CN102351362A - Treatment method for waste water with high chloride ion content in polysilicon production - Google Patents
Treatment method for waste water with high chloride ion content in polysilicon production Download PDFInfo
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Abstract
The invention relates to a treatment method for waste water with high chloride ion content in polysilicon production. The treatment method comprises steps of: A. pretreating the waste water with high chloride ion content aggregated in the pool to obtain a sodium chloride solution with a clarification degree and a pH reaching standards and deposition; B. concentrating the sodium chloride solution to obtain 40-50% sodium chloride concentrate and 50-60% reuse water and filtering the deposition; C. carrying out evaporation crystallization on the sodium chloride solution to obtain a sodium chloride solid-liquid mixture; D. filtering and drying the sodium chloride solid-liquid mixture containing crystals to obtain high purity sodium chloride salt. The invention employs a technology containing a concentration before an evaporation to change waste into valuables, reuse and save water resource as possible and produce high quality solid sodium chloride salt; besides a relative cost, steam amount and electric energy are reduced and saved.
Description
Technical field
The present invention relates in the production of polysilicon treatment process, particularly to the treatment process of the chlorine-contained wastewater of the high density that produces to tail gas and raffinate.
Background technology
In the polysilicon process, can produce the waste water of chloride ion-containing.At present in the polysilicon industry, mainly contain following several operational path for the processing of chloride ion-containing waste water:
1, adopts certain density lime slurry to carry out drip washing to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains calcium chloride of great deal of high concentration as spray liquid.Processing to this waste water at first is to get into plate-and-frame filter press to filter for the first time, and filtrating through adding lime slurry or salt acid for adjusting pH value to neutral, gets into plate-and-frame filter press afterwards once more and filters again, obtains the directly discharging of clarifying filtrating back.
2, adopt certain density lime slurry to carry out drip washing to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains calcium chloride of great deal of high concentration as spray liquid.Processing to this waste water at first is to get into plate-and-frame filter press to filter for the first time; Filtrating is again through adding lime slurry or salt acid for adjusting pH value to neutral; Getting into plate-and-frame filter press afterwards once more filters; Obtaining clarifying filtrating gets into the triple effect evaporation system and evaporates and separate out the calcium chloride crystal, oven dry again.
3, adopt certain density sodium hydroxide solution to carry out drip washing to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains sodium-chlor of great deal of high concentration as spray liquid.Processing to this waste water is at first extremely neutral through adding sodium hydroxide solution or salt acid for adjusting pH value; Add polymerize aluminum chloride coagulating agent and polyacrylamide flocculant; Clear liquid and precipitate and separate obtain clarity and pH value sodium chloride solution up to standard afterwards, directly discharging.
4, adopt certain density sodium hydroxide solution to carry out drip washing to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains sodium-chlor of great deal of high concentration as spray liquid.Processing to this waste water is at first extremely neutral through adding sodium hydroxide solution or salt acid for adjusting pH value; Add polymerize aluminum chloride coagulating agent and polyacrylamide flocculant; Clear liquid and precipitate and separate afterwards; Obtain clarity and pH value sodium chloride solution entering thin-film evaporator up to standard and carry out the evaporative crystallization processing, obtain sodium chloride crystal at last.
There is corresponding problem separately in above-mentioned four kinds of operational paths.
1, the problem of first kind of technology existence mainly contains:
1. the damage to pressure filter is bigger;
2. power consumption is bigger;
3. has bigger environmental protection risk.
Its reason mainly is: possibly there is acid-basicity in raw wastewater, directly gets into the corrosion that the filter press chance causes filter cloth and filter plate; Press filtration repeatedly, consumes energy; High chloride ion-containing direct discharging of waste water influences environment.
2, the problem of second kind of technology existence mainly contains:
1. the damage to pressure filter is bigger;
2. energy consumption is big, and cost is high.
Its reason mainly is: possibly there is acid-basicity in raw wastewater, directly gets into the corrosion that the filter press chance causes filter cloth and filter plate; Press filtration and evaporative crystallization follow-up equipment are many repeatedly, and energy consumption is big.
