CN113072233A - Treatment method for treating acid wastewater for graphite purification - Google Patents
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Abstract
The invention discloses a treatment method for treating acid wastewater generated in graphite purification, which comprises the following steps: the method comprises the following steps: removing impurities in the concentrated acid water; the recovered acid is reused in the production line; treating the multistage acid pickling filter pressing waste liquid; the low-concentration washing water is treated in multiple stages. The method has the beneficial effects that: the treatment method is suitable for treating the acidic wastewater purified by graphite, the treatment of acidic substances in the wastewater is realized by adding the neutralizing agent and the coagulant, the standard-reaching discharge of the wastewater can be realized, the effective removal of acidic ions in the wastewater can be realized, the discharge standard can be reached, the process is simple, the operation is convenient, the effective dilution and precipitation of the ions in the wastewater can be realized, the precipitated substances can be collected and treated, and the treatment method has the advantages of low construction cost, low operation cost and high treatment effect.
Description
Technical Field
The invention relates to a treatment method, in particular to a treatment method for treating acid wastewater of graphite purification, belonging to the technical field of acid wastewater treatment application.
Background
Graphite is a mineral name, usually produced in metamorphic rocks, it is coal or carbonaceous rocks are affected by regional metamorphism or magma invasion to form, graphite is an allotrope of elemental carbon, every carbon atom's periphery links the other three carbon atoms, the arrangement mode presents a plurality of hexagons of the honeycomb, there is weak van der Waals' attraction between every layer, chemical inactive, have corrosion resistance, the method of graphite purification is alkali acid method, chloridize roasting method, flotation method, high-temperature purification method and hydrofluoric acid method, the alkali acid method is the most widely applied method in graphite purification industrial production of our country, it is few to have a disposable investment, the product grade is higher, strong adaptability, etc. and the advantage that the apparatus is simple, strong versatility. The chlorination roasting method has the advantages of energy conservation, high purification efficiency and high recovery rate, but has the problems of toxic chlorine, severe corrosivity, severe environmental pollution and the like. A flotation method: graphite has good natural floatability, and substantially all of the graphite can be purified by flotation. Hydrofluoric acid method: graphite has good acid resistance, particularly hydrofluoric acid resistance, and the graphite can be purified by hydrofluoric acid. High-temperature purification method: the high-temperature method for purifying graphite has high product quality, the carbon content can reach more than 99.995%, which is the biggest characteristic of the high-temperature method, but simultaneously, the method has the disadvantages of high energy consumption, extremely high requirements on equipment, special design and high investment.
Graphite is a mineral name, the graphite is usually subjected to an alkaline-acid method, a hydrofluoric acid method and the like, waste water generated after purification seriously affects the environment and cannot reach the discharge standard, and the purification efficiency of the graphite is affected due to multiple process steps and complex operation when the waste water is treated. Therefore, a treatment method for treating acid wastewater generated in graphite purification is provided to solve the above problems.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for treating acidic wastewater from graphite purification.
The invention achieves the aim through the following technical scheme, and the treatment method for treating the acid wastewater generated by graphite purification comprises the following steps:
(1) removing impurities in the concentrated acid water, and removing the impurities in the acid by low-temperature evaporation of the concentrated acid water;
(2) the recovered acid is reused in the production line, and the concentrated acid water with impurities removed is conveyed to the production line again for utilization;
(3) treating the multistage pickling and filter pressing waste liquid, and collecting the pickling waste liquid in a waste water collecting tank;
(4) the low-concentration washing water is treated in multiple stages, and a neutralizing agent and a coagulant are added into acid water for treatment.
Preferably, in the step (1), the solid impurities are removed by low-temperature evaporation, and the solid impurities are treated.
Preferably, in the step (2), the concentrated acid water is recovered after evaporation and condensation for subsequent treatment, and the concentrated acid water with impurities removed is conveyed to the production line again for wastewater treatment.
