CN115677090A - Method for recycling electroplating chromium-containing wastewater - Google Patents
Method for recycling electroplating chromium-containing wastewater Download PDFInfo
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- CN115677090A CN115677090A CN202211229291.2A CN202211229291A CN115677090A CN 115677090 A CN115677090 A CN 115677090A CN 202211229291 A CN202211229291 A CN 202211229291A CN 115677090 A CN115677090 A CN 115677090A
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Abstract
The invention discloses a method for recycling electroplating chromium-containing wastewater, which comprises the following steps: (1) filtering the electroplating chromium-containing wastewater to remove impurities; (2) Adjusting the pH of the electroplating chromium-containing wastewater in the step (1) to 2-3, then, adjusting the pH of the effluent adsorbed by an anion resin exchange column to 5, and then, entering an cation resin exchange column for ion exchange until the concentration of Cr (VI) in the wastewater reaches the standard; the anion resin of the anion resin exchange column is chromium-specific adsorption resin; the cation resin of the cation resin exchange column is strong acid type cation exchange resin; (3) Stopping exchange, and respectively eluting and regenerating the anion resin exchange column and the cation resin exchange column; (4) And (4) leaching and regenerating the anion resin exchange column in the step (3) to obtain a regenerated liquid, removing sodium from the regenerated liquid through a sodium ion exchange column, and evaporating and concentrating to obtain a chromium plating solution, wherein the chromium plating solution is used for an electroplating process, so that the treatment cost is reduced.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to a resource utilization method of electroplating chromium-containing wastewater.
Background
Chromium plating is a common material surface treatment process, and a large amount of waste water is generated in the process, and the sources of the waste water comprise a plating part washing and bleaching process, plating bath waste liquid, a passivation process and the like. Anions present in wastewater include the following: crO 4 2- 、Cr 2 O 7 2- 、SO 4 2- 、Cl - The cation comprises: cr (chromium) component 3+ 、H + 、Cu 2+ 、Ni 2+ 、Zn 2+ And the like, two valence states of chromium mainly exist in the electroplating wastewater: trivalent chromium (Cr (III)) and hexavalent chromium (Cr (VI)), the Cr (III) being derived from cations and the Cr (VI) being derived from anions. The discharge standard of the electroplating pollutants (GB 21900-2008) requires that the concentration of Cr (VI) in the wastewater is less than 0.2mg/L [2] . In the regional electroplating industrial park in China at present, the chromium-containing wastewater accounts for about 20 percent of the total amount of the electroplating wastewater, the concentration is 500-1000mg/L, 0.8-1.2 tons of chromium-containing sludge (the water content is 70 percent) are generated in each 100 tons of chromium-containing wastewater, the disposal cost of a single ton of chromium sludge is about 750-1500 yuan, the disposal cost of sludge is reduced to water quantity of about 10-20 yuan/ton of water, and the disposal cost of chromium-containing wastewater is 20-30 yuan/ton; the cost for treating chromium-containing waste water is 480-720 ten thousand yuan per year based on the electroplating industrial park with the scale of 4000 tons/day (about 20 percent of chromium-containing water), and 1920-2880 tons of chromium mud is produced.
The treatment method aiming at the single chromium-containing wastewater comprises a chemical precipitation method, a ferrite method, a membrane separation technology, an adsorption method and an ion exchange methodMethod, extraction method, photocatalytic method, electrolytic method, biological method ] And so on. Wherein the chemical precipitation method is a method commonly adopted in domestic electroplating process, and the method comprises the steps of firstly adding iron powder, sodium sulfite and FeSO into the wastewater 4 Reducing agent to remove Cr in wastewater 6+ Conversion to Cr 3+ Then adding alkaline agent such as lime or NaOH to the obtained Cr 3+ Conversion to Cr (OH) 3 And precipitating to remove chromium in the wastewater. Although the method has the advantages of simple operation and high removal rate, the method has the defects that a large amount of chromium-containing sludge generated by precipitation can cause secondary pollution, and enterprises with hazardous solid waste disposal qualification need to be entrusted to carry out retreatment. Moreover, the obtained chromium sludge not only has low utilization value and inconvenient transportation and storage, but also needs to pay high sludge disposal cost.
Disclosure of Invention
Based on the background technology, the application provides a method for treating the electroplating chromium-containing wastewater, so that the chromium in the wastewater can be recycled and reused in a chromium plating tank after treatment, and the chromium can be used as a raw material of a chromium plating process, thereby reducing the treatment cost.