3, the problem of the third technology existence mainly contains:
1. energy consumption is big, and cost is higher;
2. has bigger environmental protection risk.
Its reason mainly is: the lower concentration brine waste is evaporated until crystallization repeatedly, consume than macro-energy; High chloride ion-containing direct discharging of waste water influences environment.
4, the problem of the 4th kind of technology existence mainly contains:
1. energy consumption is big, and cost is higher.
Its reason mainly is: evaporate repeatedly until crystallization, consumed energy is bigger.
Summary of the invention
The present invention provides in production of polysilicon for solving the problems of the technologies described above, and a kind of method of handling high chlorine-contained wastewater can make waste water reuse or standard discharge as much as possible after the processing, and produce high-quality by product-sodium chloride salt.
Technical scheme of the present invention is following:
High chloride ion-containing wastewater treatment method in the production of polysilicon is characterized in that treatment step is:
A. carry out pre-treatment and obtain clarity and pH value sodium chloride solution and deposition up to standard accumulating in high chloride ion-containing waste water in the pond; Specific targets are that < 25mg/>l, pH is 6 ~ 9 for SS.
B. the sodium chloride solution that steps A is obtained concentrates, and makes the concentration lifting at double of sodium chloride solution, obtains 40% ~ 50% sodium-chlor concentrated solution, 50% ~ 60% reuse water; And deposition filtered, obtaining the waste residue of pie after the filtration, main component is silicon-dioxide, water glass, Starso, sodium-chlor etc.;
C. the sodium-chlor concentrated solution that step B is obtained evaporates, and when crystal is separated out, saturated nacl aqueous solution is carried out crystallisation by cooling and obtains the sodium-chlor solidliquid mixture;
D. the sodium-chlor solidliquid mixture that contains xln that step C is obtained filters and dries up, and filters out the sodium chloride crystal particle, forms sodium chloride salt, filtrating recirculation evaporation.
Said pre-treatment is meant: at first in high chloride ion-containing waste water, add hydrochloric acid, alkali lye is adjusted to neutrality with waste water.Specifically be controlled to be: if high chloride ion-containing waste water for acid, then at first adds concentration in high chloride ion-containing waste water is that 32% alkali lye carries out neutralizing treatment, and add-on is carried out interlocked control by alkali lye volume pump and pH meter, guarantee in the waste water and after the pH value 6 ~ 9; If high chloride ion-containing waste water be alkalescence, then at first in high chloride ion-containing waste water, add concentration and be 30% hydrochloric acid and carry out neutralizing treatment, add-on is carried out interlocked control by hydrochloric acid volume pump and pH meter, guarantee in the waste water and after the pH value 6 ~ 9.In this reaction process, envrionment temperature and air pressure there are not particular requirement, normal temperature, normal pressure get final product.Through above-mentioned measure; The pH value of high chloride ion-containing waste water is transferred to neutrality; Adding concentration afterwards is that 10% polymerize aluminum chloride coagulating agent (add-on is controlled at the ratio of the PAC 4L of the high chloride ion-containing waste water adding 10% of 1m3) makes the suspended particle in the high chloride ion-containing waste water form alumen ustum, and adding concentration again is that 0.1% polyacrylamide flocculant (add-on is controlled at the ratio of the PAM solution 2L of the high chloride ion-containing waste water adding 0.1% of 1m3) makes the alumen ustum in the high chloride ion-containing waste water condense into bigger bulk deposition; To condense at last has block sedimentary high chloride ion-containing waste water to place settling bath to staticly settle, and clear liquid is separated with deposition, and < 25mg/>l and pH value are at 6 ~ 9 sodium chloride solution to obtain clarity SS.
