CN113073204B - Method for recovering copper from low-concentration acidic wastewater - Google Patents
Method for recovering copper from low-concentration acidic wastewater Download PDFInfo
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- CN113073204B CN113073204B CN202110347366.6A CN202110347366A CN113073204B CN 113073204 B CN113073204 B CN 113073204B CN 202110347366 A CN202110347366 A CN 202110347366A CN 113073204 B CN113073204 B CN 113073204B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The application particularly discloses a method for recovering copper from low-concentration acidic wastewater. The method of the present application comprises the steps of: s1, adding the wastewater into a concentration tank, and heating and concentrating the wastewater to obtain concentrated wastewater; s2, adding the concentrated wastewater into an impurity removal tank, introducing concentrated ammonia water into the impurity removal tank in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; s3, carrying out suction filtration on the solution in the impurity removal tank, transferring the suction filtration liquid into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the filtrate to be 2-3, adding absolute ethyl alcohol into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate; s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals; and S5, calcining the copper-containing crystal to obtain copper. The method can be used for recovering copper from the copper-iron containing waste liquid with low copper content.
Description
Technical Field
The application relates to the technical field of wastewater treatment, in particular to a method for recovering copper from low-concentration acidic wastewater.
Background
As environmental regulations become more stringent in terms of the treatment of industrial wastewater, many industrial wastewaters must be treated using more advanced treatment procedures to achieve the specified discharge standards.
In recent years, as the image resolution and additional functions are improved, the panel manufacturing process is changed from the original aluminum process to the copper process. In the printed circuit board processing industry, a lead-tin corrosion-resistant layer is pre-plated on a part of copper foil needing to be reserved on the outer layer of the existing board, then etching liquid is added to etch the rest part of the copper foil in a chemical reaction mode, and the etching is carried out. In the etching process, along with the continuous dissolution of copper, the concentration of copper ions in the etching solution is continuously increased, and when the copper ions in the etching solution reach a certain concentration limit, the etching solution loses the etching capability on copper, namely the etching waste solution.
Among the prior art, carry out the electrolysis to etching waste liquid and retrieve, can retrieve most copper ion in the etching waste liquid, but in the waste liquid that remains, still remain a small amount of copper ion and iron ion, if directly discharge the waste liquid in the environment, cause the pollution easily.
Disclosure of Invention
In order to recover copper from a copper-iron containing waste liquid with low copper content, the application provides a method for recovering copper from low-concentration acidic waste water.
The method for recovering copper from low-concentration acidic wastewater adopts the following technical scheme:
a method for recovering copper from low-concentration acidic wastewater comprises the following steps:
s1, adding wastewater with the volume of V into a concentration tank, and heating and concentrating the wastewater until the volume of the wastewater is concentrated into V1 to obtain concentrated wastewater;
s2, adding the concentrated wastewater with the volume of V1 into an impurity removal tank, stirring at the rotating speed of 50-60r/min, introducing concentrated ammonia water into the impurity removal tank in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again;
s3, carrying out suction filtration on the solution in the impurity removal tank, transferring the suction filtration liquid with the volume of V2 into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the suction filtration liquid to be between 2 and 3, adding absolute ethyl alcohol with the volume of V3 into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate;
s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals;
s5, calcining the copper-containing crystal at 650-700 ℃ to obtain copper. .
By adopting the technical scheme, in S1, the wastewater is added into a concentration tank for heating and concentration, and the volume fraction of the solvent in the wastewater is reduced, so that the volume fraction of the solute in the wastewater is relatively increased, and the effect of increasing the concentration is achieved; in S2, strong ammonia water is introduced into the concentrated wastewater during stirring, and the following reaction occurs:
Fe 3+ +3NH 3 ·H 2 O→Fe(OH) 3 ↓+3NH 4 + ——①；
Cu 2+ +2NH 3 ·H 2 O→Cu(OH) 2 ↓+2NH 4 + ——②；
so that precipitation occurs in the impurity removal tank, and after the excessive concentrated ammonia water is gradually added, the following reaction occurs:
Cu(OH) 2 +2NH 4 + +2NH 3 ·H 2 O→[Cu(NH 3 ) 4 ] 2+ +4H 2 o- (3); namely addAfter excessive concentrated ammonia water is added, dissolving copper hydroxide, namely only remaining ferric hydroxide precipitate in the impurity removal tank, namely separating copper ions from iron ions; in S3, carrying out suction filtration on the solution in the impurity removal tank, separating ferric hydroxide precipitate from the copper ion-containing solution, adding concentrated sulfuric acid to adjust the pH of the filtrate, and introducing sulfate ions and SO 4 2- And [ Cu (NH) ] 3 ) 4 ] 2+ Bound to form [ Cu (NH) 3 ) 4 ]SO 4 Adding absolute ethyl alcohol into the solution, wherein the absolute ethyl alcohol and the solvent are mutually dissolved to cause the polarity of the solvent to be reduced, and then [ Cu (NH) 3 ) 4 ]SO 4 Separating out solution, and performing suction filtration to obtain crystallization crystals and waste liquid; in S4, the wastewater is subjected to S1, S2 and S3 again, copper ions in the wastewater are further precipitated, and the crystallization precipitates obtained for many times are concentrated to obtain copper-containing crystals; in S5, the copper-containing crystal is calcined so that [ Cu (NH) 3 ) 4 ]SO 4 And (4) decomposing by heating to obtain a Cu simple substance.
