[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN102428042A - Method for purifying waste silicon slurry - Google Patents

Method for purifying waste silicon slurry Download PDF

Info

Publication number
CN102428042A
CN102428042A CN2009801591307A CN200980159130A CN102428042A CN 102428042 A CN102428042 A CN 102428042A CN 2009801591307 A CN2009801591307 A CN 2009801591307A CN 200980159130 A CN200980159130 A CN 200980159130A CN 102428042 A CN102428042 A CN 102428042A
Authority
CN
China
Prior art keywords
slurries
abrasive
water
separating machine
useless silicon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2009801591307A
Other languages
Chinese (zh)
Inventor
许明洙
李相坤
许仁郎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
RECYCLE SYSTEM Corp
Original Assignee
RECYCLE SYSTEM Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by RECYCLE SYSTEM Corp filed Critical RECYCLE SYSTEM Corp
Publication of CN102428042A publication Critical patent/CN102428042A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/037Purification
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/20Sludge processing
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The present invention relates to a method for purifying waste silicon slurry, comprising: separating solids and cutting oil included in waste silicon slurry; mixing the separated solids with water; and separating abrasives and wastewater from the slurry having solids mixed with water, and processing the separated abrasives into a purified abrasive powder.

Description

Useless silicon slurries process for extracting
Technical field
The present invention relates to useless silicon slurries process for extracting; Say so more in detail and relate in a kind of useless silicon slurries that from the semiconductor wafer manufacturing engineering, produce abrasive and the machining oil that Separation and Recovery respectively refined and utilize the useless silicon slurries process for extracting that further all waste water that produce in the useless silicon slurries extractive process is refined and utilize again.
Background technology
Recently,,, utilize the industry of solar thermal energy to receive extensive concern, the demand of silicon wafer is presented the trend of rapid increase in order to tackle the petroleum-based energy exhaustion and to prevent the global warming phenomenon along with the development of information communication and semiconductor industry.
In general, silicon wafer is through supplying with machining oil and abrasive and being made by scroll saw (wire saw) cutting to silicon ingot (silicon ingot).In addition; The silicon wafer that is cut is mixed with in being pasted with machining oil and abrasive under the state of the useless silicon slurries that cut powder (saw dust); Manufacture the silicon for solar cell wafer through cleaning process, or manufacturing semi-conductor through grinding, etching and cleaning engineering etc. uses silicon wafer.
Current; The machining oil that uses when semi-conductor is made with silicon wafer is made up of the material of blended wax system oil (80~90%), water, tensio-active agent, dispersion agent, viscosity modifier etc.; This machining oil plays between the cotton rope and silicon ingot (silicon ingot) that makes abrasive evenly enter into scroll saw (wire saw), and the effect of the heat of friction that is produced by cotton rope traction fast in the cooling working angles.
The silicon for solar cell wafer is about 180~250 μ m, is cut to become to be equivalent to about 1/3 the film of semi-conductor with silicon wafer, therefore can't use the machining oil that comprises a large amount of paraffin series oil.Replace, use the machining oil comprise 80~90% water miscible glycol ether (DEG), polyoxyethylene glycol (PEG), polyethers (PPG) etc.In order to reduce 5~30 μ m size abrasive and the sedimentation of cutting powder, continue use and comprise 80~90% water miscible glycol ether (DEG), polyoxyethylene glycol (PEG), polyethers machining oils such as (PPG).
In this silicon wafer manufacturing processed, the useless silicon slurries that silicon that comes off from silicon ingot (silicon ingot) and the powder that comes off from scroll saw (Wire Saw) and abrasive and machining oil mix will be classified as the particular surroundings waste and handle.
In general, useless silicon slurries have high viscosity, are difficult to separate through simple physical operations, and it is classified as special waste and all burns or bury processing.This treatment process has the one side of high cost in processing costs, particularly, this treatment facility is classified as and detests environmental facility recently, has facility and keeps somewhere the very problem of difficulty.And, if burn or bury, have to some extent expellant gas or leach the problem that water seriously pollutes surrounding environment.
Particularly; The machining oil that comprises 80~90% water miscible glycol ether, polyoxyethylene glycol (PEG) or polyethers (PPG) etc. that uses in the manufacturing of silicon for solar cell wafer is water-soluble; Its again utilization ratio be 40~50%, have a large amount of wastes and the problem of waste water of producing.
In addition, density is that the size of 2.3 silicon cutting powder in working angles is about 0.1 μ m, and its apparent density reduces; If but contain under the cutting oil condition; Because abrasive and cutting powder be by cohesion and the phenomenon of co-precipitation, it is more that the cutting powder that material contains is ground in regeneration, and existence can only obtain the problem of low-purity; Because the iron content that produces in the process of lapping is more; Need append nitric acid, hydrofluoric acid cleaning process, in this process, have the problem of the fluoric acid waste water that produces a large amount of regeneration and can't utilize again.
Summary of the invention
The present invention proposes under aforesaid background, the object of the present invention is to provide a kind of useless silicon slurries process for extracting, in the useless silicon slurries that from the semi-conductor manufacturing engineering, produce, and the abrasive that refined of Separation and Recovery and machining oil and utilize again respectively.
Another object of the present invention is to provide a kind of useless silicon slurries process for extracting, all waste water that produce in the useless silicon slurries extractive process are cleaned and utilization again.
In order to achieve the above object, the useless silicon slurries process for extracting according to a form of the present invention comprises: the solid substance that comprises in the useless silicon slurries of separation and the step of machining oil; With isolated solid substance and water blended step; From solid substance and water blended slurries, separate abrasive and waste water, isolated abrasive is manufactured the step of the abrasive powder of being refined.
Useless silicon slurries process for extracting according to additional form of the present invention comprises: the part that will remove in the useless silicon slurries of magnetic force composition impurity is rendered to first separating machine, in first separating machine, separates the step of first solid substance and first machining oil; With isolated first machining oil and untapped remaining useless silicon slurries blended step; Blended first machining oil and useless silicon slurries are rendered to second separating machine, in second separating machine, separate the step of second solid substance and second machining oil.