Preferably, in the step (3), multistage treatment is adopted in a pickling high-concentration wastewater collection tank, the primary pickling press-filtration waste liquid is subjected to press filtration or centrifugal dehydration, hydrochloric acid, nitric acid and hydrofluoric acid are added into the collection tank, 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 6 tons of 40% hydrofluoric acid are supplemented in a primary pickling refining system, the total amount of the primary pickling solution is 90 tons, 7.2 tons of hydrochloric acid, 3.6 tons of nitric acid, 2.4 tons of hydrofluoric acid and 54 tons of water are added, 76.5 tons of primary pickling waste liquid is subjected to press filtration or centrifugal dehydration, contains 6.12 tons of hydrochloric acid, 3.06 tons of nitric acid and 2.04 tons of hydrofluoric acid, and is subjected to precision pretreatment by a sony wastewater precision pretreatment system and then treated by an ultralow temperature mixed acid evaporation recovery system.
Preferably, after the primary acid washing solution treatment in the step (3), 13.5 tons of primary cleaning water after the primary acid washing are carried out each day, 1.08 tons of residual hydrochloric acid, 0.54 tons of nitric acid and 0.36 tons of hydrofluoric acid are subjected to filter pressing or centrifugal dehydration treatment to generate 13.5 tons of secondary primary cleaning wastewater, wherein 0.54 tons of hydrochloric acid, 0.27 tons of nitric acid and 0.18 tons of hydrofluoric acid are generated, and then the secondary primary cleaning wastewater is treated by a precision sony wastewater pretreatment system.
Preferably, in the step (3), 2.91 tons of 30% hydrochloric acid and 0.7275 tons of 60% nitric acid are supplemented into a secondary pickling solution and 84 tons of the secondary pickling solution, wherein the secondary pickling solution contains 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 54 tons of water, and after pressure filtration or dehydration treatment, 71.4 tons of secondary mixed acid waste liquid is obtained, wherein 6.12 tons of hydrochloric acid and 3.06 tons of nitric acid are treated by a precision sony waste acid pretreatment system and a low-temperature mixed acid extraction and recovery system.
Preferably, in the step (4), the first cleaning wastewater after the secondary acid washing is added into the secondary acid washing solution, so as to obtain 1.08 tons of hydrochloric acid and 0.54 tons of nitric acid.
Preferably, the first cleaning wastewater after the second cleaning in the step (4) is subjected to pressure filtration or centrifugal dehydration to obtain 12.6 tons of second-stage first cleaning wastewater, wherein the hydrochloric acid is 0.54 ton, and the nitric acid is 0.27 ton.
Preferably, after the multi-stage treatment is carried out in the step (4) to obtain a plurality of cleaning wastewater after the secondary acid cleaning, the cleaning wastewater adjusting tank 1384 tons per day is obtained, wherein 1.08 tons of hydrochloric acid, 0.54 tons of nitric acid and 0.18 tons of hydrofluoric acid are obtained, and 572.7mg/L of chloride ions, 289.8mg/L of nitrate ions and 93.0mg/L of fluoride ions are obtained, and the total salt content is 1980 mg/L.
Preferably, in the step (4), the cleaning wastewater adjusting tank is subjected to FCM catalytic self-electrolysis reaction, the removal rate of chloride ions is 10%, the residual concentration is 540mg/L, the removal rate of fluoride ions is 90%, the residual concentration of fluoride ions is 9.7mg/L, the removal rate of total salt is 12%, and the residual total salt amount is 1742mg/L, and after the treatment of the catalytic three-dimensional electrolysis reactor and the delayed neutralization precipitation system, the removal rate of chloride ions is 20%, the residual concentration is 432mg/L, the removal rate of fluoride ions is 80%, the residual concentration is 1.94mg/L, the removal rate of total salt is 15%, and the residual 1481mg/L are finally discharged after passing through the clean water tank and reaching the standard.