Concentrating described in the step B is the employing reverse osmosis technology, and reverse osmosis technology is advanced and effective at present desalination technology.Reverse osmosis is the water technology that adopts membrane separating, and its principle is under pressure, and water sees through reverse osmosis membrane becomes pure water; Impurity in the water is held back by reverse osmosis membrane and is taken out of by dense water.Utilize reverse osmosis technology can remove the magazines such as inorganic salts ion, colloid, bacterium, virus, bacterial endotoxin and most of organism in the water effectively.Reverse osmosis system desalination rate is generally 95～99%.First-stage reverse osmosis equipment water outlet resistivity is generally between 0.05～0.5M Ω cm.Two-pass reverse osmosis equipment effluent quality specific conductivity is generally at 2～5 μ S/cm.In step B, be exactly that sodium chloride solution is passed through reverse osmosis membrane, the salt concentration of the sodium-chlor concentrated solution of entering reverse osmosis membrane is roughly at 7.0% ~ 9.5%wt.
Reverse osmosis technology is to belong to physical method basically, and its desalting process has the unexistent excellent characteristics of traditional water treatment process aspect many:
The a reverse osmosis is at ambient temperature, adopts the physical method of no phase transformation to get so that water is desalinated, purifying;
The processing of b water only relies on the pressure of water as impellent, and its energy consumption is minimum in many treatment processs;
C need not be a large amount of chemical agent and acid-alkali regeneration handle;
D does not have chemical waste fluid discharging, the neutralizing treatment of no spent acid alkali, non-environmental-pollution;
The e system is simple, and is easy to operate, the product water quality stabilizing;
F is adapted to raw water quality in a big way, both has been applicable to brackish water, seawater so that the processing of sewage, is adapted to the fresh water treatment of low saline salinity again;
G saves floor space;
H running maintenance and maintenance of equipment work amount are few.
When among the said step B deposition being filtered be with pump delivery to special cell body, filter through pressure filter then; Add in the mud before filtration complementary powder granulous flocculating aids arranged that (add-on is that 1m3 sodium-chlor concentrated solution adds the ratio of 10% PAC 4L and the ratio of the PAM solution 2L of 1m3 sodium-chlor concentrated solution adding 0.1%.Through adding flocculating aids, can improve filtering rate or obtain highly clarifying filtrating, can reduce filtration resistance, can prevent that the filter residue accumulation is too closely knit, filtration is carried out smoothly; Suspended substance sedimentation speed in the deposition can be accelerated; The mud that forms can be accelerated filtration velocity when press filtration.
Evaporation described in the step C is that the sodium-chlor concentrated solution is fed in the vaporizer, when crystal is separated out, saturated nacl aqueous solution is delivered to crystallizer tank, feeds recirculated cooling water and carries out crystallisation by cooling.During this time, adopt the continuously feeding operation, can cut down the consumption of energy.In evaporating course; Need control vaporizer internal gas pressure at-90 ~-98 KPa, temperature of charge is controlled at 27 ~ 40 ℃ in the vaporizer, adopts forced circulation evaporation; When circulating-pump outlet not timing sampling is found to have xln to separate out, saturated solution is delivered to crystallizer tank carries out crystallisation by cooling.
Technique effect of the present invention is following:
The present invention optimizes the treatment process of the high chlorine-contained wastewater that produces in the production of polysilicon more, and having solved high chlorine-contained wastewater can't a Treatment Technology difficult problem, and waste water is turned waste into wealth; Reuse as far as possible; The conserve water resource can produce the higher solid sodium chloride salt of quality, and relative cost reduces; Adopt to concentrate earlier the technology of afterwards evaporating, employing vaporizer continuously feeding operation greatly promotes treatment capacity and relative steam consumption, the electric energy etc. saved; Satisfy the environmental protection demand fully, waste water can play remarkable social benefit near zero release.
Embodiment
The present invention is a high chloride ion-containing wastewater treatment method in a kind of production of polysilicon; Operational path is: adopt sodium hydroxide as leacheate; Form the waste water of sodium chloride-containing salt, obtain through overregulating series of preprocessing technologies such as pH value, flocculation, deposition, separation that clarity is very high, pH value neutral sodium chloride solution; Sodium chloride solution is realized the concentrated of sodium chloride solution, reuse water reuse through equipment series such as ultrafiltration, reverse osmosiss; Highly spissated sodium chloride solution gets into the vaporizer circulating and evaporating, and precipitated sodium chloride crystal crystallisation by cooling is Plate Filtration again, obtains the higher sodium chloride salt solid particulate of purity.