In order to solve the technical problems, the specific method is that anion resin is used for adsorbing hexavalent chromium, cation resin is used for adsorbing Cr (III), copper, zinc, nickel and iron ions, and anion resin regeneration liquid is subjected to sodium removal and concentration;
wherein, the anion resin adsorbs hexavalent chromium and the cation resin adsorbs copper, zinc, nickel and iron ions, and the main steps are as follows:
filtering the chromium-containing wastewater to remove impurities in the chromium-containing wastewater;
adjusting the pH value of the pretreated electroplating chromium-containing wastewater to 2-3 by using hydrochloric acid, introducing into an anion resin exchange column (a first exchange column) to recover anion hexavalent chromium, adjusting the pH value of effluent after anion resin adsorption to 5, and introducing into an cation resin exchange column (a second exchange column) to recover copper, zinc, nickel and iron ions to obtain chromium-removing wastewater with low index concentration, wherein the concentration of Cr (VI) is less than or equal to 0.2mg/L; and after the exchange column reaches a saturated state, eluting, desorbing and regenerating, collecting desorbed regeneration liquid of the first exchange column, removing sodium from the regeneration liquid, and concentrating.
The regeneration liquid sodium removal and concentration method mainly comprises the following steps:
introducing the chromium-containing regenerated liquid into a sodium ion exchange column for sodium removal;
evaporating and concentrating the hexavalent chromium regeneration solution subjected to sodium removal treatment;
preferably, the wastewater treated by the anion resin exchange column and the cation resin exchange column in the step (2) is used as the washing water for the pretreatment of the electroplating process.
Preferably, the concentration range of Cr (VI) in the chromium-containing electroplating wastewater is 400-900mg/L; the concentration of Cr (VI) in the wastewater after reaching the standard is less than or equal to 0.2mg/L.
Preferably, the concentration of Cr (VI) in the chromium plating solution after the evaporation concentration is 600-900g/L.
Preferably, the sulfate ion in the solution can be further removed after evaporation and concentration, and barium carbonate can be added to remove the sulfate ion. The molar ratio of barium carbonate added to sulfate was 1:1, depending on the concentration of sulfate in the solution.
Preferably, the elution of the anion exchange column is as follows: after the leacheate is washed by water, backwashing is a known means in the field, and the method specifically comprises the following steps: rinsing with clear water for 20-30min; the leacheate is 10-15wt% NaOH solution, the leacheate is leached into the exchange column from top to bottom, the mixture is kept standing for 40-60min after 20-40min, and the step is repeated until Cr (VI) is not detected by the exchange column; the cation resin exchange column is washed by 20-30wt% sulfuric acid after being washed by an eluent and back washed.
Preferably, the elution of the anion exchange column is as follows: the method comprises the following steps of leaching with an acidic leaching solution, leaching with an alkaline leaching solution, and backwashing, and specifically comprises the following steps: spraying 5-10wt% hydrochloric acid via regeneration pipeline for 20-30min by hydrochloric acid dosing device, washing with clear water to neutral, introducing 10-15wt% NaOH via liquid alkali dosing device, with spraying speed of 2BV/h, spraying time of 30-60min, and standing time of 30-60min; the Cr (VI) can not be detected when the column is reciprocated to the exchange column; washing with clear water for 30-60min;
the chromium-specific adsorption resin is strong base anion exchange resin with a polystyrene framework; the strong acid type cation exchange resin is strong acid styrene cation resin.
Advantageous effects
(1) This application is through constituting ion exchange system by anion resin (first exchange column) and cation resin (second exchange column), adsorbs chromium ion and other positive ions (copper, nickel, zinc and iron) in the electroplating effluent respectively, and each ion concentration satisfies discharge to reach standard requirement in the waste water after the processing, and can the retrieval and utilization as chromium plating pretreatment sparge water, reduction treatment cost. Meanwhile, compared with the traditional precipitation method, the occupied area is reduced.
(2) When the method is used for controlling the adsorption of the anion exchange column, the pH value of the wastewater is 2-3, because the pH value of the solution influences the existence form of Cr (VI) in the solution. Cr (VI) in neutral and alkaline solution, the main species is CrO 4 2- (ii) a In acidic solution, HCrO is mainly used -4 The form exists. The ion exchange material has the selectivity sequence of OH to anions in solution - ＞HCrO 4 - ＞CrO 4 2- . OH in solution as the pH of the solution increases - The concentration increases, and therefore the selective adsorption capacity of the anion resin for Cr (VI) decreases. In addition, if the solution is alkaline, cr (VI) exists in the form of CrO 4 2- Occupies two active positions of the anion resin, and the existence form of Cr (VI) is HCrO under the acidic condition 4 - Only one active site of the anionic resin is occupied. The two aspects are influenced together, so that the adsorption amount of Cr (VI) on the anion resin is reduced under the alkaline condition. But when the solution pH is<2, the adsorption capacity of the anion resin to chromium ions is reduced, and may be Cl in the solution - The increase in concentration of (A) inhibits exchange of the anion resin with Cr (VI), and HCrO 4 - Is gradually converted into H 2 CrO 4 Non-ionic, thereby further reducing the amount of Cr (VI) adsorbed by the alloy.
