CN101500754A - Method of recovering abrasive from abrasive slurry waste liquid and apparatus therefor - Google Patents
Method of recovering abrasive from abrasive slurry waste liquid and apparatus therefor Download PDFInfo
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- CN101500754A CN101500754A CNA2007800300911A CN200780030091A CN101500754A CN 101500754 A CN101500754 A CN 101500754A CN A2007800300911 A CNA2007800300911 A CN A2007800300911A CN 200780030091 A CN200780030091 A CN 200780030091A CN 101500754 A CN101500754 A CN 101500754A
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- abrasive slurry
- grinding agent
- waste liquid
- dispersion
- particle diameter
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- 239000007788 liquid Substances 0.000 title claims abstract description 130
- 239000002002 slurry Substances 0.000 title claims abstract description 90
- 239000002699 waste material Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 103
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 238000011084 recovery Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims description 107
- 239000002245 particle Substances 0.000 claims description 97
- 239000003795 chemical substances by application Substances 0.000 claims description 90
- 238000001914 filtration Methods 0.000 claims description 36
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 20
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 20
- 239000007859 condensation product Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 230000004888 barrier function Effects 0.000 abstract 2
- 238000005498 polishing Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 32
- 239000000377 silicon dioxide Substances 0.000 description 16
- 239000000758 substrate Substances 0.000 description 16
- 239000011521 glass Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000004087 circulation Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000006063 cullet Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 208000037805 labour Diseases 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Images
Classifications
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- 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/66—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/06—Jet mills
-
- 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
- B24B37/00—Lapping machines or devices; Accessories
-
- 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
- B24B55/00—Safety devices for grinding or polishing machines; Accessories fitted to grinding or polishing machines for keeping tools or parts of the machine in good working condition
- B24B55/02—Equipment for cooling the grinding surfaces, e.g. devices for feeding coolant
- B24B55/03—Equipment for cooling the grinding surfaces, e.g. devices for feeding coolant designed as a complete equipment for feeding or clarifying coolant
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Food Science & Technology (AREA)
- Grinding-Machine Dressing And Accessory Apparatuses (AREA)
- Treatment Of Sludge (AREA)
- Disintegrating Or Milling (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
Abstract
Not only small-diameter foreign matter but also large-diameter foreign matter mixed in polishing is effectively removed from an abrasive slurry waste liquid to thereby attain recovery of abrasive. Recovery of abrasive from an abrasive slurry waste liquid is accomplished by the use of a recovery apparatus comprising a high pressure jet disperser machine capable of mutual collision of abrasive slurry waste liquids as high pressure jet streams in a dispersion vessel; an ultrasonic strainer capable of, while applying ultrasonic waves to the dispersion liquid obtained by dispersion by means of the high pressure jet disperser machine and/or a barrier filter, straining the dispersion liquid through the barrier filter; and a cyclone capable of classifying of the filtrate liquid obtained by straining by means of the ultrasonic strainer.
Description
Technical field
The present invention relates to from the abrasive slurry waste liquid to reclaim the method and the device of grinding agent, particularly the recovery method and the device of recovery cerium oxide from uses the abrasive slurry waste liquid when as the abrasive slurry of grinding agent glass substrate being ground with cerium oxide.
Background technology
In LCD (LCD), plasma scope (PD), inorganic and display of organic electroluminescence, the field-emitter display flat-panel monitors such as (FED), the glass substrate that uses various compositions requires very high surface quality as glass substrate.Therefore, use abrasive slurry that glass substrate is carried out mirror ultrafinish, as grinding agent, although preferably use hardness to be lower than the cerium oxide that glass substrate can carry out mirror ultrafinish.
Abrasive slurry is not only ground the function deterioration in the process of using repeatedly, become and can't use, and the meetings such as lapping rejects of sneaking into because of grinding cause damage to glass substrate.Therefore, having used abrasive slurry for several times to be used as trade waste usually discards.
But,, do not wish the abrasive slurry waste liquid discarded from the angle of utilizing again of resource, particularly the resource of cerium oxide is less, worry can't stably to supply in the future, and cerium oxide and alumina abrasive etc. to compare price very high, therefore wish it is utilized again.
Reach the technology of utilizing again as the recovery that relates to grinding agents such as cerium oxide, patent documentation 1～3 is for example arranged.
