CN102351362B - 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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- CN102351362B CN102351362B CN 201110225435 CN201110225435A CN102351362B CN 102351362 B CN102351362 B CN 102351362B CN 201110225435 CN201110225435 CN 201110225435 CN 201110225435 A CN201110225435 A CN 201110225435A CN 102351362 B CN102351362 B CN 102351362B
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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 aconcentration 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 to tail gas and raffinate, particularly to the treatment process of the chlorine-contained wastewater of the high density that produces.
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 as spray liquid to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains calcium chloride of a large amount of high densitys.Processing to this waste water at first is to enter plate-and-frame filter press to filter for the first time, and filtrate by adding lime slurry or salt acid for adjusting pH value to neutral, again enters afterwards plate-and-frame filter press and filters again, directly discharging after the filtrate that obtains clarifying.
2, adopt certain density lime slurry to carry out drip washing as spray liquid to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains calcium chloride of a large amount of high densitys.Processing to this waste water at first is to enter plate-and-frame filter press to filter for the first time, filtrate is again by adding lime slurry or salt acid for adjusting pH value to neutral, again entering afterwards plate-and-frame filter press filters, the filtrate that obtains clarifying enters the triple effect evaporation system and evaporates and separate out the calcium chloride crystal, again oven dry.
3, adopt certain density sodium hydroxide solution to carry out drip washing as spray liquid to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains sodium-chlor of a large amount of high densitys.Processing to this waste water is at first extremely neutral by 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 as spray liquid to tail gas and the raffinate that produces in the production of polysilicon, thereby produce the waste water that contains sodium-chlor of a large amount of high densitys.Processing to this waste water is at first extremely neutral by adding sodium hydroxide solution or salt acid for adjusting pH value, add polymerize aluminum chloride coagulating agent and polyacrylamide flocculant, afterwards clear liquid and precipitate and separate, obtain clarity and pH value sodium chloride solution up to standard and enter thin-film evaporator and carry out evaporative crystallization and process, obtain at last sodium chloride crystal.
There is corresponding problem separately in above-mentioned four kinds of operational paths.
1, the problem of the first technique existence mainly contains:
1. the damage to pressure filter is larger;
2. power consumption is larger;
3. has larger environmental protection risk.
Its reason mainly is: may there be acid-basicity in raw wastewater, directly enters the corrosion that the filter press chance causes filter cloth and filter plate; Repeatedly press filtration consumes the energy; High chloride ion-containing direct discharging of waste water affects environment.
2, the problem of the second technique existence mainly contains:
1. the damage to pressure filter is larger;
2. energy consumption is large, and cost is high.
Its reason mainly is: may there be acid-basicity in raw wastewater, directly enters 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 large.
3, the problem of the third technique existence mainly contains:
1. energy consumption is large, and cost is higher;
2. has larger environmental protection risk.
Its reason mainly is: the lower concentration brine waste is evaporated repeatedly until crystallization consumes than macro-energy; High chloride ion-containing direct discharging of waste water affects environment.
4, the problem of the 4th kind of technique existence mainly contains:
1. energy consumption is large, and cost is higher.
Its reason mainly is: evaporation is until crystallization repeatedly, and consumed energy is larger.
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 processing high chlorine-contained wastewater can make waste water energy as much as possible reuse or standard discharge after the processing, and produce high-quality by product-sodium chloride salt.
Technical scheme of the present invention is as follows:
The treatment process of high chloride ion-containing waste water 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 precipitation up to standard being gathered in high chloride ion-containing waste water in the pond; Specific targets are SS＜25mg/l, and pH is 6 ~ 9.
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 precipitation 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 having crystal to separate 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, filtrate recirculation evaporation.
Described pre-treatment refers to: at first add hydrochloric acid in high chloride ion-containing waste water, alkali lye is adjusted to neutrality with waste water.Specifically be controlled to be: be that 32% alkali lye carries out neutralizing treatment if high chloride ion-containing waste water for acid, then at first adds concentration in high chloride ion-containing waste water, 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 is 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.By above-mentioned measure, the pH value of high chloride ion-containing waste water is transferred to neutrality, adding afterwards concentration 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 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 larger bulk precipitation again; To condense at last has the high chloride ion-containing waste water of block precipitation to place settling bath to staticly settle, and clear liquid is separated with precipitation, obtains clarity SS＜25mg/l and pH value at 6 ~ 9 sodium chloride solution.
