CN103936218B - The high fluorine-containing nitrogenous wastewater from battery production of a kind of photovoltaic industry becomes the method for zero release - Google Patents
The high fluorine-containing nitrogenous wastewater from battery production of a kind of photovoltaic industry becomes the method for zero release Download PDFInfo
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- Y—GENERAL 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
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Abstract
The invention discloses the high fluorine-containing nitrogenous wastewater from battery production of a kind of photovoltaic industry to become the method for zero release, first fluorine-containing for height nitrogenous wastewater from battery production is sent into equalizing tank homogeneous; Enter except fluorine reaction tank again, reaction tank water outlet enters settling tank; Settling tank supernatant liquor enters intermediate pool; Again through quartz filter and activated charcoal filter, fresh water enters into the process of first-stage reverse osmosis film; The dense water of reverse osmosis membrane accelerates crystallizing pond through the induction of overrich water, the calcium ion in dense water and fluorion is made to accelerate to form precipitation on crystal seed, effectively reduce calcium ion and fluorinion concentration, to improve the cycles of concentration of reverse osmosis concentration film, supernatant liquor is by cartridge filter, then entering into reverse osmosis concentration film, to carry out circulation concentrated; The a small amount of dense water of reverse osmosis concentration film enters vaporizer, and greatly reduce the expense needed for evaporation, steam condensate enters into reuse pool, and fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste.Not discharge water pollutent in whole process.
Description
Technical field
The invention belongs to sewage treatment project field, relate to the high fluorine-containing nitrogenous effluent defluorinate of a kind of photovoltaic industry, denitrogenation and reuse, and realize the method for zero release.
Background technology
China is one of whole world country that water resources is the poorest per capita.And Industrial Economic Development is while creation great wealth, cause immense pressure also to local resources environment, water environment pollution is particularly serious, exploitation advanced treatment of industrial waste water and reuse technology demand very urgent.Although the photovoltaic energy is green energy resource, still there is more serious water pollutions in photovoltaic cell production process.Photovoltaic cell produce different workshop sections generally born by different enterprises, discharge mainly contain production of polysilicon waste water (main component is nitric acid, hydrofluoric acid), silicon chip cutting wastewater (principal pollutant composition is polyoxyethylene glycol), photovoltaic cell factory effluent (main component is nitric acid, hydrofluoric acid) etc.The technological process of production that photovoltaic cell is produced is as follows: Wafer Cleaning → surface wool manufacturing → phosphorous diffusion → trimming → phosphorosilicate glass removal → antireflective coating preparation → silk screen printing → sintering → test and classify, and technique adopts HF-HNO
3system chemical method for etching, waste water principal pollutant are fluorochemical and nitrate nitrogen, and usual nitrate nitrogen concentration is greater than 200mg/L, and fluorinion concentration is greater than 500mg/L, need could meet reuse requirement except after fluorine and denitrogenation.
Evaporation technique can realize the zero release of waste water, but its quantity of steam or current consumption are greatly, and working cost is high, and fluorion has very strong corrodibility to evaporation equipment.For high fluoride waste, calcium salt precipitation method effectively can remove fluorion, and process is convenient, low cost.Reverse osmosis technology ratio of desalinization is high, it is the effective technology of Sewage advanced treatment and reuse, conventional reverse osmosis technique can reach the wastewater recycle rate of 70%, 30% dense water is through pervaporation denitrogenation, and utilize reverse osmosis membrane, effluent quality is excellent, can be used as process water water source, realize reuse completely, the denitrogenation of reverse osmosis membrane dense water conservancy evaporation technique, realizes the zero release of waste water.But, still there is multiple key technical problem in reverse osmosis process, larger pollution is there is in the excessive calcium ion that one Shi Qian road defluorinating process brings to reverse osmosis membrane, fouling membrane can make film device be difficult to normal operation, decelerating membrane pollution is the difficult point of membrane concentration, wherein reducing fluorinion in waste water and calcium ion etc. easily causes the material concentration of film fouling to be crucial, and fouling membrane is the key factor affecting reverse osmosis membrane technology popularization; Even if two be achieve 70% waste water reclamation rate, still have the waste water of 30% need evaporate.Therefore, how employing new technology, reduce waste water evaporated water, reduce the running cost of wastewater zero discharge process, is that high fluorine-containing nitrogenous photovoltaic cell factory effluent zero release can the key of practical application.
