CN116917242A - Treatment method of high-salt high-organic wastewater - Google Patents
Treatment method of high-salt high-organic wastewater Download PDFInfo
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- 235000011130 ammonium sulphate Nutrition 0.000 claims description 8
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- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a method for treating high-salinity high-organic wastewater, belonging to the technical field of wastewater treatment. The method comprises the following steps: adsorbing organic matters in the initial high-salt high-organic wastewater containing sodium sulfate by the activated carbon device, then analyzing the activated carbon device by adopting an organic solvent, and adsorbing the organic matters in the initial high-salt high-organic wastewater of the next round of analyzed activated carbon; the organic solvent contains methylene chloride. The method can effectively remove COD in the wastewater under the condition of lower treatment cost, and the COD content of the intermediate wastewater obtained after the organic matters are adsorbed by the activated carbon device can meet the requirement of directly entering an evaporative crystallization system, thereby being beneficial to continuous and stable operation of the system.
Description
Technical Field
The disclosure relates to the technical field of wastewater treatment, in particular to a method for treating high-salinity high-organic wastewater.
Background
The battery recovery industry adopts a wet leaching process to recover important metals to generate a large amount of high-salt high-organic wastewater, and the salt is mainly sodium sulfate. The wastewater has the salt content of external drainage or is subjected to desalting treatment by adopting processes such as evaporation crystallization and the like for recycling production. In order to keep the evaporative crystallization system running stably, prevent the generation of organic foam and reduce the amount of evaporation mother liquor, the COD of the incoming water must be reduced before entering the evaporative crystallization system.
Regarding removal of COD in wastewater, common methods include physical methods, chemical methods and biological methods, wherein biological methods are methods generally regarded as the lowest running cost. However, when the concentration of sodium chloride in the wastewater is not less than 4g/L or the total salt content is not less than 10g/L, the removal of COD cannot be performed by using a biological method with lower cost. Thus, such high-salt wastewater is generally treated by a process as shown in fig. 1, in which removal of COD is performed by chemical methods such as ozone oxidation or fenton, but such a treatment process is costly. The ozone oxidation method has high equipment requirement, large investment and higher power consumption. The Fenton method generates a large amount of Fenton sludge in addition to the high cost of the chemical, resulting in high sludge disposal cost.
In view of this, the present disclosure is specifically proposed.
Disclosure of Invention
The aim of the present disclosure is to provide a method for treating high-salt and high-organic wastewater, which can effectively remove COD in the wastewater under the condition of lower treatment cost, and is beneficial to subsequent desalting treatment.
The present disclosure may be implemented as follows:
the present disclosure provides a method for treating high-salinity high-organic wastewater, comprising the steps of:
adsorbing organic matters in the initial high-salt high-organic wastewater containing sodium sulfate by the activated carbon device, then analyzing the activated carbon device by adopting an organic solvent, and adsorbing the organic matters in the initial high-salt high-organic wastewater of the next round by the analyzed activated carbon device;
the organic solvent contains methylene chloride.
In an alternative embodiment, the initial high-salt high-organic wastewater includes at least one of the following characteristics:
characteristic one: the total salt content in the initial high-salt high-organic wastewater is not less than 10g/L;
and the second characteristic is: the concentration of sodium chloride in the initial high-salt high-organic wastewater is not lower than 4g/L;
and (3) the following characteristics: COD content in the initial high-salt high-organic wastewater is not less than 800mg/L.
In alternative embodiments, the total salt content in the initial high-salt high-organic wastewater is 10-300g/L, and/or the sodium chloride concentration in the initial high-salt high-organic wastewater is 4-40g/L; and/or the COD content in the initial high-salt high-organic wastewater is 800-5000mg/L; and/or the initial high-salt high-organic wastewater is high-salt high-organic wastewater in the battery recycling industry.
In an alternative embodiment, the high-salt, high-organic wastewater in the battery recovery industry includes at least one of battery recovery industry raffinate wastewater, battery recovery industry battery discharge wastewater, and battery recovery industry extracted saponification wastewater.
In an alternative embodiment, the activated carbon device is adsorbed to a saturated state and then subjected to an analytical treatment; and/or the solid-to-liquid ratio of the activated carbon to the organic solvent in the activated carbon device is 48g:1L-52g:1L.
In an alternative embodiment, the activated carbon device to be analyzed is dried first, and then the analysis treatment is performed;
drying includes at least one of the following features:
characteristic one: the water content of the activated carbon in the dried activated carbon device is not more than 10wt%;
and the second characteristic is: the drying is carried out at 100-110deg.C for 1.5-2.5 hr.
In an alternative embodiment, the organic matter is separated from the organic solvent by separating the organic matter from the separated solution.
In an alternative embodiment, the means of separation include: and converting the organic solvent in the analysis liquid into gas to be separated from the organic matters, so as to obtain the organic solvent and high-concentration organic wastewater.
In an alternative embodiment, the conversion of the organic solvent in the resolving fluid to a gas is performed at a temperature of greater than or equal to 35 ℃ and less than 100 ℃.
