CN102320701A - Device and method for recycling silicon powder in silicon processing waste water - Google Patents

Device and method for recycling silicon powder in silicon processing waste water Download PDF

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CN102320701A
CN102320701A CN201110163091A CN201110163091A CN102320701A CN 102320701 A CN102320701 A CN 102320701A CN 201110163091 A CN201110163091 A CN 201110163091A CN 201110163091 A CN201110163091 A CN 201110163091A CN 102320701 A CN102320701 A CN 102320701A
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waste water
silica flour
water
silicon
outlet
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张世文
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Boying Xiamen Science and Technology Co Ltd
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Boying Xiamen Science and Technology Co Ltd
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Priority to PCT/CN2012/072043 priority patent/WO2012171366A1/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/38Treatment of water, waste water, or sewage by centrifugal separation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/463Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
    • 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

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  • Water Supply & Treatment (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

The invention discloses a device and method for recycling silicon powder in silicon processing waste water and relates to waste water treatment. In The device and method for recycling the silicon powder in the silicon processing waste water, provided by the invention, an electrolysis technology, a centrifugal separation technology and a filter technology are combined. The device is provided with an electrolysis system, a centrifugal separation system, a drying system and a filtering system, wherein the electrolysis system is provided with a stop valve, a water supply pump, an electrolysis machine and a buffer tank; the centrifugal separation system is provided with a stop valve, a water supply pump, a centrifugal machine, a silicon powder collecting tank and a waste water storage tank; the drying system is used for drying silicon powder obtained by centrifugal separation; and the filtering system is provided with a stop valve, a water pump, a filter device, a tee joint, a backwashing pump and a recycled water storage tank. The method comprises the following steps of: electrolyzing firstly to obtain electrolytic flocculation waste water; carrying out centrifugal separation to obtain silicon powder sediments and waste water; drying to obtain a silicon powder finished product; and then filtering and introducing the filtered liquid into the recycled water storage tank to obtain recycled water.

Description

Silica flour recycle device and method thereof in a kind of silicon processing waste water
Technical field
The present invention relates to a kind of wastewater treatment, especially relate to silica flour recycle device and method thereof in a kind of silicon processing waste water.
Background technology
Along with the fast development of semi-conductor industry, the high-purity crystal silicon materials have obtained widespread use, and wherein crystalline silicon is to be drawn as silicon single crystal rod earlier, cuts into silicon chip then and is used to make chip.In recent years, along with global oil, coal equal energy source growing tension, sun power becomes most important new forms of energy in this century gradually; The solar energy industry in the whole world has got into high-speed development period, during the preparation solar cell, and need be with HIGH-PURITY SILICON casting silicon ingot; Cut into silicon chip then; No matter be used silicon single crystal of semi-conductor industry or the used polysilicon of solar cell, all need high-purity crystalline silicon be cut into silicon chip, in cutting process; Calculate theoretically and have 44% crystalline silicon and cut mill and entered into cutting slurry, lost and have in the actual course of processing up to 50%~52% crystalline silicon form with silica flour for high-purity silicon powder.No matter the polysilicon that is used for the silicon single crystal of electronic-grade or is used for solar level all need make through a large amount of energy consumptions and high cost.Therefore, along with semi-conductor industry steadily forward with the leapfrogging growth of solar energy industry, the whole world needs the total amount of cutting processing silicon single crystal and polysilicon the great-jump-forward growth to occur, also year by year phenomenal growth of the slug that produces in the cutting processing process.On the other hand, along with reshuffling and the lasting decline of profit of silicon chip cutting industry, the silicon chip cutting enterprise control production process of coincidentally beginning to fight, the idea that reduces production costs.If can the HIGH-PURITY SILICON in the slug, polyoxyethylene glycol and silit be carried out comprehensive reutilization; Will reduce environmental pollution; Improve the utilization ratio of resource; Particularly if can the silica flour in the cutting wastewater be able to reclaim effectively and be used further to make solar cell, be highly significant to alleviating China's solar energy polycrystalline silicon import volume in short supply, that reduce polysilicon, and this will produce considerable economic and social benefit; So the recovery project of raw material receives pursuing energetically of the domestic factory of cutting into slices in the silicon cutting wastewater, it is in full flourish that the silicon cutting wastewater reclaims one time of enterprise.
