CN107245585B - Electroplating waste treatment method - Google Patents
Electroplating waste treatment method Download PDFInfo
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- CN107245585B CN107245585B CN201710472981.3A CN201710472981A CN107245585B CN 107245585 B CN107245585 B CN 107245585B CN 201710472981 A CN201710472981 A CN 201710472981A CN 107245585 B CN107245585 B CN 107245585B
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses an electroplating waste treatment method, which comprises the following steps: stripping water to precipitate nickel to obtain nickel-containing waste residue; mixing nickel-containing waste residue and electroplating sludge, adding water for washing, and performing filter pressing to obtain a mixture; adding water into the mixture for slurrying, and pumping into a leaching tank; adding concentrated H in 40-50 deg.C environment 2 SO 4 Until the pH value is 2.0, filter-pressing to form leachate and filter residue; copper extraction; leaching again; secondary copper extraction; removing iron; removing calcium and magnesium; extracting impurities; nickel extraction; nickel electrodeposition and the like. By adopting the technical scheme, the electroplating waste treatment method can treat the electroplating waste, recycle harmful heavy metals in the waste and avoid environmental pollution.
Description
Technical Field
The invention relates to a method for treating electroplating waste, belonging to the technical field of metallurgy and chemical industry.
Background
Electroplating is a process of plating a thin layer of other metals or alloys on the surface of some metals by using the principle of electrolysis, and is a process of attaching a layer of metal film on the surface of a metal or other material product by using the action of electrolysis so as to prevent the oxidation (such as corrosion) of the metal, improve the wear resistance, the conductivity, the light reflection property, the corrosion resistance, the beauty and the like. The electroplating sludge is a discharge produced in the electroplating wastewater treatment process, contains a large amount of toxic heavy metals such as chromium, cadmium, nickel, zinc and the like, and has very complex components. Among 47 types of hazardous wastes listed in national records of hazardous wastes (encirclement [1998] 89), electroplating sludge accounts for 7 types of hazardous wastes, and is a typical hazardous waste. At present, most of electroplating sludge is only simply buried in land or even randomly stacked due to the problems of multiple sites, small scale, low equipment level, low pollution treatment level and the like in the electroplating industry of China, so that the environment is seriously polluted.
Deplating is a process of removing a plating layer on the surface of a workpiece. The deplating is an inevitable ring in the field of electroplating, and the method comprises two methods: the first is to soak the deplated part in the deplating solution, and the principle is to remove the electroplated layer by using a chemical dissolving method; another method is to put the deplated parts in a deplating solution for electrolysis, and the principle is to remove the electroplated layer by an electrochemical method. The deplating liquid after deplating also contains a large amount of toxic heavy metals such as chromium, cadmium, nickel, zinc and the like, and the toxic heavy metals are discharged randomly to cause serious pollution to the environment.
Disclosure of Invention
Therefore, the present invention is directed to overcoming the drawbacks of the prior art and providing a method for treating electroplating wastes.
In order to achieve the above object, a method for treating plating waste according to the present invention comprises the steps of:
1) Stripping water to precipitate nickel to obtain nickel-containing waste residue;
2) Mixing nickel-containing waste residue and electroplating sludge, adding water for washing, and performing filter pressing to obtain a mixture;
3) Adding water into the mixture obtained in the step 2 for slurrying, and pumping into a leaching tank;
4) Leaching: adding concentrated H in 40-50 deg.C environment 2 SO 4 Until the pH value is 2.0, filter-pressing to form leachate and filter residue;
5) Carrying out copper extraction process on the leaching solution obtained in the step 4;
6) Leaching the solution obtained in the step 5 again;
7) Carrying out copper extraction process on the leachate obtained in the step 6 again;
8) Heating the solution obtained in the step 7 to 70 ℃, adding soda powder to adjust the pH value to 1.0-1.5, and adding NaClO 3 Powder until no Fe is in solution 2+ Then heating to above 90 ℃, adding soda water, and gradually adjusting the pH value to 4.0; filtering, putting filter residues into a slag washing tank, and putting filtrate into a calcium and magnesium removing tank;
9) Heating the filtrate obtained in the step 8 to 60 ℃, and adding sodium fluoride powder until the mass percentage concentration of calcium and magnesium ions in the solution is less than 0.2%; filtering, putting filter residues into a residue washing tank, and extracting impurities from filtrate;
10 Carrying out impurity extraction on the filtrate obtained in the step 9, adding dilute sulfuric acid after impurity extraction to back extract metal ions in the loaded organic phase into a liquid phase; adding hydrochloric acid with over 4.5N to Fe 3+ Carrying out back extraction;
11 Carrying out nickel extraction on the solution obtained in the step 10, adding dilute sulfuric acid after nickel extraction to back extract metal ions in the loaded organic phase into a liquid phase; adding hydrochloric acid with more than 4.5N to Fe 3+ Carrying out back extraction;