The invention has the beneficial effects that: the treatment method is suitable for treating the acidic wastewater purified by graphite, the treatment of acidic substances in the wastewater is realized by adding the neutralizing agent and the coagulant, the standard-reaching discharge of the wastewater can be realized, the effective removal of acidic ions in the wastewater can be realized, the discharge standard can be reached, the process is simple, the operation is convenient, the effective dilution and precipitation of the ions in the wastewater can be realized, the precipitated substances can be collected and treated, and the treatment method has the advantages of low construction cost, low operation cost and high treatment effect.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a treatment process for treating acidic wastewater from graphite purification, the treatment process comprising the steps of:
(1) removing impurities in the concentrated acid water, and removing the impurities in the acid by low-temperature evaporation of the concentrated acid water;
(2) the recovered acid is reused in the production line, and the concentrated acid water with impurities removed is conveyed to the production line again for utilization;
(3) treating the multistage pickling and filter pressing waste liquid, and collecting the pickling waste liquid in a waste water collecting tank;
(4) the low-concentration washing water is treated in multiple stages, and a neutralizing agent and a coagulant are added into acid water for treatment.
And (2) removing the solid impurities by adopting low-temperature evaporation in the step (1) and treating the solid impurities.
And (3) recovering concentrated acid water after evaporation and condensation in the step (2) for subsequent treatment, and conveying the concentrated acid water subjected to impurity removal to a production line again for wastewater treatment.
And (3) performing multistage treatment on the pickling high-concentration wastewater collection pool in the step (3), performing filter pressing or centrifugal dehydration on the primary pickling filter-pressing waste liquid, adding hydrochloric acid, nitric acid and hydrofluoric acid into the collection pool, supplementing 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 6 tons of 40% hydrofluoric acid into a primary pickling refining system, wherein the total amount of the primary pickling solution is 90 tons, 7.2 tons of hydrochloric acid, 3.6 tons of nitric acid, 2.4 tons of hydrofluoric acid and 54 tons of water are added into the primary pickling refining system, performing filter pressing or centrifugal dehydration on the primary pickling waste liquid, obtaining 76.5 tons of primary pickling waste liquid, wherein the primary waste liquid contains 6.12 tons of hydrochloric acid, 3.06 tons of nitric acid and 2.04 tons of hydrofluoric acid, and performing treatment on the primary waste liquid by an ultralow-temperature mixed acid evaporation.
After the primary pickling solution treatment in the step (3), 13.5 tons of primary cleaning water after the primary pickling is carried out every day, 1.08 tons of residual hydrochloric acid, 0.54 tons of nitric acid and 0.36 tons of hydrofluoric acid are subjected to filter pressing or centrifugal dehydration treatment to generate 13.5 tons of secondary primary cleaning wastewater, wherein 0.54 ton of hydrochloric acid, 0.27 ton of nitric acid and 0.18 ton of hydrofluoric acid are subjected to secondary primary cleaning wastewater treatment by a precision Sanmani wastewater pretreatment system.
In the step (3), 2.91 tons of 30% hydrochloric acid and 0.7275 tons of 60% nitric acid are added into a secondary pickling solution, namely 84 tons of the secondary pickling solution, in a secondary pickling refining system, wherein the secondary pickling solution contains 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 54 tons of water, and 71.4 tons of secondary mixed acid waste liquid is obtained after filter pressing or dehydration treatment, wherein 6.12 tons of hydrochloric acid and 3.06 tons of nitric acid are treated by a precision sonny waste acid pretreatment system and a low-temperature mixed acid extraction and recovery system.
And (4) adding the first cleaning wastewater after the secondary pickling into the secondary pickling solution to obtain 1.08 tons of hydrochloric acid and 0.54 ton of nitric acid.
