example, the use of the aperture of filter membrane being 0.1 in cooling agent renovation process disclosed in patent document 2
μm organic film.
However, organic film is softer than ceramic membrane, filtered when to the used cooling agent containing tramp materials such as cutting swarfs
When, easily produce the abrasion equivalent damage of filter membrane surface.
Prior art literature
Patent document
Patent document 1：Japanese Laid-Open Patent Publication 2012-6115
Patent document 2：Japanese Laid-Open Patent Publication 2012-020365
The content of the invention
It is empty fine in use it is an object of the invention to provide a kind of cooling agent renovation process and cooling agent regenerating unit
When dimension film filters cooling agent, it is difficult to make the hollow-fibre membrane be damaged because of the tramp material of cooling agent.
Cooling agent renovation process according to one aspect of the invention, can make with scroll saw cut off crystal ingot when used it is cold
But agent is recycled, and the cooling agent renovation process includes：Filter progress so that the cooling agent with laminar condition in hollow form
The mode of flowing in each hollow bulb of one or more hollow-fibre membranes, to being supplied respectively to the cooling agent in each hollow bulb,
Wherein, the aperture of the film of the hollow-fibre membrane is less than 0.05 μm.
In addition, cooling agent regenerating unit according to a further aspect of the present invention, can make cutting off crystal ingot when institute with scroll saw
The cooling agent for using is recycled, and the cooling agent regenerating unit includes：One or more hollow-fibre membranes of hollow form；And supply
To portion, the cooling agent is supplied to the hollow bulb of each hollow-fibre membrane, wherein, the aperture of the film of the hollow-fibre membrane is
Less than 0.05 μm, the supply unit supplies institute to make the cooling agent in the way of laminar condition flows in each hollow bulb
State cooling agent.
Brief description of the drawings
Fig. 1 is the summary construction diagram of the cooling agent regenerating unit involved by present embodiment.
Fig. 2 is the fragmentary perspective cross sectional view of the Filter membrane module of the cooling agent regenerating unit.
Fig. 3 is the figure of the relation between total filtration yield and permeation flux of each membrane aperture for representing hollow-fibre membrane.
Specific embodiment
Hereinafter, referring to figs. 1 to Fig. 2, one embodiment of the present invention is illustrated.Fig. 1 is the cooling involved by present embodiment
The summary construction diagram of agent regenerating unit.Fig. 2 is the fragmentary perspective cross sectional view of the Filter membrane module of the cooling agent regenerating unit.
System of the cooling agent regenerating unit of present embodiment in the silicon wafer for being for example used in semiconductor, solar cell etc.
Make in operation, tramp material is removed from the cooling agent (coolant) used when silicon ingot is cut off with scroll saw, so that the cooling
Agent can be recycled.Additionally, the cutting-off method of silicon ingot can be any one of bonded-abrasive mode and free abrasive mode.
Cooling agent includes the water-soluble solvents such as diethylene glycol, propane diols, the polyethylene glycol of low-molecular-weight.The cooling agent it is viscous
It is 20~60cp to spend.Additionally, in the case of dilute with water cooling agent, various additives etc. are added sometimes.Therefore, cooling agent
Composition and viscosity are not limited to described composition and viscosity.
Hereinafter, reference picture 1 and Fig. 2, illustrate cooling agent regenerating unit 10.
Cooling agent regenerating unit 10 possesses storage unit 12, membrane filtration portion 14 and centrifugation portion (centrifugal separating device)
16。
Storage unit 12 has treatment trough 121 and mixing part 122.
Treatment trough 121 stores the cooling agent (used cooling agent) used when cutting off silicon ingot using scroll saw.This makes
Used cooling agent is used in following purpose, i.e.,：During to cutting off silicon ingot using scroll saw the frictional heat that produces cooled down, with
And discharged by cutting swarf (silicon cutting swarf) dispersion of the silicon ingot produced by cut-out and from cutting portion etc..Therefore, it is used cold
But the cutting swarf containing silicon, scroll saw clipped wire, abrasive particle (with the situation that free abrasive mode is cut off) in itself etc. are understood in agent
Tramp material.
Mixing part 122 with the agitator 123 being configured in treatment trough 121 and is connected with agitator by rotary shaft 124a
123 motor 124.Rotary shaft 124a is vertically extending.Motor 124 makes agitator 123 be revolved centered on rotary shaft 124a
Turn.This kind of mixing part 122 rotates agitator 123 by by motor 124, used cold in treatment trough 121 to being stored in
But agent is stirred.The mixing part 122 of present embodiment when membrane filtration portion 14 and centrifugation portion 16 work, to being stored in place
Used cooling agent in reason groove 121 is stirred.
Membrane filtration portion 14 has Filter membrane module 20, filtering side feed path (supply unit) 141, filtering side foldback path
(foldback portion) 143 and filtered fluid accumulator tank 144.14 pairs, the membrane filtration portion is stored in the used cooling agent for the treatment of trough 121
Filtered to remove the tramp material contained in the cooling agent, and the cooling agent after filtering removes tramp material is delivered to
Filtered fluid accumulator tank 144.