Useless silicon slurries process for extracting according to another additional form of the present invention comprises: solid substance and water blended slurries are rendered to the 3rd separating machine, in the 3rd separating machine, separate the step of abrasive and waste water; With isolated abrasive and water blended step; Apply vibrations to abrasive and water blended slurries, remove the cleaning step of the cutting powder that abrasive surface adheres to; To render to the 4th separating machine through the abrasive of cleaning step, separation steps by size in the 4th separating machine; Remove the step of the water that contains in the isolated abrasive; The dry step of removing the abrasive of water.
Useless silicon slurries process for extracting according to another additional form of the present invention comprises: with isolated machining oil and active carbon powder blended step; Blended machining oil and active carbon powder are rendered to the 5th separating machine, in the 5th separating machine, separate the step of machining oil; Evaporate the step of the water that contains in the isolated machining oil.
Useless silicon slurries process for extracting according to form of appending of the present invention also comprises: the step of mixed active carbon powder and precoat slurries in isolated waste water; Blended waste water and active carbon powder and precoat slurries are rendered to the 6th separating machine, in the 6th separating machine, separate the water that refined and the step of solid substance.
According to aforesaid formation, useless silicon slurries process for extracting of the present invention has the useful effect that can reclaim machining oil that is refined and the abrasive powder of being refined.
And useless silicon slurries process for extracting of the present invention can reclaim the machining oil raw material, and material is ground in the regeneration that can access the size that is suitable for cutting silicon ingot, has that the face of tool that prevents silicon wafer is twisted, a bending etc., prevents the useful effect that the silicon wafer quality reduces.
And, comprise the waste water refining step in the useless silicon slurries process for extracting of the present invention, have the waste water of minimizing output, reduce the chemical oxygen demand of waste water, reduce the useful effect of wastewater treatment load.
Description of drawings
Fig. 1 is the structure iron of expression according to the useless silicon slurries device for refining of one embodiment of the invention.
Fig. 2 is the embodiment of expression according to solid substance of the present invention and machining oil separated part 100.
Fig. 3 is the embodiment of expression according to abrasive refinement of the present invention and abrasive powder generation portion 200.
Fig. 4 is the embodiment of expression according to machining oil refinement of the present invention portion 300.
Fig. 5 is the embodiment of expression according to waste water refinement of the present invention portion 400.
Fig. 6 is the mechanical flow digram of expression according to the useless silicon slurries process for extracting of the useless silicon slurries device for refining of Fig. 1.
Fig. 7 is the mechanical flow digram of expression according to abrasive process for extracting of the present invention.
Fig. 8 is the mechanical flow digram of expression according to machining oil process for extracting of the present invention.
Fig. 9 is the mechanical flow digram of expression according to waste water process for extracting of the present invention.
Embodiment
Below, for those skilled in the art can understand and implement easily, the preferred embodiment of the form of appending with reference to accompanying drawing and record at length describes the present invention.
In this manual, useless silicon slurries are cutting powder, abrasive and the machining oil blended mixtures that come off from silicon ingot (silicon ingot) or scroll saw (Wire Saw).Solid substance is to comprise through the useless silicon slurries of magnetic force composition Impurity removal engineering to render to separating machine; The mixture that is full of cutting powder and abrasive that obtains through the engineering of separating machining oil in the separating machine, or separate the mixture of discharge in the waste water process recycling.
Fig. 1 is the structure iron of expression according to the useless silicon slurries device for refining of one embodiment of the invention; Fig. 2 is that expression is according to solid substance of the present invention and machining oil separated part 100; Fig. 3 is that expression is refined and abrasive powder generation portion 200 according to abrasive of the present invention; Fig. 4 be expression according to machining oil recoverer 310 of the present invention and machining oil base oil refinement portion 320, Fig. 5 is the embodiment of expression according to waste water refinement of the present invention portion 400.
At first; As shown in Figure 1, the useless silicon slurries device for refining in the present embodiment comprises that substantially solid substance and machining oil separated part 100, abrasive refine and abrasive powder generation portion 200, machining oil recoverer 310, machining oil base oil refinement portion 320 and waste water refinement portion 400.
Solid substance and machining oil separated part 100
Solid substance is from useless silicon slurries, to separate the device of solid substance and machining oil with machining oil separated part 100.As shown in Figure 2; In one embodiment of this invention, solid substance and machining oil separated part 100 comprise that first stirrer 111, magnetic force composition Impurity removal are with filter 112, heated and stirred case 113, first separating machine 114, machining oil safe deposit box 115, second stirrer 116 and second separating machine 117.
When first stirrer 111 gives up the silicon slurries in input, it is stirred more than 30 minutes fully, make by sedimentary solid substance and mix equably.The useless silicon slurries that obtain stirring in first stirrer 111 send magnetic force composition Impurity removal to filter 112 by taking out the pump (not shown).In order to reduce the viscosity of useless silicon slurries, in the process of magnetic force composition Impurity removal with filter 112 handovers, utilize preheating heat X (not shown) will give up the preheating of silicon slurries for example more than 30 ℃, below 50 ℃.
The silico briquette that magnetic force composition Impurity removal together condenses with filter 112 removals and iron powder.Magnetic force composition Impurity removal is configured in inside electro-magnet or PM are installed with filter 112, discharges iron powder through control current or discrete magnets.In order to discharge iron powder preferably, magnetic force composition Impurity removal be with can installing stirrer in the filter 112, or uses the iron powder of the magnet surface of absorption rotation, blade is installed discharged the iron powder that is cut and also continue filtering multiple device.