Patent documentation 1 is following technology: the centrifugal separator with the first step is handled the draining of discharging in the glass grinding, with moisture from and form the cerium oxide concentrate, centrifugal separator with second step is handled this cerium oxide concentrate, reclaims cerium oxide by this.Patent documentation 2 is following technology: add hydrochloric acid and hydrogen peroxide and heating in the grinding agent after using, reclaim grinding agent by this from the gained waste liquid.Patent documentation 3 is following technology: the abrasive slurry waste liquid is added filter, remove coarse impurities, the aperture is arranged is that the ultrafilter of the UF (milipore filter) of 2～100nm filters to apparatus then, reclaims grinding agent by this.
Patent documentation 1: the Japan Patent spy opens the 2004-306210 communique
Patent documentation 2: the Japan Patent spy opens the 2003-211356 communique
Patent documentation 3: Japanese patent laid-open 10-118899 communique
The announcement of invention
Yet silica and lapping rejects (iron powder of cullet and supplying tubing etc.) that the grinding agent in the abrasive slurry waste liquid produces when grinding mix and inter coagulation mutually, exist with the form of condensation product with viscosity.Therefore, if only as described in patent documentation 1, carry out the centrifugation processing, though then separable water can't separate silica and lapping rejects with good precision, so there is the remaining shortcoming that a large amount of silica and lapping rejects are arranged in the grinding agent that is reclaimed.In addition, exist hydrochloric acid and hydrogen peroxide to pollute the dangerous higher of grinding agent that (remaining in) reclaimed, pollutant just be reclaimed repeatedly the shortcoming of water cleaning as the recovery method of the chemistry of use hydrochloric acid as described in the patent documentation 2 and hydrogen peroxide.In addition, even carry out filtration treatment as minute multistep as described in the patent documentation 3, grinding agent in the abrasive slurry waste liquid also can be as mentioned above exists with the form of the condensation product with viscosity, therefore exists filter that the shortcoming that mesh stops up, can't use as actual device can take place at short notice.For example, though the particle diameter of cerium oxide is about 0.5～5 μ m, promptly using the aperture is that the filter of 50 μ m filters, and mesh also can take place at short notice stop up.Therefore, the maintenance of carrying out for the mesh of eliminating filter stops up will expend a large amount of time and labors.
The present invention is In view of the foregoing and the invention of doing, its objective is provides a kind of method and device that reclaims grinding agent from the abrasive slurry waste liquid, this method and device can be removed the small particle diameter foreign matter and the big particle diameter foreign matter of sneaking into because of grinding with the high rate of removing efficiently from the abrasive slurry waste liquid, thereby the recovery grinding agent, and the maintenance of retracting device is easy.
For reaching above-mentioned purpose, the invention provides a kind of method that from the abrasive slurry waste liquid, reclaims grinding agent, this method is the recovery method of recovery grinding agent from the abrasive slurry waste liquid that contains the condensation product that is formed greater than the big particle diameter foreign matter cohesion of the particle diameter of this grinding agent less than the small particle diameter foreign matter of the particle diameter of this grinding agent and particle diameter by grinding agent, particle diameter, the method is characterized in that, comprise dispersion step, filter operation and classification operation; In described dispersion step, carry out the mechanical dispersion treatment of described abrasive slurry waste liquid; In described filtration operation, the dispersion liquid after the described dispersion treatment is carried out filtration treatment, from described dispersion liquid, remove described big particle diameter foreign matter; In described classification operation, carry out classification with the filtrate of cyclone separator (cyclone) after and handle, described grinding agent in this filtrate and the classification of described small particle diameter foreign matter to described filtration treatment.
According to the present invention, in dispersion step, carry out mechanical dispersion treatment, the grinding agent, small particle diameter foreign matter and the big particle diameter foreign matter that constitute the condensation product in the abrasive slurry waste liquid are disperseed separately.Here, " grinding agent, small particle diameter foreign matter and the big particle diameter foreign matter that constitute condensation product are disperseed " to be meant for condensation product being disintegrated and resolving into grinding agent, small particle diameter foreign matter and big particle diameter foreign matter and carry out dispersion treatment, be not meant fully condensation product to be dispersed into grinding agent, small particle diameter foreign matter and big particle diameter foreign matter.By this dispersion liquid being carried out filtration treatment, can from the abrasive slurry waste liquid, remove big particle diameter foreign matter effectively, and can prevent for a long time that the mesh of filter from stopping up with filter.Here, " removing big particle diameter foreign matter by filtration treatment " is meant in order to remove big particle diameter foreign matter and carries out filtration treatment, be not meant and can fully remove big particle diameter foreign matter.At last, filtrate is carried out classification handle, with grinding agent and the classification of small particle diameter foreign matter.At this moment, through dispersion step and filtration operation, can be effectively with grinding agent classification from the small particle diameter foreign matter.Here, " handling grinding agent and the classification of small particle diameter foreign matter by classification " is meant that not being meant can be fully with the classification of small particle diameter foreign matter for grinding agent and the classification of small particle diameter foreign matter are carried out the cyclonic separation processing.