In an alternative embodiment, the separated organic solvent is subjected to the next round of activated carbon device analysis; and/or carrying out biochemical system treatment on the separated high-concentration organic wastewater.
In an alternative embodiment, the wastewater after the biochemical system treatment is subjected to the advanced treatment system treatment.
In an alternative embodiment, the initial high-salt high-organic wastewater is subjected to a conditioning tank treatment and a heavy coagulating sedimentation unit treatment, and then is subjected to an organic adsorption treatment by an activated carbon device.
In an alternative embodiment, the auxiliary agent is added during the treatment of the heavy coagulating sedimentation unit, so as to be regulatedHeavy metal and F in the first intermediate wastewater obtained after pool treatment - And forming a precipitate, and removing the precipitate to obtain second intermediate wastewater.
In an alternative embodiment, the processing method further comprises: carrying out reaction tank treatment on the third intermediate wastewater remained after the activated carbon device adsorbs organic matters;
in the treatment process of the reaction tank, ammonium bicarbonate and sodium sulfate in the third intermediate wastewater are added for double decomposition reaction.
In an alternative embodiment, the fourth intermediate wastewater obtained after the treatment in the reaction tank is subjected to solid-liquid separation to obtain sodium bicarbonate and fifth intermediate wastewater.
In an alternative embodiment, sodium bicarbonate is calcined to obtain sodium carbonate;
and/or deaminizing the fifth intermediate wastewater to obtain ammonia water and sixth intermediate wastewater.
In an alternative embodiment, ammonia is made into ammonium bicarbonate and returned to the reaction tank.
In an alternative embodiment, the sixth intermediate wastewater is subjected to a freeze crystallization treatment to yield sodium sulfate solids and a mother liquor.
In an alternative embodiment, solid sodium sulfate is added as a nucleus during the freeze crystallization process.
In an alternative embodiment, the sodium sulfate solids resulting from the freeze crystallization process are returned to the reaction tank.
In an alternative embodiment, the mother liquor is subjected to an evaporative crystallization treatment to yield ammonium sulfate and water.
In an alternative embodiment, the water from the evaporative crystallization process is used to dilute the initial high-salt, high-organic wastewater or effluent from the lower run.
The beneficial effects of the present disclosure include:
by using the activated carbon device, the activated carbon contained in the activated carbon device has a developed pore structure, and can effectively adsorb organic matters in the initial high-salt high-organic wastewater, thereby achieving the effect of separating the organic matters from the initial high-salt high-organic wastewater. The active carbon in the active carbon device is resolved through dichloromethane, so that organic matters adsorbed by the active carbon can be resolved more fully and thoroughly than other resolving agents, and the active carbon can be released more thoroughly, so that the active carbon device is favorable for having higher organic matter adsorption rate in each repeated use, improving the treatment capacity and reducing the treatment cost, and can maintain a relatively stable adsorption effect in each adsorption.
The method can effectively remove COD in the wastewater under the condition of lower treatment cost, and the COD content of the intermediate wastewater obtained after organic matters are adsorbed by the activated carbon device can meet the desalting requirement of directly entering an evaporative crystallization system, so that the continuous and stable operation of the system is facilitated, and the salt is effectively removed.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present disclosure, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present disclosure and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a process flow diagram for treating high-salt wastewater in the prior art;
fig. 2 is a flow chart of a process for treating high-salinity and high-organic wastewater in an embodiment of the disclosure.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The method for treating the high-salinity high-organic wastewater provided by the disclosure is specifically described below.
The disclosure provides a method for treating high-salt high-organic wastewater, which comprises the following steps: adsorbing organic matters in the initial high-salt high-organic wastewater containing sodium sulfate by the activated carbon device, then analyzing the activated carbon device by adopting an organic solvent, and adsorbing the organic matters in the initial high-salt high-organic wastewater of the next round by the analyzed activated carbon device;
the organic solvent contains methylene chloride.
For reference, the "salt" in the "high salt" includes at least sodium sulfate, and optionally sodium chloride and other forms of salt in the wastewater, and "high" means that the total salt content in the initial high-salt high-organic wastewater is not less than 10g/L. In some embodiments, the total salt content in the initial high-salt, high-organic wastewater may be 10-300g/L,10g/L, 20g/L, 30g/L, 40g/L, 50g/L, 60g/L, 70g/L, 80g/L, 90g/L, 100g/L, 150g/L, 200g/L, 250g/L, 300g/L, etc., and may be any other value in the range of 10-300 g/L.
"organic" in "high organic" refers to the COD content, COD refers to the chemical oxygen demand, which is the amount of reducing substances to be oxidized in a chemically measured water sample; "high" means that the organic content in the initial high-salt high-organic wastewater is not less than 800mg/L (i.e., the COD content in the initial high-salt high-organic wastewater is not less than 800 mg/L). In some embodiments, the organic content of the initial high-salt high-organic wastewater may be 800-5000mg/L (i.e., the COD content of the initial high-salt high-organic wastewater is 800-5000 mg/L), such as 800mg/L, 1000mg/L, 1500mg/L, 2000mg/L, 2500mg/L, 3000mg/L, 3500mg/L, 4000mg/L, 4500mg/L, 5000mg/L, etc., and may be any other value in the range of 800-5000 mg/L.