And (4) performing filter pressing or centrifugal dehydration on the first cleaning wastewater obtained after the second-stage cleaning in the step (4) to obtain 12.6 tons of second-stage first cleaning wastewater, wherein the hydrochloric acid is 0.54 ton, and the nitric acid is 0.27 ton.
And (4) after multi-stage treatment is carried out in the step (4) to obtain a plurality of cleaning wastewater after secondary pickling, cleaning wastewater adjusting tanks 1384 tons per day are obtained, wherein 1.08 tons of hydrochloric acid, 0.54 tons of nitric acid and 0.18 tons of hydrofluoric acid are obtained, and 572.7mg/L of chloride ions, 289.8mg/L of nitrate ions and 93.0mg/L of fluoride ions are obtained, and the total salt content is 1980 mg/L.
And (4) carrying out FCM catalytic self-electrolysis reaction on the cleaning wastewater adjusting tank in the step (4), wherein the removal rate of chloride ions is 10%, the residual concentration is 540mg/L, the removal rate of fluoride ions is 90%, the residual concentration of fluoride ions is 9.7mg/L, the removal rate of full salt is 12%, and the residual amount of full salt is 1742mg/L, and after treatment of a catalytic three-dimensional electrolysis reactor and a delayed neutralization and precipitation system, the removal rate of chloride ions is 20%, the residual concentration is 432mg/L, the removal rate of fluoride ions is 80%, the residual concentration is 1.94mg/L, the removal rate of full salt is 15%, the residual concentration is 1481mg/L, and finally, the waste water is discharged after reaching the standard through a clean water tank.
The method is suitable for wastewater treatment with low total salt removal rate and low standard discharge effect, and has low requirement on wastewater treatment.
Example two:
a treatment process for treating acidic wastewater from graphite purification, the treatment process comprising the steps of:
(1) removing impurities in the concentrated acid water, and removing the impurities in the acid by low-temperature evaporation of the concentrated acid water;
(2) the recovered acid is reused in the production line, and the concentrated acid water with impurities removed is conveyed to the production line again for utilization;
(3) treating the multistage pickling and filter pressing waste liquid, and collecting the pickling waste liquid in a waste water collecting tank;
(4) the low-concentration washing water is treated in multiple stages, and a neutralizing agent and a coagulant are added into acid water for treatment.
And (2) removing the solid impurities by adopting low-temperature evaporation in the step (1) and treating the solid impurities.
And (3) recovering concentrated acid water after evaporation and condensation in the step (2) for subsequent treatment, and conveying the concentrated acid water subjected to impurity removal to a production line again for wastewater treatment.
And (3) performing multistage treatment on the pickling high-concentration wastewater collection pool in the step (3), performing filter pressing or centrifugal dehydration on the primary pickling filter-pressing waste liquid, adding hydrochloric acid, nitric acid and hydrofluoric acid into the collection pool, supplementing 24 tons of 40% hydrochloric acid, 6 tons of 60% nitric acid and 6 tons of 50% hydrofluoric acid into a primary pickling refining system, wherein the total amount of the primary pickling solution is 90 tons, 7.2 tons of hydrochloric acid, 3.6 tons of nitric acid, 2.4 tons of hydrofluoric acid and 54 tons of water are added into the primary pickling refining system, performing filter pressing or centrifugal dehydration on the primary pickling waste liquid, obtaining 76.5 tons of primary pickling waste liquid, wherein the primary waste liquid contains 6.12 tons of hydrochloric acid, 3.06 tons of nitric acid and 2.04 tons of hydrofluoric acid, and performing treatment on the primary waste liquid by an ultralow-temperature mixed acid evaporation.
After the primary pickling solution treatment in the step (3), 13.5 tons of primary cleaning water after the primary pickling is carried out every day, 1.08 tons of residual hydrochloric acid, 0.54 tons of nitric acid and 0.36 tons of hydrofluoric acid are subjected to filter pressing or centrifugal dehydration treatment to generate 13.5 tons of secondary primary cleaning wastewater, wherein 0.54 ton of hydrochloric acid, 0.27 ton of nitric acid and 0.18 ton of hydrofluoric acid are subjected to secondary primary cleaning wastewater treatment by a precision Sanmani wastewater pretreatment system.