By this, can be efficiently from the abrasive slurry waste liquid that contains the condensation product that forms greater than the big particle diameter foreign matter cohesion of the particle diameter of this grinding agent less than the small particle diameter foreign matter of the particle diameter of this grinding agent and particle diameter by grinding agent, particle diameter, remove these foreign matters etc. with the high rate of removing, thereby recovery grinding agent, and the mesh that can suppress the filter in the filtration treatment stops up, so the maintenance times of device reduces, and maintenance becomes easy.In addition, because do not use chemical treatment fully, so there is not chemical substance to remain in danger in the grinding agent that is reclaimed as pollutant yet.
Preferred implementation of the present invention is characterised in that described grinding agent is that particle diameter is the cerium oxide of 0.5～5 μ m.
Use under the situation of cerium oxide as grinding agent of high price, recycling extremely helps to reduce cost, and in addition, the resource of cerium oxide is less, worries can't stably supply in the future, so the present invention is effective especially.
Preferred implementation of the present invention is characterised in that described dispersion step is to make the high pressure jet stream of described abrasive slurry waste liquid formation more than two strands, and the high pressure collision that described high pressure jet stream is collided is mutually handled.
Method as mechanical dispersion treatment, various process for dispersing such as pearl mill (beads mill) method are arranged, but dispersion for the condensation product that forms by grinding agent, small particle diameter foreign matter and the cohesion of big particle diameter foreign matter, effectively make the high pressure jet stream of abrasive slurry waste liquid formation more than two strands especially, and the high pressure collision that this high pressure jet stream is collided is mutually handled.
In addition, preferred implementation of the present invention is characterised in that, in described filtration operation, when filtering described dispersion liquid with filter, described dispersion liquid and/or filter is applied ultrasonic wave, carries out ultrasonic wave and handles.
By hyperacousticly filtering simultaneously in that the dispersion liquid that filtered and/or filter are applied as mentioned above, can improve filter efficiency.That is,, can prevent that dispersed grinding agent, small particle diameter foreign matter and big particle diameter foreign matter condense once more in dispersion step by dispersion liquid is applied ultrasonic wave.In addition, by filter is applied ultrasonic wave, can make filter be difficult to take place mesh and stop up.Therefore, special good is that dispersion liquid and filter are applied ultrasonic wave.
Preferred implementation of the present invention is characterised in that, in described filtration operation, implements intermittently with backwash water the backwash that filter carries out backwash to be handled.
With backwash water the backwash that filter carries out backwash is handled by carrying out as mentioned above intermittently, can further be made filter be difficult to take place mesh and stop up.
For reaching above-mentioned purpose, the present invention also provides a kind of device that reclaims grinding agent from the abrasive slurry waste liquid, and this device is characterised in that, comprises high pressure jet stream dispersion machine, ultrasonic wave filter and cyclone separator; Described high pressure jet stream dispersion machine makes the high pressure jet stream of described abrasive slurry waste liquid formation more than two strands, and makes the collision mutually in dispersion cup of described high pressure jet stream; Described ultrasonic wave filter hyperacousticly filters this dispersion liquid with described filter simultaneously in that the dispersion liquid after disperseing with described high pressure jet stream dispersion machine and/or filter are applied; Described cyclone separator is handled carry out classification with the particle in the described ultrasonic wave filter filtrate filtered.
Utilize above-mentioned grinding agent retracting device, can handle the abrasive slurry waste liquid with high pressure jet stream dispersion machine, ultrasonic wave filter, cyclone separator successively, so can from the abrasive slurry waste liquid, remove foreign matter etc. with the high rate of removing efficiently, thereby reclaim grinding agent.
The present invention handles by the abrasive slurry waste liquid of sneaking into foreign matter etc. because of grinding is carried out dispersion treatment, filtration treatment and classification, can remove foreign matter etc. with the high rate of removing from the abrasive slurry waste liquid efficiently, thereby reclaims grinding agent.
The simple declaration of accompanying drawing
Fig. 1 is the overall structure figure that reclaims the device of grinding agent from the abrasive slurry waste liquid of the present invention.