Filter membrane module 20 have will a large amount of (multiple) hollow-fibre membranes 22,22 ... the He of filter house 21 of harness
House the housing 25 of filter house 21.At the length direction both ends (adhesive layer) 24 of filter house 21, adjacent hollow-fibre membrane 22,
22 is bonded to each other by resin binder 27 etc..Accordingly, maintain multiple hollow-fibre membranes 22,22 ... by harness into columned
State.In addition, the gap between adhesive layer 24, adjacent hollow-fibre membrane 22,22 is blocked by described adhesive 27 etc..Accordingly,
When used cooling agent is supplied in each hollow bulb 23 of a large amount of hollow-fibre membranes 22,22 ... of harness, Bu Huijin
Between entering hollow-fibre membrane 22,22.That is, between preventing used cooling agent from entering hollow-fibre membrane 22,22.
Each hollow-fibre membrane 22 is the hollow form of both ends open.That is, in hollow-fibre membrane 22, the week of hollow bulb 23 is surrounded
Wall is the film for being filtered, and the liquid to be treated being supplied in hollow bulb 23 (is the cooling comprising tramp material in present embodiment
Agent) pass through perisporium towards direction outside footpath, so that liquid to be treated is filtered.The hollow-fibre membrane 22 of present embodiment is by organic
The organic hollow fiber film that film is constituted.Additionally, from softness and being easily formed from the viewpoint of processing, the material of hollow-fibre membrane 22
It is preferred that organic film.Even for example, such as the small hollow-fibre membrane 22 of the internal diameter of present embodiment, (in present embodiment, external diameter is 1
~4mm), also can easy to manufacture.
In the hollow-fibre membrane 22 of present embodiment, for example, external diameter is 1~4mm, internal diameter (diameter of hollow bulb 23) being
0.5~3mm.From the viewpoint of effective film filter area from ease of manufacturing and when being processed into module, preferably external diameter is 1.5
~2.5mm, internal diameter are 0.8~1.5mm.In addition, the molecular cut off of the hollow-fibre membrane 22 is, for example, 13000, in being formed at
The diameter (membrane aperture) in the hole of the perisporium (film) of hollow fiber film 22 is, for example, 0.003 μm.The membrane aperture is based on used cooling
The average grain diameter of the tramp material contained by agent and be set, preferably 0.001~0.05 μm.Additionally, present embodiment is used
The particle diameter distribution of the tramp material contained by cooling agent is about 0.15~5 μm.
Additionally, in the present embodiment, filtration test is carried out using several standard particle samples, and by particle diameter and grain
The relationship graph of the rejection (filtering rate) of son, the grain that rejection is 90% is obtained by the curve of approximation for obtaining
Footpath, and using the particle diameter as membrane aperture.
Housing 25 has shell main body 250, liquid to be treated introduction part 251, concentrate discharge unit 252 and filtered fluid discharge unit
253。
Shell main body 250 has drum, internally houses filter house 21 (beam of hollow-fibre membrane 22).Liquid to be treated is led
Enter the side (left side in Fig. 2) that portion 251 is arranged on shell main body 250, the liquid to be treated that will be externally supplied is (in this embodiment party
It is the used cooling agent before filtering in formula) guide to an end-side openings of each hollow-fibre membrane 22.Concentrate discharge unit 252
The another side (right side in Fig. 2) of shell main body 250 is arranged on, by what is discharged from the another side opening of each hollow-fibre membrane 22
Concentrate (cooling agent of the state being concentrated for tramp material in the present embodiment) is expelled to outside.Filtered fluid discharge unit 253
Extend towards direction outside footpath from the outer peripheral face of shell main body 250, by the hollow bulb and ft connection of shell main body 250.The filtered fluid is discharged
Portion 253 will reach filter house 21 (beam of hollow-fibre membrane 22) with shell main body 250 by the perisporium of each hollow-fibre membrane 22
Filtered fluid (being in the present embodiment the cooling agent after filtering) between inner peripheral surface is expelled to outside.
At the both ends of such housing 25 for constituting, o-ring 26 is provided between shell main body 250 and filter house 21.This is O-shaped
Ring 26 will block into liquid-tight shape between the outer peripheral face of the inner peripheral surface of shell main body 250 and filter house 21 (beam of hollow-fibre membrane 22)
State.Hereby it is possible to prevent the concentrate in the liquid to be treated and concentrate discharge unit 252 in liquid to be treated introduction part 251 from entering
Enter between the inner peripheral surface and filter house 21 (beam of hollow-fibre membrane 22) of shell main body 250.
With the liquid to be treated introduction part 251 of Filter membrane module 20 be connected treatment trough 121 by filtering side feed path 141, will
Used cooling agent in treatment trough 121 is guided to the liquid to be treated introduction part 251 of Filter membrane module 20.Supplied in the filtering side
Pump 142 is provided with to path 141.Driven by the pump 142, the used cooling agent in treatment trough 121 is supplied by filtering side
Path 141 and be supplied to Filter membrane module 20.