12 Nickel electrodeposition of nickel-containing waste obtained in the nickel extraction process.
The electroplating waste treatment method further comprises the following steps: and (4) carrying out copper electrodeposition on the copper-containing waste obtained by the copper extraction process in the steps (5) and (7).
The electroplating waste treatment method further comprises the following steps:
13.1 Sulfuric acid is added into the waste residue obtained after copper electrodeposition, the iron-containing waste residue obtained in the step 8 and the calcium-containing magnesium waste residue obtained in the step 9 for washing;
13.2 Water is added to the substance obtained in step 13.1 for washing, and the waste residue after washing is recovered.
By adopting the technical scheme, the electroplating waste treatment method can treat the electroplating waste, recycle harmful heavy metals in the waste and avoid environmental pollution.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the detailed description.
As shown in the drawings, the present embodiment provides a method for treating electroplating wastes, comprising the following steps:
1. deplating and precipitating nickel;
the reason is as follows: containing NO 3 - Is harmful to the copper extractant.
The method comprises the following steps: heating to 50-60 deg.C, adding Na 2 CO 3 Adjusting the pH value of the powder to 7.5-8.0, and performing filter pressing; if the filter residue contains NO3 - High, one wash is also required.
The mechanism is as follows: ni (NO) 3 ) 2 +Na 2 CO 3 ＝Ni 2 CO 3 ↓+2NaNO 3 。
2. Electroplating sludge or crude NiCO 3 Washing.
The reason is as follows: containing a small amount of NO 3 -hazardous to copper extractants.
The method comprises the following steps: and fully slurrying the slurry in the tank by using tap water, and performing filter pressing.
3. And (6) pulping.
The purpose is as follows: the pipeline conveying is convenient, the labor amount is reduced, the labor intensity is reduced, and other areas in the workshop are kept sanitary and clean.
The method comprises the following steps: tap water (or primary slag washing water) and clean solid raw materials are fully pulped and then pumped into a leaching tank.
The mechanism is as follows: and (4) physical processes.
4. And (4) leaching.
The purpose is as follows: by H 2 SO 4 Dissolving NiCO 3 。
The method comprises the following steps: slowly add concentrated H 2 SO 4 And (4) performing pressure filtration at the temperature of 40-50 ℃ when the PH = 2.0. Putting the filter residue into a residue washing tank, filtering the filtrate for the second time, and extracting copper; the solution after copper extraction is subjected to a leaching process and a secondary copper extraction process again, and the obtained solution enters a subsequent iron removal process for the purposes of: (1) The acid generated after copper extraction can be recycled, and (2) the concentration of nickel is improved.
The mechanism is as follows: acid-base neutralization.
NiCO 3 +H 2 SO 4 ＝NiSO 4 +CO 2 ↑+H 2 O
Ni(OH) 2 +H 2 SO 4 ＝NiSO 4 +2H 2 O
5. Iron removal
The purpose is as follows: removal of NiSO 4 Iron ions in solution.
The method comprises the following steps: (1) heating to 70 deg.C, adding soda powder, adjusting pH to 1.0-1.5, adding appropriate amount of NaClO 3 Powder, and reacting for 30 minutes;
(2) confirmation of absence of Fe 2 After + heating to above 90 ℃, dilute soda lye is added to adjust the PH =3.5-4.0, end point PH =4.0.
(3) Filtering, putting the filter residue into a slag washing tank, and putting the filtrate into a calcium and magnesium removing tank.
The mechanism is as follows: first, the sodium jarosite is generated, and the rest of the trace Fe 3 + to form Fe (OH) 3 And (4) precipitating.