Fig. 2 is the key diagram that the particle diameter of the grinding agent that contains in the abrasive slurry waste liquid, small particle diameter foreign matter and big particle diameter foreign matter distributes.
Fig. 3 is the key diagram of explanation high pressure jet stream dispersion machine.
Fig. 4 is the respectively key diagram of the effect of processing that explanation is carried out with high pressure jet stream dispersion machine, ultrasonic wave filter, cyclone separator.
Fig. 5 is the key diagram of the dispersion effect of explanation high pressure jet stream dispersion machine.
Fig. 6 is that explanation is carried out the effect of Combination key diagram with high pressure jet stream dispersion machine and ultrasonic wave filter.
Fig. 7 is that explanation is carried out the effect of Combination key diagram with high pressure jet stream dispersion machine, ultrasonic wave filter and cyclone separator.
Symbol description
10 ... from the abrasive slurry waste liquid, reclaim the device of grinding agent, 12 ... grinder, 14 ... glass substrate, 16 ... turntable, 18 ... nozzle, 20 ... grinding tool, 22 ... grinding pad, 24 ... the abrasive slurry waste liquid, 26 ... the waste liquid bucket, 28 ... the waste liquid pipe arrangement, 30 ... the high pressure jet stream dispersion machine, 32 ... the ultrasonic wave filter, 34 ... cyclone separator, 36 ... waste liquid tank, 38 ... supplying tubing, 40 ... dispersion cup, 42 ... jet nozzle, 44 ... discharge pipe, 46 ... high-pressure pump, 48 ... dispersion liquid, 50 ... filter with jar, 52 ... triple valve, 54 ... valve, 56 ... supplying tubing, 58 ... filter and use pump, 60 ... filtering container, 62 ... filter, 64 ... ultrasonic oscillator, 66 ... valve, 68 ... return pipe arrangement, 70 ... filtrate, 72 ... the cyclone separator jar, 74 ... the filtrate pipe arrangement, 76 ... first valve, 78 ... second valve, 80 ... the backwash pump, 82 ... washwater tank, 84 ... supplying tubing, 86 ... the cyclone separator pump, 88 ... cyclone separating tower, 90 ... the circulation pipe arrangement, 92 ... the abrasive slurry recycling can, 94 ... small particle diameter foreign matter recycling can, A ... grinding agent, B ... the small particle diameter foreign matter, C ... big particle diameter foreign matter, D ... condensation product
The best mode that carries out an invention
Below, from the abrasive slurry waste liquid, reclaim the method for grinding agent and the preferred implementation of device describes according to accompanying drawing to of the present invention.
Fig. 1 is the overall structure figure that reclaims the device 10 of grinding agent from the abrasive slurry waste liquid of the present invention, be the example that reclaims grinding agent A from abrasive slurry waste liquid 24, this abrasive slurry waste liquid 24 is the abrasive slurry waste liquids that utilize when cerium oxide ground as 12 pairs of glass substrates 14 of grinder of grinding agent.
As shown in Figure 1, grinder 12 is fixed in glass substrate 14 mountings turntable 16 and makes its rotation.Then, when supplying with the grinder slurry, press the grinding tool 20 of rotation from the top of turntable 16, utilize 22 pairs of glass substrates 14 of grinding pad to grind by nozzle 18.In addition, the structure as grinder 12 is not limited to said structure, can use various grinders.
Then, the abrasive slurry waste liquid 24 after the use of using in grinding is situated between and is transported to retracting device 10 with waste liquid bucket 26 by waste liquid pipe arrangement 28.Here, in the abrasive slurry waste liquid 24, the particle diameter that grinding agent A, the particle diameter that produces because of grinding produce less than the silicon dioxide granule of the particle diameter of grinding agent A (below be called " small particle diameter foreign matter B ") with because of grinding condenses greater than the cullet of the particle diameter of grinding agent A and the iron rust of grinding agent supplying tubing etc. (below be called " big particle diameter foreign matter C "), exists with the form of condensation product D with viscosity.
As shown in Figure 2, grinding agent A, small particle diameter foreign matter B and big particle diameter foreign matter C particle diameter separately are distributed as: roughly in the scope of 0.5～5 μ m, small particle diameter foreign matter B is roughly less than 0.5 μ m grinding agent A (cerium oxide), and big particle diameter foreign matter C is roughly greater than 5 μ m.Here, particle diameter is meant the maximum particle diameter of each particle.If under remaining situation about having, abrasive slurry is utilized again as the silicon dioxide granule of small particle diameter foreign matter B, then " passivation " can take place, nonferromagnetic substance descends.