In some embodiments, the initial high-salt high-organic wastewater has a sodium chloride concentration of not less than 4g/L, further may be 4-40g/L, such as 4g/L, 10g/L, 15g/L, 20g/L, 25g/L, 30g/L, 35g/L, 40g/L, etc., and may be any other value in the range of 4-40 g/L.
The concentration of sodium chloride and the total salt content are related to the tolerance degree of microorganisms, and the concentration of sodium chloride is less than 4g/L or the total salt content is less than 10g/L, so that the microbial agent can be suitable for the survival of common microorganisms.
The initial high-salt high-organic wastewater used in the present disclosure may be, for example, high-salt high-organic wastewater in the battery recycling industry, and the total salt content and sodium chloride concentration in such wastewater satisfy the above ranges.
As an example, the high-salt and high-organic wastewater in the battery recycling industry can be raffinate wastewater in the battery recycling industry, wherein the salt in the wastewater is mainly sodium sulfate, and the wastewater also contains Ca 2+ And Mg (magnesium) 2+ And (3) plasma metal ions. The high-salt high-organic wastewater in the battery recycling industry can also be battery discharge wastewater in the battery recycling industry, the salt in the wastewater is mainly sodium sulfate, and the wastewater also contains F - And Ca 2+ And (3) plasma. The high-salt and high-organic wastewater in the battery recycling industry can also be the saponification wastewater extracted in the battery recycling industry, the salt in the wastewater is mainly sodium sulfate, and the wastewater also contains substances such as oil content, suspended matters and the like. Above Ca 2+ 、Mg 2+ All of the F-, oil and suspended matter can be removed by the heavy coagulating sedimentation unit treatment described below.
In some embodiments, the initial high-salt high-organic wastewater can be subjected to a conditioning tank treatment and a heavy coagulating sedimentation unit treatment, and then subjected to an organic adsorption treatment by an activated carbon device.
For convenience of distinction, the organic wastewater treated by the regulating reservoir is hereinafter referred to as "first intermediate wastewater", the organic wastewater regulated by the pH regulator is hereinafter referred to as "second intermediate wastewater", and the wastewater remaining after the activated carbon device adsorbs the organic matter is hereinafter referred to as "third intermediate wastewater".
In the present disclosure, the effect of the regulating tank mainly includes regulating water quantity and balancing water quality, and the initial high-salt high-organic wastewater can be regulated after entering the regulating tank, so that the water quality is uniform and the water quantity is stable.
The heavy coagulating sedimentation unit is mainly used for leading Ca in the first intermediate wastewater 2+ 、Mg 2+ 、F - Substances such as oil and/or suspended substances form precipitates, which can be removed therefrom by solid-liquid separation (e.g., filtration, etc.).
When the high-salt high-organic wastewater in the battery recycling industry isWhen the raffinate waste water in the battery recycling industry is treated by the heavy coagulating sedimentation unit, the pH regulator is added into the waste water to ensure that Ca in the first intermediate waste water 2+ And Mg (magnesium) 2+ And forming a precipitate, and removing the precipitate to obtain second intermediate wastewater.
By way of example, the pH adjuster may include NaOH. That is, in some embodiments, the pH adjuster may be a mixture of NaOH and other substances that have a similar effect as pH adjusters. In other embodiments, the pH adjuster may also be NaOH alone.
Ca in the first intermediate wastewater can be caused by using NaOH as a pH regulator 2+ And Mg (magnesium) 2+ Form hydroxide precipitate and Na in NaOH + Ca in the first intermediate wastewater 2+ And Mg (magnesium) 2+ The hardness of the second intermediate wastewater is greatly reduced compared with that of the first organic intermediate wastewater.
As a reference, ca in the first intermediate wastewater 2+ And Mg (magnesium) 2+ The precipitate can be formed at a pH of 10-11. The pH may be 10, 10.1, 10.2, 10.3, 10.4, 10.5, 10.6, 10.7, 10.8, 10.9 or 11, etc., or any other value within the range of 10 to 11. At this pH range, ca in the first intermediate wastewater can be caused to 2+ And Mg (magnesium) 2+ And the like are sufficiently precipitated.
When the high-salt high-organic wastewater in the battery recycling industry is the battery discharge wastewater in the battery recycling industry, sulfuric acid and calcium hydroxide are added in the treatment process of the heavy coagulating sedimentation unit, and the pH value of the system is controlled to be 9-10 so as to ensure that F in the first intermediate wastewater - The calcium fluoride precipitate formed is removed. Then adding calcium carbonate to make Ca in the first intermediate waste water 2+ Is removed in the form of calcium carbonate precipitate.