For the recovery method and the technology of silicon single crystal and polysilicon cutting wastewater, the researchist also does a lot of work, and has applied for relevant patent.But in the recovery method of cutting wastewater, major part all is polyoxyethylene glycol and the silit that reclaims in the slip, and ripe not enough for the recovery method of silica flour in the slip.For the recovery of silica flour, at present, technology relatively more commonly used is that chemical industry is merged with the mining industry processing technology mutually; The bond material machining characteristics; Utilize spinning dispersion, matting, flocculation, extraction etc. to separate principle and method,, and reclaim silica flour the contaminant removal in the cutting wastewater.For example; Chinese patent ZL 200710018636.9 discloses a kind of method that from the cutting waste mortar, reclaims silica flour and carborundum powder, and it is to remove suspension agent and sticker in the waste material through organic solvent, and solid-state sand material is carried out gas flotation; Obtain the Si powder of certain purity; Further this Si powder is carried out liquid floatation and gravitational segregation, again the silica flour that sub-elects is carried out pickling, obtain the method for highly purified silica flour.Chinese patent ZL200810118666.1 discloses a kind of method of from grinding waste liquid, extracting silica flour; It is to add hydrochloric acid toward grinding waste liquid, and pH is 1.0~6.0 in control, and concentration of hydrochloric acid is 0.1%~37%; The hydrochloric acid temperature is 15~60 ℃, through leave standstill, separate, dry and reclaim the method for silica flour.Chinese patent ZL 200910155689.4 discloses a kind of method that from the cutting waste mortar, reclaims polycrystal silicon ingot, carborundum powder and polyoxyethylene glycol; It is according to weight ratio 1: 0.5~5 mixed agglomerates with the silicon powder that makes and fusing assistant; In vacuum high temperature furnace, carry out pyroprocessing; Temperature ranges is 1450~1800 ℃, and the treatment time, scope was at 1~10h; Then the molten state HIGH-PURITY SILICON after the pyroprocessing is carried out directional freeze, obtain polycrystal silicon ingot.Yet though utilize these methods can both reclaim silica flour, its application still has certain limitation.Subject matter has: the treatment process of waste water is unreasonable in (1) recovery technology: in the silica flour removal process, produce great amount of wastewater, also not have several enterprises to accomplish up to standard or zero release at present.(2) Financial cost is high: matting, extraction or adding fusing assistant pyroprocessing reclaim silica flour; These methods or add a large amount of chemical agents, or required energy consumption and height are though can realize reclaiming the purpose of silica flour; But running cost; Weigh from economical standard, still not fully up to expectations, in the silicon cutting wastewater, reclaim silica flour and can't realize mass-producing.(3) reclaim the secondary pollution problem that produces in the technology: in the silicon cutting wastewater, add flocculation agent in the regenerated using treating processes of waste water; Colloid thing, solid particulate in the waste water precipitate; This not only increases running cost; And environment caused certain pollution, increase the difficulty of subsequent disposal, not environmental protection.
In sum; Monocrystalline and polysilicon all obtain through high energy consumption is expensive; And most of monocrystalline of China and polysilicon are dependence on import, thus in the cutting wastewater recovery value of silica flour far above silit and polyoxyethylene glycol, in cutting process; Lose in the form entering cutting wastewater of 50% crystalline silicon with silica flour; Research and development are fit to safe, reliable, efficient, the less energy-consumption of China's economic present situation and developmental level, low investment, silica flour and waste water reclamation utilize in the silicon cutting wastewater cheaply device and method, reclaim the silica flour in the cutting wastewater effectively, not only can turn waste into wealth, improve the cost of resource utilization, reduction silicon chip; And can alleviate the problem of environmental pollution that waste water produces, and important social effect and commercial value are arranged to alleviating China's silicon raw material import volume in short supply, that reduce the silicon raw material.
