CN116119876A - Method for recycling desulfurization wastewater - Google Patents
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- CN116119876A CN116119876A CN202310138766.5A CN202310138766A CN116119876A CN 116119876 A CN116119876 A CN 116119876A CN 202310138766 A CN202310138766 A CN 202310138766A CN 116119876 A CN116119876 A CN 116119876A
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- C—CHEMISTRY; METALLURGY
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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Abstract
The invention discloses a desulfurization wastewater recycling method, which comprises the following steps: discharging the desulfurization wastewater to a buffer tank, reducing the COD value in the wastewater through stirring aeration, precipitating suspended matters in the water, and filtering to obtain filtrate A and filter residue A; adding the filtrate A into a reaction tank, and adding a calcium reagent and an aluminum reagent into the reaction tank, wherein the molar ratio of the calcium reagent to the aluminum reagent to the chloride ion content in the filtrate A is 5:2.5:1; carrying out solid-liquid separation on the solid-liquid mixture, and filtering to obtain filtrate B and filter residue B; flowing the filtrate B into a clarification tank, adding PAM for flocculation precipitation reaction, and filtering to obtain filtrate C and filter residue C; the filtrate C enters a low-temperature vacuum evaporation system to obtain reclaimed water A; and discharging the reclaimed water A into a biochemical pool for ammonia nitrogen biochemical treatment to obtain reclaimed water B. The method has the advantages of being capable of efficiently removing the chlorine, fluorine, COD and ammonia nitrogen content in the desulfurization tower wastewater, enabling the produced reclaimed water to meet the use standard of industrial production and reducing the waste of water resources.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy of industrial wastewater, in particular to a method for recycling desulfurization wastewater.
Background
A great deal of research is carried out on the treatment of industrial wastewater containing chlorine, fluorine, COD and ammonia nitrogen at home and abroad, and a lot of progress is also made on the research on chlorine removal technology and related basic theory. Flue gas containing a large amount of sulfur, nitrogen, chlorine, fluorine and other components generated by the pyrometallurgy of the electroplating sludge and the roasting of the spent catalyst is absorbed by a desulfurization tower, sulfur, fluorine and the like are absorbed by calcium oxide to form desulfurized gypsum and calcium fluoride, and chloride ions and part of nitrogen form ammonium radicals to exist in a liquid phase, and after enrichment and concentration, the chloride ions can reach more than 15 g/L. At present, the treatment methods of chlorine-containing desulfurization wastewater mainly comprise an adsorption method, an electrocoagulation method, a reverse osmosis method, an ion exchange method, a chemical precipitation method, a coagulation sedimentation method and the like, wherein the ion exchange method has high cost and strict requirements on the water quality of the wastewater, the electrocoagulation method and the reverse osmosis method have complex devices and high power consumption, so that the methods are rarely adopted, and the chemical precipitation method, the coagulation sedimentation method and the adsorption method are frequently adopted, but the defects of unstable water quality of effluent, small adsorption capacity, large addition amount of required reagents and the like are also caused.
Reducing chloride ions, fluoride ions and sulfate radicals in the waste water of the desulfurizing tower in the production process, and the produced calcium aluminate can also be used as a building material fire metallurgy fluxing agent for cement, brick making and the like. Wherein the chemical precipitation method is to generate calcium fluoride precipitate by utilizing the reaction of calcium hydroxide and hydrofluoric acid in the wastewater, and the sulfate radical generates calcium sulfate precipitate, so that fluoride ions and sulfate radical can be removed from the wastewater. Chloride ions are common corrosive ions in water, so that the cavitation erosion of stainless steel is easy to cause, and sodium metaaluminate and slaked lime are utilized to treat wastewater containing the chloride ions. Therefore, there is a need to develop a method for simultaneously removing chlorine and fluorine ions in desulfurization wastewater by using calcium hydroxide and sodium metaaluminate so that the desulfurization wastewater can be recycled.