When the high-salt high-organic wastewater in the battery recovery industry is the saponification wastewater extracted in the battery recovery industry, a coagulant (such as polyaluminum chloride (PAC) and a flocculant (such as Polyacrylamide (PAM)) can be added in the treatment process of the heavy coagulation sedimentation unit to form sediment for oil content and suspended matters in the first intermediate wastewater and remove the sediment.
In the present disclosure, the activated carbon device may be an activated carbon column, and in addition, may be other activated carbon-containing adsorption devices.
By using the activated carbon device, the activated carbon contained in the activated carbon device has a developed pore structure, and can effectively adsorb organic matters in the initial high-salt high-organic wastewater, thereby achieving the effect of separating the organic matters from the initial high-salt high-organic wastewater.
In some embodiments, the activated carbon device is adsorbed to saturation and then subjected to a desorption treatment.
For reference, the solid to liquid ratio of activated carbon to organic solvent in the activated carbon device may be 48g:1L-52g:1L, such as 48g:1L, 48.5g:1L, 49g:1L, 49.5g:1L, 50g:1L, 50.5g:1L, 51g:1L, 51.5g:1L, or 52g:1L, etc., and may be any other value in the range of 48g:1L-52g:1L.
If the solid-to-liquid ratio of the activated carbon to the organic solvent in the activated carbon device is lower than 48g:1L (e.g., 45 g:1L), the organic solvent is excessive, thus increasing unnecessary cost and further increasing the subsequent rectification operation cost; if the solid-to-liquid ratio of the activated carbon to the organic solvent in the activated carbon device is higher than 48 g/1L (e.g., 50 g/1L), the analysis of COD in the activated carbon and the circulation of the activated carbon are not facilitated.
In some embodiments, the organic solvent is pure dichloromethane; in other embodiments, the organic solvent may be a mixed solution of dichloromethane and other solvents capable of adsorbing organic matters.
The activated carbon is analyzed by the organic solvent, so that organic matters adsorbed by the activated carbon can be transferred into the organic solvent, and the regeneration and the recycling of the activated carbon are realized.
The inventor researches and creatively obtains that: the active carbon in the active carbon device is resolved by methylene dichloride, so that organic matters adsorbed by the active carbon can be resolved more fully and thoroughly than other resolving agents, and the active carbon is released more thoroughly, so that the active carbon device is favorable for having higher organic matter adsorption rate in each repeated use, thereby being favorable for improving the treatment capacity and reducing the treatment cost, and is favorable for keeping a relatively stable adsorption effect in each adsorption.
In some embodiments, the activated carbon device to be parsed may be dried prior to the parsing process.
The moisture content of the activated carbon in the activated carbon device after drying is not more than 10wt%, for example, the moisture content of the activated carbon in the activated carbon device after drying may be 10wt%, 9wt%, 8wt%, 7wt%, 6wt%, 5wt%, 4wt%, 3wt%, 2wt% or 1wt%, etc., or may be any other value within a range of not more than 10wt%.
Illustratively, the drying may be performed at 100-110deg.C (e.g., 100deg.C, 112 deg.C, 115deg.C, 118 deg.C or 120deg.C, etc.) for 1.5-2.5h (e.g., 1.5h, 2h or 2.5h, etc.). The water content of the activated carbon can be reduced to not more than 10wt% after drying according to the method.
The active carbon device to be resolved is firstly dried and then resolved, so that the water content of the active carbon can be reduced, and the phenomenon that part of organic matters are mutually soluble with water, so that the organic matters are brought out of the water mutually soluble with the organic matters in the process of transferring the organic matters to dichloromethane is avoided, and the resolution of the dichloromethane to the organic matters is reduced.
Further, separating the organic matters from the organic solvent by using the analysis solution for analyzing the organic matters to obtain the separated organic solvent and the high-concentration organic wastewater after the organic solvent is removed.
For reference, the separation means may include: and converting the organic solvent in the analysis liquid into gas to be separated from the organic matters, so as to obtain the organic solvent and high-concentration organic wastewater.
In some embodiments, the conversion of the organic solvent in the resolved liquid to a gas is performed at a temperature greater than or equal to 35 ℃ and less than 100 ℃. The process can be carried out in a rectifying tower, and the organic solvent is fully converted into gas under the temperature condition by utilizing the difference of the boiling points of the organic solvent and the organic matters in the analysis liquid, and meanwhile, the organic matters still keep the original phase state (non-gaseous state), so that the separation of the organic solvent and the organic matters in the analysis liquid is realized. Under the above conditions, water is still in liquid form.
It is noted that the condition of 35 ℃ or higher can reduce the energy consumption; if the temperature is too high, part of organic matters in the analysis liquid can be carried out, so that the recovered organic solvent is impure, and the analysis effect of the next round of activated carbon device after subsequent recovery is affected.
Further, the separated organic solvent is recovered, and the recovered organic solvent can be used for next round of analysis of the activated carbon device. The recovery of the organic solvent may be carried out by condensation, for example.