Summary of the invention
The objective of the invention is to problem to silica flour in the existing silicon cutting wastewater and the existence of waste water reclamation utilization technology; Overcome and existing reclaim from the silicon cutting wastewater that the investment that silica flour produced is big, running cost is high, environment is produced secondary pollution and can not realize defectives such as wastewater to reach standard or zero release, silica flour recycle device and method thereof in a kind of silicon processing waste water that electrolysis tech, centrifugal separation technique and filtering technique are combined is provided.
The silica flour recycle device is provided with electrolytic system, centrifugal separation system, dehumidification system and filtering system in the said silicon processing waste water;
Said electrolytic system is used for the electrolysis and the precipitation process of silicon cutting wastewater, decomposes the organism in the waste water through electrolytic oxidation, reduces COD significantly, under electric field action, improves the waste water settling condition simultaneously, quickens the sedimentation of waste water waste water; Said electrolytic system is provided with stopping valve, working shaft, electrolysis machine and surge tank; The external silicon cutting wastewater of the import of stopping valve relief outlet, the import of working shaft connects the outlet of stopping valve, and the water supply pump outlet connects the import of electrolysis machine, and the outlet of electrolysis machine connects the import of surge tank, and the outlet of surge tank connects with centrifugal separation system;
Said centrifugal separation system is used for the silica flour rapid subsidence of waste water is separated; Said centrifugal separation system is provided with stopping valve, working shaft, whizzer, silica flour holding tank and waste water basin; The import of stopping valve connects the wastewater outlet of electrolytic system surge tank; The outlet of stopping valve connects the import of working shaft; The water supply pump outlet connects with the import of whizzer, and the deposition outlet of whizzer connects with the silica flour holding tank, and the wastewater outlet of whizzer connects with the waste water basin;
Said dehumidification system is used for the silica powder drying with the spinning gained;
Said filtering system is used for that waste water with the centrifugal separation system gained filters, separating treatment gets regenerated recycle-water; Said filtering system is provided with stopping valve, water pump, filtration unit, threeway, backwashing pump and reprocessing cycle water basin; The import of stopping valve connects the outlet of centrifugal separation system waste water basin; The import of the outlet water pump of stopping valve; The import of filter device is taken in the outlet of water pump, and the outlet of filtration unit connects the import of threeway, and two outlets of threeway connect backwashing pump and reprocessing cycle water basin respectively.
The anode of said electrolysis machine is a noble electrode, and said anodic substrate can be titanium-base or plastic base etc., and the top layer of said substrate can be coated with precious metal oxide coating; Cathode material in the electrolyzer of said electrolysis machine can be a kind of in the alloy of graphite, titanium, iron, aluminium, zinc, copper, lead, nickel, molybdenum, chromium, metal etc.; The WV of adjacent two electrode pads of said electrolysis machine can be 2~18V, and the optimum operation WV is 3~8V; The working current density of electrolysis machine can be 5~200mA/cm 2, optimum current density is 30~120mA/cm 2
Said dehumidification system can adopt a kind of in kiln drier, blast drier, Vacuumdrier, the freeze drier etc.
The recoverying and utilizing method of silica flour in the said silicon processing waste water adopts silica flour recycle device in the above-mentioned silicon processing waste water, may further comprise the steps:
1) electrolysis: with the silicon cutting wastewater after working shaft extracts, carry out electrolysis in the input electrolysis machine after, get into surge tank, electrolytic flocculation waste water;
In step 1), said silicon cutting wastewater is meant the waste water that high-purity crystalline silicon produces in cutting into the process of silicon chip, and silica flour content is 60~200mg/L in the waste water, waste water COD≤100mg/L; Said electrolysis is that the silicon cutting wastewater is made it to generate the hydroxyl [OH] of status nascendi and the oxygen [O] of status nascendi through electrolysis; In order to the organism in the oxygenolysis waste water; Simultaneously, under electric field action, make suspended substance, colloid, charged corpuscle cohesion in the waste water form larger particles; The nano-catalytic anode material is installed in the electrolyzer of said electrolysis machine; It is the MOX inertia catalyst coatings of 10~35nm that there is crystal grain on its top layer, and it is active and stable that kind electrode has higher electrocatalytic reaction, can reduce electrolytic overpotential significantly; Its WV can be 2~250V; Adjacent two interelectrode voltages are 2~18V, and adjacent two interelectrode optimum voltages are 3~8V, and current density is 5~200mA/cm 2, the best is 30~120mA/cm for current density 2, the residence time of waste water in electrolysis machine is 3~15min, the process electrolysis of silicon cutting wastewater is after valve gets into centrifugal separation system.