In addition, if under remaining situation about having, abrasive slurry is utilized again, then when grinding, can cause damage to glass substrate 14 as the cullet of big particle diameter foreign matter C and iron rust etc.
As shown in Figure 1, retracting device 10 mainly is made of high pressure jet stream dispersion machine 30, ultrasonic wave filter 32 and cyclone separator 34, and these machines 30,32,34 are situated between and connect continuously with pipe arrangement and jar.Below, the recovery method (flow process of operation) that reclaims grinding agent A to the structure of retracting device 10 with from abrasive slurry waste liquid 24 describes.
Jie is transported to high pressure jet stream dispersion machine 30 by waste liquid tank 36 interior abrasive slurry waste liquids 24 Jie that waste liquid pipe arrangement 28 is stored in retracting device 10 to supply with pipe arrangement 38 with waste liquid bucket 26.High pressure jet stream dispersion machine 30 is that the long side direction both sides of dispersion cup 40 dispose a pair of jet nozzle 42,42 relatively at the closed container that forms withstand voltage tubular as shown in Figure 3.In addition, be connected with the discharge pipe 44 that the dispersion liquid after the dispersion treatment 48 is discharged in the central portion side of dispersion cup 40.On the other hand, as shown in Figure 1, supplying tubing 38 is provided with high-pressure pump 46, and supplying tubing 38 is in the discharge side branch of high-pressure pump 46, is connected with above-mentioned a pair of jet nozzle 42,42.By this, in dispersion cup 40, abrasive slurry waste liquid 24 collides mutually with the form of high pressure jet stream, the energy that utilizes this collision to produce, and shown in Fig. 4 (A), the condensation product D in the abrasive slurry waste liquid 24 is disperseed.Preferred 50～the 100MPa of ejection pressure of the abrasive slurry waste liquid 24 of self-injection flow nozzle 42 ejections, the more preferably scope of 50～70MPa.Fig. 5 is the result who carries out abrasive slurry waste liquid 24 and carry out the settling test of the dispersion liquid 48 after the dispersion treatment with 30 pairs of abrasive slurry waste liquids of high pressure jet stream dispersion machine 24.Fig. 5 (A) is after the stirrer paddle with 360rpm stirs abrasive slurry waste liquid 24, and its developmental tube of packing into is left standstill situation after 15 minutes.Fig. 5 (B) is after similarly above-mentioned dispersion liquid 48 being stirred, and its developmental tube of packing into is left standstill situation after 15 minutes.Fig. 5 (C) is after similarly untapped abrasive slurry being stirred, and its developmental tube of packing into is left standstill situation after 15 minutes.By Fig. 5 (A) as can be known, the abrasive slurry waste liquid 24 that grinding agent A, small particle diameter foreign matter B and big particle diameter foreign matter C exist with the form of condensation product D with viscosity still serve as the troubled liquor after the stirring, and Separation of Solid and Liquid does not take place.On the other hand, shown in Fig. 5 (B), carry out dispersion liquid 48 after the dispersion treatment in the roughly center position generation Separation of Solid and Liquid of developmental tube with 30 pairs of abrasive slurry waste liquids of high pressure jet stream dispersion machine 24, approximate with the Separation of Solid and Liquid state of the untapped abrasive slurry shown in Fig. 5 (C).As mentioned above, grinding agent A, small particle diameter foreign matter B and big particle diameter foreign matter C become easily by Separation of Solid and Liquid, and this expression can disperse the condensation product D in the abrasive slurry waste liquid 24 effectively by the dispersion treatment of high pressure jet stream dispersion machine 30.
As dispersion machine, if mechanical dispersion machine, then except that the high pressure jet stream dispersion machine, can use ultrasonic dispersing machine, pearl mill dispersion machine etc., but special preferably to the high pressure jet stream dispersion machine 30 of dispersive property the best of condensation product D.
Carrying out dispersion liquid 48 after the dispersion treatment with high pressure jet stream dispersion machine 30 is transported to by discharge pipe 44 and filters with jars 50.At this moment, be arranged at the triple valve 52 of discharge pipe 44, dispersion liquid 48 is returned to waste liquid tank 36 (circuit shown in the dotted line) once more by switching, can be with abrasive slurry waste liquid more than 24 time by high pressure jet stream dispersion machine 30.Therefore, be preferably according to the complexity of the dispersion of condensation product D and set dispersion treatment number of times (number of pass times).In addition, when carrying out repeatedly dispersion treatment, be preferably under the state of valve 54 temporary closes that will be arranged at waste liquid pipe arrangement 28 and carry out.