Concentrated described in the step B is to adopt reverse osmosis technology, and reverse osmosis technology is present advanced and effective 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 effectively remove magazines such as inorganic salts ion, colloid, bacterium, virus, bacterial endotoxin and most of organism in the water.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.Second-level reverse osmosis device effluent quality specific conductivity is generally at 2～5 μ S/cm.In step B, be exactly with sodium chloride solution by reverse osmosis membrane, enter the salt concentration of sodium-chlor concentrated solution of reverse osmosis membrane 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 method in all many-sides:
The a reverse osmosis is at ambient temperature, adopts the physical method without 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 process;
D discharges without chemical waste fluid, without the neutralizing treatment of spent acid alkali, non-environmental-pollution;
The e system is simple, and is easy to operate, the product water water conditioning;
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 again the fresh water treatment of low saline salinity;
G saves floor space;
H running maintenance and maintenance of equipment work amount are few.
When among the described step B precipitation being filtered be with pump delivery to special cell body, then pass through Filter Press; (add-on is that 1m3 sodium-chlor concentrated solution adds the ratio that the ratio of 10% PAC 4L and 1m3 sodium-chlor concentrated solution add 0.1% PAM solution 2L to add flocculating aids that complementary granular is arranged in the mud before filtration.By adding flocculating aids, the filtrate that can improve filtering rate or highly be clarified can be reduced filtration resistance, can prevent that the filter residue accumulation is too closely knit, and filtration is carried out smoothly; Suspended substance sedimentation speed in the precipitation can be accelerated; The mud that forms can be accelerated filtration velocity when press filtration.
Evaporation is that the sodium-chlor concentrated solution is passed in the vaporizer described in the step C, when having crystal to separate out saturated nacl aqueous solution is delivered to crystallizer tank, passes into recirculated cooling water and carries out crystallisation by cooling.During this time, adopt the continuously feeding operation, can reduce energy consumption.In the process of evaporation, 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 as follows:
The present invention optimizes the treatment process of the high chlorine-contained wastewater that produces in the production of polysilicon more, has solved the technical barrier that high chlorine-contained wastewater can't be processed, and waste water is turned waste into wealth, as far as possible reuse, saving water resource can produce the higher solid sodium chloride salt of quality, and relative cost reduces; Adopt to concentrate first the technique of evaporating afterwards, adopt vaporizer continuously feeding operation, make the very big lifting for the treatment of capacity and relatively save steam consumption, electric energy etc.; Satisfy the environmental protection demand fully, waste water can play significant social benefit near zero release.
Embodiment
The present invention is the treatment process of high chloride ion-containing waste water in a kind of production of polysilicon, operational path is: adopt sodium hydroxide as leacheate, form the waste water of chloride containing sodium salt, obtain the sodium chloride solution that clarity is very high, the pH value is neutral through overregulating the series of preprocessing techniques such as pH value, flocculation, precipitation, separation; Sodium chloride solution is realized the concentrated of sodium chloride solution, reuse water reuse by equipment series such as ultrafiltration, reverse osmosiss; Highly concentrated sodium chloride solution enters 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.
The 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 a large amount of high densitys.The water quality of this part waste water is carried out control on the source.Because the wastewater eluting acid-basicity disunity of elution circuit discharging, some is acid, and some is alkalescence, remittance will neutralize in the former pond time and separate out in a large number hydrolyzate, be very easy to stop up pond and pipeline, and alkaline water is discharged to three wastes operation, also caused to a certain extent the waste of raw material.So, control wastewater eluting water quality well, discharge this type of waste water when reacceesing neutrality to three wastes treatment process, when processing, comparatively easy like this.
In addition, as far as possible the stably manufactured system enters the chlorosilane tail gas amount of drip washing with minimizing.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 to the concrete treatment step of high chloride ion-containing waste water be:
(1) pre-treatment
The 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 a large amount of high densitys.This kind waste water ph is alkalescence or acid, and solid suspension content is larger, and millpond is collected specially.
Then in high chloride ion-containing waste water, add hydrochloric acid, alkali lye.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 and after the pH value 6 ~ 9; High chloride ion-containing waste water in the pond is alkalescence, then at first adds concentration and is 30% ~ 32% hydrochloric acid in high chloride ion-containing waste water 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.By above-mentioned control, the pH value of high chloride ion-containing waste water is transferred to neutrality, then adding concentration is that 9% ~ 12%(is generally 10%) polymerize aluminum chloride coagulating agent (add-on is controlled at the ratio that the former water of 1m3 adds 10% PAC 4L) make the suspended particle in the high chloride ion-containing waste water form alumen ustum, adding concentration is that 0.08% ~ 0.12%(is generally 0.1% again) polyacrylamide flocculant (add-on is controlled at the ratio that the former water of 1m3 adds 0.1% PAM solution 2L) make the alumen ustum in the high chloride ion-containing waste water condense into larger bulk precipitation; To condense at last has the high chloride ion-containing waste water of block precipitation to place settling bath to staticly settle, and supernatant liquor is separated with precipitation, obtains clarity SS＜25mg/l and pH value at 6 ~ 9 sodium chloride solution.