2) spinning: will pass through purifying liquid waste of electrolytic system processing gained and get into centrifugal separation system through pipeline, the cf-that rotation is produced by whizzer comes the separating substances of different sizes and different densities, gets silica flour throw out and waste water;
In step 2) in, the working speed of whizzer can be 1000~15000rpm in the said centrifugal separation system, can be 30~300s working time, and the optimum operation rotating speed can be 1500~3000rpm, and the optimum operation time can be 30~150s.
3) drying: the silica flour throw out of centrifugal separation system gained is placed drying machine, reduce the water ratio in the silica flour throw out, get the silica flour finished product through super-dry;
4) filter: the waste water of centrifugal separation system gained is got in the filtration unit through water pump lifting, waste water is carried out filtering separation, the filtrating of filtering generation enters into the reuse water basin and gets reuse water.
In step 4), said filtration unit can be multi-medium filtering device or micro-filtration filtration unit etc.; The filtrate of said multi-medium filtering device can be silica sand, hard coal and cobble, and filtration velocity can be 7.5~20m/h.Multi-medium filtering device WP≤0.6MPa, 0.04MPa≤water feeding pressure≤0.4MPa, back flushing water feeding pressure>=0.15MPa; Inlet outlet pressure differential is 0.01~0.015MPa; Back washing strength is 4~25L/ (sm), and back flushing lasts 3~7min, and the backwash expansion rate is 40%~50%; The said condition that waste water is carried out filtering separation can be WP≤0.6MPa, 0.04MPa≤water feeding pressure≤0.4MPa, back flushing water feeding pressure>=0.15MPa.
The present invention carries out advanced treatment with the silicon cutting wastewater, turns waste into wealth, and in cutting wastewater, purifies liquid waste the device and method that makes the waste water reclamation recycle in the recovery silica flour finished product.This invention equipment is simple, and running cost is low, does not produce secondary pollution; And the silica flour finished product that reclaims can also utilize again; Regenerated recycle-water also can recycle in production technique, not only can improve resource utilization, can also alleviate the problem of environmental pollution that waste water produces; Increase economic efficiency; Particularly adopt this method the silica flour of most worthy in the silicon cutting wastewater to be reclaimed and utilize, can reduce consumption of raw materials, this is to alleviating the significant and commercial value of import volume that China's silicon raw material is in short supply, reduce the silicon raw material.Adopt this technological line to solve the difficult problem that silica flour and waste water reclamation utilize in the existing silicon cutting wastewater, have following advantage:
1) adopt electrolysis to have following outstanding effect: (1) under galvanic action, the hydroxyl [OH] of the status nascendi that electrolysis produces and the oxygen [O] of status nascendi make and residue in oxidation operation decomposition in the sewage, reduce COD fast, improve the biodegradability of sewage.(2) suspended substance, colloid, charged corpuscle in the waste water condensed under electric field action and form larger particles, accelerate precipitation, and improve the separation efficiency of follow-up centrifugal separation system.
