CN104812532A - Coolant regeneration method and coolant regeneration device - Google Patents

Coolant regeneration method and coolant regeneration device Download PDF

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Publication number
CN104812532A
CN104812532A CN201280077378.0A CN201280077378A CN104812532A CN 104812532 A CN104812532 A CN 104812532A CN 201280077378 A CN201280077378 A CN 201280077378A CN 104812532 A CN104812532 A CN 104812532A
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China
Prior art keywords
cooling agent
hollow
fibre membrane
membrane
treatment trough
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CN201280077378.0A
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CN104812532B (en
Inventor
井上一真
延藤芳树
荻田大
西田高治
玉井雅之
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Kuraray Co Ltd
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Kuraray Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D63/00Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/02Hollow fibre modules
    • B01D63/034Lumen open in more than two directions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/147Microfiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B27/00Other grinding machines or devices
    • B24B27/06Grinders for cutting-off
    • B24B27/0633Grinders for cutting-off using a cutting wire
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B57/00Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
    • B24B57/02Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B28D5/0076Accessories 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2315/00Details relating to the membrane module operation
    • B01D2315/14Batch-systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D63/00Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/02Hollow fibre modules

Abstract

The invention provides a coolant regeneration method for making coolant, which has been used when cutting an ingot using a wire saw, reusable is characterized in that coolant is supplied respectively into the respective hollow sections of one or multiple hollow fiber membranes that are hollow from one end of each hollow fiber membrane and the membrane pore size in the hollow fiber membrane is 0.05 mum or less so that the coolant flows in the hollow sections in a laminar flow.

Description

Cooling agent renovation process and cooling agent regenerating unit
Technical field
The present invention relates to a kind of cooling agent renovation process and cooling agent regenerating unit, remove the tramp materials such as cutting swarf the cooling agent used when cutting off the crystal ingots such as silicon from using scroll saw, thus this cooling agent is recycled.
Background technology
Silicon wafer for solar cell etc. obtains by using scroll saw to cut off (section) to silicon ingot.The method cutting off silicon ingot has bonded-abrasive mode and free abrasive mode two kinds.Bonded-abrasive mode uses cuts off silicon ingot by the scroll saw of the abrasive particle sets such as carborundum and cooling agent (cooling fluid).In addition, free abrasive mode uses scroll saw and the cooling agent (mud) containing abrasive particle to cut off silicon ingot.
In general, from the view point of manufacturing cost, the cooling agent used in the cut-out operation of silicon ingot (used cooling agent) is recycled.Cutting swarf (following, also referred to as " cutting swarf ") containing silicon in this used cooling agent, the tramp material such as clipped wire, abrasive particle (carrying out situation about cutting off in free abrasive mode) of scroll saw itself.Therefore, if directly recycle used cooling agent, the scuffing of silicon wafer surface, the breakage of silicon wafer, the deterioration etc. of cutting machine may be caused.Therefore, used cooling agent is reused after by tramp materials such as removing cutting swarf such as filtration, centrifugations.
Such as, patent document 1 discloses a kind of cooling agent to using in the cut-out operation of silicon ingot and carries out membrane filtration and the method (cooling agent renovation process) that can recycle.In this cooling agent renovation process, filter membrane is used to filter used cooling agent, accordingly, from described cooling agent removing tramp material.Be described in detail as follows.
Described cooling agent renovation process uses the aperture (membrane aperture) in the hole of filter membrane to be that the ceramic membrane of 1 ~ 10 μm is as filter membrane.This filter membrane is hollow tube-shape (drum).And, by so-called cross flow one (cross-flow) mode from tramp materials such as used cooling agent removing cutting swarfs, this cross flow configuration is the mode that side allows used cooling agent flow abreast relative to the surface (filter membrane surface) of filter membrane in or beyond the hollow bulb of the filter membrane of this hollow tube-shape.
In the filtration of this cross flow configuration, usually the flow velocity of used cooling agent relative to filter membrane surface is increased.Accordingly, utilize the flowing of used cooling agent to strike off the tramp materials such as the cutting swarf that will be piled up in filter membrane surface, therefore, tramp material is inhibited to the accumulation of filter membrane surface, its result, and the film blocking of filter membrane is inhibited.
At this, in cooling agent renovation process, if use ceramic membrane cost to rise, therefore, use organic filter film (organic film) in recent years.Such as, in cooling agent renovation process disclosed in patent document 2, the aperture of use filter membrane is the organic film of 0.1 μm.
But organic film is softer than ceramic membrane, when filtering the used cooling agent containing tramp materials such as cutting swarfs, easily produce the abrasion equivalent damage of filter membrane surface.