Summary of the invention
For the problems referred to above existed in nitrogenous photovoltaic cell production wastewater treatment method fluorine-containing in prior art, the invention provides the high fluorine-containing nitrogenous wastewater from battery production of a kind of photovoltaic industry and to become the novel method of zero release.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry becomes the method for zero release, comprises the steps:
(1) first fluorine-containing for height nitrogenous wastewater from battery production is sent into equalizing tank homogeneous;
(2) enter again except fluorine reaction tank, add calcium hydroxide wherein, regulate wastewater pH to 8 ~ 9, fluorion and calcium ion is made to form calcium fluoride precipitate, then add coagulating agent and flocculation agent successively, reaction tank water outlet enters settling tank, and the outer row of precipitation is as sludge treatment, supernatant liquor enters intermediate pool, adds sulphuric acid soln and regulates wastewater pH to 7 ~ 8;
(3) again through quartz filter and activated charcoal filter, remove suspended impurity and the organic impurities of larger particles in waste water respectively, water outlet after filtration is first by ultrafiltration membrane treatment, and the dense water of ultra-filtration membrane gets back to equalizing tank, and fresh water enters into the process of first-stage reverse osmosis film;
(5) first-stage reverse osmosis film fresh water delivers to reuse pool, and dense water accelerates crystallizing pond through the induction of overrich water, adds induction crystal seed wherein, makes the calcium ion in dense water and fluorion accelerate to form precipitation on crystal seed;
(6) supernatant liquor passes through cartridge filter, enter into again reverse osmosis concentration film carry out circulation concentrate, namely reuse pool is delivered in the water outlet of reverse osmosis concentration film, the concentrated dense water of film again enters the induction of dense water and accelerates crystallizing pond acceleration sofening treatment, pass through cartridge filter, fill cycle as reverse osmosis concentration film uses, until when effluent index is about to higher than industrial reuse water-quality guideline, stops circulation concentrated;
(7) the dense water of reverse osmosis concentration film enters vaporizer again and evaporates, and steam condensate enters into reuse pool, and fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste.Not discharge water pollutent in whole process.
In described step (2), the supernatant liquor of settling tank enters intermediate pool successively after deliming reaction tank and second-level settling pond, concrete steps are: the supernatant liquor of settling tank enters deliming reaction tank, add sodium carbonate wherein, the calcium ion unnecessary with prime forms precipitation of calcium carbonate, then adds flocculation agent, and water outlet enters second-level settling pond, the outer row of precipitation is as sludge treatment, and second-level settling pond supernatant liquor enters intermediate pool.
Wherein, the fluorine-containing nitrogenous wastewater from battery production of described height is the photovoltaic industry wastewater from battery production of nitrate nitrogen concentration >200mg/L and fluorinion concentration >500mg/L.
Wherein, described ultra-filtration membrane is hollow-fibre membrane, tubular membrane or flat sheet membrane.
Wherein, described induction is accelerated crystallizing pond and is divided into reaction zone and settling region, adds and have induced crystallization crystal seed in reaction zone, and the crystal seed in settling region under precipitation is back to reaction zone, settling region supernatant liquor water outlet.
Wherein, described crystal seed is calcite sand or quartz sand, and particle diameter is 50 order ~ 500 orders.
Wherein, described cartridge filter, filtering accuracy is less than or equal to 5 μm.
Wherein, described reverse osmosis concentration film is sea water desalination membrane or low pressure high desalination reverse osmosis membrane.