6Fe 2+ +NaClO 3 +6H + ＝6Fe 3+ +NaCl+3H 2 O (Oxidation)
6Fe 3+ +Na 2 SO 4 +12H 2 O＝Na 2 Fe 6 (SO 4 ) 4 (OH) 12 ↓+6H 2 SO 4 (Chengfeng)
Fe 3+ +3H 2 O＝Fe(OH) 3 ↓+3H + (precipitation)
H 2 SO 4 +Na 2 CO 3 ＝Na 2 SO 4 +CO 2 ↑+H 2 O (acid-base neutralization)
6. Removing calcium and magnesium
The purpose is as follows: removing calcium and magnesium ions and purifying the extraction environment.
The method comprises the following steps: (1) heating to 60 ℃, adding a proper amount of sodium fluoride powder, reacting for 6-8 m, wherein the calcium and magnesium are all less than or equal to 0.002.
(2) Filtering, putting the filter residue into a residue washing tank, and carrying out secondary filtration on the filtrate to enter an impurity extraction process.
The mechanism is as follows: caF 2 And MgF 2 Is a poorly soluble solid.
Ca 2+ +2NaF↓＝CaF 2 ↓+2Na + Mg 2+ +2NaF＝MgF 2 ↓+2Na +
7. Extract of miscellaneous plants
The purpose is as follows: removal of metal ions, e.g. Fe, detrimental to nickel electrodeposition 3+ 、Zn 2+ 、Mn 2+ 、Cu 2+ 、Cr 3+ And the like.
The mechanism is as follows: the chemical process is divided into 5 sections, and different metal ions are extracted with different difficulty degrees (Fe 3+ > Zn2+ > Ca2+ > Mn2+ > Ni2+ > Na + > H +) according to P507;
①
na soap;
the principle is as follows: h 3 M+3NaOH＝Na 3 M+3H 2 O。
(2) Extracting impurities; na (Na) 3 M+Re 2+ ＝Re 3 M 2 +3Na + 。
(3) Washing; with dilute H 2 SO 4 Mix Ni 2+ Back extraction into liquid phase for the purpose ofThe loaded organic phase entering the stripping section does not contain Ni 2+ 。
(4) Back extraction; with dilute H 2 SO 4 And (3) completely introducing the metal ions in the loaded organic phase into a liquid phase, which is also called organic phase regeneration.
(5) Counter Fe 3+ (ii) a Due to Fe 3+ Easy extraction and difficult back extraction, so that the back extraction needs hydrochloric acid with the concentration of more than 4.5N.
8. Nickel extraction
The purpose is as follows: increasing the concentration of nickel ions in the solution, and removing harmful anions such as Cl-and NO 3 - 、F - And the like.
The mechanism is as follows: performing simultaneous extraction and impurity reaction, extracting by 5 sections (1) with Na soap (2), washing (3), and back extracting (5) to remove Fe.
9. Electrodeposition of copper
The purpose is as follows: so that the Cu < 2+ > forms simple substance metal to deposit on the cathode plate by losing electrons.
The mechanism is as follows: and (3) cathode reaction: cu 2+ -2e→Cu 2H + +2e→H 2 And × (when the acidity is large).
And (3) anode reaction: 2OH - +2e→O 2 +2H + 。
Therefore, not only Cu and H are generated in the electrodeposition process 2 And also generate H 2 SO 4 And oxygen.
10. Nickel electrodeposition
The mechanism is as follows: and (3) cathode reaction: ni 2+ -2e→Ni。
And (3) anode reaction: 2OH - +2e→O 2 +2H + 。
11. Slag washing:
the purpose is as follows: valuable metals in the slag are recovered, the recovery rate is improved, and environmental pollution is avoided.
11.1 washing slag once, and adding a small amount of sulfuric acid.