Prior art document
Patent document
Patent document 1: No. 2012-6115, Japanese Laid-Open Patent Publication
Patent document 2: No. 2012-020365, Japanese Laid-Open Patent Publication
Summary of the invention
The object of the present invention is to provide a kind of cooling agent renovation process and cooling agent regenerating unit, when in use hollow fiber film filters cooling agent, not easily make described hollow-fibre membrane damage because of the tramp material of cooling agent.
According to the cooling agent renovation process of one aspect of the invention, the cooling agent recycling used when cutting off crystal ingot with scroll saw can be made, described cooling agent renovation process comprises: filter progress, in the mode making described cooling agent flow in each hollow bulb of one or more hollow-fibre membranes of hollow form with laminar condition, described cooling agent is supplied respectively in described each hollow bulb, wherein, the aperture of the film of described 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 the cooling agent recycling used when cutting off crystal ingot with scroll saw, described cooling agent regenerating unit comprises: one or more hollow-fibre membranes of hollow form; And supply unit, described cooling agent is supplied in the hollow bulb of each hollow-fibre membrane, wherein, the aperture of the film of described hollow-fibre membrane is less than 0.05 μm, and described supply unit supplies described cooling agent in the mode making described cooling agent and flow in described each hollow bulb with laminar condition.
Accompanying drawing explanation
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 described cooling agent regenerating unit.
Fig. 3 is the figure of the relation between total filtration yield of each membrane aperture representing hollow-fibre membrane and permeation flux.
Detailed description of the invention
Below, referring to figs. 1 through Fig. 2, one embodiment of the present invention is described.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 described cooling agent regenerating unit.
The cooling agent regenerating unit of present embodiment is in the manufacturing process of silicon wafer being such as used in semiconductor, solar cell etc., remove tramp material from the cooling agent (cooling fluid) used when cutting off silicon ingot with scroll saw, thus this cooling agent is recycled.In addition, the cutting-off method of silicon ingot can be any one of bonded-abrasive mode and free abrasive mode.
Cooling agent comprises the water-soluble solvents such as diethylene glycol, propane diols, low-molecular-weight polyethylene glycol.The viscosity of this cooling agent is 20 ~ 60cp.In addition, when dilute with water cooling agent, sometimes various additives etc. are added.Therefore, the composition of cooling agent and viscosity are not limited to described composition and viscosity.
Below, with reference to Fig. 1 and Fig. 2, cooling agent regenerating unit 10 is illustrated.
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 using scroll saw to cut off silicon ingot.This used cooling agent is used in following object, that is: to the frictional heat that produces when using scroll saw to cut off silicon ingot cool and will cut off the silicon ingot produced cutting swarf (silicon cutting swarf) dispersion and from cutting portion discharge etc.Therefore, the cutting swarf of silicon, the tramp material such as clipped wire, abrasive particle (carrying out situation about cutting off in free abrasive mode) of scroll saw itself can be contained in used cooling agent.
Mixing part 122 has the agitator 123 be configured in treatment trough 121 and the motor 124 being connected with agitator 123 by rotating shaft 124a.Rotating shaft 124a extends along the vertical direction.Motor 124 makes agitator 123 rotate centered by rotating shaft 124a.This kind of mixing part 122, by making agitator 123 rotate by motor 124, is stirred the used cooling agent be stored in treatment trough 121.The mixing part 122 of present embodiment, when membrane filtration portion 14 works with centrifugation portion 16, is stirred the used cooling agent be stored in treatment trough 121.
Membrane filtration portion 14 has Filter membrane module 20, filters side feed path (supply unit) 141, filters foldback path, side (foldback portion) 143 and filtered fluid accumulator tank 144.This membrane filtration portion 14 filters to remove the tramp material contained in this cooling agent to the used cooling agent being stored in treatment trough 121, and will remove the coolant feed after tramp material by filtering to filtered fluid accumulator tank 144.
Filter membrane module 20 has the housing 25 by the filter house 21 of a large amount of (multiple) hollow-fibre membrane 22,22 ... harness and collecting 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 membrane 22,22...... become columned state by harness.In addition, at adhesive layer 24, the gap between adjacent hollow-fibre membrane 22,22 is by blockings such as described adhesives 27.Accordingly, when in each hollow bulb 23 that used cooling agent is supplied to a large amount of hollow-fibre membranes 22 of harness, 22......, can not enter between hollow-fibre membrane 22,22.That is, prevent used cooling agent from entering between hollow-fibre membrane 22,22.
Each hollow-fibre membrane 22 is hollow forms of both ends open.Namely, in hollow-fibre membrane 22, the perisporium surrounding hollow bulb 23 is the film carrying out filtering, and the liquid to be treated (for comprising the cooling agent of tramp material in present embodiment) be supplied in hollow bulb 23 passes through perisporium towards direction outside footpath, thus liquid to be treated is filtered.The hollow-fibre membrane 22 of present embodiment is the organic hollow tunica fibrosa be made up of organic film.In addition, from the view point of soft and easy formed machining, the preferred organic film of material of hollow-fibre membrane 22.Such as, even the hollow-fibre membrane 22 (in present embodiment, external diameter is 1 ~ 4mm) that the internal diameter as present embodiment is little, also can easily manufacture.