Beneficial effect of the present invention:
Present method adopts dense water to induce and accelerates crystallization, the calcium ion in the dense water of reverse osmosis membrane and fluorion is made to form precipitation on induced crystallization crystal seed, and be efficiently removed, reduce the possibility of fouling membrane, improve the cycles of concentration of reverse osmosis concentration film, accelerate the dense water of crystallization through induction to enter into reverse osmosis concentration film again to carry out circulation concentrated, the waste water total yield of membranous system is made to reach more than 90%, namely the wastewater from battery production amount entering vaporizer cuts down more than 90%, thus the expense greatly reduced needed for evaporation, and make high fluorine-containing nitrogenous wastewater from battery production zero release.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The high fluorine-containing nitrogenous wastewater from battery production of a kind of photovoltaic industry of the present invention become zero release method technical process as shown in Figure 1, comprise the steps:
(1) first fluorine-containing for height nitrogenous wastewater from battery production is sent into equalizing tank homogeneous;
(2) enter again except fluorine reaction tank, add calcium hydroxide wherein, regulate wastewater pH to 8 ~ 9, fluorion and calcium ion is made to form calcium fluoride precipitate, then add polymerize aluminum chloride and polyacrylamide coagulation successively, reaction tank water outlet enters settling tank, and the outer row of precipitation is as sludge treatment;
(3) supernatant liquor enters deliming reaction tank, adds sodium carbonate wherein, and the calcium ion unnecessary with prime forms precipitation of calcium carbonate, then adds polyacrylamide flocculant, and water outlet enters second-level settling pond, and the outer row of precipitation is as sludge treatment;
(4) second pond supernatant liquor enters intermediate pool, adds sulphuric acid soln and regulates wastewater pH to 7 ~ 8; Again through quartz filter and activated charcoal filter, remove suspended impurity and the organic impurities of larger particles in waste water respectively, the water outlet after filtration is first by ultrafiltration membrane treatment, and the dense water of ultra-filtration membrane gets back to equalizing tank, and fresh water enters into the process of first-stage reverse osmosis film;
(5) first-stage reverse osmosis film fresh water delivers to reuse pool, and dense water accelerates crystallizing pond through the induction of overrich water, adds induction crystal seed wherein, makes the calcium ion in dense water and fluorion accelerate to form precipitation on crystal seed.
(6) supernatant liquor passes through cartridge filter, enter into again reverse osmosis concentration film carry out circulation concentrate, namely reuse pool is delivered in the water outlet of reverse osmosis concentration film, the concentrated dense water of film again enters the induction of dense water and accelerates crystallizing pond acceleration sofening treatment, pass through cartridge filter, fill cycle as reverse osmosis concentration film uses, until when effluent index is about to higher than industrial reuse water-quality guideline, stops circulation concentrated.
(7) the dense water of reverse osmosis concentration film enters vaporizer again and evaporates, and steam condensate enters into reuse pool, and fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste.Not discharge water pollutent in whole process.
As preferred version of the present invention, wherein, high fluorine-containing nitrogenous wastewater from battery production is the photovoltaic industry wastewater from battery production of nitrate nitrogen concentration >200mg/L and fluorinion concentration >500mg/L; Ultra-filtration membrane is hollow-fibre membrane, tubular membrane or flat sheet membrane; Induction is accelerated crystallizing pond and is divided into reaction zone and settling region, adds and have induced crystallization crystal seed in reaction zone, and the crystal seed in settling region under precipitation is back to reaction zone, settling region supernatant liquor water outlet; Crystal seed is calcite sand or quartz sand, and particle diameter is 50 order ~ 500 orders; Cartridge filter, filtering accuracy is less than or equal to 5 μm; Reverse osmosis concentration film is sea water desalination membrane or low pressure high desalination reverse osmosis membrane.
Contrast case (using fluorine-containing nitrogenous photovoltaic cell production wastewater treatment method of the prior art):
The high fluorine-containing nitrogenous wastewater from battery production of certain photovoltaic industry, water quality characteristic is as follows: NO
3 --N460mg/L, F
-1100mg/L, specific conductivity 2920 μ s/cm.Fluorine-containing for height nitrogenous wastewater from battery production as shown in Figure 1, is first sent into equalizing tank homogeneous by wastewater treatment concrete technology flow process; Enter except fluorine reaction tank again, add calcium hydroxide wherein and regulate wastewater pH to 8.5, make fluorion and calcium ion form calcium fluoride precipitate, then add polymerize aluminum chloride and polyacrylamide coagulation successively, reaction tank water outlet enters settling tank, and the outer row of precipitation is as sludge treatment; Supernatant liquor enters intermediate pool, adds sulphuric acid soln and regulates wastewater pH to 7.5; Again through quartz filter and activated charcoal filter, remove suspended impurity and the organic impurities of larger particles in waste water respectively, water outlet after filtration is first by hollow fiber ultrafiltration membrane process, the dense water of ultra-filtration membrane gets back to equalizing tank, fresh water enters into the process of first-stage reverse osmosis film, first-stage reverse osmosis film waste water reclamation rate is 60%, dense water (i.e. raw wastewater 40%) enters vaporizer and evaporates, steam condensate enters into reuse pool, fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste.Not discharge water pollutent in whole process.