The useless silicon slurries heating that heated and stirred case 113 will be removed magnetic force composition impurity is more than 30 ℃, below 50 ℃ and stir, and the viscosity that reduces useless silicon slurries also prevents its deposition.Heated and stirred case 113 is configured to install level switch or level controller, useless silicon slurries overflow or the situation of empty van under, prevent to take out pump startup.Heated and stirred case 113 is heated by multiple thermals source such as steam, electric current, warm water; Mounting temperature sensor and temperature control valve use with the steam trap (steam trap) that is used for removing swimmingly water of condensation respectively, or temperature control (Control) valve and a steam trap use are installed.
In order to reduce in the heated and stirred case 113 time of heating, from magnetic force composition Impurity removal with filter 112 to the process of heated and stirred case 113 handovers, utilize the heat exchanger (not shown) preheating silicon slurries that give up.Through supplying with thermal source to heat exchanger and heated and stirred case 113, the silicon slurries that will give up heat more than 30 ℃, below 50 ℃, to reduce the viscosity of useless silicon slurries.
Throw in the part of the useless silicon slurries of the removal magnetic force composition impurity that stores in the heated and stirred case 113 in first separating machine 114, be separated into first solid substance and first machining oil.First separating machine 114 is configured to be made up of pressure filter or separating centrifuge.As an example, separating centrifuge is to remove that 1 μ m is above, size below the 10mm, and the concentration of handling solid substance occupies the separating centrifuge of the useless silicon slurries of 1~50 (%).In this separating centrifuge, screw rod low speed rotates, and discharges the solid substance that is moved to wall by cf-, and the cutting powder of cf-less effect relatively and machining oil overflow after being stacked in the separating machine.For according to the temperature of useless silicon slurries, concentration, viscosity and change speed is installed motor and phase inverter and unit (controller) use at rotor and screw rod respectively in the separating centrifuge.
115 keepings of machining oil safe deposit box are from first separating machine, 114 isolating first machining oils.All the other parts of the useless silicon slurries of the removal magnetic force composition impurity that stores in first machining oil of taking care of in the input machining oil safe deposit box 115 in second stirrer 116 and the heated and stirred case 113 stir and make the machining oil slurries.As an example, in order to reduce the viscosity of mixture, second stirrer 116 heats through multiple thermals source such as steam, electric current, warm water.And second stirrer 116 is configured to throw in the water of recycling.
Second separating machine 117 is thrown in the machining oil slurries from second stirrer 116, be separated into second solid substance and second machining oil.As an example, second separating machine 117 is configured to comprise precoat filter (precoat filter) and turbidometer and precoat slurries case.The precoat slurries for example are that the amount that is mixed into solid substance is filtration chamber's volumetrical of precoat filter (precoat filter) more than 30%, below 70%, and the concentration of machining oil is the slurries more than 30%, below 50%.Precoat filter (precoat filter) is made and supplied to these precoat slurries in precoat slurries case.Precoat filter (precoat filter) only is applied to the filter surface with the part of the macroparticle that comprises in the precoat slurries of supplying with, and little example is little by little blocked between the macroparticle and formed precoat.
Precoat filter (precoat filter) is when second stirrer 116 is supplied with the machining oil slurries with certain pressure, regular hour, subsequently from precoat slurries case with predefined pressure and time to precoat filter (precoat filter) supply precoat slurries.When carrying out this process for several times repeatedly, solid substance is residued in precoat filter (precoat filter), and machining oil is then passed through.As an example, also carry out the heat of compression air of the heat more than 50 ℃ is supplied with 10 minutes, the warm air pressurization engineering that residual machining oil is also discharged in the heating precoat filter (precoat filter).When this project finishes, separate solid substance from precoat filter (precoat filter).
Machining oil from precoat filter (precoat filter) is discharged when the result who is detected by turbidometer does not reach the turbidity of setting, will be sent to second stirrer 116 and circulation again.On the contrary, the machining oil that reaches the turbidity of setting will arrive machining oil safe deposit box (label 311 of Fig. 4) certainly.
Abrasive refines and abrasive powder generation portion 200
In Fig. 1, abrasive refines and abrasive powder generation portion 200 separates abrasive in isolating first, second solid substance by size from solid substance and machining oil separating machine 100, and the device of the manufacturing abrasive powder of being refined.As shown in Figure 3; In one embodiment of this invention, abrasive refine and abrasive powder generation portion 200 be configured to comprise first mixing machine 211, magnetic force composition Impurity removal with filter 212, the 3rd separating machine 213, second mixing machine 214, cleaning machine 215, the 4th separating machine 216, net formula filter 217 (screen filter), water extracter 218, drying machine 219 and handover portion 220.
First mixing machine 211 is that first and second separating machine 114,117 from solid substance and machining oil separated part 100 is separated and first, second solid substance of supplying with and the for example water more than 50 ℃, below 70 ℃ mix and make the device of aqueous slurry.First mixing machine 211 comprises stirrer and level detection sensor, and its ratio of mixture that is used in water and solid substance is mixed into more than 2: 1, melts the machining oil that contains in the solid substance.
Magnetic force composition Impurity removal makes to melt in first mixing machine 211 with filter 212 has the aqueous slurry of residual machining oil to pass through, and removes the foreign substances (for example, silicon) with the iron powder cohesion.Magnetic force composition Impurity removal is configured in inside electro-magnet or PM are installed with filter 212, discharges iron powder through control current or discrete magnets.In order to discharge iron powder preferably, magnetic force composition Impurity removal be with can installing stirrer in the filter 212, or can use the magnet surface mounting filtering net in rotation, discharges simultaneously with iron powder and the multiple device of continuous filtration.
The 3rd separating machine 213 separates abrasive from the aqueous slurry of removing magnetic force composition impurity, and separates and remove all the other foreign substances.As an example, the 3rd separating machine 213 is configured to 300~600rpm separating centrifuge, in separating centrifuge; Together discharge the cutting powder with water; Be sent to first mixing machine 211 again by the slurries of spinning, reach below the benchmark value (for example, 0.5%) until the cutting content of powder.Wherein, separating centrifuge when 600rpm, is together discharged 3 μ ms with interior cutting powder with water according to its speed of rotation, when 400rpm, together discharges 5 μ m with interior cutting powder with water.