Disclosure of Invention
The invention aims to provide a method for recycling desulfurization wastewater. The method has the advantages of being capable of efficiently removing chlorine, fluorine, COD and ammonia nitrogen content in the desulfurization tower wastewater, enabling the produced reclaimed water to meet the use standard of industrial production and reducing the waste of water resources.
The technical scheme of the invention is as follows: the method for recycling the desulfurization wastewater comprises the following steps:
s1: discharging the desulfurization wastewater to a buffer tank, reducing the COD value in the wastewater by stirring and aeration, reducing the COD value to below 103mg/L, precipitating suspended matters in the water, and filtering to obtain filtrate A and filter residue A;
s2: adding the filtrate A in the step S1 into a reaction tank, and adding a calcium reagent and an aluminum reagent into the reaction tank, wherein the molar ratio of the calcium reagent to the aluminum reagent to the chloride ion content in the filtrate A is 5:2.5:1;
s3: carrying out solid-liquid separation on the solid-liquid mixture after the reaction of S2, and filtering through a plate frame to obtain filtrate B and filter residue B;
s4: flowing the filtrate B of the step S3 into a clarifier and adding 5 drops of PAM for flocculation precipitation reaction, and filtering to obtain filtrate C and filter residue C;
s5: the filtrate C of the S4 enters a low-temperature vacuum evaporation system, and the filtrate C is treated in a low-temperature reduced pressure distillation mode to obtain reclaimed water A;
s6: and (3) discharging the regenerated water A of the S5 into a biochemical pool for ammonia nitrogen biochemical treatment, and adding an ammonia nitrogen treating agent to reduce the ammonia nitrogen content to obtain regenerated water B.
Compared with the prior art, the invention has the beneficial effects that: by using calcium hydroxide or calcium oxide and sodium metaaluminate in proper proportion, namely, the adding mole ratio of chloride ion content to the calcium reagent and the aluminum reagent is 1:5:2.5, under the condition of proper temperature, PH value and stirring reaction, the chloridion is adsorbed and removed, the once removal rate can reach more than 60 percent, and the removal rate of the fluorinion and sulfate ion can reach more than 70 percent; evaporating and crystallizing in a low-temperature vacuum decompression mode, and preventing residual chloride ions, fluoride ions, COD, ammonia nitrogen and the like from being evaporated in a vacuum state of-97 kpa at 30-35 ℃, so that the physicochemical indexes in the reclaimed water can be reduced to milligram-level content, and the water supplementing requirement in wet production can be truly met; the continuous operation of the low-temperature vacuum decompression evaporation technology can realize unattended operation, the cost is only power consumption, the cost of electricity charge per ton of water treatment is within 80KWH, more than 90% of regenerated water and less than 10% of solid waste can be produced, the whole process is managed in a closed mode, no harmful waste gas and the like are produced, the working environment meets the requirements of green production, and the maximization of resource utilization and the reduction of hazardous waste are realized.
In the method for recycling the desulfurization wastewater, the stirring speed in the step S1 is 300-400r/min, and the COD value in the wastewater is reduced by continuous air aeration for 30-40 min.
In the method for recycling desulfurization wastewater, chloride ions, a calcium reagent and an aluminum reagent in the S2 are subjected to stirring reaction to remove the chloride, the stirring speed is 300-400r/min, the reaction temperature is 40 ℃, the reaction time is 60min, and finally the content of the chloride ions in the filtrate B in the S3 is reduced to below 40% of the original wastewater.
In the method for recycling desulfurization wastewater, the calcium reagent in the step S2 is calcium hydroxide or calcium oxide, and the aluminum reagent is sodium metaaluminate.
In the method for recycling desulfurization wastewater, when the calcium reagent in the S2 is calcium hydroxide, the calcium hydroxide, sodium metaaluminate and chloride ion content in the filtrate A are mixed according to the following mass parts: 100 parts of calcium hydroxide, 57 parts of sodium metaaluminate and 10 parts of chloride ions in filtrate A.