The high-concentration organic wastewater obtained by the separation contains little salt, and even if the high-concentration organic wastewater contains salt, the high-concentration organic wastewater contains the salt, the content of the high-concentration organic wastewater is a concentration which can be adapted to a microbiological method, such as the concentration of sodium chloride is less than 4g/L or the total salt content is less than 10g/L. Therefore, the high-concentration organic wastewater can directly enter a biochemical system, and COD in the high-concentration organic wastewater is degraded by adopting a biological method.
Furthermore, the wastewater treated by the biochemical system can enter the advanced treatment system for treatment, so that the COD in the corresponding wastewater can reach the discharge standard.
In the present disclosure, the third intermediate wastewater may also be subjected to a reaction tank treatment.
For reference, ammonium bicarbonate may be added during the tank process to double-decompose with sodium sulfate in the third intermediate wastewater to produce sodium bicarbonate and ammonium sulfate.
For convenience of distinction, the wastewater obtained after the treatment in the reaction tank is referred to as "fourth intermediate wastewater".
Further, the fourth intermediate wastewater is subjected to solid-liquid separation to obtain sodium bicarbonate and fifth intermediate wastewater.
For reference, the sodium bicarbonate obtained may be calcined to obtain soda ash (which may be recycled for production). In addition, the fifth intermediate wastewater may be deaminated in a deamination system to obtain ammonia and a sixth intermediate wastewater.
Further, ammonia water can be recovered and then reacted with carbon dioxide to prepare ammonium bicarbonate, and the ammonium bicarbonate can be returned to the reaction tank again for recycling. In addition, the sixth intermediate wastewater can be subjected to freezing crystallization treatment in a freezing crystallization system, and the ammonium sulfate is crystallized from the liquid by cooling and controlling the temperature, so that sodium sulfate solid and mother liquor are obtained. In some alternative embodiments, solid sodium sulfate may be added as a nucleus during the freeze crystallization process to increase the crystallization rate of sodium sulfate.
The sodium sulfate solid obtained by the freezing crystallization treatment can be returned to the reaction tank at the front end for recycling. In addition, the mother liquor obtained in the freezing crystallization treatment process can be subjected to evaporation crystallization treatment in an evaporation crystallization system to obtain ammonium sulfate and water. The evaporative crystallization system converts water in the mother liquor into steam in a heating mode, and distilled water is formed after the steam is condensed. Most of ammonium sulfate in the mother liquor is separated out to form solid particle crystals, and the rest small part of the mother liquor enters a mother liquor treatment system for further treatment. It is noted that most COD in the initial high-salt high-organic wastewater is separated and removed by the activated carbon device, and COD in the water obtained by freezing and crystallizing treatment meets the requirement of directly entering an evaporation and crystallization system, so that the system can continuously and stably run.
Further, the distilled water obtained by the evaporation and crystallization treatment can be used for diluting high-concentration organic wastewater or directly recycling production or directly discharging.
The features and capabilities of the present disclosure are described in further detail below in connection with the examples.
Example 1
The embodiment provides a treatment process of raffinate (high-salt high-organic) wastewater in a battery recycling industry, referring to fig. 2, comprising the following steps:
step (1): the raffinate (high-salt high-organic) wastewater is used as initial high-salt high-organic wastewater to enter an adjusting tank first, so as to obtain first intermediate wastewater. Feeding the first intermediate wastewater into a heavy coagulating sedimentation unit which controls the pH to 10-11 by adding sodium hydroxide so that the Mg in the first intermediate wastewater 2+ And Ca 2+ And hydroxide precipitate is formed and removed to obtain second intermediate wastewater.
The raffinate (high-salt and high-organic) wastewater in the battery recycling industry contains sodium sulfate and COD, wherein the concentration of the sodium sulfate is 150g/L, and the concentration of the COD is 1200mg/L.
Step (2): and (3) enabling the second intermediate wastewater to enter an activated carbon column, and enabling the activated carbon column to adsorb and filter organic matters contained in the second intermediate wastewater until the activated carbon column is saturated in adsorption. Subsequently, the saturated activated carbon column was subjected to a drying treatment at 105℃for 2 hours. And analyzing the dried activated carbon column by using dichloromethane, so that the organic matters adsorbed in the activated carbon column are transferred into the dichloromethane, wherein the solid-to-liquid ratio of the activated carbon in the activated carbon column to the dichloromethane is 50 g/1L.
And (3) carrying out organic adsorption on the initial high-salt high-organic wastewater to be treated in the next round by the resolved regenerated active carbon column.
And (3) sending the dichloromethane containing the organic matters into a rectifying tower, heating to 35 ℃ to change the dichloromethane into steam, condensing and recycling the steam, and then analyzing the steam by using an activated carbon column for the next round. In this way, the organics are concentrated and the salt content is very low. The COD index of the third intermediate wastewater remained after the organic matters are adsorbed by the activated carbon column is stable, and the whole equipment is convenient to operate and manage.