Second mixing machine 214 comprises stirrer and water level monitoring transmitter, for example, is used in the water more than 50 ℃, below 70 ℃ with from the ratio mixed of the 3rd separating machine 213 isolating abrasives according to 5: 2.Cleaning machine 215 is in abrasive in second mixing machine 214 and water blended slurries, to insert vibrations, removes the cutting powder that abrasive surface is adhered to, and the device of together discharging with water.As an example, cleaning machine 215 is configured to Ultrasonic Cleaners, utilizes the mechanical cleaning machine of cleaning brush etc.
The 4th separating machine 216 is with the isolating by size device of the abrasive that obtains through cleaning process.The 4th separating machine 216 is configured to comprise that giving case, water tank, a plurality of screwed valve, flow takes into account overflow lip (overflow nozzle).Supply to when giving case through under meter and screwed valve at the water of water tank to the abrasive of the underfeed of giving case; Big relatively abrasive particle is deposited upon the bottom; Effectively size abrasive is swum; Little size abrasive is by on floating, and is discharged to through the overflow lip (overflow nozzle) that the filter with the net more than the 3 μ m, below the 5 μ m is installed and gives the case outside.Give the case inner side and be configured to mounting permanent magnet, to remove magnetic force composition impurity.Giving case inside, according to being little size abrasive from top, is that the order of big abrasive obtains separating to the bottom.
Net formula filter 217 is removed the also not separated and for example abrasive more than the 20 μ m of cohesion in the 4th separating machine 216.Water extracter 218 is removed the water that from the abrasive of the 4th separating machine 216 and discharge, contains.Water extracter 218 is configured to be equipped with the pressure filter of 200~400 aperture plates (mesh) filter cloth.
Remove the abrasive of water in the drying machine 219 drying and dehydrating machines 218.Drying machine 219 is configured to supply with the abrasive screw rod drying machine of steam.The screw rod drying machine is rotated through screw rod, mixes, dismisses abrasive, and it is contacted and evaporation drying water with the area of heat transfer of wide area.In drying process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus abrasive feed rate or adjusting screw(rod) speed of rotation are to regulate the moisture content in the abrasive.
Handover portion 220 is transplanted on retrieving arrangement with obtaining the exsiccant abrasive powder in the drying machine 219.Handover portion 220 is configured to conveyer (conveyer); In conveyer (conveyer), install under the situation of electro-magnet iron powder remover; Remove the iron powder that contains in the abrasive powder, be recovered to the abrasive that the content of cutting powder has the purity of 1ppm with pulverulence.
Machining oil recoverer 310 and machining oil base oil refinement portion 320
In Fig. 1; Machining oil recoverer 310 is to reclaim solid substance and the device of the machining oil that will comprise as base oil from machining oil separated part 100 isolated paraffin series oil, and machining oil base oil refinement portion 320 is the devices that refine the machining oil that water-soluble glycol ether (DEG), polyoxyethylene glycol (PEG) or polyethers (PPG) are comprised as base oil.As shown in Figure 4; In one embodiment of this invention; Machining oil recoverer 310 is configured to comprise machining oil safe deposit box 311, rapid steamer 312 and refined machining oil safe deposit box 313, and machining oil base oil refinement portion 320 is configured to comprise the 3rd mixing machine 321, the 5th separating machine 322, rapid steamer 323 and has refined machining oil base oil safe deposit box 324.
311 keepings of machining oil safe deposit box are reached the machining oil of the turbidity of setting by the result of turbidometer detection from the machining oil of 117 separation of second separating machine and discharge.The water that rapid steamer 312 evaporations contain from the machining oil that machining oil safe deposit box 311 is supplied with.Rapid steamer 312 is configured to by steam-heated water rapid steamer.In evaporative process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus regulates the machining oil feed rate, to regulate the moisture content in the machining oil.Refine machining oil safe deposit box 313 and taken care of the machining oil that refines from the quilt of rapid steamer 312 discharges.
The 3rd mixing machine 321 will mix with active carbon powder from the machining oil that machining oil safe deposit box 311 is supplied with.The additive that contains in the active carbon powder absorption machining oil, for example tensio-active agent, dispersion agent, viscosity modifier.
The 5th separating machine 322 separates blended machining oil and active carbon powder in the 3rd mixing machine 321.The 5th separating machine 322 is configured to precoat filter (precoat filter).In precoat filter (precoat filter); The absorption additive; For example the Powdered Activated Carbon of tensio-active agent, dispersion agent, viscosity modifier is filtered, and separates water-soluble glycol ether (DEG), polyoxyethylene glycol (PEG) or polyethers (PPG) as the machining oil raw material.The water that rapid steamer 323 evaporations contain from the machining oil that the 5th separating machine 322 is supplied with.Rapid steamer 323 is configured to by steam-heated water rapid steamer.In evaporative process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus regulates the machining oil feed rate, to regulate the moisture content in the machining oil.Refine machining oil base oil safe deposit box 324 and taken care of the machining oil base oil that refines from the quilt of rapid steamer 323 discharges.
Waste water refinement portion 400
In Fig. 1, waste water refinement portion 400 is the devices that refine all waste water that produce in abrasive refinement and the abrasive powder generation portion 200.As shown in Figure 5, in one embodiment of this invention, waste water refinement portion 400 is configured to comprise precoat slurries safe deposit box 411, waste water safe deposit box 412, the 6th separating machine 413 and has refined water safe deposit box 414.
Precoat slurries safe deposit box 411 stores the precoat slurries.Wherein, the precoat slurries are with the active carbon powder mixing and the slurries of manufacturing with the solid substance of discharging from the 6th separating machine 413 and recycled water.
The waste water that produces in 412 keeping abrasives refinements of waste water safe deposit box and the abrasive powder generation portion 200, and, from the waste water that the 6th separating machine 413 is discharged, do not reach the waste water of the turbidity of setting by the result of turbidometer detection as an example.
The 6th separating machine 313 supplies to the precoat slurries from precoat slurries safe deposit box 411, supplies to waste water from waste water safe deposit box 412, separates recycled water and solid substance.As an example, the 6th separating machine 413 is configured to comprise precoat filter (precoat filter) and turbidometer.A part of separating the solid substance of discharging from the 6th separating machine 413 is used in manufacturing precoat slurries, and all the other are used as the cement manufacturing and use with the energy.