In the method for recycling desulfurization wastewater, the pH value of the filtrate B in the step S3 is controlled to be 7-9.
In the method for recycling desulfurization wastewater, the concentration of the solution after the PAM is added in the S4 is controlled within 5 PPM.
In the method for recycling desulfurization wastewater, the filtrate C in the step S5 is evaporated and boiled at 30 ℃ under the vacuum state of-97 kpa.
In the method for recycling desulfurization wastewater, the filtrate C in the step S5 is separated into 10 parts of concentrated waste liquid and 90 parts of reclaimed water A after being subjected to low-temperature reduced-pressure distillation condensation treatment.
In the method for recycling desulfurization wastewater, the ammonia nitrogen content of the reclaimed water B in the S6 is below 130 mg/L.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a view showing the raw water of desulfurization wastewater of the present invention;
FIG. 3 is a calcium aluminate precipitate after dechlorination according to the invention;
FIG. 4 shows the regenerant water and concentrate after low temperature vacuum evaporation according to example 1 of the present invention;
FIG. 5 shows the regenerant water and concentrate obtained after low-temperature vacuum evaporation in example 2 according to the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not intended to be limiting.
Example 1: the method for recycling the desulfurization wastewater comprises the following steps:
s1: discharging desulfurization wastewater generated in the desulfurization tower to a buffer tank, primarily reducing the COD value in the wastewater through stirring aeration oxidation, reducing the final COD value to below 103mg/L, precipitating suspended matters in the water to obtain filtrate A and filter residue A, and continuously performing air aeration for 30-40 min at a stirring rate of 300-400 r/min;
s2: adding the filtrate A in the step S1 into a reaction tank, adding calcium hydroxide and sodium metaaluminate into desulfurization wastewater in a certain proportion in the reaction tank, and removing most of chloride ions in the wastewater to obtain calcium aluminate precipitate; measuring 1000ml of desulfurization wastewater, measuring the chloride ion content of the desulfurization wastewater to be 10.56g/L, keeping the stirring speed to be 300-400r/min, keeping the temperature at 40 ℃, adding 57g of sodium metaaluminate to dissolve, continuously adding 101g of calcium hydroxide for 60 minutes, and filtering to obtain the filtrate, wherein the chloride ion content of the filtrate is measured to be 4.08g/L, and the chloride ion content is reduced by more than 60%;
s3: after the reaction is finished, carrying out solid-liquid separation on the solid-liquid mixture after the reaction of S2, and carrying out plate-frame filter pressing to obtain filtrate B and filter residue B, wherein the filtrate B is chlorine-removing wastewater, and the filter residue B is calcium aluminum fluorite and can be used as building material additives such as cement;
s4: allowing the filtrate B with reduced chloride ions to flow into a clarifying tank for clarification, dripping about 5 drops of PAM for flocculation precipitation, and filtering to obtain filtrate C and filter residue C;
s5: and (3) the filtrate C of the S4 enters a low-temperature vacuum evaporation system to set the evaporation temperature to be 30-35 ℃, and the evaporation is carried out under a vacuum state of-97 kpa to obtain regenerated water A with the entering quantity of about 90% and concentrated waste liquid with the chloride ion content of 0.39g/L, wherein the chloride ion reaches the standard of regeneration and reuse of waste water of a desulfurizing tower, so that the condition of co-boiling of chemicals in a high-temperature state is avoided.
S6: and (3) discharging the regenerated water A of the S5 into a biochemical pond for ammonia nitrogen biochemical treatment, further reducing the ammonia nitrogen content to below 130mg/L by adding a proper amount of ammonia nitrogen treating agent, finally reducing the ammonia nitrogen content to the content of a normal water body, wherein the COD (chemical oxygen demand) is 84.6mg/L, the ammonia nitrogen content is less than 100mg/L, and the regenerated water meets the requirement of industrial reuse water.
The results of the wastewater, reclaimed water and concentrate of example 1 are shown in Table 1.