Step (3): and (3) feeding the third intermediate wastewater into a reaction tank, and adding 83g/L of ammonium bicarbonate and sodium sulfate in the third intermediate wastewater to perform double decomposition reaction to obtain fourth intermediate wastewater containing sodium bicarbonate and ammonium sulfate. And carrying out solid-liquid separation on the fourth intermediate wastewater to obtain sodium bicarbonate and fifth intermediate wastewater. Calcining the sodium bicarbonate solid at 280 ℃ to obtain sodium carbonate for reuse in production.
Step (4): and (3) introducing the fifth intermediate wastewater into a deamination system for deamination treatment to obtain ammonia water and sixth intermediate wastewater. Introducing carbon dioxide into ammonia water, and introducing the ammonia water into a reaction tank in the step (3) with the mass ratio of 1:1.6 to prepare ammonium bicarbonate.
Step (5): and (3) carrying out freezing crystallization treatment on the sixth intermediate wastewater in a freezing crystallization system, wherein the freezing temperature is 10 ℃, so that ammonium sulfate is crystallized out of the liquid, and sodium sulfate solid and mother liquor are obtained. In the process of the freezing and crystallizing treatment, 0.15g/L solid sodium sulfate is added into a freezing and crystallizing system to serve as crystal nucleus. And (3) returning the sodium sulfate solid obtained by freezing and crystallizing treatment to the reaction tank of the step (3) again for continuous reaction.
Step (6): and (3) carrying out evaporation crystallization treatment on the mother liquor obtained in the step (5) in an evaporation crystallization system, wherein the evaporation temperature is 105 ℃, the evaporation reaction time is about 2 hours, water in the mother liquor is converted into steam, the steam is condensed to form distilled water, and part of the distilled water is used for diluting the high-concentration organic wastewater according to the COD concentration condition of the high-concentration organic wastewater, and the part of the distilled water is directly recycled for production. Most of COD in the initial high-salt high-organic wastewater is separated and removed by the activated carbon column, and COD in the mother liquor meets the requirement of directly entering an evaporative crystallization system, so that the system can continuously and stably run.
Step (7): the COD concentration of the high-concentration organic matter wastewater separated by the activated carbon column in the step (2) is about 60000mg/L, and salt is hardly brought in from the wastewater, and the salt in the high-concentration organic matter wastewater is the concentration adaptable to a microbiological method, so that the COD in the high-concentration organic matter wastewater is directly degraded by a biological method, and after biological treatment, the COD can be further treated by an advanced treatment system to reach the discharge standard.
Example 2
This embodiment differs from embodiment 1 in that: the initial high-salt high-organic wastewater is battery discharge (high-salt high-organic) wastewater in the battery recycling industry, and the battery discharge (high-salt high-organic) wastewater in the battery recycling industry contains fluoride ions, sodium sulfate, COD and the like, wherein the concentration of the fluoride ions is 150mg/L, the concentration of the sodium sulfate is 55g/L, and the concentration of the COD is 5000mg/L.
The wastewater treatment process comprises the following steps:
step (1): and (3) discharging the battery (high-salt high-organic) wastewater firstly enters an adjusting tank, and adjusting the water quality and the water quantity to obtain first intermediate wastewater. The first intermediate wastewater enters a defluorination and coagulation precipitation unit, and the pH value of the unit is controlled to be 9-10 by adding sulfuric acid and calcium hydroxide, so that fluoride ions in the first intermediate wastewater can form calcium fluoride precipitates for removal. Subsequently, the wastewater after the removal of fluoride ions is sent to a calcium-removing coagulating sedimentation unit, which adds sodium carbonate to make Ca in the first intermediate wastewater 2+ And forming calcium carbonate precipitate for further removal to obtain second intermediate wastewater.
The rest of the procedure is the same as in example 1.
Example 3
This embodiment differs from embodiment 1 in that: the initial high-salt high-organic wastewater is the extraction saponification (high-salt high-organic) wastewater in the battery recycling industry, and the extraction saponification (high-salt high-organic) wastewater in the battery recycling industry contains oil content, sodium sulfate, COD and the like, wherein the oil content is 80mg/L, the sodium sulfate content is 12000mg/L, and the COD concentration is 800mg/L.
The wastewater treatment process comprises the following steps:
step (1): the extraction and saponification (high-salt and high-organic) wastewater firstly enters an adjusting tank, and the water quality and the water quantity are adjusted to obtain first intermediate wastewater. And (3) the first intermediate wastewater enters a heavy coagulating sedimentation unit, and the unit enables oil content and suspended matters in the first intermediate wastewater to form sediment and further remove the sediment under the coagulating sedimentation effect by adding PAC and PAM, so as to obtain second intermediate wastewater.
Example 4
This embodiment differs from embodiment 1 in that: the solid-to-liquid ratio of the activated carbon to the organic solvent in the activated carbon device was 48g:1L.
Example 5
This embodiment differs from embodiment 1 in that: the solid-to-liquid ratio of the activated carbon to the organic solvent in the activated carbon device was 50g:1L.
Example 6
This embodiment differs from embodiment 1 in that: drying was carried out at 100℃for 2.5h.
Example 7
This embodiment differs from embodiment 1 in that: drying was carried out at 110℃for 1.5h.