Refine water safe deposit box 414 and stored the water that refines from the quilt of the 6th separating machine 413 supplies.Having refined the recycled water that stores in the water safe deposit box 414 is the water that is reached the turbidity of setting by the result that turbidometer detects, and it is used as useless silicon slurries refinement water and re-uses.
Fig. 6 is the mechanical flow digram of expression according to the useless silicon slurries process for extracting of useless silicon slurries device for refining of the present invention.
As shown in the figure, according to useless silicon slurries process for extracting of the present invention, it comprises substantially: the step S10 that from useless silicon slurries, separates the machining oil of solid substance; Refine abrasive from solid substance, and make the step S20 of the abrasive powder of being refined; Refine the step S30 of machining oil base oil; The step S40 of the waste water that refinement begins to produce from the step of refining abrasive.
At first the step S10 that separates solid substance and machining oil is described, the silicon slurries that will give up are rendered to stirrer S11.In order to regulate the viscosity of the useless silicon slurries of throwing in the stirrer, throw in machining oil or water to stirrer, mix with useless silicon slurries and stir S13.
Subsequently, utilize and to take out the pump silicon slurries that will give up and be transplanted on magnetic force composition Impurity removal from stirrer and use filter.Remove the magnetic force composition impurity S15 that contains in the useless silicon slurries at magnetic force composition Impurity removal in filter.In order to reduce the viscosity of useless silicon slurries, in the process of transferring with filter to magnetic force composition Impurity removal, utilize preheating heat X (not shown) will give up the preheating of silicon slurries for for example more than 30 ℃, below 50 ℃.
As an example, in useless silicon slurries process for extracting of the present invention, can begin to carry out repeatedly once more from the magnetic force composition being removed the step S11 that renders to stirrer again with the useless silicon slurries of removing magnetic force composition impurity the filter.
Subsequently, separate first solid substance and the first machining oil S17 that comprises in the useless silicon slurries of removing magnetic force composition impurity.According to distinctive form of the present invention, step S17 renders to first separating machine with the part in the useless silicon slurries of removing magnetic force property impurity, in first separating machine, separates the step of first solid substance and first machining oil.
As an example, first separating machine is configured to pressure filter or separating centrifuge.As an example, separating centrifuge is to remove that 1 μ m is above, size below the 10mm, and the concentration of handling solid substance occupies the separating centrifuge of the useless silicon slurries of 1~50 (%).In this separating centrifuge, screw rod low speed rotates, and discharges the solid substance that is moved to wall by cf-, and the cutting powder of cf-less effect relatively and machining oil overflow after being deposited in the separating machine.For according to the temperature of useless silicon slurries, concentration, viscosity and change speed is installed motor and phase inverter and unit (controller) use at rotor and screw rod respectively in the separating centrifuge.
Subsequently, untapped all the other useless silicon slurries among isolated first machining oil among the step S17 and the step S17 are mixed, in stirrer, make machining oil slurries S18.Machining oil and useless silicon slurries blended machining oil slurries are rendered to second separating machine, in second separating machine, separate second solid substance and the second machining oil S19.
As an example, second separating machine is configured to comprise precoat filter (precoat filter) and turbidometer and precoat slurries case.The precoat slurries for example are that the amount that is mixed into solid substance is filtration chamber's volumetrical of precoat filter (precoat filter) more than 30%, below 70%, and the concentration of machining oil is the slurries more than 30%, below 50%.Precoat filter (precoat filter) is made and supplied to these precoat slurries in precoat slurries case.Precoat filter (precoat filter) only is applied to the filter surface with the part of the macroparticle that comprises in the precoat slurries of supplying with, and little particle is little by little blocked between the macroparticle and formed precoat.
Precoat filter (precoat filter) is when stirrer is supplied with the machining oil slurries with certain pressure, regular hour, from precoat slurries case with predefined pressure and time to precoat filter (precoat filter) supply precoat slurries.When carrying out this process for several times repeatedly, solid substance is residued in precoat filter (precoat filter), and machining oil is then passed through.As an example, also carry out the heat of compression air of the heat more than 50 ℃ is supplied with 10 minutes, the warm air pressurization engineering that residual machining oil is also discharged in the heating precoat filter (precoat filter).When this project finishes, separate solid substance from precoat filter (precoat filter).
Machining oil from precoat filter (precoat filter) is discharged when the result who is detected by turbidometer does not reach the turbidity of setting, will be sent to stirrer and circulation again.On the contrary, the machining oil that reaches the turbidity of setting will arrive the machining oil safe deposit box certainly.
Below; Step S20 to also make the abrasive powder of being refined from solid substance refinement abrasive describes; Isolated solid substance is sent to first mixing machine in step S17, S19; In first mixing machine, fixture is mixed with the for example water more than 50 ℃, below 70 ℃ and makes aqueous slurry S21.First mixing machine comprises stirrer and level detection sensor, and its ratio of mixture that is used in water and solid substance is mixed into more than 2: 1, melts the machining oil that contains in the solid substance.
Subsequently, from solid substance and water blended aqueous slurry, remove magnetic force composition impurity S23, from the aqueous slurry of removing magnetic force composition impurity, separate abrasive, make the abrasive powder S25 that is refined.
Below, also make the step S25 of the abrasive powder of being refined with reference to Fig. 7 to Fig. 9 to separating abrasive, refine the step S30 of machining oil base oil, refinement is carried out detailed explanation from the step S40 of the waste water that the step of refining abrasive begins to produce.
Fig. 7 is the mechanical flow digram of expression according to abrasive refinement of the present invention and abrasive powder method of manufacture.
Blended aqueous slurry in first mixing machine (the step S23 of Fig. 6) is rendered to the 3rd separating machine, in the 3rd separating machine, separate abrasive S251.As an example; The 3rd separating machine is configured to 300~600rpm separating centrifuge; In separating centrifuge, together discharge the cutting powder with water, aforesaid first mixing machine among the step S21 of Fig. 6 be sent to again by the slurries of spinning; Reach below the benchmark value (for example, 0.5%) until the cutting content of powder.Wherein, separating centrifuge when 600rpm, is together discharged 3 μ ms with interior cutting powder with water according to its speed of rotation, when 400rpm, together discharges 5 μ m with interior cutting powder with water.