2) reduce the waste water COD total release; Significantly improve wastewater biodegradability: traditional biochemical end adds membrane filtration technique; Though water reuse in can implementation part can not reduce the total release of COD of sewage, the hydroxyl [OH] of the status nascendi that electrolysis of the present invention produces makes the oxidation operation decomposition with the oxygen [O] of status nascendi; Not only reduce the total release of COD of sewage significantly, and improve the biodegradability of waste water;
3) the reuse water rate high, realize zero release basically: in the silica flour removal process; Not only do not produce new waste water, and can purify liquid waste simultaneously, the reclamation rate of waste water is up to 80%~95%; Reuse water directly recycle in production technique; Sewage effluent is few, realizes zero release basically, has solved the problem of environmental pollution that discharge of wastewater produces;
4) Financial cost is low: adopt electrolysis tech and centrifugal separation technique that the silicon in the silicon cutting wastewater is recycled, need not add a large amount of cleanings, extraction chemistry medicament, or the energy consumption of consume significant, cost is lower, and is comparatively worthwhile economically.
5) do not produce secondary pollution: in the silicon cutting wastewater, need not add chemical substances such as flocculation agent in the regenerated using treating processes of waste water, not only save cost, and practice thrift material consumption and do not produce secondary pollution.
6) utilize whizzer that the silicon cutting wastewater is carried out the solid-liquid separating treatment, can shorten the isolating distance of silica flour natural subsidence in waste water greatly, velocity of separation is accelerated, improve separation efficiency, improved isolating effect simultaneously.
Description of drawings
Fig. 1 is that the structure of silica flour recycle device embodiment in the silicon processing waste water according to the invention is formed synoptic diagram.
Embodiment
The present invention be after the comparative study of composition, character and the existing processing scheme of existing silicon cutting wastewater being goed deep into system completion to the silicon cutting wastewater in silica flour and waste water reclamation utilize the design of technology; Through the combination utilization of technologies such as electrolytic system, centrifugal separation system, dehumidification system and filtering system, thereby form silica flour and waste water reclamation use device and method in a kind of silicon cutting wastewater.
Following embodiment will combine accompanying drawing that the present invention is further described.
Referring to Fig. 1, silica flour recycle device embodiment is provided with in the silicon processing waste water according to the invention:
Electrolytic system: electrolytic system is used for electrolysis treatment, and electrolytic system is provided with stopping valve 11, working shaft 12, electrolysis machine 13 and surge tank 14.The external silicon cutting wastewater of the import of stopping valve 11 relief outlet P; The import of working shaft 12 connects the outlet of stopping valve 11; The outlet of working shaft 12 connects the import of electrolysis machine 13, and the outlet of electrolysis machine 13 connects the import of surge tank 14, and the outlet of surge tank 14 connects with centrifugal separation system through stopping valve.
Centrifugal separation system: centrifugal separation system is used for that purifying waste water of electrolysis gained carried out spinning to be handled, and obtains silica flour throw out and waste water.Centrifugal separation system is provided with stopping valve 21, working shaft 22, whizzer 23, silica flour holding tank 24, stopping valve 25, waste water basin 26; The import of stopping valve 21 connects the outlet that electrolytic system is purified liquid waste, and the process of purifying liquid waste working shaft 22 entering whizzers 23 carry out spinning and get silica flour throw out and waste water; The silica flour throw out that produces is collected in the silica flour holding tank 24, and the outlet of silica flour holding tank 24 connects the import of dehumidification system; And the wastewater collection that produces is in waste water basin 26, and the import of filtering system is taken in the outlet of waste water basin 26.
Dehumidification system: the silica flour throw out that dehumidification system is used for dry centrifugal separation system gained gets the silica flour finished product.Dehumidification system is provided with drying machine 31, and the import of drying machine 31 connects the outlet of silica flour holding tank 24 in the centrifugal separation system.
Filtering system: filtering system is used for that waste water with the centrifugal separation system gained filters, separating treatment gets regenerated recycle-water.Filtering system is provided with stopping valve 41, water pump 42, filtration unit 43, stopping valve 44, threeway 45, stopping valve 46, backwashing pump 47, stopping valve 48, reprocessing cycle water basin 49; The import of stopping valve 41 connects the outlet of centrifugal separation system waste water basin 28, and waste water gets into filtration units 43 through water pump 42, and the outlet of filtration unit is divided into two-way through threeway 45, and one the tunnel connects with reprocessing cycle water basin 49 through stopping valve 44; Another road connects with reprocessing cycle water basin 49 through stopping valve 46, backwashing pump 47, stopping valve 48 successively.