In the hollow-fibre membrane 22 of present embodiment, such as, external diameter is 1 ~ 4mm, internal diameter (diameter of hollow bulb 23) is 0.5 ~ 3mm.Effective film filter area from the view point of ease of manufacturing and when being processed into module, preferred external diameter is 1.5 ~ 2.5mm, internal diameter is 0.8 ~ 1.5mm.In addition, the molecular cut off of this hollow-fibre membrane 22 is such as 13000, and the diameter (membrane aperture) being formed at the hole of the perisporium (film) of hollow-fibre membrane 22 is such as 0.003 μm.This membrane aperture based on the tramp material contained by used cooling agent average grain diameter and be set, preferably 0.001 ~ 0.05 μm.In addition, the domain size distribution of the tramp material contained by used cooling agent of present embodiment is about 0.15 ~ 5 μm.
In addition, in the present embodiment, several standard particle sample is used to carry out filtration test, and by the relation pictorialization of the rejection (filtering rate) of particle diameter and particle, the particle diameter that rejection is 90% is obtained by the curve of approximation obtained, and using this particle diameter as membrane aperture.
Housing 25 has shell main body 250, liquid to be treated introduction part 251, concentrate discharge portion 252 and filtered fluid discharge portion 253.
Shell main body 250 has drum, in inside collecting filter house 21 (bundle of hollow-fibre membrane 22).Liquid to be treated introduction part 251 is arranged on the end side (left side in Fig. 2) of shell main body 250, the liquid to be treated supplied (being the used cooling agent before filtration in the present embodiment) is guided to the end side opening of each hollow-fibre membrane 22 from outside.Concentrate discharge portion 252 is arranged on another side (right side in Fig. 2) of shell main body 250, and the concentrate of being discharged by the other end side opening from each hollow-fibre membrane 22 (cooling agent of the state be concentrated for tramp material in the present embodiment) is expelled to outside.Filtered fluid discharge portion 253 extends, by the hollow bulb of shell main body 250 and ft connection from the outer peripheral face of shell main body 250 towards direction footpath.The filtered fluid (being the cooling agent after filtering in the present embodiment) that perisporium by each hollow-fibre membrane 22 arrives between filter house 21 (bundle of hollow-fibre membrane 22) and the inner peripheral surface of shell main body 250 by this filtered fluid discharge portion 253 is expelled to outside.
At the both ends of the housing 25 so formed, between shell main body 250 and filter house 21, be provided with O type ring 26.This O type ring 26 blocks into liquid tight condition by between the inner peripheral surface of shell main body 250 with the outer peripheral face of filter house 21 (bundle of hollow-fibre membrane 22).Accordingly, can prevent the concentrate in the liquid to be treated in liquid to be treated introduction part 251 and concentrate discharge portion 252 from entering between the inner peripheral surface of shell main body 250 and filter house 21 (bundle of hollow-fibre membrane 22).
Filter side feed path 141 treatment trough 121 is connected with the liquid to be treated introduction part 251 of Filter membrane module 20, the used cooling agent in treatment trough 121 is guided to the liquid to be treated introduction part 251 of Filter membrane module 20.Pump 142 is provided with at this filtration side feed path 141.Driven by this pump 142, the used cooling agent in treatment trough 121 is supplied to Filter membrane module 20 by filtering side feed path 141.
This filtration side feed path 141 is to allow used cooling agent from end side (left end Fig. 2) towards another side (right-hand end in Fig. 2) in the mode that laminar condition flows in the hollow bulb 23 of each hollow-fibre membrane 22, and adjustment is supplied to the flow etc. of the used cooling agent of liquid to be treated introduction part 251.Specifically, filter side feed path 141 and cooling agent is supplied to processed liquid introduction part 251 as follows, that is: the Reynolds number preferably 10 ~ 2000 of the cooling agent of flowing in the hollow bulb 23 of each hollow-fibre membrane 22, more preferably 10 ~ 500, further preferably 10 ~ 200.
Filter foldback path, side 143 the concentrate discharge portion 252 of Filter membrane module 20 is connected with treatment trough 121, the cooling agent be concentrated in Filter membrane module 20 (useless cooling agent) is guided in treatment trough 121.This useless cooling agent is the cooling agent that the concentration of tramp material uprises the state of (namely tramp material is concentrated) by the membrane filtration of Filter membrane module 20.
Filtered fluid accumulator tank 144 stores the cooling agent of the process of discharging from the filtered fluid discharge portion 253 of Filter membrane module 20.