The removal efficiency of principal pollutant index is in table 1.
Table 1 technique unit removal efficiency table
Case study on implementation (use the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry of the present invention become the method for zero release):
The high fluorine-containing nitrogenous wastewater from battery production of certain photovoltaic industry, water quality characteristic is as follows: NO
3 --N460mg/L, F
-1100mg/L, specific conductivity 2920 μ s/cm.Fluorine-containing for height nitrogenous wastewater from battery production as shown in Figure 1, is first sent into equalizing tank homogeneous by wastewater treatment concrete technology flow process; Enter except fluorine reaction tank again, add calcium hydroxide wherein and regulate wastewater pH to 8.5, make fluorion and calcium ion form calcium fluoride precipitate, then add polymerize aluminum chloride and polyacrylamide coagulation successively, reaction tank water outlet enters settling tank, and the outer row of precipitation is as sludge treatment; Supernatant liquor enters deliming reaction tank, add enough sodium carbonate wherein, the calcium ion unnecessary with prime forms precipitation of calcium carbonate, add polyacrylamide flocculant again, water outlet enters second-level settling pond, the outer row of precipitation is as sludge treatment, and second pond supernatant liquor enters intermediate pool, adds sulphuric acid soln and regulates wastewater pH to 7.5; Again through quartz filter and activated charcoal filter, remove suspended impurity and the organic impurities of larger particles in waste water respectively, water outlet after filtration is first by hollow fiber ultrafiltration membrane process, the dense water of ultra-filtration membrane gets back to equalizing tank, fresh water enters into the process of first-stage reverse osmosis film, and first-stage reverse osmosis film waste water reclamation rate is 70%; Reverse osmosis membrane fresh water delivers to reuse pool, dense water accelerates crystallizing pond through the induction of overrich water, wherein add and have the 100 order calcite sand of 10g/L as induction crystal seed, make the calcium ion in dense water and fluorion accelerate to form precipitation on crystal seed, supernatant liquor is the cartridge filter of 5 μm by precision; Enter into again reverse osmosis concentration film carry out circulation concentrate, namely reuse pool is delivered in the water outlet of reverse osmosis concentration film, the concentrated dense water of film again enters the induction of dense water and accelerates crystallizing pond acceleration sofening treatment, and by cartridge filter, the fill cycle as reverse osmosis concentration film uses.When reverse osmosis concentration film waste water reclamation rate is 67%, namely membranous system waste water total yield reaches 90.1%, the concentrated dense water of film (i.e. raw wastewater 9.9%) enters vaporizer and evaporates, steam condensate enters into reuse pool, fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste.Not discharge water pollutent in whole process.
The removal efficiency of principal pollutant index is in table 2.