Then, be transported to and filter with jars 50 dispersion liquid 48 as shown in Figure 1, being situated between is supplied to ultrasonic wave filter 32 by filtering with pump 58 to supply with pipe arrangement 56.In the ultrasonic wave filter 32, filtering container 60 is that the boundary is divided into 60A of filter chamber (the last chamber of Fig. 1) and the 60B of filtrate chamber (the following chamber of Fig. 1) with filter 62, and is provided with above the 60A of filter chamber to the hyperacoustic ultrasonic oscillator 64 of filter 62 vibrations.As hyperacoustic condition, export preferred 500～1000W, the more preferably scope of 500～800W, the preferred 15～25kHz of frequency, the more preferably scope of 17～22kHz.The sidewall of the 60A of filter chamber be connected with possess valve 66 return pipe arrangement 68, the dispersion liquid 48 that is supplied to the 60A of filter chamber is situated between and is circulated to and filters with jars 50 to return pipe arrangement 68.The bottom of the 60B of filtrate chamber is connected with and will be delivered to the filtrate pipe arrangement 74 of cyclone separator with jar 72 with filter 62 filtrate filtered 70, and is provided with first valve 76 in the way of pipe arrangement 74.Filtrate pipe arrangement 74 is in the upstream branch of first valve, and being situated between is connected with washwater tank 82 with pump 80 with second valve 78 and backwash.Store the rinse water that is used for cleaning filter 62 in the washwater tank 82.
When filtering, open, drive under second valve, 78 closing state and filter with pump 58 at first valve 76 with the 32 pairs of dispersion liquids 48 of ultrasonic wave filter that constitute as mentioned above.By this, be stored in to filter and be situated between with the 60A of filter chamber and return pipe arrangement 68 circulations, and, filter with 62 pairs of dispersion liquids 48 of filter being subjected to hyperacoustic while that ultrasonic oscillator 64 vibrates with jars 50 dispersion liquid 48.As the aperture of filter 62, use that grinding agent A in the dispersion liquid 48 and small particle diameter foreign matter B can can't pass through by, big particle diameter foreign matter C, for example the aperture about 10 μ m gets final product.By this, shown in Fig. 4 (B), accumulate among the 60B of filtrate chamber to have and removed big particle diameter foreign matter C, mix the filtrate 70 that grinding agent A and small particle diameter foreign matter B are arranged, this filtrate 70 is situated between and is transported to cyclone separator with jars 72 with filtrate pipe arrangement 74.In this filtration treatment,, can prevent to condense once more with high pressure jet stream dispersion machine 30 dispersed grinding agent A, small particle diameter foreign matter B and big particle diameter foreign matter C by to dispersion liquid 48 in the filtering container 60 and filter 62 vibration ultrasonic waves.In addition, because of ultrasonic wave causes filter 62 vibrations, the mesh that can suppress filter 62 stops up.
If continue to carry out filtration treatment for a long time, then filter pressure can rise, so be preferably the backwash of carrying out filter 62.Backwash is to drive backwash pump 80 under the state that filtration stops with pump 58, first valve 76 cuts out, second valve 78 is opened.By this, the rinse water that is stored in washwater tank 82 is passed through filter 62 along the direction opposite with filtration treatment, filter 62 is carried out backwash, so can reduce filter pressure.
Fig. 6 carries out after the dispersion treatment carrying out the present invention of filtration treatment and directly with the ultrasonic wave filter abrasive slurry waste liquid 24 being carried out the comparison diagram of strainability of the comparative example of filtration treatment with ultrasonic wave filter 32 with 30 pairs of abrasive slurry waste liquids of high pressure jet stream dispersion machine 24.The aperture of employed filter 62 is set at the 10 μ ms bigger slightly than the upper limit 5 μ m of the particle diameter of cerium oxide.
As shown in Figure 6, the filtering traffic among the present invention is reduced to about about 800 (mL/ branches) through about 1500 (the mL/ branches) when just beginning to filter after 60 minutes, is stabilized in about 800 (mL/ branches) afterwards.On the other hand, the filtering traffic in the comparative example is exactly the low discharge of about 100 (mL/ branches) when just beginning to filter, and also is about 100 (mL/ branches) afterwards always.By this result as can be known, in advance with 30 pairs of abrasive slurry waste liquids of high pressure jet stream dispersion machine 24 carry out dispersion treatment, the filtering traffic of the present invention of filtering with ultrasonic wave filter 32 then is the comparative example that just filters without dispersion treatment about 8 times.