Provide the specific embodiment of the recoverying and utilizing method of silica flour in the silicon processing waste water below in conjunction with Fig. 1.
Embodiment 1
Silica flour and waste water reclamation utilize engineering in the 1000 ton per day silicon cutting wastewater.
The water quality situation of said silicon cutting wastewater is as shown in table 1.
The water quality situation of table 1 silicon cutting wastewater
Figure BDA0000068349430000061
Step 1, electrolysis: start working shaft 12, sewage is with 50m 3/ h flow velocity gets into electrolysis machine 13 through stopping valve 11 and carries out electrolysis, gets into surge tank 14 again and precipitates.The WV of said electrolysis machine is 12V, and two interpolar voltages are 3.5~8.0V, current density 80mA/cm 2The residence time of waste water in electrolysis machine is 9~15min; Under galvanic action, the organism of the hydroxyl [OH] of the status nascendi that electrolysis produces and the oxygen strong oxidizing property material oxygenolysis waste water such as [O] of status nascendi reduces COD; And make suspended substance, colloid, charged corpuscle in the silicon cutting wastewater under electric field action, form larger particles, be convenient to spinning.Electrolytic system is handled each item water-quality guideline such as the table 2 of after waste water.
The water quality situation of purifying liquid waste after table 2 electrolysis
Figure BDA0000068349430000062
Step 2, spinning: handle purifying liquid waste of gained through electrolytic system and get into centrifugal separation system through pipeline; The cf-that 23 rotations are produced by whizzer; The separating substances of different sizes and different densities is come; Get silica flour throw out and waste water, collect respectively in silica flour holding tank 24 and the waste water basin 26.
The working speed of whizzer is 1800~2000rpm in the said centrifugal separation system, and be 210s working time.
Step 3, drying: the silica flour of centrifugal separation system gained through super-dry, is reduced the water ratio in the silica flour throw out, the silica flour finished product, the recovery of silica flour is up to 92%.
Step 4, filtration: the waste water in the waste water storage tank 26 in the centrifugal separation system is promoted entering filtration units 43 through water pump 42, waste water is filtered, separates, the filtrating of filtering generation enters into reprocessing cycle water basin 49 and gets reuse water.Every operation for some time; Regularly the filtrate in the filtration unit 43 is carried out back flushing; The process of back flushing is: utilize backwashing pump 47 that the reuse water in the reprocessing cycle water basin 49 is got into from filtration unit 43 exits, carry out back flushing, the waste water that back flushing produces discharges through filtration unit 43 imports.
Filtration unit 43 is the multi-medium filtering device in the said filtering system, and the filtrate of multi-medium filtering device is silica sand, hard coal and cobble, and filtration velocity is 8~10m/h.Multi-medium filtering device WP is 0.3MPa, and water feeding pressure is 0.1MPa, and the back flushing water feeding pressure is 02MPa, and back washing strength is 6~15L/ (sm), and back flushing lasts 5min, and the backwash expansion rate is 45%.
The Wastewater Recovery rate is 90%, and the water quality situation of reuse water is as shown in table 3.
The water quality situation of table 3 reuse water
Figure BDA0000068349430000071
Embodiment 2
Silica flour and waste water reclamation utilize engineering in the 2000 ton per day silicon cutting wastewater.
The water quality situation of said silicon cutting wastewater is as shown in table 3.