Table 2 technique unit removal efficiency table
Contrast above-mentioned case can find out: for the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry, utilize calcium salt precipitation method effectively can remove fluorion, utilize reverse osmosis membrane, effluent quality is excellent, can be used as process water water source, realize reuse completely, the denitrogenation of reverse osmosis membrane dense water conservancy evaporation technique, realizes the zero release of waste water.But conventional reverse osmosis technique only reaches the wastewater recycle rate of former water 70%, and fouling membrane can make film device be difficult to normal operation, and decelerating membrane pollution is the difficult point of membrane concentration, wherein reduces fluorinion in waste water and calcium ion etc. and easily causes the material concentration of film fouling to be crucial.The become method of zero release of the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry of the present invention adopts dense water to induce to accelerate crystallization, the calcium ion in the dense water of reverse osmosis membrane and fluorion is made to form precipitation on induced crystallization crystal seed, and be efficiently removed, reduce the possibility of fouling membrane, improve the cycles of concentration of reverse osmosis concentration film, accelerate the dense water of crystallization through induction to enter into reverse osmosis concentration film again to carry out circulation concentrated, the waste water total yield of membranous system is made to reach more than 90%, namely the wastewater from battery production amount entering vaporizer cuts down more than 90%, thus the expense greatly reduced needed for evaporation, and make high fluorine-containing nitrogenous wastewater from battery production zero release.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention.All any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry becomes a method for zero release, and it comprises the following steps:
(1) first fluorine-containing for height nitrogenous wastewater from battery production is sent into equalizing tank homogeneous;
(2) enter except fluorine reaction tank, make fluorion and calcium ion form calcium fluoride precipitate, then add coagulating agent and flocculation agent successively, reaction tank water outlet enters settling tank again, and the outer row of precipitation is as sludge treatment, and supernatant liquor enters intermediate pool; Be specially, the supernatant liquor of settling tank enters intermediate pool successively after deliming reaction tank and second-level settling pond, the supernatant liquor of settling tank enters deliming reaction tank, add sodium carbonate wherein, the calcium ion unnecessary with prime forms precipitation of calcium carbonate, then adds flocculation agent, and water outlet enters second-level settling pond, the outer row of precipitation is as sludge treatment, and second-level settling pond supernatant liquor enters intermediate pool;
(3) again through quartz filter and activated charcoal filter, remove suspended impurity and the organic impurities of larger particles in waste water respectively, water outlet after filtration is first by ultrafiltration membrane treatment, and the dense water of ultra-filtration membrane gets back to equalizing tank, and fresh water enters into the process of first-stage reverse osmosis film;
(4) first-stage reverse osmosis film fresh water delivers to reuse pool, and dense water accelerates crystallizing pond through the induction of overrich water, adds induction crystal seed wherein, makes the calcium ion in dense water and fluorion accelerate to form precipitation on crystal seed;
(5) supernatant liquor passes through cartridge filter, enter into again reverse osmosis concentration film carry out circulation concentrate, namely reuse pool is delivered in the water outlet of reverse osmosis concentration film, the concentrated dense water of film again enters the induction of dense water and accelerates crystallizing pond acceleration sofening treatment, pass through cartridge filter, fill cycle as reverse osmosis concentration film uses, until when effluent index is about to higher than industrial reuse water-quality guideline, stops circulation concentrated;
(6) the dense water of reverse osmosis concentration film enters vaporizer again and evaporates, and steam condensate enters into reuse pool, and fully recovering is in process water, and the residue that evaporation produces is as disposition of solid waste; Not discharge water pollutent in whole process.
2. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: in described step (2), waste water enters except after fluorine reaction tank, add calcium hydroxide wherein, regulate waste water ph to 8 ~ 9, make fluorion and calcium ion form calcium fluoride precipitate.
3. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: in described step (2), after settling tank supernatant liquor enters intermediate pool, add sulphuric acid soln and regulate waste water ph to 7 ~ 8.
4. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: the fluorine-containing nitrogenous wastewater from battery production of described height is the photovoltaic industry wastewater from battery production of nitrate nitrogen concentration >200mg/L and fluorinion concentration >500mg/L.
5. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: described ultra-filtration membrane is hollow-fibre membrane, tubular membrane or flat sheet membrane.
6. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: described dense water induction is accelerated crystallizing pond and is divided into reaction zone and settling region, add in reaction zone and have induced crystallization crystal seed, crystal seed in settling region under precipitation is back to reaction zone, settling region supernatant liquor water outlet.
7. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, and it is characterized in that: described crystal seed is calcite sand or quartz sand, particle diameter is 50 order ~ 500 orders.
8. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, and it is characterized in that: described cartridge filter, filtering accuracy is less than or equal to 5 μm.
9. the high fluorine-containing nitrogenous wastewater from battery production of photovoltaic industry according to claim 1 becomes the method for zero release, it is characterized in that: described reverse osmosis concentration film is sea water desalination membrane or low pressure high desalination reverse osmosis membrane.
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| CN114853204A (en) * | 2022-04-11 | 2022-08-05 | 江苏道同环境科技有限公司 | Metal silicide BOE etching wastewater zero-discharge treatment device and method |
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