As shown in Figure 1, after filtration treatment, be transported to cyclone separator is supplied to three liquid divergence types with pump 86 by cyclone separator with supply pipe arrangement 84 with filtrate 70 Jie of jar 72 cyclone separator 34.Then, the filtrate 70 that is supplied to the top of cyclone separating tower 88 becomes circulation because of cyclone separator with the discharge pressure (0.6MPa) of pump 86, flows in cyclone separating tower 88.Because this circulation, filtrate 70 is subjected to centrifugal force, and the grinding agent A that proportion is heavier concentrates on the internal perisporium side of cyclone separating tower 88 and descends simultaneously, and on the other hand, the small particle diameter foreign matter B that proportion is lighter concentrates on the central portion of cyclone separating tower 88 and rises simultaneously.Therefore, shown in Fig. 4 (C), discharge the high specific gravity liquid that contains grinding agent A, discharge the low-gravity liquid that contains small particle diameter foreign matter B from the top from the bottom of cyclone separating tower 88.
In addition, the middle proportion liquid that grinding agent A and small particle diameter foreign matter B mix mutually is situated between and is back to cyclone separator with jar 72 with circulation pipe arrangement 90, carries out classification repeatedly with cyclone separator and handles.Then, high specific gravity liquid is stored in abrasive slurry recycling can 92, utilizes as abrasive slurry again.In addition, low-gravity liquid is stored in small particle diameter foreign matter jar 94.By this, can from abrasive slurry waste liquid 24, reclaim grinding agent A with the high foreign matter rate of removing efficiently.
Fig. 7 will carry out the filtrate 70 of abrasive slurry waste liquid 24 after through high pressure jet stream dispersion machines 30, ultrasonic wave filter 32 with 34 pairs in cyclone separator the present invention of classification, the direct comparative example 1 that carries out classification with 34 pairs of abrasive slurry waste liquids of cyclone separator 24, only compare with the comparative example 2 that cyclone separator 34 carries out classification, study the result of its classification performance through ultrasonic wave filter 32 backs.The dioxide-containing silica that the research of classification performance is stored in the liquid of abrasive slurry recycling can 92 by inquiry carries out.Here, the dioxide-containing silica that contains in the abrasive slurry waste liquid 24 is 195mg/L, and the dioxide-containing silica in the untapped abrasive slurry is about 60mg/L.Therefore, the silica of the 135mg/L in the abrasive slurry waste liquid 24 is the silica that the grinding because of glass substrate 14 produces.
As shown in Figure 7, the dioxide-containing silica in the comparative example 1 is 195mg/L, fails to carry out the classification of grinding agent A and small particle diameter foreign matter (silica) B fully.In addition, in the comparative example 2, can remove small particle diameter foreign matter (silica) B of 20mg/L.Relative therewith, among the present invention, can remove small particle diameter foreign matter (silica) B of 98mg/L.As a result, remaining silica is 97mg/L, and is close with the dioxide-containing silica of untapped abrasive slurry.
As mentioned above, will from grinding agent A, particle diameter greater than the big particle diameter foreign matter C of the particle diameter of this grinding agent A cohesion takes place less than the small particle diameter foreign matter B of the particle diameter of this grinding agent A and particle diameter and the abrasive slurry waste liquid 24 that exists with the form of condensation product D reclaim grinding agent A, importantly each that use high pressure jet stream dispersion machine 30, ultrasonic wave filter 32 and cyclone separator 34 with said sequence handled.
In addition, in the embodiments of the present invention, to reclaim grinding agent A from utilize the abrasive slurry waste liquid 24 when cerium oxide ground glass substrate 14 as the grinder of grinding agent A is that example describes, but the present invention also can be used for using the situation of other grinding agent, or is used for the grinding agent that the grinding of grinding object, for example semiconductor substrate etc. beyond the glass substrate is used.
The possibility of utilizing on the industry
The present invention is specially adapted to from using with cerium oxide to the abrasive slurry of grinding agent glass substrate Reclaim cerium oxide in the abrasive slurry waste liquid when grinding.
In addition, here quote the Japanese patent application 2006 of filing an application on August 16th, 2006-All the elements of No. 222000 specification, claims, accompanying drawing and summary illustrate as the present invention The announcement of book.