(2) In the adsorption process of the electroplating wastewater, after the exchange of the anion resin (the first exchange column) is saturated, the chromium ion exchange system is desorbed and regenerated by sodium hydroxide with the mass fraction of 10-15%, and the obtained regenerated solution can be reused in a chromium plating tank after sodium removal and concentration, so that the chromium environmental pollution is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a diagram of a simple single-column test apparatus used in the examples of the present application;
FIG. 2 is a graph of adsorption efficiency for example 1;
FIG. 3 is a graph of adsorption efficiency for comparative example 1;
FIG. 4 is a graph showing the concentrations of desorption regeneration liquids of different resins of example 1 and comparative example 1;
FIG. 5 is the drawing of three puffs of example 2;
FIG. 6 shows the resin pairs Cr of example 3 3+ Drawing;
FIG. 7 is a graph showing the resin pairs Cr of comparative example 2 3+ And (5) absorbing the attached drawings.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
A1 anion resin is from Kahaisi, and the resin is strong base anion exchange resin with polystyrene structure; the B1 positive resin is from Kaihsia, and the resin is strong acid styrene positive resin.
The ion concentration detection method in the application is a conventional detection method in the field, for example, cr (VI) is detected by a dibenzoyl dihydrazide spectrophotometry, and the detected concentration range is 0-0.2mg/L.
In a factory which discharges chromium-containing wastewater in Fujian spring region, chromium ions in the wastewater are treated and recovered, and the concentrations of chromium and other ions in the chromium-containing wastewater in an electroplating factory are respectively determined by the following methods: cr (VI) is measured by spectrophotometry, and total chromium (T) Cr ) And the copper, the zinc and the nickel are measured by an atomic absorption spectrophotometry. The raw water pH was measured with a pH meter. The water source for all experiments was the parkThe chromium-containing wastewater in the reaction kettle contains the following anions: crO 4 2- 、Cr 2 O 7 2- 、SO 4 2- 、Cl - Cation: cr (chromium) component 3+ 、H + 、Cu 2+ 、Ni 2 + 、Zn 2+ And the detection result of the concentration of the metal ions in the chromium-containing wastewater is as follows:
the method comprises the following steps in the process of treating the wastewater:
filtering the chromium-containing wastewater in advance to remove suspended matters and particle solid impurities in the wastewater;
effluent water obtained after wastewater is adsorbed by the A1 anion resin is subjected to pH adjustment to 5 and then enters the B1 cation resin to form an ion exchange system in series, effluent liquid obtained after the system is treated is sampled and analyzed every half hour, and the concentration of hexavalent chromium in an analysis result is less than or equal to 0.2mg/L, the concentration of cationic copper, nickel, zinc and iron is less than or equal to 0.2mg/L, so that the effluent water reaches the standard of washing water for chrome plating pretreatment.
And when the first exchange column (anion resin exchange column) is saturated, stopping introducing the wastewater, performing desorption regeneration, and concentrating the regenerated solution to reuse the regenerated solution in the chromium plating tank.
Example 1
A1 anion resin is used as Cr special adsorption resin, and through a single-column small experiment, the water inflow rate is 5BV/h. The result of ion adsorption is shown in figure 2, the effluent concentration of Cr (VI) is 0mg/L, and the adsorption rate of Cr (VI) can reach 100%. But a cation (Cu) 2+ 、Ni 2+ 、Zn 2+ ) The concentration of inlet and outlet water is not changed greatly, which shows that A1 anion resin has almost no adsorption capacity to cations, and the total Cr adsorption rate is only 61.2 percent, which also shows that the resin can adsorb Cr 3+ The adsorption efficiency of (2) is low.