Centrifugation portion 16 has centrifugal separator 161, separator accumulator tank 166, separation side feed path 167 and separation side foldback path 169.This centrifugation portion 16 is separated the larger tramp material of particle diameter contained (removing) this cooling agent by centrifugation from the cooling agent be stored in treatment trough 121, and by the cooling agent foldback treatment trough 121 after this 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 162, in upside for cylindric and downside is cone shape shape.The lower ending opening of this bowl of body 163.In addition, the rotating shaft 164a that bowl body 163 is extended by above-below direction is connected with motor 164.Motor 164 drives rotating shaft 164a and makes it rotate, thus bowl body 163 is rotated centered by rotating shaft 164a.Scraper plate 165 utilizes its side end to scrape the tramp material of the internal face being attached to bowl body 163.
The centrifugal force that this centrifugal separator 161 utilizes the rotation based on bowl body 163 and produces, by the cooling agent be supplied in bowl body 163, (clipped wire, the abrasive particle (carrying out situation about cutting off in free abrasive mode) of silicon cutting swarf, scroll saw itself are separated with tramp material.The centrifugal separator 161 of present embodiment is so-called longitudinal type centrifugal separator, but also can be the rotation axis horizontal of bowl body or the so-called horizontal type centrifugal separator of approximate horizontal configuration.
In this centrifugal separator 161, when scraping, under the state making the rotary speed of bowl body 163 reduce, to make the side end of scraper plate 165 close to the mode mobile scraper 165 of the internal face of bowl body 163.The tramp material using scraper plate 165 to scrape is discharged to separator accumulator tank 166 by the opening of the lower end of bowl body 163.
Treatment trough 121 is connected with the introduction part (omit and illustrate) of centrifugal separator 161 by separation side feed path 167, and the cooling agent in treatment trough 121 is guided to centrifugal separator 161.Pump 168 is provided with at this separation side feed path 167.By the driving of this pump 168, the cooling agent in treatment trough 121 is supplied to the described introduction part of centrifugal separator 161 by separation side feed path 167.
The discharge portion of centrifugal separator 161 (omitting diagram) is connected with treatment trough 121 by separation side foldback path 169, the cooling agent (isolated cooling agent) being separated larger tramp material guided in treatment trough 121 in centrifugal separator 161.
The cooling agent regenerating unit 10 formed as described above regenerates the cooling agent that the concentration of such as tramp material is more than 10 % by weight and can recycle.
Such as, this cooling agent regenerating unit 10 carries out batch processing to the used cooling agent used when cut-out 2 ~ 3 silicon ingots.When the size of silicon ingot be 15cm × 15cm × 45cm, silicon proportion is 2.3, the loss of silicon ingot (becoming the ratio of cutting swarf during cut-out) is about 50%, if cut off 2 silicon ingots, the cutting swarf produced etc. are about 23kg.Now, the amount of the cooling agent of use is 200kg.In the case, the concentration (% by weight) of the tramp material of used cooling agent is (23/223) × 100=10.3%.
Cooling agent regenerating unit 10 processes (removing tramp material) to this kind of used cooling agent and can recycle.
In this process, in the cooling agent regenerating unit 10 of present embodiment, because used cooling agent flows in the hollow bulb 23 of each hollow-fibre membrane 22 in membrane filtration portion 14 with laminar condition, so, compare with the situation in turbulent condition current downflow, the tramp material contained in used cooling agent is not easy to collide the inner peripheral surface (surrounding the filter membrane surface of hollow bulb 23) in hollow-fibre membrane 22.Therefore, when utilizing the mistake of hollow-fibre membrane 22 to filter the tramp material of used cooling agent, the damage of the hollow-fibre membrane 22 that can effectively prevent from resulting from the abrasion etc. of the filter membrane surface (inner peripheral surface) of the collision of tramp material to cause.Details are as follows.
In cooling agent renovation process in the past, if use organic hollow tunica fibrosa, then the easy filter membrane surface at this organic hollow tunica fibrosa produces abrasion equivalent damage.Through the result studied the reason of this damage, find because used cooling agent is large relative to the flow velocity of filter membrane surface, so the flowing of cooling agent near filter membrane surface becomes turbulent condition, the tramp material contained in used cooling agent collides in filter membrane surface because of this turbulent flow, therefore, there is the damage of filter membrane surface.To this, in cooling agent regenerating unit 10, flow in the hollow bulb 23 of hollow-fibre membrane 22 with laminar condition by allowing used cooling agent, described tramp material is inhibited to the collision of the inner peripheral surface (filter membrane surface) of hollow-fibre membrane 22, accordingly, the damage of hollow-fibre membrane 22 is prevented.