The filtering side feed path 141 is allowing used cooling agent from a side (left end in Fig. 2) towards another
One side (right-hand end in Fig. 2) in the way of flowing, is adjusted by laminar condition in the hollow bulb 23 of each hollow-fibre membrane 22
Supply to the flow of used cooling agent etc. of liquid to be treated introduction part 251.Specifically, filtering side feed path 141 with
Following manner supplies to processed liquid introduction part 251 cooling agent, i.e.,：The flowing in the hollow bulb 23 of each hollow-fibre membrane 22
Cooling agent Reynolds number preferably 10~2000, more preferably 10~500, further preferred 10~200.
With treatment trough 121 be connected the concentrate discharge unit 252 of Filter membrane module 20 by filtering side foldback path 143, will be
In cooling agent (useless cooling agent) guiding to the treatment trough 121 being concentrated in Filter membrane module 20.This useless cooling agent is by filtering
The membrane filtration of film module 20 and the concentration of tramp material uprise the cooling agent of the state of (i.e. tramp material is concentrated).
Filtered fluid accumulator tank 144 stores the treated cooling discharged from the filtered fluid discharge unit 253 of Filter membrane module 20
Agent.
Centrifugation portion 16 has centrifugal separator 161, separator accumulator tank 166, separation side feed path 167 and separates
Side foldback path 169.The centrifugation portion 16 is separated from the cooling agent being stored in treatment trough 121 by centrifugation and (removed
Go) the larger tramp material of contained in cooling agent particle diameter, and by the cooling agent foldback treatment trough 121 after the separation tramp material.
Centrifugal separator 161 has housing 162, bowl body 163, motor 164 and scraper plate 165.Bowl body 163 is configured in housing
In 162, in upside be cylindric and downside is coniform shape.The lower ending opening of the bowl body 163.In addition, bowl body 163 passes through
The rotary shaft 164a that above-below direction extends is connected with motor 164.Motor 164 drives rotary shaft 164a and rotates it, so that
Bowl body 163 is rotated centered on rotary shaft 164a.Scraper plate 165 scrapes the internal face that is attached to bowl body 163 using its side end
Tramp material.
The centrifugal force that the centrifugal separator 161 is produced using the rotation based on bowl body 163, is fed in bowl body 163
Cooling agent and tramp material (silicon cutting swarf, scroll saw clipped wire, abrasive particle in itself (with the situation that free abrasive mode is cut off)
Separate.The centrifugal separator 161 of present embodiment is so-called longitudinal type centrifugal separator, but is alternatively the rotation axis horizontal of bowl body
Or the so-called horizontal type centrifugal separator of approximate horizontal configuration.
In the centrifugal separator 161, in scraping, in the state of the rotary speed reduction for making bowl body 163, so as to scrape
Mode mobile scraper 165 of the side end of plate 165 close to the internal face of bowl body 163.The tramp material scraped using scraper plate 165 is passed through
The opening of the lower end of bowl body 163 is discharged to separator accumulator tank 166.
With the introduction part (omitting diagram) of centrifugal separator 161 be connected treatment trough 121 by separation side feed path 167, and
Cooling agent in treatment trough 121 is guided to centrifugal separator 161.Pump 168 is provided with the separation side feed path 167.Pass through
The driving of the pump 168, the cooling agent in treatment trough 121 is supplied to centrifugal separator 161 by separation side feed path 167
The introduction part.
With treatment trough 121 be connected the discharge unit (omitting diagram) of centrifugal separator 161 by separation side foldback path 169, will
The separated cooling agent of larger tramp material (separate cooling agent) guiding is to treatment trough 121 in centrifugal separator 161
It is interior.
The concentration of the 10 pairs of such as tramp materials of cooling agent regenerating unit for constituting as described above is more than 10 weight % cold
But agent is regenerated and can be recycled.
For example, 10 pairs of used cooling agents used when 2~3 silicon ingots are cut off of the cooling agent regenerating unit enter
Row batch processing.The size of silicon ingot be 15cm × 15cm × 45cm, loss that silicon proportion is 2.3, silicon ingot (during cut-out into
It is the ratio of cutting swarf) it is about in the case of 50%, if the about 23kg such as 2 silicon ingots of cut-out, produced cutting swarf.This
When, the amount of the cooling agent for using is 200kg.In the case, the concentration (weight %) of the tramp material of used cooling agent is
(23/223) × 100=10.3%.
Cooling agent regenerating unit 10 is processed this kind of used cooling agent (removing tramp material) and can be again
Utilize.
In managing in this place, in the cooling agent regenerating unit 10 of present embodiment, because used cooling agent is with laminar flow
State flowing in the hollow bulb 23 of each hollow-fibre membrane 22 in membrane filtration portion 14, so, with the feelings flowed under turbulent condition
Condition compares, and the inner peripheral surface that the tramp material contained in used cooling agent is not easy to collide in hollow-fibre membrane 22 (is surrounded hollow
The filter membrane surface in portion 23).Therefore, in the tramp material for being filtered to remove used cooling agent using hollow-fibre membrane 22,
The hollow-fibre membrane that can effectively prevent from resulting from abrasion of filter membrane surface (inner peripheral surface) of collision of tramp material etc. to cause
22 damage.Details are as follows.