Claims (8)
1. method that from the abrasive slurry waste liquid, reclaims grinding agent, this method is the recovery method of recovery grinding agent from the abrasive slurry waste liquid that contains the condensation product that is formed greater than the big particle diameter foreign matter cohesion of the particle diameter of this grinding agent less than the small particle diameter foreign matter of the particle diameter of this grinding agent and particle diameter by grinding agent, particle diameter, it is characterized in that, comprise dispersion step, filter operation and classification operation;
In described dispersion step, carry out the mechanical dispersion treatment of described abrasive slurry waste liquid;
In described filtration operation, the dispersion liquid after the described dispersion treatment is carried out filtration treatment, from described dispersion liquid, remove described big particle diameter foreign matter;
In described classification operation, carry out classification with the filtrate of cyclone separator after and handle, described grinding agent in this filtrate and the classification of described small particle diameter foreign matter to described filtration treatment.
2. the method that reclaims grinding agent from the abrasive slurry waste liquid as claimed in claim 1 is characterized in that described grinding agent is that particle diameter is the cerium oxide of 0.5～5 μ m.
3. the method that from the abrasive slurry waste liquid, reclaims grinding agent as claimed in claim 1 or 2, it is characterized in that, described dispersion step is to make the high pressure jet stream of described abrasive slurry waste liquid formation more than two strands, and the high pressure collision that described high pressure jet stream is collided is mutually handled.
4. as each described method that from the abrasive slurry waste liquid, reclaims grinding agent in the claim 1～3, it is characterized in that, in described filtration operation, when filtering described dispersion liquid with filter, described dispersion liquid and/or filter are applied ultrasonic wave, carry out ultrasonic wave and handle.
5. the method that reclaims grinding agent from the abrasive slurry waste liquid as claimed in claim 4 is characterized in that, in described filtration operation, implements intermittently with backwash water the backwash that described filter carries out backwash to be handled.
6. as each described method that from the abrasive slurry waste liquid, reclaims grinding agent in the claim 1～5, it is characterized in that in described dispersion step, repeated multiple times is carried out the dispersion treatment of abrasive slurry waste liquid.
7. as each described method that from the abrasive slurry waste liquid, reclaims grinding agent in the claim 1～5, it is characterized in that, in described classification operation, the middle proportion liquid that grinding agent and small particle diameter foreign matter are mixed mutually takes out from cyclone separator, carries out classification repeatedly and handles.
8. a device that reclaims grinding agent from the abrasive slurry waste liquid is characterized in that, comprises high pressure jet stream dispersion machine, ultrasonic wave filter and cyclone separator;
Described high pressure jet stream dispersion machine makes the high pressure jet stream of described abrasive slurry waste liquid formation more than two strands, and makes the collision mutually in dispersion cup of described high pressure jet stream;
Described ultrasonic wave filter hyperacousticly filters this dispersion liquid with described filter simultaneously in that the dispersion liquid after disperseing with described high pressure jet stream dispersion machine and/or filter are applied;
Described cyclone separator is handled carry out classification with the particle in the described ultrasonic wave filter filtrate filtered.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006222000 | 2006-08-16 | ||
| JP222000/2006 | 2006-08-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101500754A true CN101500754A (en) | 2009-08-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007800300911A Pending CN101500754A (en) | 2006-08-16 | 2007-06-14 | Method of recovering abrasive from abrasive slurry waste liquid and apparatus therefor |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JPWO2008020507A1 (en) |
| KR (1) | KR20090009266A (en) |
| CN (1) | CN101500754A (en) |
| TW (1) | TW200810880A (en) |
| WO (1) | WO2008020507A1 (en) |
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| KR100310234B1 (en) * | 1999-08-20 | 2001-11-14 | 안복현 | Preparation method of metal oxide slurry for cmp of semiconductor |
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- 2007-06-14 WO PCT/JP2007/062046 patent/WO2008020507A1/en active Application Filing
- 2007-06-14 CN CNA2007800300911A patent/CN101500754A/en active Pending
- 2007-06-14 JP JP2008529824A patent/JPWO2008020507A1/en not_active Withdrawn
- 2007-06-14 KR KR1020087028925A patent/KR20090009266A/en active Search and Examination
- 2007-06-26 TW TW096123063A patent/TW200810880A/en unknown
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Also Published As
| Publication number | Publication date |
|---|---|
| TW200810880A (en) | 2008-03-01 |
| KR20090009266A (en) | 2009-01-22 |
| JPWO2008020507A1 (en) | 2010-01-07 |
| WO2008020507A1 (en) | 2008-02-21 |
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