In the step (3), 2.91 tons of 30% hydrochloric acid and 0.7275 tons of 60% nitric acid are added into a secondary pickling solution, namely 84 tons of the secondary pickling solution, in a secondary pickling refining system, wherein the secondary pickling solution contains 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 54 tons of water, and 71.4 tons of secondary mixed acid waste liquid is obtained after filter pressing or dehydration treatment, wherein 6.12 tons of hydrochloric acid and 3.06 tons of nitric acid are treated by a precision sonny waste acid pretreatment system and a low-temperature mixed acid extraction and recovery system.
And (4) adding the first cleaning wastewater after the secondary pickling into the secondary pickling solution to obtain 1.08 tons of hydrochloric acid and 0.54 ton of nitric acid.
And (4) performing filter pressing or centrifugal dehydration on the first cleaning wastewater obtained after the second-stage cleaning in the step (4) to obtain 12.6 tons of second-stage first cleaning wastewater, wherein the hydrochloric acid is 0.54 ton, and the nitric acid is 0.27 ton.
And (4) after multi-stage treatment is carried out in the step (4) to obtain a plurality of cleaning wastewater after secondary pickling, cleaning wastewater adjusting tanks 1384 tons per day are obtained, wherein 1.08 tons of hydrochloric acid, 0.54 tons of nitric acid and 0.18 tons of hydrofluoric acid are obtained, and 572.7mg/L of chloride ions, 289.8mg/L of nitrate ions and 93.0mg/L of fluoride ions are obtained, and the total salt content is 1980 mg/L.
And (4) carrying out FCM catalytic self-electrolysis reaction on the cleaning wastewater adjusting tank in the step (4), wherein the removal rate of chloride ions is 10%, the residual concentration is 540mg/L, the removal rate of fluoride ions is 90%, the residual concentration of fluoride ions is 9.7mg/L, the removal rate of full salt is 12%, and the residual amount of full salt is 1742mg/L, and after treatment of a catalytic three-dimensional electrolysis reactor and a delayed neutralization and precipitation system, the removal rate of chloride ions is 20%, the residual concentration is 432mg/L, the removal rate of fluoride ions is 80%, the residual concentration is 1.94mg/L, the removal rate of full salt is 15%, the residual concentration is 1481mg/L, and finally, the waste water is discharged after reaching the standard through a clean water tank.
The method is suitable for wastewater treatment with high total salt removal rate and high standard discharge effect, and has high requirements on wastewater treatment.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A treatment method for treating acid wastewater of graphite purification is characterized by comprising the following steps: the processing method comprises the following steps:
(1) removing impurities in the concentrated acid water, and removing the impurities in the acid by low-temperature evaporation of the concentrated acid water;
(2) the recovered acid is reused in the production line, and the concentrated acid water with impurities removed is conveyed to the production line again for utilization;
(3) treating the multistage pickling and filter pressing waste liquid, and collecting the pickling waste liquid in a waste water collecting tank;
(4) the low-concentration washing water is treated in multiple stages, and a neutralizing agent and a coagulant are added into acid water for treatment.
2. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (2) removing the solid impurities by adopting low-temperature evaporation in the step (1) and treating the solid impurities.
3. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (3) recovering concentrated acid water after evaporation and condensation in the step (2) for subsequent treatment, and conveying the concentrated acid water subjected to impurity removal to a production line again for wastewater treatment.
4. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (3) performing multistage treatment on the pickling high-concentration wastewater collection pool in the step (3), performing filter pressing or centrifugal dehydration on the primary pickling filter-pressing waste liquid, adding hydrochloric acid, nitric acid and hydrofluoric acid into the collection pool, supplementing 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 6 tons of 40% hydrofluoric acid into a primary pickling refining system, wherein the total amount of the primary pickling solution is 90 tons, 7.2 tons of hydrochloric acid, 3.6 tons of nitric acid, 2.4 tons of hydrofluoric acid and 54 tons of water are added into the primary pickling refining system, performing filter pressing or centrifugal dehydration on the primary pickling waste liquid, obtaining 76.5 tons of primary pickling waste liquid, wherein the primary waste liquid contains 6.12 tons of hydrochloric acid, 3.06 tons of nitric acid and 2.04 tons of hydrofluoric acid, and performing treatment on the primary waste liquid by an ultralow-temperature mixed acid evaporation.
5. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: after the primary pickling solution treatment in the step (3), 13.5 tons of primary cleaning water after the primary pickling is carried out every day, 1.08 tons of residual hydrochloric acid, 0.54 tons of nitric acid and 0.36 tons of hydrofluoric acid are subjected to filter pressing or centrifugal dehydration treatment to generate 13.5 tons of secondary primary cleaning wastewater, wherein 0.54 ton of hydrochloric acid, 0.27 ton of nitric acid and 0.18 ton of hydrofluoric acid are subjected to secondary primary cleaning wastewater treatment by a precision Sanmani wastewater pretreatment system.
6. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: in the step (3), 2.91 tons of 30% hydrochloric acid and 0.7275 tons of 60% nitric acid are added into a secondary pickling solution, namely 84 tons of the secondary pickling solution, in a secondary pickling refining system, wherein the secondary pickling solution contains 24 tons of 30% hydrochloric acid, 6 tons of 60% nitric acid and 54 tons of water, and 71.4 tons of secondary mixed acid waste liquid is obtained after filter pressing or dehydration treatment, wherein 6.12 tons of hydrochloric acid and 3.06 tons of nitric acid are treated by a precision sonny waste acid pretreatment system and a low-temperature mixed acid extraction and recovery system.
7. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (4) adding the first cleaning wastewater after the secondary pickling into the secondary pickling solution to obtain 1.08 tons of hydrochloric acid and 0.54 ton of nitric acid.
8. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (4) performing filter pressing or centrifugal dehydration on the first cleaning wastewater obtained after the second-stage cleaning in the step (4) to obtain 12.6 tons of second-stage first cleaning wastewater, wherein the hydrochloric acid is 0.54 ton, and the nitric acid is 0.27 ton.
9. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (4) after multi-stage treatment is carried out in the step (4) to obtain a plurality of cleaning wastewater after secondary pickling, cleaning wastewater adjusting tanks 1384 tons per day are obtained, wherein 1.08 tons of hydrochloric acid, 0.54 tons of nitric acid and 0.18 tons of hydrofluoric acid are obtained, and 572.7mg/L of chloride ions, 289.8mg/L of nitrate ions and 93.0mg/L of fluoride ions are obtained, and the total salt content is 1980 mg/L.
10. The treatment method for treating the acid wastewater generated in the purification of graphite according to claim 1, characterized in that: and (4) carrying out FCM catalytic self-electrolysis reaction on the cleaning wastewater adjusting tank in the step (4), wherein the removal rate of chloride ions is 10%, the residual concentration is 540mg/L, the removal rate of fluoride ions is 90%, the residual concentration of fluoride ions is 9.7mg/L, the removal rate of full salt is 12%, and the residual amount of full salt is 1742mg/L, and after treatment of a catalytic three-dimensional electrolysis reactor and a delayed neutralization and precipitation system, the removal rate of chloride ions is 20%, the residual concentration is 432mg/L, the removal rate of fluoride ions is 80%, the residual concentration is 1.94mg/L, the removal rate of full salt is 15%, the residual concentration is 1481mg/L, and finally, the waste water is discharged after reaching the standard through a clean water tank.
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