In addition, in the cooling agent regenerating unit 10 of present embodiment, parallel (simultaneously) carries out utilizing the membrane filtration of hollow-fibre membrane 22 and utilizing the centrifugation of whizzer.Accordingly, the larger cutting swarf etc. contained effectively is removed in used cooling agent by centrifugation, further, utilize hollow-fibre membrane to isolate from the used cooling agent containing (namely less) tramp material being difficult to the size removed by centrifugation the cooling agent processed simultaneously.Its result, in the cooling agent regenerating unit 10 of present embodiment, can obtain the re-generatively cooled agent of high-quality (namely tramp material is less) at short notice from the cooling agent that the concentration of tramp material is high.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 (being 0.003 μm in the present embodiment), membrane aperture is set smaller than the domain size distribution (about 0.15 ~ 5 μm) of the tramp material of used cooling agent.In addition, allow used cooling agent flow in hollow bulb 23 with laminar condition, be difficult to collide the inner peripheral surface in hollow-fibre membrane 22 to allow the tramp material of used cooling agent (cutting swarf etc.).Accordingly, in the cooling agent regenerating unit 10 of present embodiment, even if to the high used cooling agent of the concentration of tramp material (such as, the concentration of tramp material is the cooling agent of more than 10 % by weight) when carrying out processing, also be difficult to film blocking occurs in each hollow-fibre membrane 22 of Filter membrane module 20, membrane filtration can be carried out long-term and stably.That is, even if the used cooling agent high to the concentration of tramp material filters, also be difficult in hollow-fibre membrane 22 film blocking occurs, therefore, even if process the used cooling agent that can carry out the tramp material concentration of centrifugation high with high efficiency, also membrane filtration can be carried out long-term and stably.Accordingly, centrifugation is utilized effectively to remove in used cooling agent the larger cutting swarf etc. contained, further, utilize hollow-fibre membrane to isolate from the used cooling agent containing (namely less) tramp material being difficult to the size removed by centrifugation the cooling agent processed simultaneously.Its result, in the cooling agent regenerating unit 10 of present embodiment, can obtain the re-generatively cooled agent of high-quality (namely tramp material is less) in the short time from the cooling agent that the concentration of tramp material is high.
In addition, in the filtration of inner pressed (making the filter type that liquid to be treated flows at hollow bulb) using hollow-fibre membrane in the past, when the fluid that the viscosity of filtering similar cooling agent is high, the hollow-fibre membrane that membrane aperture is large is employed.In addition, in the mode that liquid to be treated is large relative to the flow velocity of inner peripheral surface (filter membrane surface), liquid to be treated is supplied in hollow bulb.This is to utilize the liquid to be treated scraping of disturbance state for being piled up in the tramp material of the inner peripheral surface of hollow-fibre membrane.Owing to using the hollow-fibre membrane that membrane aperture is large, so tramp material enters hollow-fibre membrane interior (surrounding in the perisporium of hollow bulb) and the film blocking of hollow-fibre membrane easily occurs, if do not filter the used cooling agent that the concentration ratio of tramp material can carry out the concentration of centrifugation also low with high efficiency, then there is film blocking at short notice and stably cannot carry out membrane filtration.And, because the used cooling agent flowed in the hollow bulb of hollow-fibre membrane is in sinuous flow state, so cause inner peripheral surface abrasion etc. and easily cause the damage of hollow-fibre membrane because of the collision of tramp material.
The cooling agent regenerating unit 10 of present embodiment carries out backwash (backwash) termly in membrane filtration portion 14.Accordingly, 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 less tramp material of the particle diameter of the inner peripheral surface of hollow-fibre membrane 22 becomes the block with to a certain degree size and peels off from inner peripheral surface.The block of this stripping, when backwash, flows into treatment trough 121 by filtering side feed path 141.The tramp material turning back to the behavior of described piece of this treatment trough 121 large with particle diameter is identical, therefore, is preferably separated from used cooling agent in centrifugation portion 16.
Cooling agent regenerating unit of the present invention and cooling agent renovation process are not limited to above-mentioned embodiment, certainly can do various change without departing from the gist of the present invention.
The cooling agent regenerating unit 10 of above-mentioned embodiment can make cooling agent recycling (regeneration) used when cutting off silicon ingot, but also can the cooling agent used when cutting off the crystal ingot beyond silicon crystal ingots such as (such as) sapphires be regenerated.
In addition, in the cooling agent regenerating unit 10 of above-mentioned embodiment, carry out the centrifugation utilizing the membrane filtration of hollow-fibre membrane 22 He utilize centrifugal separator 161 simultaneously, but be not limited to this structure.Such as, cooling agent regenerating unit also can be the structure of only carrying out the membrane filtration utilizing hollow-fibre membrane 22.In the structure shown here, used cooling agent is supplied in the hollow bulb 23 of each hollow-fibre membrane 22 by the mode also becoming laminar condition with the used cooling agent of flowing in hollow bulb 23, thus the damage of the hollow-fibre membrane 22 caused because of the collision of the tramp material of used cooling agent is inhibited.And by the membrane aperture of hollow-fibre membrane 22 is set to less than 0.05 μm, the film blocking that tramp material causes also is inhibited, and can carry out membrane filtration long-term and stably.