Subsequently, isolated abrasive is sent to second mixing machine, in second mixing machine, with abrasive and for example mixing of the water more than 50 ℃, below 70 ℃ and manufacturing slurries S252.Wherein, second mixing machine comprises stirrer and water level monitoring transmitter, and it is used in water and the separated abrasive ratio mixed according to 5: 2.
Subsequently, abrasive and water blended slurries are transplanted on magnetic force composition Impurity removal and use filter.Magnetic force composition Impurity removal with filter in, remove foreign substances (for example, the silicon) S253 that together condenses with iron powder that contains in the slurries.Behind step S253, slurries are rendered to second mixing machine again, and begin to carry out repeatedly once more from step S252.
Subsequently, in cleaning machine, insert vibrations, remove the cutting powder that abrasive surface is adhered to, and together discharge S254 with water to the aqueous slurry of removing magnetic force composition impurity.As an example, cleaning machine is configured to Ultrasonic Cleaners, utilizes the mechanical cleaning machine of cleaning brush etc.
Subsequently, will render to the 4th separating machine, in the 4th separating machine, separate S255 by size through the abrasive of cleaning step S254.The 4th separating machine is configured to comprise that giving case, water tank, a plurality of screwed valve, flow takes into account overflow lip (overflow nozzle).Supply to when giving case through under meter and screwed valve at the water of water tank to the abrasive of the underfeed of giving case; Big relatively abrasive particle is deposited upon the bottom; Effectively size abrasive is swum; Little size abrasive is by on floating, and is discharged to through the overflow lip (overflow nozzle) that the filter with the net more than the 3 μ m, below the 5 μ m is installed and gives the case outside.Give the case inner side and be configured to mounting permanent magnet, to remove magnetic force composition impurity.Giving case inside, is little size abrasive according to top, is that the order of big abrasive obtains separating to the bottom.
Subsequently, isolated abrasive is sent to water extracter, in water extracter, removes the water S256 that contains in the abrasive.As an example, water extracter is configured to be equipped with the pressure filter of 200~400 aperture plates (mesh) filter cloth.
Subsequently, the dry abrasive S257 that is removed water in drying machine.Drying machine is configured to supply with the abrasive screw rod drying machine of steam.The screw rod drying machine is rotated through screw rod, mixes, dismisses abrasive, and it is contacted and evaporation drying water with the area of heat transfer of wide area.In drying process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus abrasive feed rate or adjusting screw(rod) speed of rotation are to regulate the moisture content in the abrasive.
Subsequently, in drying machine, obtain the exsiccant abrasive and be transplanted on the retrieving arrangement that is used to reclaim abrasive powder by handover portion.Handover portion is configured to conveyer (conveyer), in conveyer (conveyer), installs under the situation of electro-magnet iron powder remover, removes the magnetic force composition impurity S258 that contains in the abrasive powder.
Fig. 8 is the mechanical flow digram of expression according to machining oil process for extracting of the present invention.
According to the machining oil base oil process for extracting of one embodiment of the invention, realize by water that contains in the isolating machining oil among the step S19 of evaporation Fig. 6 in rapid steamer and the method for refining.Rapid steamer is configured to by steam-heated water rapid steamer.In evaporative process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus regulates the machining oil feed rate, to regulate the moisture content in the machining oil.
Machining oil base oil process for extracting according to another embodiment of the present invention, isolated machining oil and active carbon powder mixing S31 among the step S19 with Fig. 6 in the 3rd mixing machine.The additive that contains in the active carbon powder absorption machining oil, for example tensio-active agent, dispersion agent, viscosity modifier.
Subsequently, blended machining oil and active carbon powder are rendered to the 5th separating machine, in the 5th separating machine, separate machining oil S32.The 5th separating machine is configured to precoat filter (precoat filter).In precoat filter (precoat filter); The absorption additive; For example the Powdered Activated Carbon of tensio-active agent, dispersion agent, viscosity modifier is filtered, and reclaims water-soluble glycol ether (DEG), polyoxyethylene glycol (PEG) or polyethers (PPG) as the machining oil raw material, re-uses as raw material.
Subsequently, in rapid steamer, evaporate the water S33 that contains in the isolated base oil, to refine machining oil base oil S33.Rapid steamer is configured to by steam-heated water rapid steamer.In evaporative process, detect moisture content through moisture meter, steam regulation pressure and feed rate, make its reach a certain amount of in, or plus-minus regulates the machining oil feed rate, to regulate the moisture content in the machining oil.
Fig. 9 is the mechanical flow digram of expression according to waste water process for extracting of the present invention.
As shown in the figure, in refining the method for waste water, mixed active carbon powder and precoat slurries S41 in the isolated waste water in the step S25 of Fig. 6.Blended waste water and active carbon powder and precoat slurries are rendered to the 6th separating machine, in the 6th separating machine, separate recycled water and solid substance S42.Wherein, the precoat slurries are that water and active carbon powder that solid substance and quilt from the discharge of the 6th separating machine are refined are mixed and the slurries of manufacturing.
In the waste water of in the 6th separating machine, discharging, the result who is detected by turbidometer does not reach the waste water of the turbidity of setting, with the step S41 through mixed active carbon powder and precoat slurries once more.A part of separating the solid substance of discharging from the 6th separating machine is used in manufacturing precoat slurries, and all the other are used as the cement manufacturing and use with the energy.The result who is detected by turbidometer reaches the water of the turbidity of setting, and it is used as useless silicon slurries and refines water and re-use.
More than; Embodiment with reference to shown in the accompanying drawing describes the present invention; So that those skilled in the art understand and embodiment of the present invention easily; But it is the embodiment of exemplary, it will be appreciated by those skilled in the art that to realize various deformation and other impartial with it embodiment from embodiments of the invention.Therefore, technical protection scope of the present invention is defined by claims.