Preferably, in S1, V: v1=1: (0.2-0.3).
Preferably, in the S2, strong ammonia water is introduced into the impurity removing tank at the flow rate of V4/min, and the ratio of V1: v4=1: (0.08-0.12).
Preferably, the total volume of the concentrated ammonia water introduced into the impurity removal tank is V5, and the volume ratio of V1: v5=1: (0.5-0.6).
Preferably, in S3, during the suction filtration, the precipitate after suction filtration is washed with concentrated ammonia water, and the washed concentrated ammonia water is incorporated into the filtrate.
Preferably, in S1, the wastewater in the concentration tank is heated and concentrated by using a hot air blower.
Preferably, the hot air blower blows hot air with the temperature of 120-150 ℃.
Preferably, in S5, the copper-containing crystal is calcined in a nitrogen atmosphere.
In summary, the present application has the following beneficial effects:
1. the method comprises the following steps: s1, adding wastewater with the volume of V into a concentration tank, and heating and concentratingWastewater is obtained until the volume of the wastewater is concentrated to be V1, and concentrated wastewater is obtained; s2, adding the concentrated wastewater with the volume of V1 into an impurity removal tank, stirring at the rotating speed of 50-60r/min, introducing concentrated ammonia water into the impurity removal tank in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; s3, carrying out suction filtration on the solution in the impurity removal tank, transferring the suction filtration liquid with the volume of V2 into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the suction filtration liquid to be between 2 and 3, adding absolute ethyl alcohol with the volume of V3 into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate; s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals; s5, calcining the copper-containing crystals at 650-700 ℃ to obtain copper; in S1, adding the wastewater into a concentration tank for heating and concentration, and reducing the volume fraction of a solvent in the wastewater, so that the volume fraction of a solute in the wastewater is relatively increased, and the effect of increasing the concentration is achieved; in S2, strong ammonia water is introduced into the concentrated wastewater during stirring, and the following reaction occurs: fe 3+ +3NH 3 ·H 2 O→Fe(OH) 3 ↓+3NH 4 + ；Cu 2 + +2NH 3 ·H 2 O→Cu(OH) 2 ↓+2NH 4 + (ii) a Therefore, precipitation occurs in the impurity removing tank, and after excessive concentrated ammonia water is gradually added, the following reaction occurs: cu (OH) 2 +2NH 4 + +2NH 3 ·H 2 O→[Cu(NH 3 ) 4 ] 2+ +4H 2 O; after excessive concentrated ammonia water is added, dissolving copper hydroxide, namely only remaining ferric hydroxide precipitate in the impurity removal tank, namely separating copper ions from iron ions; in S3, carrying out suction filtration on the solution in the impurity removal tank, separating ferric hydroxide precipitate from the copper ion-containing solution, adding concentrated sulfuric acid to adjust the pH of the filtrate, and introducing sulfate ions and SO 4 2- And [ Cu (NH) 3 ) 4 ] 2+ Bound to form [ Cu (NH) 3 ) 4 ]SO 4 Adding absolute ethyl alcohol into the solution, wherein the absolute ethyl alcohol and the solvent are mutually dissolved to cause the polarity of the solvent to be reduced, and then [ Cu (NH) 3 ) 4 ]SO 4 Separating out solution, and performing suction filtration to obtain crystallization crystals and waste liquid; in S4, the wastewater is subjected to S1, S2 and S3 again, copper ions in the wastewater are further precipitated, and the crystallization precipitates obtained for many times are concentrated to obtain copper-containing crystals; in S5, the copper-containing crystal is calcined so that [ Cu (NH) 3 ) 4 ]SO 4 And (4) decomposing by heating to obtain a Cu simple substance.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
The method of this example 1 includes the following steps:
s1, adding 100L of wastewater into a concentration tank, blowing and heating the surface of the wastewater by using an air heater to concentrate the wastewater, wherein the temperature of an air outlet of the air heater is 120 ℃ until the volume of the wastewater is concentrated to 30L, so as to obtain concentrated wastewater;
s2, adding 30L of concentrated wastewater into an impurity removal tank, stirring the concentrated wastewater at a rotating speed of 60r/min, and introducing concentrated ammonia water into the impurity removal tank at a flow rate of 3.6L/min in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; the total volume of the concentrated ammonia water introduced into the impurity removing tank is 18L;
s3, carrying out suction filtration on the solution in the impurity removal tank, transferring 48L of suction filtration liquid into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the filtrate liquid to be 2-3, adding 10L of absolute ethyl alcohol into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate; in the suction filtration process, the suction filtration precipitate is washed by concentrated ammonia water, and the washing liquid is combined with the wastewater;
s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals;
s5, calcining the copper-containing crystal in a nitrogen atmosphere at 650 ℃ to obtain copper.