In addition, the concentration of the tramp material of the used cooling agent of cooling agent regenerating unit 10 process of above-mentioned embodiment is more than 10 % by weight, but is not limited to this concentration.That is, cooling agent regenerating unit 10 concentration that also can process tramp material lower than 10 % by weight used cooling agent.The concentration of this tramp material lower than the used cooling agent of 10 % by weight, such as, produces in the situation (silicon ingot of cut-out is the situation of one or cuts off the situation etc. less than the silicon ingot of above-mentioned embodiment) that the amount of the silicon ingot cut off is few.In the case, cooling agent regenerating unit 10 also can make centrifugation portion 16 stop and only making membrane filtration portion 14 work.
In addition, in the cooling agent regenerating unit 10 of above-mentioned embodiment, used cooling agent by being configured at a large amount of (multiple) hollow-fibre membrane 22 in housing 25,22 ... and be filtered, but is not limited to this structure.Also can be the structure such as only configuring a hollow-fibre membrane 22 in housing 25.
Embodiment
At this, in order to the effect of the cooling agent regenerating unit and cooling agent renovation process that confirm above-mentioned embodiment, use the cooling agent regenerating unit of above-mentioned embodiment, and change the membrane aperture of hollow-fibre membrane, carried out the process of used cooling agent respectively.It will the results are shown in Fig. 3 and following table 1.
In addition, the membrane aperture of the hollow-fibre membrane now used is 0.003 μm (aperture identical with above-mentioned embodiment) (embodiment 1 ~ 3 of table 1, comparative example 3), 0.02 μm (embodiment 4 of table 1), 0.04 μm (embodiment 5 of table 1), 0.1 μm (comparative example 1 of table 1), 2 μm (comparative example 2 of table 1).The particle diameter that retains of these each hollow-fibre membranes is 13000, and effective film filter area is 10m 2.In addition, the initial value of flux (flux) is adjusted to 20L/m 2hr, about backwash, makes filtered fluid every 30 minutes one time adverse current 15 seconds.In addition, the concentration of the tramp material of cooling agent before treatment is about 10 % by weight.
Table 1
(1) permeation flux drops to initial setting value (20 (L/hrm 2)) 80% till filtration yield.
(2) permeation flux drops to initial setting value (20 (L/hrm 2)) 80% till filtration time.
As can be known from these results, the membrane aperture of hollow-fibre membrane is less, then be more less likely to occur film blocking.That is, membrane aperture is less, then filter run is longer.In addition, known by making the membrane aperture of hollow-fibre membrane fully be less than the domain size distribution (about 0.15 ~ 5 μm) of the tramp material contained in cooling agent (in the present embodiment, be such as the situation of 0.003 μm), even if Zong filtration yield becomes 10000L/m 2, the permeation flux of hollow-fibre membrane also declines hardly.In addition, the particle diameter that retains of the hollow-fibre membrane of embodiment 1 ~ 5 is 13000, but when use retain particle diameter be 5000 hollow-fibre membrane carry out the regeneration process of cooling agent similar to the above, even if Zong filtration yield becomes 10000L/m 2, the permeation flux of hollow-fibre membrane also declines hardly.
According to above embodiment, can confirm by making the used cooling agent flowed in the hollow bulb of hollow-fibre membrane become laminar condition, and membrane aperture is set to is less than tramp material, can effectively suppress the film of hollow-fibre membrane to block.
[summary of embodiment]
Summarize above embodiment then as described below.
Namely, in the cooling agent renovation process involved by above-mentioned embodiment, the cooling agent recycling used when cutting off crystal ingot with scroll saw can be made, described cooling agent renovation process comprises: filter progress, in the mode making described cooling agent flow in each hollow bulb of one or more hollow-fibre membranes of hollow form with laminar condition, in described each hollow bulb, supply described cooling agent respectively, wherein, the aperture of the film of described hollow-fibre membrane is less than 0.05 μm.
According to this structure, because cooling agent flows in the hollow bulb of each hollow-fibre membrane with laminar condition, therefore, compared with situation about flowing with turbulent condition, the tramp materials such as the cutting swarf of the crystal ingot contained in cooling agent, the clipped wire of scroll saw itself, abrasive particle (cutting off the situation of crystal ingot in free abrasive mode) are difficult to collide the inner peripheral surface (surrounding the filter membrane surface of hollow bulb) in hollow-fibre membrane.Accordingly, during the tramp material of in use hollow fiber film throw away the refrigerant, effectively can prevent from resulting from the damage of the hollow-fibre membrane (filter membrane) of the collision of tramp material.