Claims (13)

1. a useless silicon slurries process for extracting is characterized in that, comprising:
A) solid substance that comprises in the useless silicon slurries of separation and the step of machining oil;
B) with said isolated solid substance and water blended step;
C) from said solid substance and water blended slurries, separate abrasive and waste water, isolated abrasive is manufactured the step of the abrasive powder of being refined.
2. useless silicon slurries process for extracting according to claim 1 is characterized in that said a) step comprises:
A-1) said useless silicon slurries are rendered to the step of stirrer;
A-2) step of the useless silicon slurries in the said stirrer is rendered in heating and stirring;
The step of the magnetic force composition impurity that a-3) contains in the said useless silicon slurries of removal;
A-4) remove in the useless silicon slurries of said magnetic force composition impurity, its part is rendered in first separating machine, in said first separating machine, separate the step of first solid substance and first machining oil;
A-5) with said a-4) in the step isolated first machining oil with at said a-4) in the step untapped remaining remove the useless silicon slurries blended step of magnetic force composition impurity; And
A-6) with said a-5) blended first machining oil and useless silicon slurries are rendered in second separating machine in the step, in said second separating machine, separate the step of second solid substance and second machining oil.
3. useless silicon slurries process for extracting according to claim 2 is characterized in that, said first separating machine is in pressure filter or the separating centrifuge any one, and said second separating machine is a precoat filter of throwing in the precoat slurries.
4. useless silicon slurries process for extracting according to claim 1 is characterized in that said c) step also comprises:
C-1) step of removal magnetic force composition impurity in said solid substance and water blended slurries;
C-2) said solid substance and water blended slurries are rendered in the 3rd separating machine, in said the 3rd separating machine, separated the step of abrasive and waste water;
C-3) with said isolated abrasive and water blended step;
C-4) implement vibrations to said abrasive and water blended slurries, remove the cleaning step of the cutting powder that said abrasive surface adheres to;
C-5) will render in the 4th separating machine separation steps by size in said the 4th separating machine through the abrasive of said cleaning step;
The step of the water that c-6) is contained in the said isolated abrasive of removal;
C-7) step of the abrasive of dry said removal water.
5. useless silicon slurries process for extracting according to claim 4 is characterized in that said c-3) step also comprises:
Remove the step of the magnetic force composition impurity that contains in said abrasive and the water blended slurries.
6. useless silicon slurries process for extracting according to claim 4 is characterized in that said c) step also comprises:
The step of the magnetic force composition impurity that c-8) contains in the said abrasive that is dried of removal.
7. useless silicon slurries process for extracting according to claim 4 is characterized in that said the 3rd separating machine is a separating centrifuge, and said the 4th separating machine comprises gives case.
8. useless silicon slurries process for extracting according to claim 1 is characterized in that, said useless silicon slurries process for extracting also comprises:
D) refine the step of the base oil of isolated machining oil in the said a) step.
9. useless silicon slurries process for extracting according to claim 8 is characterized in that said d) step comprises:
D-1) with isolated machining oil in the said a) step and active carbon powder blended step;
D-2) with said d-1) blended machining oil and active carbon powder are rendered to the 5th separating machine in the step, in said the 5th separating machine, separate the step of machining oil;
The step of the water that d-3) contains in the said isolated machining oil of evaporation.
10. useless silicon slurries process for extracting according to claim 9 is characterized in that said the 5th separating machine is the precoat filter.
11. useless silicon slurries process for extracting according to claim 1 is characterized in that, said useless silicon slurries process for extracting also comprises:
E) step of isolated waste water in step refinement c).
12. useless silicon slurries process for extracting according to claim 11 is characterized in that said e) step comprises:
E-1) at said c) step of mixed active carbon powder and precoat slurries in the isolated waste water in the step;
E-2) with said e-1) blended waste water and active carbon powder and precoat slurries are rendered to the 6th separating machine in the step, in said the 6th separating machine, separate the water that refined and the step of solid substance.
13. useless silicon slurries process for extracting according to claim 12 is characterized in that, said the 6th separating machine is a precoat filter of throwing in the precoat slurries.
CN2009801591307A 2009-09-17 2009-09-18 Method for purifying waste silicon slurry Pending CN102428042A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
KR10-2009-0087910 2009-09-17
KR20090087910A KR100948612B1 (en) 2009-09-17 2009-09-17 Method for refining silicon slurry
PCT/KR2009/005332 WO2011034224A1 (en) 2009-09-17 2009-09-18 Method for purifying waste silicon slurry