In conventional cooling agent renovation process, if using organic hollow fiber film, easily in the organic hollow fiber
The filter membrane surface of film produces abrasion equivalent damage.The result that the reason for through to the damage is studied, finds because used cold
But agent is big relative to the flow velocity of filter membrane surface, so the flowing of the cooling agent near filter membrane surface turns into turbulent condition,
The tramp material contained in used cooling agent is collided in filter membrane surface because of the turbulent flow, therefore, there is filter membrane surface
Damage.In this regard, in cooling agent regenerating unit 10, by allowing used cooling agent with laminar condition in hollow-fibre membrane 22
Flowing in hollow bulb 23, the tramp material is inhibited to the collision of the inner peripheral surface (filter membrane surface) of hollow-fibre membrane 22, according to
This, prevents the damage of hollow-fibre membrane 22.
In addition, in the cooling agent regenerating unit 10 of present embodiment, parallel (while) carry out using hollow-fibre membrane 22
Membrane filtration and using whizzer centrifugation.Accordingly, used cooling agent is effectively removed by centrifugation
In the larger cutting swarf that contains etc., also, using hollow-fibre membrane simultaneously from big containing be difficult to remove by centrifugation
The used cooling agent of small (i.e. less) tramp material isolates treated cooling agent.As a result, in present embodiment
Cooling agent regenerating unit 10 in, high-quality can be obtained from the concentration of tramp material cooling agent high in a short time and (be mixed into
Thing is less) re-generatively cooled agent.Details are as follows.
In cooling agent regenerating unit 10, the membrane aperture of each hollow-fibre membrane 22 is set as less than 0.05 μm (in this reality
Apply in mode as 0.003 μm), membrane aperture is set smaller than the particle diameter distribution (about 0.15 of the tramp material of used cooling agent
~5 μm).In addition, allow the flowing in the hollow bulb 23 with laminar condition of used cooling agent, to allow the mixed of used cooling agent
Enter thing (cutting swarf etc.) to be difficult to collide in the inner peripheral surface of hollow-fibre membrane 22.Accordingly, the cooling agent in present embodiment regenerates dress
Put in 10, even if in the used cooling agent high of the concentration to tramp material (for example, the concentration of tramp material is more than 10 weight %
Cooling agent) processed in the case of, be also difficult in each hollow-fibre membrane 22 of Filter membrane module 20 occur film block, energy
It is enough to carry out membrane filtration long-term and stably.Even if that is, the used cooling agent high to the concentration of tramp material was carried out
Filter, is also difficult to film blocking in hollow-fibre membrane 22, therefore, even if to the tramp material that can be centrifuged with high efficiency
Concentration used cooling agent high is processed, it is also possible to carry out membrane filtration long-term and stably.Accordingly, using centrifugation
Effectively remove larger cutting swarf for containing in used cooling agent etc., also, using hollow-fibre membrane simultaneously from containing
The used cooling agent of (i.e. less) tramp material for the size for being difficult to remove by centrifugation is isolated treated cold
But agent.As a result, in the cooling agent regenerating unit 10 of present embodiment, can be in the short time from high cold of the concentration of tramp material
But agent obtains the re-generatively cooled agent of high-quality (i.e. tramp material is less).
Additionally, in the inner pressed (filter type for making liquid to be treated be flowed in hollow bulb) using conventional hollow-fibre membrane
Filtering in, in the case of the viscosity of the similar cooling agent of filtering fluid high, used the hollow-fibre membrane that membrane aperture is big.Separately
Outward, liquid to be treated is supplied to hollow bulb in the liquid to be treated mode big relative to the flow velocity of inner peripheral surface (filter membrane surface).
This is to scrape the tramp material of the inner peripheral surface of hollow-fibre membrane to be piled up in using the liquid to be treated of disturbance state.Due to using
The big hollow-fibre membrane of membrane aperture, so tramp material enters in hollow-fibre membrane (surround in the perisporium of hollow bulb) and is susceptible to
The film of hollow-fibre membrane is blocked, if the also low use of the concentration that can be centrifuged with high efficiency to the concentration ratio of tramp material
The cooling agent crossed is filtered, then film occurs in a short time and blocks and cannot stably carry out membrane filtration.And, because hollow
The used cooling agent of flowing is in sinuous flow state in the hollow bulb of tunica fibrosa, so because the collision of tramp material causes inner peripheral surface
Abrasion etc. and easily cause the damage of hollow-fibre membrane.
The cooling agent regenerating unit 10 of present embodiment regularly carries out backwash (backwash) in membrane filtration portion 14.According to
This, the film of each hollow-fibre membrane 22 blocks more difficult generation.