The A1 anion resin with saturated adsorption is regenerated by using a sodium hydroxide solution, as shown in figure 4, and the A1 anion resin generates a regeneration liquid with the concentration of total Cr reaching 15307mg/L, wherein 99.4 percent is Cr (VI). After the regeneration liquid is subjected to sodium removal and concentration, sulfate ions in the solution can be further removed, and barium carbonate can be added to remove the sulfate ions. According to the concentration of sulfate radical in the solution, the molar ratio of the added barium carbonate to the sulfate radical is 1:1, the solution is filtered, and the filtrate is reused as the chromium plating raw material in the chromium plating bath. Through single-column small-scale test, the regeneration liquid can generate high-concentration total Cr which is a necessary condition for recycling the total Cr in the chromium tank, and a good theoretical basis is laid for achieving the aim of recycling.
Comparative example 1
The results of changing the kind of anion resin to a weakly basic anion exchange resin and examining the adsorption regeneration of the different resins as in example 1 are shown in FIG. 3.
As can be seen from the data of example 1 and comparative example 1, the adsorption efficiencies of the resin of comparative example 1 to Cr (VI) and total Cr were 90.0% and 92.1%, respectively, and to Cu 2+ 、Ni 2+ 、Zn 2+ The adsorption efficiency of metal cations was over 99.7%, however, the resin of comparative example 1 was regenerated, as shown in FIG. 4, with metal cations (Cu) in the regeneration liquid 2+ 、Ni 2+ 、Zn 2+ ) The higher content indicates that the resin of comparative example 1 is susceptible to cation leakage and cannot effectively separate Cr (VI) from other impurities. The resin selected in the embodiment 1 has excellent Cr (VI) adsorption capacity, the regeneration liquid can generate high-concentration total Cr which is a necessary condition for recycling the high-concentration total Cr in a chromium tank, and a good theoretical basis is laid for realizing the aim of recycling.
Example 2
The experiment is carried out three times of adsorption and two times of regeneration; the concentration of the Cr (VI) in the inlet water is referred to the actual electroplating wastewater, the concentration range of the Cr (VI) is 400-900mg/L, and outlet sampling analysis is carried out every 0.5 h.
As shown in FIG. 5, the A1 anion resin selected in the present application begins to decrease in removal rate after the first reaction adsorption is continued for 16 hours, the effluent concentration exceeds 0.2mg/L, and the adsorption is terminated. After regeneration treatment, the regeneration process adopted in the experiment comprises the steps of firstly washing with 10% alkali liquor for 20min, then standing for 40min, repeating the steps until no Cr (VI) is detected, eluting and regenerating with 10wt% alkali liquor, basically and effectively removing chromium ions of the A1 anion resin serving as the Cr-specific adsorption resin, and finally rinsing with clear water for 20min to finish the backwashing stage.
And (3) carrying out a secondary adsorption experiment, similar to the process of the primary adsorption experiment, and similarly, after the A1 negative resin is used as the Cr special adsorption resin for adsorption time lasting for 16 hours, the removal rate is reduced. Performing secondary regeneration, specifically spraying 5% hydrochloric acid via a regeneration pipeline for 20min by a hydrochloric acid dosing device, washing with clear water to neutrality, introducing 10% NaOH by a liquid alkali dosing device, with a spraying speed of 2BV/h, a spraying time of 30min, and a standing time of 30min; the Cr (VI) can not be detected when the column is reciprocated to the exchange column; washing with clear water for 30min; in the second regeneration process, compared with the first regeneration process, the acid washing stage is added, and the sludge-like substances generated in the adsorption process are effectively removed, so that the adsorption time and the adsorption capacity are improved.
And (4) carrying out three times of adsorption experiments, wherein after the second regeneration, the reaction adsorption time is not reduced, but the reaction adsorption time can be continuously operated for 21 hours. From the above results, it was found that although the color of the A1 negative resin changed after it was regenerated as a Cr specific adsorption resin, the structure of the resin did not change at all, so that the adsorption performance had good stability.
Collecting the regenerated liquid twice, removing sodium from the regenerated liquid, concentrating, further removing sulfate ions in the solution, and optionally adding barium carbonate to remove sulfate ions. According to the concentration of sulfate radical in the solution of 0.5-1g/L, the molar ratio of the added barium carbonate to the sulfate radical is 1:1, filtering the solution, and reusing the filtrate as the chromium plating raw material in the chromium plating bath.
Example 3
The pH of the wastewater after adsorption in example 2 was adjusted to 5 and then introduced into a cation resin exchange column (B1 cation resin), and as a result, as shown in FIG. 6, when the pH of the influent was adjusted to 5, the adsorption times were 2h,4h,6h,8h and 10h, the effluent was clear, and Cr was precipitated 3+ The concentration is lower than 10mg/L, the removal rate exceeds 87%, and a layer of solid suspended matter begins to appear on the surface layer of the resin after the operation for a period of time. After an adsorption time of 10h, cr 3+ The concentration exceeds 10mg/L, but the removal rate still reaches more than 80 percent.