Publications (1)

Publication Number Publication Date
CN102428042A true CN102428042A (en) 2012-04-25

Family

ID=42183573

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2009801591307A Pending CN102428042A (en) 2009-09-17 2009-09-18 Method for purifying waste silicon slurry

Country Status (4)

Country Link
JP (1) JP2013505144A (en)
KR (1) KR100948612B1 (en)
CN (1) CN102428042A (en)
WO (1) WO2011034224A1 (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101435021B1 (en) 2012-11-29 2014-09-15 쌍용양회공업(주) Processing Silicon Sludge For Cement Manufacturing Raw Materials
KR101472486B1 (en) 2013-07-02 2014-12-12 주식회사 시알에스 Recycling system for waste sludge
KR101579840B1 (en) * 2014-07-22 2015-12-24 주식회사 세신머티리얼즈 Water soluble waste slurry recycling method and device
KR101622295B1 (en) * 2014-10-13 2016-05-18 주식회사 포스코 Manufacturing method of heat increasing and component controlling briquette used in steel manufacturing process
KR101793274B1 (en) * 2016-06-02 2017-11-02 김경태 Si Sludge Regeneration System
PL239376B1 (en) * 2019-04-01 2021-11-29 Ht Solutions Spolka Cywilna A method of recycling post-production mineral abrasive for its secondary use
CN115193101B (en) * 2021-04-09 2024-02-13 中国矿业大学 A method for recovering coolant from wire cutting

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4449185B2 (en) * 2000-07-13 2010-04-14 株式会社新菱 Abrasive recovery method
JP4335541B2 (en) * 2003-01-20 2009-09-30 隼次 芝田 Method and apparatus for separating SiO2 particles and SiC particles, and separation and recovery SiC
KR100625283B1 (en) * 2004-09-24 2006-09-18 장영철 Waste Sludge Regeneration Apparatus and Method Generated in Semiconductor Wafer Fabrication
KR100626252B1 (en) * 2004-12-24 2006-09-21 (주)풍남반도체테크 Regeneration process of wire saw abrasive
JP4718854B2 (en) * 2005-02-04 2011-07-06 株式会社安永 Recycling method of waste slurry in slurry type processing apparatus and regeneration processing apparatus used therefor
KR100786644B1 (en) * 2007-06-15 2007-12-21 주식회사 유스테크코리아 Waste Slurry Recycling Method in Semiconductor Wafer Manufacturing Process and Regeneration System
JP5090191B2 (en) * 2008-01-24 2012-12-05 三和油化工業株式会社 Method for recovering dispersion medium from waste slurry slurry

Also Published As

Publication number Publication date
WO2011034224A1 (en) 2011-03-24
JP2013505144A (en) 2013-02-14
KR100948612B1 (en) 2010-03-18

Similar Documents

Publication Publication Date Title
CN102428042A (en) Method for purifying waste silicon slurry
CN101681808B (en) Regenerating process and regenerating system to regenerate waste slurry from semiconductor wafer manufacturing process
CN101528597B (en) Silicon reclamation apparatus and method of reclaiming silicon
CN102925191B (en) Method and device for extracting asphalt from oil sand through solvent extraction
KR20160060684A (en) Treatment method for cement kiln extracted gas, chlorine bypass system, and cement firing device
KR20120059857A (en) Recycling method and system of sludge in semi-conductor producing process
CN101684028B (en) A method and device for processing silicon crystal plate cutting waste
CN102746934A (en) Method for recovering water-soluble cutting fluid from silicon wafer cutting fluid
CN103347654A (en) Coolant regeneration method
JP3776675B2 (en) Recycling equipment for inorganic abrasive waste liquid
TWI579441B (en) Method for producing briquettes and briquettes produced using the same
KR20050096328A (en) System for recycling waste sludge of semiconductor wafer
JP3768919B2 (en) Method for treating oil-adhered particles
CN101935581B (en) Separation regeneration production process of cutting waste mortar by silicon wafer line
KR101047383B1 (en) Waste Slurry Recycling Method and Device
CN201912833U (en) Treatment device for recovering recycled oil from silicon wafer cutting waste oil sludge
JP3950391B2 (en) Wire saw slurry management system
CN101805663A (en) Resource utilization method of silicon slice cutting and processing mortar of propylene glycol system
KR101020151B1 (en) Waste Slurry Recycling Equipment and Recycling Method
WO2007119308A1 (en) Method of recovering silicon-containing material
CN102952621B (en) Method and equipment for recycling silicon wafer cutting and grinding waste
TW201013745A (en) Wafer/photovoltaic panel cutting waste handling process and equipment
RU2217510C2 (en) Method of processing metalliferrous waste and device for processing the waste
KR102268889B1 (en) Apparatus for removing impuritiy of cement kiln dust and method therefor
KR101331446B1 (en) Method For Purificating Abrasive Cutting Sludge

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20120425