In addition, in cooling agent regenerating unit 10, by carrying out backwash, being piled up in the grain of the inner peripheral surface of hollow-fibre membrane 22
The less tramp material in footpath turns into be had the block of size to a certain degree and is peeled off from inner peripheral surface.The block of the stripping passes through in backwash
Filtering side feed path 141 flows into treatment trough 121.Return to that described piece of the treatment trough 121 of behavior is big with particle diameter to be mixed into
Thing is identical, it is therefore preferable that being separated from used cooling agent in centrifugation portion 16.
Cooling agent regenerating unit of the invention and cooling agent renovation process are not limited to above-mentioned implementation method, certainly not
Various changes can be made in the range of main points of the invention.
The cooling agent regenerating unit 10 of above-mentioned implementation method can make the cooling agent used when silicon ingot is cut off sharp again
With (regeneration), but it is also possible to which the cooling agent to being used in crystal ingot (for example, the crystal ingot such as sapphire) beyond cutting off silicon is carried out
Regeneration.
In addition, in the cooling agent regenerating unit 10 of above-mentioned implementation method, while carrying out using the film of hollow-fibre membrane 22
Filtering and the centrifugation using centrifugal separator 161, but it is not limited to the structure.For example, cooling agent regenerating unit is alternatively
Only carry out the structure using the membrane filtration of hollow-fibre membrane 22.In the structure shown here, also with using for being flowed in hollow bulb 23
Cooling agent turn into laminar condition mode used cooling agent is supplied to the hollow bulb 23 of each hollow-fibre membrane 22, from
And the damage of the hollow-fibre membrane 22 caused by the collision of the tramp material of used cooling agent is inhibited.And, pass through
The membrane aperture of hollow-fibre membrane 22 is set to less than 0.05 μm, the film that tramp material is caused is blocked and is also inhibited, can be for a long time
Stably carry out membrane filtration.
In addition, the concentration of the tramp material of the used cooling agent of the treatment of cooling agent regenerating unit 10 of above-mentioned implementation method
It is more than 10 weight %, but is not limited to the concentration.That is, cooling agent regenerating unit 10 can also process the concentration of tramp material less than 10
The used cooling agent of weight %.Used cooling agent of the concentration of the tramp material less than 10 weight %, such as in cut-out
The few situation of amount of silicon ingot (silicon ingot of cut-out is the situation of one or cuts off smaller than the silicon ingot of above-mentioned implementation method
Situation etc.) under produce.In the case, cooling agent regenerating unit 10 can also make centrifugation portion 16 stop and only make membrane filtration portion
14 work.
Additionally, in the cooling agent regenerating unit 10 of above-mentioned implementation method, used cooling agent is by being configured at housing
A large amount of (multiple) hollow-fibre membranes 22 in 25,22 ... and filtered, but be not limited to the structure.Or for example in shell
A structure for hollow-fibre membrane 22 is only configured in body 25.
Embodiment
Here, in order to confirm the cooling agent regenerating unit of above-mentioned implementation method and the effect of cooling agent renovation process, making
With the cooling agent regenerating unit of above-mentioned implementation method, and change the membrane aperture of hollow-fibre membrane, carried out respectively used cold
But the treatment of agent.Result is shown in Fig. 3 and following table 1 by it.
Additionally, the membrane aperture of the hollow-fibre membrane for now using is 0.003 μm (with above-mentioned implementation method identical aperture)
(embodiment 1~3, comparative example 3 of table 1), 0.02 μm (embodiment 4 of table 1), 0.04 μm (embodiment 5 of table 1), 0.1 μm of (table 1
Comparative example 1), 2 μm (comparative example 2 of table 1).The molecular cut off of these each hollow-fibre membranes is 13000, effective film filtering surface
Product is 10m2.In addition, the initial value of flux (flux) is adjusted to 20L/m2Hr, on backwash, makes filtered fluid every 30 minutes
Once adverse current 15 seconds.In addition, the concentration of the tramp material of the cooling agent of before processing is about 10 weight %.
Table 1
(1) permeation flux drops to initial setting value (20 (L/hrm2)) 80% untill filtration yield.
(2) permeation flux drops to initial setting value (20 (L/hrm2)) 80% untill filtration time.
As can be known from these results, the membrane aperture of hollow-fibre membrane is smaller, then be less susceptible to film blocking.That is, membrane aperture
Smaller, then filter run is more long.In addition, understanding by making to contain in the membrane aperture of hollow-fibre membrane sufficiently smaller than cooling agent
Tramp material particle diameter distribution (about 0.15~5 μm) (in the present embodiment, for example, 0.003 μm of situation), even if total filtering
Amount turns into 10000L/m2, the permeation flux of hollow-fibre membrane also hardly declines.Additionally, the doughnut of embodiment 1~5
The molecular cut off of film be 13000, but carried out using the hollow-fibre membrane that molecular cut off is 5000 it is similar to the above cold
But in the case that the regeneration of agent is processed, even if total filtration yield turns into 10000L/m2, the permeation flux of hollow-fibre membrane is also hardly
Can decline.