TABLE 1 results of various tests on wastewater, regenerant and concentrate from example 1
| Cl - (g/L) | COD(mg/L) | Ammonia nitrogen (mg/L) | Liquid chromaticity | |
| Desulfurization waste water | 10.56 | 3000 | 1020 | Yellow colour |
| One-time chlorine removal | 4.08 | 2000 | 800 | Yellow colour |
| Concentrated solution | 40.0 | 5000 | 1000 | Brown color |
| Reclaimed water | 0.39 | 84.6 | ＜100 | Colorless and colorless |
As is clear from Table 1, after one chlorine removal, the chlorine ion content was removed by 60% or more, but the COD and ammonia nitrogen reducing effect was limited. After low-temperature vacuum evaporation, the chloride ions in the concentrated solution are enriched, and 10% of concentrated solution is produced. The chloride ions, COD and ammonia nitrogen in the reclaimed water are reduced to the requirement of the production reuse water.
Example 2: the method for recycling the desulfurization wastewater comprises the following steps:
s1: discharging desulfurization wastewater generated in the desulfurization tower to a buffer tank, primarily reducing the COD value in the wastewater through stirring aeration oxidation, reducing the final COD value to below 103mg/L, precipitating suspended matters in the water to obtain filtrate A and filter residue A, and continuously performing air aeration for 30-40 min at a stirring rate of 300-400 r/min;
s2: adding the filtrate A in the step S1 into a reaction tank, adding calcium hydroxide and sodium metaaluminate into desulfurization wastewater in a certain proportion in the reaction tank, and removing most of chloride ions in the wastewater to obtain calcium aluminate precipitate; measuring 1000ml of desulfurization wastewater, measuring the chloride ion content of the desulfurization wastewater to be 15.21g/L, keeping the stirring speed to be 300-400r/min, keeping the temperature at 40 ℃, adding 82g of sodium metaaluminate to be dissolved, continuously adding 164g of calcium hydroxide for 60 minutes, and filtering to obtain the filtrate, wherein the chloride ion content of the filtrate is measured to be 4.02g/L, and the chloride ion content is reduced by more than 60%;
s3: after the reaction is finished, carrying out solid-liquid separation on the solid-liquid mixture after the reaction of S2, and carrying out plate-frame filter pressing to obtain filtrate B and filter residue B, wherein the filtrate B is chlorine-removing wastewater, and the filter residue B is calcium aluminum fluorite and can be used as building material additives such as cement;
s4: allowing the filtrate B with reduced chloride ions to flow into a clarifying tank for clarification, dripping about 5 drops of PAM for flocculation precipitation, and filtering to obtain filtrate C and filter residue C;
s5: the filtrate C of the S4 enters a low-temperature vacuum evaporation system to set the evaporation temperature to be 30-35 ℃, and the evaporation is carried out under a vacuum state of-97 kpa to obtain regenerated water A with the entering amount of about 90% and concentrated waste liquid with the chloride ion content of 0.39g/L, wherein the chloride ion reaches the standard of regeneration and reuse of waste water of a desulfurizing tower, so that the condition of co-boiling of chemicals in a high-temperature state is avoided;
s6: and (3) discharging the regenerated water A of the S5 into a biochemical pond for ammonia nitrogen biochemical treatment, further reducing the ammonia nitrogen content to below 130mg/L by adding a proper amount of ammonia nitrogen treating agent, finally reducing the ammonia nitrogen content to the content of a normal water body, wherein the COD (chemical oxygen demand) is 102.6mg/L, the ammonia nitrogen content is less than 128mg/L, and the regenerated water meets the requirement of industrial reuse water.
The results of the wastewater, reclaimed water and concentrate of example 2 are shown in Table 2.