Comparative example 2
The difference from example 3 is that the pH of the wastewater entering the cation exchange column was not adjusted, and the pH of the wastewater was 2 to 4, and the results are shown in FIG. 7.
Comparison of data shows that Cr in effluent is obtained after pH is adjusted in the examples of the application 3+ The concentration is relatively lower, and the removal rate is higher.
Claims (10)
1. A method for recycling electroplating chromium-containing wastewater is characterized by comprising the following steps:
(1) Filtering the electroplating chromium-containing wastewater to remove impurities,
(2) Adjusting the pH of the electroplating chromium-containing wastewater in the step (1) to 2-3, then, adjusting the pH of the effluent adsorbed by an anion resin exchange column to 5, and then, entering an cation resin exchange column for ion exchange until the concentration of Cr (VI) in the wastewater reaches the standard; the anion resin of the anion resin exchange column is chromium-specific adsorption resin; the cation resin of the cation resin exchange column is strong acid type cation exchange resin;
(3) Stopping exchange, and respectively eluting and regenerating the anion resin exchange column and the cation resin exchange column;
(4) And (4) leaching and regenerating the anion resin exchange column in the step (3) to obtain a liquid as a regenerated liquid, removing sodium from the regenerated liquid through a sodium ion exchange column, and evaporating and concentrating to obtain a chromium plating solution, wherein the chromium plating solution is used for an electroplating process.
2. The method for treating and recycling chromium-containing electroplating wastewater as claimed in claim 1, wherein the wastewater treated by the anion resin exchange column and the cation resin exchange column in sequence in step (2) is used as the washing water for the pretreatment of electroplating process.
3. The method for recycling electroplating chromium-containing wastewater as claimed in claim 1, wherein in the step (1), the concentration range of Cr (VI) in the electroplating chromium-containing wastewater is 400-900mg/L; in the step (2), the concentration of Cr (VI) in the wastewater reaching the standard is less than or equal to 0.2mg/L.
4. The method for recycling chromium-containing electroplating wastewater as claimed in claim 1, wherein the concentration of Cr (VI) in the chromium plating solution obtained by evaporation and concentration in the step (4) is 600-900g/L.
5. The method for recycling chromium-containing electroplating wastewater as claimed in claim 1, wherein in step (4), part of sulfate radicals in the chromium plating solution are removed.
6. The method for recycling chromium-containing electroplating wastewater as claimed in claim 5, wherein in step (4), barium carbonate for removing sulfate ions is added to the chromium plating solution.
7. The method for recycling the electroplating chromium-containing wastewater is characterized in that the elution of the anion resin exchange column is as follows: back washing after the leacheate is washed by water; the leacheate is 10-15wt% NaOH solution, the leacheate is leached into the exchange column from top to bottom, the mixture is kept standing for 40-60min after 20-40min, and the step is repeated until Cr (VI) is not detected by the exchange column; the cation resin exchange column is washed by 20-30wt% sulfuric acid after being washed by an eluent and back washed.
8. The method for recycling electroplating chromium-containing wastewater as claimed in claim 7, wherein the elution of the anion resin exchange column is as follows: the method comprises the following steps of leaching with an acidic leaching solution, leaching with an alkaline leaching solution, and backwashing, and specifically comprises the following steps: leaching with 5-10% hydrochloric acid for 20-30min, washing with clear water to neutrality, leaching with 10-15wt% NaOH at a spray speed of 2BV/h for 30-60min, and standing for 30-60min; the Cr (VI) can not be detected when the column is reciprocated to the exchange column; washing with clear water for 30-60min.
9. The method for recycling chromium-containing electroplating wastewater as claimed in claim 1, wherein the filtration in step (1) removes suspended matters and particulate solid impurities.
10. The method for recycling electroplating chromium-containing wastewater as claimed in claim 1, wherein the chromium-specific adsorption resin is a strong base anion exchange resin with a polystyrene framework; the strong acid type cation exchange resin is strong acid styrene cation resin.
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| CN115571948A (en) * | 2022-10-09 | 2023-01-06 | 泉州中节能水处理科技有限公司 | Method for treating and recycling electroplating chromium-containing wastewater through ion exchange |
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| CN115571948A (en) * | 2022-10-09 | 2023-01-06 | 泉州中节能水处理科技有限公司 | Method for treating and recycling electroplating chromium-containing wastewater through ion exchange |
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