According to above example, the used cooling by making to be flowed in the hollow bulb of hollow-fibre membrane is able to confirm that
Agent turns into laminar condition, and the film that membrane aperture is set to effectively suppress less than tramp material hollow-fibre membrane is blocked.
[summary of implementation method]
The implementation method for summarizing the above is then as described below.
That is, in the cooling agent renovation process involved by above-mentioned implementation method, can make cutting off crystal ingot when institute with scroll saw
The cooling agent for using is recycled, and the cooling agent renovation process includes：Filter progress, so that the cooling agent is existed with laminar condition
The mode of flowing in each hollow bulb of one or more hollow-fibre membranes of hollow form, to being supplied respectively to institute in each hollow bulb
Cooling agent is stated, wherein, the aperture of the film of the hollow-fibre membrane is less than 0.05 μm.
According to the structure, because cooling agent is flowed with laminar condition in the hollow bulb of each hollow-fibre membrane, therefore, with
The situation of turbulent condition flowing is compared, and cutting swarf, the scroll saw of the crystal ingot contained in cooling agent clipped wire, abrasive particle in itself are (to swim
The situation of crystal ingot is cut off from abrasive particle mode) etc. the tramp material inner peripheral surface that is difficult to collide in hollow-fibre membrane (surround the mistake of hollow bulb
Filter membrane surface).Accordingly, in use the tramp material of hollow fiber film throw away the refrigerant when, effectively can prevent from resulting from being mixed into
The damage of the hollow-fibre membrane (filter membrane) of the collision of thing.
Further, since the aperture of the film of hollow-fibre membrane is less than 0.05 μm, so the aperture (membrane aperture) of film is less than making
The particle diameter of the tramp material contained in used cooling agent, therefore, tramp material is difficult to enter in hollow-fibre membrane and (surrounds hollow bulb
In perisporium), accordingly, hollow-fibre membrane is not easy film blocking because of tramp material.Therefore, even if because cooling agent is with Laminar Flow
And there is tramp material to be piled up in the situation of inner peripheral surface (filter membrane surface), it is also possible to prevent the lost of life of hollow-fibre membrane.
In the cooling agent renovation process of above-mentioned implementation method, for example, it is also possible to be：Flowed in each hollow bulb
The Reynolds number of cooling agent is 10~2000.
Additionally, in the cooling agent renovation process of above-mentioned implementation method, the tramp material of cooling agent is difficult to collide in hollow fibre
The inner peripheral surface of film is tieed up, and the film of hollow-fibre membrane is less likely to occur and blocked, therefore, even if being supplied to cold in the hollow bulb
But the concentration of the tramp material of agent is more than 10 weight %, it is also possible to carry out suitable membrane filtration for a long time.
In addition, in the cooling agent renovation process of above-mentioned implementation method, or：During the hollow-fibre membrane is organic
Hollow fiber film.
Organic filter film (organic film) is easily formed processing than inoranic membrane softness.Therefore, it is possible to easily formed internal diameter (in
The diameter in empty portion) small hollow-fibre membrane.
In addition, the cooling agent renovation process in above-mentioned implementation method also includes：Foldback operation, will lead in the filter progress
The hollow bulb of crossing each hollow-fibre membrane and the cooling agent that is concentrated is returned to store and is used when the crystal ingot is cut off
Cooling agent treatment trough.Also, it is preferred that in the filter progress, be stored in the treatment trough cooling agent be supplied to it is described
In the hollow bulb of each hollow-fibre membrane.
According to the structure, cooling agent can be made to be circulated between treatment trough and hollow-fibre membrane and persistently be filtered.According to
This, the tramp material that more reliably can contain in throw away the refrigerant.
Additionally, the cooling agent renovation process of above-mentioned implementation method also includes：Centrifugal separation process, to being stored in the treatment
The cooling agent of groove is centrifuged, and the cooling agent after centrifugation is returned into the treatment trough.Also, it is preferred that institute
Filter progress and the foldback operation are stated with the centrifugal separation process while carrying out.
Generally, inner pressed (mode for making the fluid before filtering be flowed in the hollow bulb) filtering of hollow fiber film in use
In, in the case where the cooling agent high of the concentration to tramp material is filtered, in the short time film can be caused to block up in hollow-fibre membrane
Plug, so as to membrane filtration cannot be carried out long-term and stably.But, the cooling agent renovation process according to above-mentioned implementation method, even if
In the case where the cooling agent high of the concentration to tramp material is processed, also it is difficult to film blocking in each hollow-fibre membrane, according to
This, can long-term and stably carry out membrane filtration.And, processed by the cooling agent high of the concentration to tramp material, can
Expeditiously it is centrifuged, thus it is possible to obtain the re-generatively cooled of high-quality (that is, tramp material is less) in a short time
Agent.
Additionally, by larger cutting swarf for containing in centrifugation effectively throw away the refrigerant etc., also, by hollow
Tunica fibrosa is simultaneously from the used cooling containing (i.e. less) cutting swarf of size for being difficult to remove by centrifugation etc.