TABLE 2 results of various tests on wastewater, regenerant and concentrate from example 2
| Cl - (g/L) | COD(mg/L) | Ammonia nitrogen (mg/L) | Liquid chromaticity | |
| Desulfurization waste water | 15.21 | 3100 | 1420 | Yellow colour |
| One-time chlorine removal | 4.02 | 2032 | 810 | Yellow colour |
| Concentrated solution | 45.0 | 5300 | 1200 | Brown color |
| Reclaimed water | 0.51 | 102.6 | 128 | Colorless and colorless |
As is clear from Table 2, the removal test of chlorine ions in high content in the desulfurization tower wastewater was conducted, and the same effect of chlorine ion removal was found. COD and ammonia nitrogen meet the requirements of the production and reuse water, and the reuse water is clear.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (10)
1. The method for recycling the desulfurization wastewater is characterized by comprising the following steps of:
s1: discharging the desulfurization wastewater to a buffer tank, reducing the COD value in the wastewater through stirring aeration, precipitating suspended matters in the water, and filtering to obtain filtrate A and filter residue A;
s2: adding the filtrate A in the step S1 into a reaction tank, and adding a calcium reagent and an aluminum reagent into the reaction tank, wherein the molar ratio of the calcium reagent to the aluminum reagent to the chloride ion content in the filtrate A is 5:2.5:1;
s3: carrying out solid-liquid separation on the solid-liquid mixture after the reaction of S2, and filtering to obtain filtrate B and filter residue B;
s4: flowing the filtrate B of the step S3 into a clarifier and putting PAM into the clarifier to perform flocculation precipitation reaction, and filtering to obtain filtrate C and filter residue C;
s5: the filtrate C of the S4 enters a low-temperature vacuum evaporation system, and the filtrate C is treated in a low-temperature reduced pressure distillation mode to obtain reclaimed water A;
s6: and (3) discharging the regenerated water A of the S5 into a biochemical pool for ammonia nitrogen biochemical treatment, and adding an ammonia nitrogen treating agent to reduce the ammonia nitrogen content to obtain regenerated water B.
2. The method for recycling desulfurization wastewater according to claim 1, wherein: the stirring speed in the step S1 is 300-400r/min, and the COD value in the wastewater is reduced by continuous air aeration for 30-40 min.
3. The method for recycling desulfurization wastewater according to claim 1, wherein: and (3) chlorine ions, a calcium reagent and an aluminum reagent in the S2 are subjected to stirring reaction to remove chlorine, wherein the stirring speed is 300-400r/min, the reaction temperature is 40 ℃, and the reaction time is 60min, so that the chlorine ion content in the filtrate B in the S3 is reduced to below 40% of the original wastewater.
4. A method for recycling desulfurization waste water according to claim 3, wherein: the calcium reagent in the S2 is calcium hydroxide or calcium oxide, and the aluminum reagent is sodium metaaluminate.
5. The method for recycling desulfurization wastewater according to claim 4, wherein: when the calcium reagent in the S2 is calcium hydroxide, the calcium hydroxide, sodium metaaluminate and chloride ion content in the filtrate A are mixed according to the following mass parts: 100 parts of calcium hydroxide, 57 parts of sodium metaaluminate and 10 parts of chloride ions in filtrate A.
6. The method for recycling desulfurization wastewater according to claim 1, wherein: the pH value of the filtrate B in the step S3 is controlled between 7 and 9.
7. The method for recycling desulfurization wastewater according to claim 1, wherein: and controlling the concentration of the solution after the PAM is added in the S4 to be within 5 PPM.
8. The method for recycling desulfurization wastewater according to claim 1, wherein: the filtrate C in S5 was boiled by evaporation at 30℃under a vacuum of-97 kpa.
9. The method for recycling desulfurization wastewater according to claim 1, wherein: and (3) separating the filtrate C in the step S5 into 10 parts of concentrated waste liquid and 90 parts of regenerated water A after low-temperature reduced pressure distillation condensation treatment.
10. The method for recycling desulfurization wastewater according to claim 1, wherein: and the ammonia nitrogen content of the regenerated water B in the S6 is below 130 mg/L.
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