Comparative example 1
The difference between this comparative example and example 1 is that: the raffinate (high-salt high-organic) wastewater was subjected to biological degradation of COD in the high-salt wastewater, and then to steps (1) to (6) in example 1.
Comparative example 2
The difference between this comparative example and example 2 is that: the COD in the high-salt wastewater is degraded by a biological method firstly by discharging the battery (high-salt high-organic) wastewater, and then the steps (1) to (7) in the embodiment 2 are carried out.
Comparative example 3
The difference from example 2 is that: the COD in the high-salt wastewater is degraded by the biological method firstly by the wastewater of extraction and saponification (high-salt high-organic matter), and then the steps (1) to (7) in the embodiment 3 are carried out.
Comparative example 4
The difference from example 1 is that: the activated carbon column was resolved using petroleum ether.
Test examples
The initial high-salt high-organic wastewater was treated as in examples 1-7 and comparative examples 1-4, each of which was repeated for 5 rounds of all steps, except for round 1, with the activated carbon columns used in each round of treatment being the corresponding regenerated activated carbon columns after the 1 st round of resolution. The COD content and the metal ion concentration in distilled water obtained after the evaporative crystallization treatment during the last 1 round of treatment were examined, and the results are shown in Table 1.
TABLE 1 COD content and Metal ion concentration in distilled water
As can be seen from the comparison of example 1 and comparative example 1, example 2 and comparative example 2, example 3 and comparative example 3: the method provided by the embodiment of the disclosure has higher COD and metal ion removal effect than the corresponding comparative example. As can be seen from comparative example 1 and comparative example 4: the dichloromethane is adopted to analyze the activated carbon column, so that the analyzed activated carbon column has better COD adsorption effect after repeated use compared with petroleum ether (probably because the dichloromethane can more thoroughly and fully analyze the organic matters adsorbed in the activated carbon column compared with other organic reagents, more re-acting space is provided, and further higher organic matter adsorption capacity is stably maintained during each repeated use), so that the COD content in distilled water obtained after the evaporation and crystallization treatment is obviously reduced.
In addition, in comparative examples 1 to 3, COD in the high-salt wastewater is degraded by a biological method, the requirement on related microorganisms is high, and the high-salt-resistant microorganisms are needed, so that the treatment cost is greatly increased and the running stability of a biochemical system is reduced; and the COD in the degraded wastewater hardly reaches the standard of direct discharge, and the residual COD is required to be adsorbed and removed by using activated carbon continuously. According to the embodiment of the disclosure, the activated carbon device is adopted to adsorb COD in the initial high-salt high-organic wastewater, so that the high-concentration organic wastewater which hardly contains salt or has very low salt can be obtained, and based on the high-concentration organic wastewater, the COD in the high-concentration organic wastewater can be degraded by adopting general microorganisms (without being high-salt-resistant microorganisms).
In summary, the present disclosure uses an activated carbon device to separate organic matters from the initial high-salt high-organic wastewater, the COD concentration of the separated high-organic wastewater is about 60000mg/L, and almost no salt is carried in from the wastewater, thereby satisfying the conditions of direct treatment by a microbiological method. The biological method is used for degrading organic matters in the wastewater, and compared with the conventional technology using ozone oxidation, fenton and other chemical methods under the same salt, the method has the advantage that the running cost is greatly saved. And the organic matters are separated from the initial high-salt high-organic wastewater by using the activated carbon device, so that the concentration of the organic matters is concentrated to 3-50 times of the original concentration, the total water content of the filtrate from the activated carbon column is 2% -33% of the original wastewater, and the scale and the running cost of the subsequent COD treatment facilities can be greatly reduced. In addition, the active carbon in the active carbon device is resolved by methylene dichloride, and organic matters adsorbed by the active carbon can be resolved more fully and thoroughly than other resolving agents, so that the active carbon can be released more thoroughly, on one hand, the active carbon device is favorable for having higher organic matter adsorption rate in each repeated use, thereby being favorable for improving the treatment capacity and reducing the treatment cost, and on the other hand, the active carbon device is favorable for keeping a more stable adsorption effect in each adsorption.
Industrial applicability
The method for treating the high-salt and high-organic wastewater is simple to operate, and can effectively adsorb organic matters in the initial high-salt and high-organic wastewater by using the activated carbon device, so that the effect of separating the organic matters from the initial high-salt and high-organic wastewater is achieved. The active carbon in the active carbon device is resolved through dichloromethane, so that organic matters adsorbed by the active carbon can be resolved sufficiently and thoroughly, on one hand, the method is favorable for having higher organic matter adsorption rate in each repeated use, is favorable for improving the treatment capacity and reducing the treatment cost, and on the other hand, the method is favorable for keeping relatively stable adsorption effect in each adsorption. The treatment method provided by the disclosure can effectively remove COD in the wastewater under the condition of lower treatment cost, and the COD content of the intermediate wastewater obtained after organic matters are adsorbed by the activated carbon device can meet the requirement of desalting by directly entering the evaporation crystallization system, so that the continuous and stable operation of the system is facilitated, and the salt is effectively removed.