Example 2
The method of embodiment 2 comprises the following steps:
s1, adding 100L of wastewater into a concentration tank, blowing and heating the surface of the wastewater by using an air heater to concentrate the wastewater, wherein the temperature of an air outlet of the air heater is 150 ℃ until the volume of the wastewater is concentrated to 20L, so as to obtain concentrated wastewater;
s2, adding 20L of concentrated wastewater into an impurity removal tank, stirring the concentrated wastewater at a rotating speed of 50r/min, and introducing concentrated ammonia water into the impurity removal tank at a flow rate of 1.6L/min in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; the total volume of the concentrated ammonia water introduced into the impurity removing tank is 10L;
s3, carrying out suction filtration on the solution in the impurity removal tank, transferring 30L of suction filtration liquid into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the filtrate liquid to be 2-3, adding 5L of absolute ethyl alcohol into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate; in the suction filtration process, concentrated ammonia water is used for washing suction filtration precipitation, and washing liquid is combined with wastewater;
s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals;
and S5, calcining the copper-containing crystal in a nitrogen atmosphere at 700 ℃ to obtain copper.
Example 3
The method of embodiment 3 includes the following steps:
s1, adding 100L of wastewater into a concentration tank, and blowing and heating the surface of the wastewater by using an air heater to concentrate the wastewater, wherein the temperature of an air outlet of the air heater is 140 ℃ until the volume of the wastewater is concentrated to 25L, so as to obtain concentrated wastewater;
s2, adding 25L of concentrated wastewater into an impurity removal tank, stirring the concentrated wastewater at a rotating speed of 50r/min, and introducing concentrated ammonia water into the impurity removal tank at a flow rate of 2.5L/min in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; the total volume of the concentrated ammonia water introduced into the impurity removing tank is 15L;
s3, carrying out suction filtration on the solution in the impurity removal tank, transferring 40L of suction filtration liquid into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the filtrate liquid to be between 2 and 3, adding 7L of absolute ethyl alcohol into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate; in the suction filtration process, the suction filtration precipitate is washed by concentrated ammonia water, and the washing liquid is combined with the wastewater;
s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals;
s5, calcining the copper-containing crystal in a nitrogen atmosphere at 700 ℃ to obtain copper.
Comparative example
Comparative example 1
The waste liquor is subjected to electrolysis to recover copper using conventional methods.
Performance test
Test method
The formulation contains 0.01mol/LCu 2+ And 0.1mol/LFe 3+ The four mixed solutions 400L were divided into 4 parts of an average amount of 100L, and the four mixed solutions were subjected to copper recovery by the methods of examples 1 to 3 and comparative example 1, respectively, and the mass of the obtained copper was measured, and the results are shown in Table 1.