Tail gas that produces in the production of polysilicon and raffinate adopt certain density sodium hydroxide solution to carry out drip washing as spray liquid, thereby produce the waste water that contains sodium-chlor of great deal of high concentration.Water quality to this part waste water is carried out the control on the source.Because the wastewater eluting acid-basicity disunity of elution circuit discharging, some is acid, and some is alkalescence; Will neutralize when converging in former pond and separate out hydrolyzate in a large number; Be very easy to stop up pond and pipeline, and alkaline water is discharged to three wastes operation, also caused the waste of raw material to a certain extent.So, control wastewater eluting water quality well, discharge this type of waste water to three wastes treatment process when reacceesing neutrality, when handling, comparatively easy like this.
In addition, try one's best the stably manufactured system to reduce the chlorosilane tail gas amount that gets into drip washing.Drip washing tail gas amount reduces, and the alkali lye consumption reduces on the one hand, and chloride ion content reduces in the wastewater eluting on the other hand, and is when three wastes operation dechlorinates processing, comparatively easy like this.
Therefore the concrete treatment step to high chloride ion-containing waste water is:
(1) pre-treatment
Tail gas that produces in the production of polysilicon and raffinate adopt certain density sodium hydroxide solution to carry out drip washing as spray liquid, thereby produce the waste water that contains sodium-chlor of great deal of high concentration.This kind waste water ph is alkalescence or acid, and solid suspension content is bigger, and millpond is collected specially.
In high chloride ion-containing waste water, add hydrochloric acid, alkali lye then.Specifically be controlled to be: the high chloride ion-containing waste water in the pond is for acid; Then at first in high chloride ion-containing waste water, add concentration and be 30% ~ 32% alkali lye and carry out neutralizing treatment; Add-on is carried out interlocked control by alkali lye volume pump and pH meter, guarantee in the waste water with after the pH value 6 ~ 9; High chloride ion-containing waste water in the pond is alkalescence, then at first in high chloride ion-containing waste water, adds concentration and is 30% ~ 32% hydrochloric acid and carry out neutralizing treatment, and add-on is carried out interlocked control by hydrochloric acid volume pump and pH meter, guarantee in the waste water and after the pH value 6 ~ 9.In this reaction process, envrionment temperature and air pressure there are not particular requirement, normal temperature, normal pressure get final product.Through above-mentioned control; The pH value of high chloride ion-containing waste water is transferred to neutrality; The polymerize aluminum chloride coagulating agent (add-on is controlled at the ratio that the former water of 1m3 adds 10% PAC 4L) that adds concentration then and be 9% ~ 12% (being generally 10%) makes the suspended particle in the high chloride ion-containing waste water form alumen ustum, and the polyacrylamide flocculant (add-on is controlled at the ratio that the former water of 1m3 adds 0.1% PAM solution 2L) that adds concentration again and be 0.08% ~ 0.12% (being generally 0.1%) makes the alumen ustum in the high chloride ion-containing waste water condense into bigger bulk deposition; To condense at last has block sedimentary high chloride ion-containing waste water to place settling bath to staticly settle, and supernatant liquor is separated with deposition, and < 25mg/>l and pH value are at 6 ~ 9 sodium chloride solution to obtain clarity SS.
To special cell body, the entrance pressure filter filters deposition with pump delivery.In filter operation, in order to reduce filtration resistance, increase filtering rate or obtain a kind of complementary powder shape material that highly clarifying filtrating adds, be called flocculating aids.Flocculating aids can improve the filtrating filtration efficiency, can prevent that the filter residue accumulation is too closely knit, and filtration is carried out smoothly.Introduce flocculating aids, the suspended substance sedimentation speed in the waste water can be accelerated; The mud that forms can be accelerated filtration velocity when press filtration.
(2) concentrate
The sodium chloride solution that produces after the pre-treatment gets into concentration systems, and wherein sodium-chlor is concentrated, and makes the concentration lifting at double of sodium chloride solution, obtains 40% ~ 50% sodium-chlor concentrated solution, 50% ~ 60% reuse water; And deposition filtered, obtaining the waste residue of pie after the filtration, main component is silicon-dioxide, water glass, Starso, sodium-chlor etc.;
Concentration technology adopts reverse osmosis technology, exactly sodium chloride solution is concentrated through reverse osmosis membrane, removes bulk impurity, with the qualified water reuse or efflux the concentrated solution of remaining high density.