To special cell body, the entrance pressure filter filters precipitation with pump delivery.In filter operation, in order to reduce filtration resistance, a kind of complementary granular material that increase filtering rate or the filtrate of highly being clarified add is called flocculating aids.Flocculating aids can improve the filtrate 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) concentrated
The sodium chloride solution that produces after the pre-treatment enters 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 precipitation 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 by reverse osmosis membrane, removes bulk impurity, with the qualified water reuse or efflux the concentrated solution of remaining high density.
Enter concentrated former water and need substantially possess following salt concentration: the salt concentration of sodium-chlor concentrated solution is roughly at 7.0% ~ 9.5%wt.
(3) evaporative crystallization
The sodium-chlor concentrated solution entered in the vaporizer evaporate, adopt the operation of continuously feeding, to reduce energy consumption.When having crystal to separate out, saturated nacl aqueous solution is delivered to crystallizer tank, passes into recirculated cooling water and carry out crystallisation by cooling.In the process of evaporation, 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 filtrate enters 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 the higher moisture content of quality about 5% or following, the salt.Satisfy the environmental protection demand fully, waste water can play significant social benefit near zero release.
Claims (7)
1. the treatment process of high chloride ion-containing waste water 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 precipitation up to standard being gathered in high chloride ion-containing waste water in the pond, specific targets are SS＜25mg/l, and 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 precipitation filtered, obtain the waste residue of pie after the filtration;
C. the sodium-chlor concentrated solution that step B is obtained evaporates, and when having crystal to separate 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, filtrate recirculation evaporation;
Described pre-treatment refers to: 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 and 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 again polyacrylamide flocculant and make the alumen ustum in the high chloride ion-containing waste water condense into larger bulk precipitation; To condense at last has the high chloride ion-containing waste water of block precipitation to place settling bath to staticly settle, and supernatant liquor is separated with precipitation, obtains clarity SS＜25mg/l and pH value at 6 ~ 9 sodium chloride solution.
2. the treatment process of high chloride ion-containing waste water in the production of polysilicon according to claim 1, it is characterized in that: the polymerize aluminum chloride coagulant concentration of adding is 9% ~ 12%, and add-on is: 1m
3The ratio of the polymerize aluminum chloride 4L of high chloride ion-containing waste water adding 10%.
3. the treatment process of high chloride ion-containing waste water in the production of polysilicon according to claim 1, 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: 1m
3High chloride ion-containing waste water adding compound concentration is 0.1% polyacrylamide flocculant 2L.
4. the treatment process of high chloride ion-containing waste water in the production of polysilicon according to claim 1 is characterized in that: the concentrated reverse osmosis that adopts described in the step B, by reverse osmosis membrane, water sees through reverse osmosis membrane becomes pure water, i.e. reuse water with sodium chloride solution.
5. the treatment process of high chloride ion-containing waste water according to claim 1 or in the 4 described production of polysilicon is characterized in that: be to filter by plate-and-frame filter press when among the described step B precipitation being filtered; Mud before filtration is to add complementary flocculating aids is arranged, and add-on is: 1m
3The concentration of sodium-chlor concentrated solution adding 4L is 10% polymerize aluminum chloride and 1m
3The concentration of sodium-chlor concentrated solution adding 2L is 0.1% polyacrylamide flocculant solution.
6. the treatment process of high chloride ion-containing waste water in the production of polysilicon according to claim 1, it is characterized in that: evaporation is that the sodium-chlor concentrated solution is passed in the vaporizer described in the step C, when having crystal to separate out, saturated nacl aqueous solution is delivered to crystallizer tank, passes into recirculated cooling water and carry out crystallisation by cooling.
7. the treatment process of high chloride ion-containing waste water in the production of polysilicon according to claim 6, it is characterized in that: in the process of evaporation, 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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| CN103145150B (en) * | 2013-03-17 | 2015-01-28 | 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 |
| CN103466871B (en) * | 2013-08-22 | 2014-09-10 | 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 |
| 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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| BRPI0815245A2 (en) * | 2007-08-23 | 2015-03-31 | Dow Global Technologies Inc | Process for brine purification, process for reducing organic contamination of a brine stream in a chemical process, brine purification apparatus and chemical process apparatus for producing purified brine |
| CN101519259A (en) * | 2009-04-27 | 2009-09-02 | 南通金三角石墨制造有限公司 | Desalination process for waste water |
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