TABLE 1 examples 1 to 3 of the present application for the recovery of copper
| Example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Cu mass/g | 45.32 | 44.89 | 45.83 | 23.12 |
| Percent recovery% | 71.37 | 70.69 | 72.17 | 36.41 |
Combining examples 1-3 and comparative example 1, and table 1, it can be seen that the process of the present application provides significantly higher copper recovery than conventional electrolytic recovery of the prior art.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (6)
1. A method for recovering copper from low-concentration acidic wastewater, which is characterized by comprising the following steps:
s1, adding wastewater with the volume of V into a concentration tank, and heating and concentrating the wastewater until the volume of the wastewater is concentrated into V1 to obtain concentrated wastewater;
s2, adding the concentrated wastewater with the volume of V1 into an impurity removal tank, stirring at the rotating speed of 50-60r/min, introducing concentrated ammonia water into the impurity removal tank in the stirring process until precipitation appears in the impurity removal tank, and dissolving part of the precipitation again; and introducing concentrated ammonia water into the impurity removal tank at the flow speed of V4/min, wherein the flow speed of V1: v4=1: (0.08-0.12); the total volume that concentrated aqueous ammonia lets in the edulcoration groove is V5, V1: v5=1: (0.5-0.6);
s3, carrying out suction filtration on the solution in the impurity removal tank, transferring the suction filtration liquid with the volume of V2 into a precipitation tank, adding concentrated sulfuric acid into the precipitation tank, adjusting the pH of the suction filtration liquid to be between 2 and 3, adding absolute ethyl alcohol with the volume of V3 into the suction filtration liquid, separating out crystals in the precipitation tank, and carrying out suction filtration to obtain wastewater and crystallization precipitate;
s4, repeating S1, S3 and S3 on the wastewater in the S3 until no obvious crystal is separated out in the S3, and concentrating the crystallization precipitate obtained in the S3 to obtain copper-containing crystals;
s5, calcining the copper-containing crystal at 650-700 ℃ to obtain copper.
2. The method for recovering copper from low-concentration acidic wastewater according to claim 1, wherein the method comprises the following steps: in the S1, V: v1=1: (0.2-0.3).
3. The method for recovering copper from low-concentration acidic wastewater according to claim 1, wherein the method comprises the following steps: in the S3, in the suction filtration process, the precipitate after suction filtration is washed by concentrated ammonia water, and the washed concentrated ammonia water is merged into the filtrate.
4. The method for recovering copper from low-concentration acidic wastewater according to claim 1, wherein the method comprises the following steps: and in the S1, heating and concentrating the wastewater in the concentration tank by using an air heater.
5. The method for recovering copper from low-concentration acidic wastewater according to claim 4, wherein the method comprises the following steps: the hot air blower blows hot air with the temperature of 120-150 ℃.
6. The method for recovering copper from low-concentration acidic wastewater according to claim 1, wherein the method comprises the following steps: and in the S5, calcining the copper-containing crystal in a nitrogen environment.
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| CN101984097A (en) * | 2010-11-24 | 2011-03-09 | 苏州市环境工程有限责任公司 | Method for comprehensive recovery of heavy metal from spent solder stripper |
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| CN1191142C (en) * | 2003-08-12 | 2005-03-02 | 北京科技大学 | Method for mfg nano copper powder |
| WO2008139021A1 (en) * | 2007-05-16 | 2008-11-20 | Pp Recycling Ltd. | Metthod of regeneration method of acid cupper(ii)chloride etching waste |
| CN101713025B (en) * | 2009-12-08 | 2011-08-10 | 浙江工业大学 | Method for wet separation of mixed solution containing nickel and zinc |
| CN103966446A (en) * | 2014-05-08 | 2014-08-06 | 南京大学 | Method for separating and recovering copper, nickel and iron from electroplating sludge |
| CN106282567A (en) * | 2015-05-29 | 2017-01-04 | 陕西瑞凯环保科技有限公司 | A kind of method reclaiming metal from useless acidic etching liquid |
| CN107287429B (en) * | 2017-07-05 | 2018-08-17 | 盛隆资源再生（无锡）有限公司 | A kind of iron content is high, the low electroplating sludge of cupro-nickel content recovery and treatment method |
| CN107338359B (en) * | 2017-07-13 | 2018-11-30 | 盛隆资源再生（无锡）有限公司 | It is a kind of containing gold, copper, nickel waste nitric acid in heavy metal classified reclaiming method |
| CN109319823B (en) * | 2017-07-31 | 2021-02-23 | 中国瑞林工程技术股份有限公司 | Method for treating copper-containing etching waste liquid |
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| CN101984097A (en) * | 2010-11-24 | 2011-03-09 | 苏州市环境工程有限责任公司 | Method for comprehensive recovery of heavy metal from spent solder stripper |
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| Title |
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| 铜氨废水处理与废铜液回收;宫本涛等;《电镀与精饰》;20020131;第24卷(第1期);31-34 * |
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