Treated cooling agent (cooling agent after membrane filtration) is isolated in agent, high therefore, it is possible to the concentration in a short time by tramp material
Cooling agent obtain high-quality re-generatively cooled agent.
In addition, the cooling agent regenerating unit of above-mentioned implementation method, can make to be used when crystal ingot is cut off with scroll saw is cold
But agent is recycled, and the cooling agent regenerating unit includes：One or more hollow-fibre membranes of hollow form；And supply unit, by institute
Cooling agent is stated to supply to the hollow bulb of each hollow-fibre membrane.Also, the aperture of the film of the hollow-fibre membrane be 0.05 μm with
Under, the supply unit supplies the cooling to make the cooling agent in the way of laminar condition flows in each hollow bulb
Agent.
According to the structure, because cooling agent is flowed with laminar condition in the hollow bulb of each hollow-fibre membrane, therefore, with
The situation of turbulent condition flowing is compared, and the tramp material contained in cooling agent is difficult to collide the inner peripheral surface in hollow-fibre membrane.Accordingly,
In use during the tramp material of hollow fiber film throw away the refrigerant, can effectively prevent from resulting from the hollow fibre of the collision of tramp material
Tie up the damage of film.
Further, since the aperture of the film of hollow-fibre membrane is less than 0.05 μm, so the aperture (membrane aperture) of film is less than cold
The particle diameter of the tramp material for but containing in agent, therefore, tramp material is difficult to enter in hollow-fibre membrane (surround in the perisporium of hollow bulb),
Accordingly, hollow-fibre membrane is not easy film blocking because of tramp material.Therefore, even if because cooling agent is mixed into Laminar Flow
Thing is piled up in the situation of inner peripheral surface (filter membrane surface), it is also possible to prevent the lost of life of hollow-fibre membrane.
Additionally, the cooling agent regenerating unit of above-mentioned implementation method also includes：Treatment trough, stores when the crystal ingot is cut off
The cooling agent for being used；Foldback portion, the cooling agent foldback that will be concentrated by the hollow bulb of each hollow-fibre membrane
To the treatment trough；And centrifugal separating device, the cooling agent in the treatment trough is centrifuged, and by centrifugation
Cooling agent afterwards is returned to the treatment trough.Also, it is preferred that the supply unit will be stored in the cooling agent supply of the treatment trough
To the hollow bulb of each hollow-fibre membrane.
According to the structure, even if in the case where the cooling agent high of the concentration to tramp material is processed, in each hollow fibre
Dimension film is also difficult to film blocking, hereby it is possible to carry out membrane filtration long-term and stably.And, by the concentration to tramp material
Cooling agent high is processed, and can be expeditiously centrifuged, thus it is possible to obtain high-quality (i.e., in a short time
Tramp material is less) re-generatively cooled agent.
Additionally, by larger cutting swarf for containing in centrifugation effectively throw away the refrigerant etc., also, by hollow
Tunica fibrosa (i.e. less) cutting swarf of size that removing is difficult to remove by centrifugation simultaneously etc., therefore, it is possible in short-term
The interior concentration by tramp material cooling agent high obtains the re-generatively cooled agent of high-quality.
Industrial applicability
The present invention provides cooling agent renovation process and cooling agent regenerating unit.
Claims (8)
1. a kind of cooling agent renovation process, it is characterised in that the cooling agent used when crystal ingot is cut off with scroll saw can be made again
Utilize, the cooling agent renovation process includes：
Filter progress so that the cooling agent with laminar condition one or more hollow-fibre membranes of hollow form each hollow bulb
The mode of interior flowing, to the cooling agent is supplied respectively in each hollow bulb, is supplied to described cold in the hollow bulb
But agent is filtered towards direction outside footpath by the perisporium of the hollow-fibre membrane, wherein,
The cooling agent contains tramp material,
Cutting swarf of the tramp material comprising the crystal ingot,
The hollow-fibre membrane is organic hollow fiber film,
The aperture of the film of the hollow-fibre membrane is less than 0.05 μm and less than the particle diameter distribution of the tramp material.
2. cooling agent renovation process according to claim 1, it is characterised in that：
The Reynolds number of the cooling agent flowed in each hollow bulb is 10~2000.
3. cooling agent renovation process according to claim 1, it is characterised in that：
It is more than 10 weight % to the concentration of the tramp material of the cooling agent supplied in the hollow bulb.
4. cooling agent renovation process according to claim 2, it is characterised in that：
It is more than 10 weight % to the concentration of the tramp material of the cooling agent supplied in the hollow bulb.
5. cooling agent renovation process according to any one of claim 1 to 4, it is characterised in that also include：
Foldback operation, the cooling agent foldback that will be concentrated by the hollow bulb of each hollow-fibre membrane in the filter progress
To the treatment trough for storing the cooling agent used when the crystal ingot is cut off, wherein,
In the filter progress, the cooling agent for being stored in the treatment trough is supplied to the hollow bulb of each hollow-fibre membrane
It is interior.