Claims (20)
1. The method for treating the high-salinity high-organic wastewater is characterized by comprising the following steps of:
adsorbing organic matters in the initial high-salt high-organic wastewater containing sodium sulfate by using the activated carbon device, then analyzing the activated carbon device by using an organic solvent, and adsorbing the organic matters in the initial high-salt high-organic wastewater of the next round by using the analyzed activated carbon device;
the organic solvent contains methylene dichloride.
2. The process of claim 1, wherein the initial high-salt, high-organic wastewater comprises at least one of the following characteristics:
characteristic one: the total salt content in the initial high-salt high-organic wastewater is not less than 10g/L;
and the second characteristic is: the concentration of sodium chloride in the initial high-salt high-organic wastewater is not lower than 4g/L;
and (3) the following characteristics: the COD content in the initial high-salt high-organic wastewater is not less than 800mg/L.
3. The process according to claim 2, wherein the total salt content in the initial high-salt high-organic wastewater is 10-300g/L and/or the sodium chloride concentration in the initial high-salt high-organic wastewater is 4-40g/L; and/or the COD content in the initial high-salt high-organic wastewater is 800-5000mg/L; and/or the initial high-salt high-organic wastewater is high-salt high-organic wastewater in the battery recycling industry.
4. The method of claim 3, wherein the high-salt, high-organic wastewater in the battery recovery industry comprises at least one of battery recovery industry raffinate wastewater, battery recovery industry battery discharge wastewater, and battery recovery industry extraction saponification wastewater.
5. The method according to any one of claims 1 to 4, wherein the activated carbon device is adsorbed to a saturated state and then subjected to a desorption treatment;
and/or the solid-to-liquid ratio of the activated carbon in the activated carbon device to the organic solvent is 48g:1L-52g:1L.
6. The method according to any one of claims 1 to 5, wherein the activated carbon device to be analyzed is dried and then subjected to the analysis treatment;
drying includes at least one of the following features:
characteristic one: the water content of the activated carbon in the dried activated carbon device is not more than 10wt%;
and the second characteristic is: the drying is carried out at 100-110deg.C for 1.5-2.5 hr.
7. The method according to any one of claims 1 to 6, wherein the organic matter and the organic solvent are separated from the solution for analysis of the organic matter.
8. The method of claim 7, wherein the separating means comprises: and converting the organic solvent in the analysis liquid into gas to be separated from the organic matters, so as to obtain the organic solvent and high-concentration organic wastewater.
9. The method according to claim 8, wherein the conversion of the organic solvent in the analytical solution into a gas is performed at a temperature of 35 ℃ or higher and 100 ℃ or lower.
10. The process according to claim 8 or 9, wherein the separated organic solvent is subjected to a next round of activated carbon device resolution; and/or carrying out biochemical system treatment on the separated high-concentration organic wastewater.
11. The method according to claim 10, wherein the wastewater treated by the biochemical system is subjected to further treatment by the advanced treatment system.
12. The process according to claims 1-11, wherein the initial high-salt high-organic wastewater is subjected to a conditioning tank treatment and a heavy coagulating sedimentation unit treatment, followed by an organic adsorption treatment with an activated carbon device.
13. The method according to claim 12, wherein an auxiliary agent is added during the treatment of the heavy coagulating sedimentation unit to make the heavy metals and F in the first intermediate wastewater obtained after the treatment of the regulating reservoir - And forming a precipitate, and removing the precipitate to obtain second intermediate wastewater.
14. The process of any one of claims 1-13, further comprising: carrying out reaction tank treatment on the third intermediate wastewater remained after the activated carbon device adsorbs organic matters;
and in the treatment process of the reaction tank, adding ammonium bicarbonate and sodium sulfate in the third intermediate wastewater to carry out double decomposition reaction.
15. The method according to claim 14, wherein the fourth intermediate wastewater obtained after the treatment in the reaction tank is subjected to solid-liquid separation to obtain sodium bicarbonate and a fifth intermediate wastewater.
16. The process of claim 15, wherein the sodium bicarbonate is calcined to provide sodium carbonate;
and/or deaminizing the fifth intermediate wastewater to obtain ammonia water and sixth intermediate wastewater.
17. The process of claim 16, wherein the aqueous ammonia is made into ammonium bicarbonate and returned to the reaction tank;
and/or performing freezing crystallization treatment on the sixth intermediate wastewater to obtain sodium sulfate solid and mother liquor.
18. The method according to claim 17, wherein sodium sulfate as a crystal nucleus is added during the freeze crystallization treatment.
19. The method according to claim 17, wherein the sodium sulfate solid obtained by the freeze crystallization treatment is returned to the reaction tank;
and/or evaporating and crystallizing the mother solution to obtain ammonium sulfate and water.
20. The process of claim 19, wherein the water from the evaporative crystallization process is used to dilute the initial high-salt high-organic wastewater or effluent from the lower run.
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