In addition, aperture due to the film of hollow-fibre membrane is less than 0.05 μm, so the aperture of film (membrane aperture) is less than the particle diameter of the tramp material contained in used cooling agent, therefore, tramp material is difficult to enter (perisporium surrounding hollow bulb is interior) in hollow-fibre membrane, accordingly, hollow-fibre membrane is not easy film blocking occurs because of tramp material.Therefore, even if having tramp material to be piled up in the situation of inner peripheral surface (filter membrane surface) with Laminar Flow because of cooling agent, the lost of life of hollow-fibre membrane can also be prevented.
In the cooling agent renovation process of above-mentioned embodiment, such as, also can be: the Reynolds number of the cooling agent flowed in described each hollow bulb is 10 ~ 2000.
In addition, in the cooling agent renovation process of above-mentioned embodiment, the tramp material of cooling agent is difficult to collide the inner peripheral surface in hollow-fibre membrane, and the film blocking of hollow-fibre membrane is less likely to occur, therefore, even if the concentration being supplied to the tramp material of the cooling agent in described hollow bulb is more than 10 % by weight, the membrane filtration be applicable to also can be carried out for a long time.
In addition, in the cooling agent renovation process of above-mentioned embodiment, also can be: described hollow-fibre membrane is organic hollow tunica fibrosa.
Organic filter film (organic film) is soft and easy formed machining than inoranic membrane.Therefore, it is possible to easily form the little hollow-fibre membrane of internal diameter (diameter of hollow bulb).
In addition, also comprising at the cooling agent renovation process of above-mentioned embodiment: foldback operation, the described cooling agent be concentrated being returned to the treatment trough storing the cooling agent used when cutting off described crystal ingot at described filter progress by the hollow bulb of each hollow-fibre membrane.Further, preferably at described filter progress, the cooling agent being stored in described treatment trough is supplied in the hollow bulb of described each hollow-fibre membrane.
According to this structure, cooling agent can be made to circulate between treatment trough and hollow-fibre membrane and continue to filter.Accordingly, the tramp material that can contain in throw away the refrigerant more reliably.
In addition, the cooling agent renovation process of above-mentioned embodiment also comprises: centrifugal separation process, carries out centrifugation, and the cooling agent after centrifugation is returned to described treatment trough to the described cooling agent being stored in described treatment trough.Further, preferred described filter progress and described foldback operation and described centrifugal separation process are carried out simultaneously.
Usually, during in use the inner pressed (making the mode that the fluid before filtration flows in hollow bulb) of hollow fiber film filters, when the cooling agent high to the concentration of tramp material filters, can film be caused to block at hollow-fibre membrane in the short time, thus membrane filtration cannot be carried out long-term and stably.But, according to the cooling agent renovation process of above-mentioned embodiment, even if when the cooling agent high to the concentration of tramp material processes, be also difficult to film blocking occurs at each hollow-fibre membrane, accordingly, membrane filtration can be carried out long-term and stably.And, processed by the cooling agent high to the concentration of tramp material, centrifugation can be carried out expeditiously, so, the re-generatively cooled agent of high-quality (that is, tramp material is less) can be obtained at short notice.
In addition, by the larger cutting swarf etc. contained in centrifugation effectively throw away the refrigerant, and, simultaneously isolate from the used cooling agent containing (namely less) cutting swarf etc. being difficult to the size removed by centrifugation the cooling agent (cooling agent after membrane filtration) processed by hollow-fibre membrane, therefore, it is possible to obtained the re-generatively cooled agent of high-quality at short notice by the cooling agent that the concentration of tramp material is high.
In addition, the cooling agent regenerating unit of above-mentioned embodiment, can make the cooling agent recycling used when cutting off crystal ingot with scroll saw, described cooling agent regenerating unit comprises: one or more hollow-fibre membranes of hollow form; And supply unit, described cooling agent is supplied in the hollow bulb of each hollow-fibre membrane.Further, the aperture of the film of described hollow-fibre membrane is less than 0.05 μm, and described supply unit supplies described cooling agent in the mode making described cooling agent and flow in described each hollow bulb with laminar condition.
According to this structure, because cooling agent flows in the hollow bulb of each hollow-fibre membrane with laminar condition, therefore, compared with situation about flowing with turbulent condition, the tramp material contained in cooling agent is difficult to collide the inner peripheral surface in hollow-fibre membrane.Accordingly, during the tramp material of in use hollow fiber film throw away the refrigerant, effectively can prevent from resulting from the damage of the hollow-fibre membrane of the collision of tramp material.