Get into spissated former water and need possess following salt concentration basically: the salt concentration of sodium-chlor concentrated solution is roughly at 7.0% ~ 9.5%wt.
(3) evaporative crystallization
With evaporating in the sodium-chlor concentrated solution entering vaporizer, adopt the operation of continuously feeding, to cut down the consumption of energy.When crystal is separated out, saturated nacl aqueous solution is delivered to crystallizer tank, feeds recirculated cooling water and carry out crystallisation by cooling.In evaporating course; Need control vaporizer internal gas pressure at-90KPa ~-98 KPa, temperature of charge is controlled at 27 ~ 40 ℃ in the vaporizer, adopts forced circulation evaporation; When circulating-pump outlet not timing sampling is found to have xln to separate out, saturated solution is delivered to crystallizer tank carries out crystallisation by cooling.
(4) press filtration
The sodium-chlor solidliquid mixture that will contain xln is delivered to pressure filter and filters and dry up, and filters out the sodium chloride crystal particle, forms sodium chloride salt, and filtrating gets into storage tank recirculation evaporation.
After the processing, waste water can be turned waste into wealth, obtain every day more than reuse water 50 sides, can produce the solid sodium chloride salt of content more than 95% of sodium-chlor in higher moisture content of quality about 5% or following, the salt.Satisfy the environmental protection demand fully, waste water can play remarkable social benefit near zero release.
Claims (8)
1. high chloride ion-containing wastewater treatment method in the production of polysilicon is characterized in that treatment step is:
A. carry out pre-treatment and obtain clarity and pH value sodium chloride solution and deposition up to standard accumulating in high chloride ion-containing waste water in the pond, specific targets be SS 25mg/l, pH is 6 ~ 9;
B. the sodium chloride solution that steps A is obtained concentrates, and obtains 40% ~ 50% sodium-chlor concentrated solution and 50% ~ 60% reuse water; And deposition filtered, obtain the waste residue of pie after the filtration;
C. the sodium-chlor concentrated solution that step B is obtained evaporates, and when crystal is separated out, saturated nacl aqueous solution is carried out crystallisation by cooling and obtains the sodium-chlor solidliquid mixture;
D. the sodium-chlor solidliquid mixture that contains xln that step C is obtained filters and dries up, and filters out the sodium chloride crystal particle, forms sodium chloride salt, filtrating recirculation evaporation.
2. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 1; It is characterized in that: said pre-treatment is meant: when the high chloride ion-containing waste water in the pond is acidity; At first in high chloride ion-containing waste water, add concentration and be 30% ~ 32% alkali lye and carry out neutralizing treatment; Add-on is carried out interlocked control by alkali lye volume pump and pH meter, guarantee in the waste water with after the pH value 6 ~ 9; When the high chloride ion-containing waste water in the pond is when alkalescence, at first in high chloride ion-containing waste water, add concentration and be 30% ~ 32% hydrochloric acid and carry out neutralizing treatment, add-on is carried out interlocked control by hydrochloric acid volume pump and pH meter, guarantee in the waste water and after the pH value 6 ~ 9;
After the pH value of high chloride ion-containing waste water transferred to neutrality, add the polymerize aluminum chloride coagulating agent and make the suspended particle in the high chloride ion-containing waste water form alumen ustum, add polyacrylamide flocculant again and make the alumen ustum in the high chloride ion-containing waste water condense into bigger bulk deposition; To condense at last has block sedimentary high chloride ion-containing waste water to place settling bath to staticly settle, and supernatant liquor is separated with deposition, and < 25mg/>l and pH value are at 6 ~ 9 sodium chloride solution to obtain clarity SS.
3. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 2; It is characterized in that: the polymerize aluminum chloride coagulant concentration of adding is 9% ~ 12%, and add-on is: the ratio of the polymerize aluminum chloride 4L of the high chloride ion-containing waste water adding 10% of 1m3.
4. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 2; It is characterized in that: the polyacrylamide flocculant of adding is the white powder material; Anionic; Molecular weight is more than 8,000,000; Adding clear water, to be mixed with concentration be 0.08% ~ 0.12% solution, and add-on is: it is 0.1% polyacrylamide flocculant 2L that the high chloride ion-containing waste water of 1m3 adds compound concentration.
5. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 1 is characterized in that: concentrate described in the step B and adopt reverse osmosis, through reverse osmosis membrane, water sees through reverse osmosis membrane becomes pure water, i.e. reuse water with sodium chloride solution.
6. according to high chloride ion-containing wastewater treatment method in claim 1 or the 5 described production of polysilicon, it is characterized in that: when among the said step B deposition being filtered is to filter through plate-and-frame filter press; Mud before filtration is to add complementary flocculating aids is arranged, and add-on is: the concentration that 1m3 sodium-chlor concentrated solution adds 4L is that the concentration of 10% polymerize aluminum chloride and 1m3 sodium-chlor concentrated solution adding 2L is 0.1% polyacrylamide flocculant solution.
7. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 1; It is characterized in that: evaporation described in the step C is that the sodium-chlor concentrated solution is fed in the vaporizer; When crystal is separated out, saturated nacl aqueous solution is delivered to crystallizer tank, feeds recirculated cooling water and carry out crystallisation by cooling.
8. high chloride ion-containing wastewater treatment method in the production of polysilicon according to claim 7; It is characterized in that: in evaporating course; The vaporizer internal gas pressure is :-90KPa ~-98 KPa; Temperature of charge is in the vaporizer: 27 ~ 40 ℃; Adopt forced circulation evaporation; When circulating-pump outlet not timing sampling is found to have xln to separate out, saturated solution is delivered to crystallizer tank carries out crystallisation by cooling.
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| CN103145150A (en) * | 2013-03-17 | 2013-06-12 | 上虞市佳和化工有限公司 | Technology and device for recycling sodium chloride from wastewater generated in process of producing silica sol by ion exchange method |
| CN103466871A (en) * | 2013-08-22 | 2013-12-25 | 苏州苏净环保工程有限公司 | Treatment method and recycling system for industrial wastewater of polycrystalline silicon batteries |
| CN104291523A (en) * | 2014-09-18 | 2015-01-21 | 波鹰(厦门)科技有限公司 | Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater |
| CN106082519A (en) * | 2016-08-12 | 2016-11-09 | 安徽皖维高新材料股份有限公司 | A kind of polyvinyl alcohol produces the recovery and treatment method of waste liquid |
| CN108911343A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Polysilicon zero emission method of wastewater and system |
| CN111087115A (en) * | 2019-12-31 | 2020-05-01 | 四川永祥多晶硅有限公司 | Polycrystalline silicon wastewater treatment method and wastewater treatment system |
| CN113772873A (en) * | 2021-10-09 | 2021-12-10 | 北部湾大学 | Method for preparing industrial salt from pickling waste liquid by using waste heat |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104291523A (en) * | 2014-09-18 | 2015-01-21 | 波鹰(厦门)科技有限公司 | Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater |
| CN106082519A (en) * | 2016-08-12 | 2016-11-09 | 安徽皖维高新材料股份有限公司 | A kind of polyvinyl alcohol produces the recovery and treatment method of waste liquid |
| CN108911343A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Polysilicon zero emission method of wastewater and system |
| CN111087115A (en) * | 2019-12-31 | 2020-05-01 | 四川永祥多晶硅有限公司 | Polycrystalline silicon wastewater treatment method and wastewater treatment system |
| CN113772873A (en) * | 2021-10-09 | 2021-12-10 | 北部湾大学 | Method for preparing industrial salt from pickling waste liquid by using waste heat |
| CN113772873B (en) * | 2021-10-09 | 2023-08-25 | 北部湾大学 | Method for preparing industrial salt from pickling waste liquid by utilizing waste heat |
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| CN102351362B (en) | 2013-04-10 |
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