6. cooling agent renovation process according to claim 5, it is characterised in that also include：
Centrifugal separation process, the cooling agent to being stored in the treatment trough is centrifuged, and by after centrifugation
Cooling agent is returned to the treatment trough, wherein,
The filter progress and the foldback operation are carried out simultaneously with the centrifugal separation process.
7. a kind of cooling agent regenerating unit, it is characterised in that the cooling agent used when crystal ingot is cut off with scroll saw can be made again
Utilize, the cooling agent regenerating unit includes：
One or more hollow-fibre membranes of hollow form；And
Supply unit, the cooling agent is supplied to the hollow bulb of each hollow-fibre membrane, wherein,
The cooling agent contains tramp material,
Cutting swarf of the tramp material comprising the crystal ingot,
The hollow-fibre membrane is organic hollow fiber film,
The aperture of the film of the hollow-fibre membrane is less than 0.05 μm and less than the particle diameter distribution of the tramp material,
The supply unit supplies the cooling to make the cooling agent in the way of laminar condition flows in each hollow bulb
Agent, be supplied to the cooling agent in the hollow bulb towards direction outside footpath by the perisporium of the hollow-fibre membrane by mistake
Filter.
8. cooling agent regenerating unit according to claim 7, it is characterised in that also include：
Treatment trough, stores the cooling agent used when the crystal ingot is cut off；
Foldback portion, the treatment is returned to by the cooling agent being concentrated by the hollow bulb of each hollow-fibre membrane
Groove；And
Centrifugal separating device, is centrifuged to the cooling agent in the treatment trough, and the cooling agent after centrifugation is returned
The treatment trough is delivered to, wherein,
The supply unit will be stored in the cooling agent of the treatment trough and supply to the hollow bulb of each hollow-fibre membrane.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2012/007651 WO2014083590A1 (en) | 2012-11-28 | 2012-11-28 | Coolant regeneration method and coolant regeneration device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104812532A CN104812532A (en) | 2015-07-29 |
| CN104812532B true CN104812532B (en) | 2017-05-31 |
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| CN201280077378.0A Expired - Fee Related CN104812532B (en) | 2012-11-28 | 2012-11-28 | Cooling agent renovation process and cooling agent regenerating unit |
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| JP (1) | JP5941995B2 (en) |
| CN (1) | CN104812532B (en) |
| WO (1) | WO2014083590A1 (en) |
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| JP2016203321A (en) * | 2015-04-24 | 2016-12-08 | 株式会社安永 | Wire saw, and manufacturing method of manufacturing plurality of sliced articles from workpiece using wire saw |
| JP6525709B2 (en) * | 2015-04-24 | 2019-06-05 | 株式会社安永 | Wire saw and manufacturing method for manufacturing a plurality of sliced products from a work using the wire saw |
| WO2018173376A1 (en) * | 2017-03-23 | 2018-09-27 | 住友電気工業株式会社 | Grinding fluid regeneration device and grinding fluid regeneration method |
| CN109764736B (en) * | 2018-12-21 | 2020-12-11 | 北京空间飞行器总体设计部 | Space microporous membrane evaporation efficient heat dissipation device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5171767A (en) * | 1991-05-06 | 1992-12-15 | Rohm And Haas Company | Utrafiltration process for the recovery of polymeric latices from whitewater |
| JPH06134264A (en) * | 1992-10-28 | 1994-05-17 | Mitsubishi Rayon Co Ltd | Turbidity removing device for semiconductor wafer grinding solution |
| JP4353665B2 (en) * | 2001-10-31 | 2009-10-28 | 三洋アクアテクノ株式会社 | Filtration device |
| JP2005334992A (en) * | 2004-05-25 | 2005-12-08 | Seiko Epson Corp | Waste fluid treating device, waste fluid treating method, and manufacturing system for semiconductor device |
| JP5261090B2 (en) * | 2008-09-11 | 2013-08-14 | 野村マイクロ・サイエンス株式会社 | Method and apparatus for treating wastewater containing silicon |
| CN101474511B (en) * | 2008-12-17 | 2011-05-04 | 西安通鑫半导体辅料有限公司 | Process for recovering polyethylene glycol and silicon carbide from silicon wafer wire cutting waste mortar |
| CN101804306B (en) * | 2010-04-22 | 2013-07-31 | 吉林市金赛科技开发有限公司 | High-performance polyethersulfone separating membrane and device for recycling sewage |
| JP2012061383A (en) * | 2010-09-14 | 2012-03-29 | Kobelco Eco-Solutions Co Ltd | Hollow fiber membrane unit, water treatment apparatus, and water treatment method |
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2012
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- 2012-11-28 WO PCT/JP2012/007651 patent/WO2014083590A1/en active Application Filing
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| CN104812532A (en) | 2015-07-29 |
| JPWO2014083590A1 (en) | 2017-01-05 |
| JP5941995B2 (en) | 2016-06-29 |
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