In addition, aperture due to the film of hollow-fibre membrane is less than 0.05 μm, so the aperture of film (membrane aperture) is less than the particle diameter of the tramp material contained in cooling agent, therefore, tramp material is difficult to enter (perisporium surrounding hollow bulb is interior) in hollow-fibre membrane, accordingly, hollow-fibre membrane is not easy film blocking occurs because of tramp material.Therefore, even if having tramp material to be piled up in the situation of inner peripheral surface (filter membrane surface) with Laminar Flow because of cooling agent, the lost of life of hollow-fibre membrane can also be prevented.
In addition, the cooling agent regenerating unit of above-mentioned embodiment also comprises: treatment trough, stores the cooling agent used when cutting off described crystal ingot; Foldback portion, the described cooling agent be concentrated by the hollow bulb by described each hollow-fibre membrane is returned to described treatment trough; And centrifugal separating device, centrifugation is carried out to the cooling agent in described treatment trough, and the cooling agent after centrifugation is returned to described treatment trough.Further, the cooling agent being stored in described treatment trough is supplied in the hollow bulb of described each hollow-fibre membrane by preferred described supply unit.
According to this structure, even if when the cooling agent high to the concentration of tramp material processes, be also difficult to film blocking occurs at each hollow-fibre membrane, accordingly, membrane filtration can be carried out long-term and stably.And, processed by the cooling agent high to the concentration of tramp material, centrifugation can be carried out expeditiously, so, the re-generatively cooled agent of high-quality (that is, tramp material is less) can be obtained at short notice.
In addition, by the larger cutting swarf etc. contained in centrifugation effectively throw away the refrigerant, and, removed (namely less) cutting swarf etc. being difficult to the size removed by centrifugation by hollow-fibre membrane simultaneously, therefore, it is possible to obtained the re-generatively cooled agent of high-quality at short notice by the cooling agent that the concentration of tramp material is high.
Utilizability in industry
The invention provides cooling agent renovation process and cooling agent regenerating unit.

Claims (8)

1. a cooling agent renovation process, is characterized in that, can make the cooling agent recycling used when cutting off crystal ingot with scroll saw, described cooling agent renovation process comprises:
Filter progress, in the mode making described cooling agent flow in each hollow bulb of one or more hollow-fibre membranes of hollow form with laminar condition, supplies described cooling agent respectively in described each hollow bulb, wherein,
The aperture of the film of described hollow-fibre membrane is less than 0.05 μm.
2. cooling agent renovation process according to claim 1, is characterized in that:
The Reynolds number of the cooling agent flowed in described each hollow bulb is 10 ~ 2000.
3. cooling agent renovation process according to claim 1 and 2, is characterized in that:
The concentration of the tramp material of the cooling agent supplied in described hollow bulb is more than 10 % by weight.
4. cooling agent renovation process according to any one of claim 1 to 3, is characterized in that:
Described hollow-fibre membrane is organic hollow tunica fibrosa.
5. cooling agent renovation process according to any one of claim 1 to 4, characterized by further comprising:
Foldback operation, is returned to the treatment trough storing the cooling agent used when cutting off described crystal ingot by the described cooling agent be concentrated by the hollow bulb of each hollow-fibre membrane at described filter progress, wherein,
At described filter progress, the cooling agent being stored in described treatment trough is supplied in the hollow bulb of described each hollow-fibre membrane.
6. cooling agent renovation process according to claim 5, characterized by further comprising:
Centrifugal separation process, carries out centrifugation to the described cooling agent being stored in described treatment trough, and the cooling agent after centrifugation is returned to described treatment trough, wherein,
Described filter progress and described foldback operation and described centrifugal separation process are carried out simultaneously.
7. a cooling agent regenerating unit, is characterized in that, can make the cooling agent recycling used when cutting off crystal ingot with scroll saw, described cooling agent regenerating unit comprises:
One or more hollow-fibre membranes of hollow form; And
Supply unit, is supplied in the hollow bulb of each hollow-fibre membrane by described cooling agent, wherein,
The aperture of the film of described hollow-fibre membrane is less than 0.05 μm,
Described supply unit supplies described cooling agent in the mode making described cooling agent and flow in described each hollow bulb with laminar condition.
8. cooling agent regenerating unit according to claim 7, characterized by further comprising:
Treatment trough, stores the cooling agent used when cutting off described crystal ingot;
Foldback portion, the described cooling agent be concentrated by the hollow bulb by described each hollow-fibre membrane is returned to described treatment trough; And
Centrifugal separating device, carries out centrifugation to the cooling agent in described treatment trough, and the cooling agent after centrifugation is returned to described treatment trough, wherein,
The cooling agent being stored in described treatment trough is supplied in the hollow bulb of described each hollow-fibre membrane by described supply unit.
CN201280077378.0A 2012-11-28 2012-11-28 Cooling agent renovation process and cooling agent regenerating unit Expired - Fee Related CN104812532B (en)

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