The water quality situation of table 3 silicon cutting wastewater
Step 1, electrolysis: starting working shaft 12, the silicon cutting wastewater is with 100m 3/ h flow velocity gets into electrolysis machine 13 through stopping valve 11 and carries out electrolysis, gets into surge tank 14 again and precipitates.The WV of said electrolysis machine is 18V, and two interpolar voltages are 3.5~5.0V, current density 120mA/cm 2The residence time of waste water in electrolysis machine is 5~8min; Under galvanic action, the organism of the hydroxyl [OH] of the status nascendi that electrolysis produces and the oxygen strong oxidizing property material oxygenolysis waste water such as [O] of status nascendi reduces COD; And make suspended substance, colloid, charged corpuscle in the silicon cutting wastewater under electric field action, form larger particles, be convenient to spinning.Electrolytic system is handled each item water-quality guideline such as the table 4 of after waste water.
The water quality situation of purifying liquid waste after table 4 electrolysis
Figure BDA0000068349430000081
Step 2, spinning: handle purifying liquid waste of gained through electrolytic system and get into centrifugal separation system through pipeline; The cf-that 23 rotations are produced by whizzer; The separating substances of different sizes and different densities is come; Get silica flour throw out and waste water, collect respectively in silica flour holding tank 24 and the waste water basin 26.
The working speed of whizzer is 2600~3000rpm in the said centrifugal separation system, and be 150s working time.
Step 3, drying: the silica flour of centrifugal separation system gained through super-dry, is reduced the water ratio in the silica flour throw out, must reclaim the silica flour finished product, the recovery of silica flour is up to 93%.
Step 4, filtration: the waste water in the waste water storage tank 26 in the centrifugal separation system is promoted entering micro-filtration filtration units 43 through water pump 42, waste water is filtered, separates, the filtrating of filtering generation enters into reprocessing cycle water basin 49 and gets reuse water.Every operation for some time; Regularly micro-filtration filtration unit 43 is carried out back flushing; The process of back flushing is: utilize backwashing pump 47 that the reuse water in the reprocessing cycle water basin 49 is got into from micro-filtration filtration unit 43 exits; Carry out back flushing, the waste water that back flushing produces discharges through 43 imports of micro-filtration filtration unit.
The Wastewater Recovery rate is 95%, and the water quality situation of reuse water is as shown in table 5.
The water quality situation of table 5 reuse water
Figure BDA0000068349430000082

Claims (10)

1. silica flour recycle device in the silicon processing waste water is characterized in that being provided with electrolytic system, centrifugal separation system, dehumidification system and filtering system;
Said electrolytic system is used for the electrolysis and the precipitation process of silicon cutting wastewater, and said electrolytic system is provided with stopping valve, working shaft, electrolysis machine and surge tank; The external silicon cutting wastewater of the import of stopping valve relief outlet, the import of working shaft connects the outlet of stopping valve, and the water supply pump outlet connects the import of electrolysis machine, and the outlet of electrolysis machine connects the import of surge tank, and the outlet of surge tank connects with centrifugal separation system;
Said centrifugal separation system is used for the silica flour rapid subsidence of waste water is separated; Said centrifugal separation system is provided with stopping valve, working shaft, whizzer, silica flour holding tank and waste water basin; The import of stopping valve connects the wastewater outlet of electrolytic system surge tank; The outlet of stopping valve connects the import of working shaft; The water supply pump outlet connects with the import of whizzer, and the deposition outlet of whizzer connects with the silica flour holding tank, and the wastewater outlet of whizzer connects with the waste water basin;
Said dehumidification system is used for the silica powder drying with the spinning gained;
Said filtering system is used for that waste water with the centrifugal separation system gained filters, separating treatment gets regenerated recycle-water; Said filtering system is provided with stopping valve, water pump, filtration unit, threeway, backwashing pump and reprocessing cycle water basin; The import of stopping valve connects the outlet of centrifugal separation system waste water basin; The import of the outlet water pump of stopping valve; The import of filter device is taken in the outlet of water pump, and the outlet of filtration unit connects the import of threeway, and two outlets of threeway connect backwashing pump and reprocessing cycle water basin respectively.
2. silica flour recycle device in a kind of silicon processing waste water as claimed in claim 1, the anode that it is characterized in that said electrolysis machine is a noble electrode, said anodic substrate is titanium-base or plastic base; The top layer of said substrate is coated with precious metal oxide coating.