Ni(OH) 2 +H 2 SO 4 →NiSO 4 +2H 2 O
NiCO 3 +H 2 SO 4 →NiSO 4 +CO 2 ↑+H 2 O
NiF 2 +H 2 SO 4 →NiSO 4 +2HF
11.2 washing the slag for the second time, directly washing the slag by tap water, recovering valuable metals in the slag, improving the recovery rate and simultaneously improving the PH value of the slag, mainly physical entrainment.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (1)
1. The electroplating waste treatment method is characterized by comprising the following steps:
1) Stripping water to precipitate nickel to obtain nickel-containing waste residue;
2) Mixing nickel-containing waste residue and electroplating sludge, adding water for washing, and performing filter pressing to obtain a mixture;
3) Adding water into the mixture obtained in the step 2 for slurrying, and pumping into a leaching tank;
4) Leaching: adding concentrated H in 40-50 deg.C environment 2 SO 4 Until the pH value is 2.0, filter-pressing to form leachate and filter residue;
5) Carrying out copper extraction process on the leaching solution obtained in the step 4;
6) Leaching the solution obtained in the step 5 again;
7) Carrying out copper extraction process again on the leachate obtained in the step 6;
8) Heating the solution obtained in the step 7 to 70 ℃, adding soda powder to adjust the pH value to 1.0-1.5, and adding NaClO 3 Powder until no Fe is in solution 2+ Then heating to above 90 ℃, adding soda water, and gradually adjusting the pH value to 4.0; filtering, putting filter residues into a slag washing tank, and putting filtrate into a calcium and magnesium removing tank;
9) Heating the filtrate obtained in the step 8 to 60 ℃, and adding sodium fluoride powder until the mass percentage concentration of calcium and magnesium ions in the solution is less than 0.2%; filtering, putting filter residues into a residue washing tank, and extracting impurities from filtrate;
10 Carrying out impurity extraction on the filtrate obtained in the step 9, adding dilute sulfuric acid after impurity extraction to back extract metal ions in the loaded organic phase into a liquid phase; adding hydrochloric acid with over 4.5N to Fe 3+ Carrying out back extraction;
11 Carrying out nickel extraction on the solution obtained in the step 10, adding dilute sulfuric acid after nickel extraction to back extract metal ions in the loaded organic phase into a liquid phase; adding hydrochloric acid with more than 4.5N to Fe 3+ Performing back extraction;
12 Nickel electrodeposition is carried out on the nickel-containing waste obtained in the nickel extraction process;
the electroplating waste treatment method further comprises the following steps: carrying out copper electrodeposition on the copper-containing waste obtained by the copper extraction process in the steps 5 and 7;
the electroplating waste treatment method further comprises the following steps:
13.1 Sulfuric acid is added into the waste residue obtained after copper electrodeposition, the waste residue containing iron obtained in the step 8 and the waste residue containing calcium and magnesium obtained in the step 9 for washing;
13.2 Water is added to the material obtained in step 13.1 for washing, and the waste residue after washing is recovered.
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| CN113061724B (en) * | 2021-03-09 | 2022-10-18 | 金川集团股份有限公司 | Method for eluting nickel sulfide and removing nickel and chloride ions in copper tailings |
| CN114405979A (en) * | 2021-12-20 | 2022-04-29 | 荆门市格林美新材料有限公司 | Cobalt-nickel tailing treatment method |
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|---|---|---|---|---|
| US6432167B1 (en) * | 1999-07-08 | 2002-08-13 | Cognis Corporation | Processes for the recovery of copper from aqueous solutions containing nitrate ions |
| CN102417987A (en) * | 2011-08-09 | 2012-04-18 | 朱小红 | Method for recovering valuable metal from electroplating sludge |
| CN103274483A (en) * | 2013-06-06 | 2013-09-04 | 重庆莘然高分子材料有限公司 | Technology for recovering nickel from nickel coating stripping waste liquid |
| CN104451159A (en) * | 2014-12-02 | 2015-03-25 | 赣州中联环保科技开发有限公司 | Process for recycling metals from electroplating wastewater |
| CN105256141A (en) * | 2015-10-26 | 2016-01-20 | 广西银亿再生资源有限公司 | Electroplating-sludge resourceful treatment and comprehensive recycling method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6432167B1 (en) * | 1999-07-08 | 2002-08-13 | Cognis Corporation | Processes for the recovery of copper from aqueous solutions containing nitrate ions |
| CN102417987A (en) * | 2011-08-09 | 2012-04-18 | 朱小红 | Method for recovering valuable metal from electroplating sludge |
| CN103274483A (en) * | 2013-06-06 | 2013-09-04 | 重庆莘然高分子材料有限公司 | Technology for recovering nickel from nickel coating stripping waste liquid |
| CN104451159A (en) * | 2014-12-02 | 2015-03-25 | 赣州中联环保科技开发有限公司 | Process for recycling metals from electroplating wastewater |
| CN105256141A (en) * | 2015-10-26 | 2016-01-20 | 广西银亿再生资源有限公司 | Electroplating-sludge resourceful treatment and comprehensive recycling method |
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