3. silica flour recycle device in a kind of silicon processing waste water as claimed in claim 1 is characterized in that cathode material in the electrolyzer of said electrolysis machine is a kind of in the alloy of graphite, titanium, iron, aluminium, zinc, copper, lead, nickel, molybdenum, chromium, metal.
4. silica flour recycle device in a kind of silicon processing waste water as claimed in claim 1, the WV that it is characterized in that adjacent two electrode pads of said electrolysis machine is 2~18V, the optimum operation WV is 3~8V; The working current density of electrolysis machine is 5~200mA/cm 2, optimum current density is 30~120mA/cm 2
5. silica flour recycle device in a kind of silicon processing waste water as claimed in claim 1 is characterized in that said dehumidification system is selected from a kind of in kiln drier, blast drier, Vacuumdrier, the freeze drier.
6. the recoverying and utilizing method of silica flour in the said silicon processing waste water is characterized in that adopting silica flour recycle device in a kind of silicon processing waste water as claimed in claim 1, and said recoverying and utilizing method may further comprise the steps:
1) electrolysis: with the silicon cutting wastewater after working shaft extracts, carry out electrolysis in the input electrolysis machine after, get into surge tank, electrolytic flocculation waste water;
2) spinning: will pass through purifying liquid waste of electrolytic system processing gained and get into centrifugal separation system through pipeline, the cf-that rotation is produced by whizzer comes the separating substances of different sizes and different densities, gets silica flour throw out and waste water;
3) drying: the silica flour throw out of centrifugal separation system gained is placed drying machine, reduce the water ratio in the silica flour throw out, get the silica flour finished product through super-dry;
4) filter: the waste water of centrifugal separation system gained is got in the filtration unit through water pump lifting, waste water is carried out filtering separation, the filtrating of filtering generation enters into the reuse water basin and gets reuse water.
7. the recoverying and utilizing method of silica flour in the silicon processing waste water as claimed in claim 6; It is characterized in that in step 1); Said silicon cutting wastewater is meant the waste water that high-purity crystalline silicon produces in cutting into the process of silicon chip, silica flour content is 60~200mg/L in the waste water, waste water COD≤100mg/L.
8. the recoverying and utilizing method of silica flour in the silicon processing waste water as claimed in claim 6; It is characterized in that in step 1) the nano-catalytic anode material is installed in the electrolyzer of said electrolysis machine, and it is the MOX inertia catalyst coatings of 10~35nm that there is crystal grain on its top layer; WV is 2~250V; Adjacent two interelectrode voltages are 2~18V, and adjacent two interelectrode optimum voltages are 3~8V, and current density is 5~200mA/cm 2, the best is 30~120mA/cm for current density 2, the residence time of waste water in electrolysis machine is 3~15min.
9. the recoverying and utilizing method of silica flour in the silicon processing waste water as claimed in claim 6; It is characterized in that in step 2) in; The working speed of whizzer is 1000~15000rpm in the said centrifugal separation system; Be 30~300s working time, and the optimum operation rotating speed is 1500~3000rpm, and the optimum operation time is 30~150s.
10. the recoverying and utilizing method of silica flour is characterized in that in step 4) in the silicon processing waste water as claimed in claim 6, and said filtration unit is multi-medium filtering device or micro-filtration filtration unit; The filtrate of said multi-medium filtering device is silica sand, hard coal and cobble, and filtration velocity is 7.5~20m/h; Multi-medium filtering device WP≤0.6MPa, 0.04MPa≤water feeding pressure≤0.4MPa, back flushing water feeding pressure>=0.15MPa, inlet outlet pressure differential are 0.01~0.015MPa, back washing strength is 4~25L/ (sm), backwashing time 3~7min; The said condition that waste water is carried out filtering separation is WP≤0.6MPa, 0.04MPa≤water feeding pressure≤0.4MPa, back flushing water feeding pressure>=0.15MPa.
CN201110163091A 2011-06-15 2011-06-15 Device and method for recycling silicon powder in silicon processing waste water Pending CN102320701A (en)

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