CN113151863A - Method for removing copper ions in nickel production process by electrodeposition - Google Patents
Method for removing copper ions in nickel production process by electrodeposition Download PDFInfo
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- CN113151863A CN113151863A CN202110289090.0A CN202110289090A CN113151863A CN 113151863 A CN113151863 A CN 113151863A CN 202110289090 A CN202110289090 A CN 202110289090A CN 113151863 A CN113151863 A CN 113151863A
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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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
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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
- C22B15/0002—Preliminary treatment
- C22B15/001—Preliminary treatment with modification of the copper constituent
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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
- C22B15/0056—Scrap treating
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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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- 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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- 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
Abstract
A method for removing copper ions in the process of producing nickel by electrodeposition relates to a method for removing copper ions in an electrodeposition system in the process of producing electrolytic nickel by a wet method. The method is characterized in that the method comprises the following steps: (1) reacting the sodium sulfide solution with the nickel electrolyte solution to prepare nickel sulfide solution; (2) adding the prepared nickel sulfide liquid into the pressurized leaching liquid to carry out copper removal reaction; (3) and (3) filtering the reacted solution except copper, taking the produced filter residue as high-copper tailing and adding the filter residue to a copper smelting system for pyrometallurgy, and returning the filtrate as leaching preparation solution. The method of the invention reduces the concentration of copper ions in the two-stage pressurized leachate, simultaneously produces high-copper tailings with high copper content and low nickel content, and takes the high-copper tailings as raw materials to enter a copper smelting system for smelting. The process is simple to operate and low in production cost.
Description
Technical Field
A method for removing copper ions in the process of producing nickel by electrodeposition relates to a method for removing copper ions in an electrodeposition system in the process of producing nickel by electrodeposition by a wet method.
Background
At present, the technological process in the process of producing electrodeposited nickel mainly comprises the working procedures of pressure leaching-extraction-electrodeposition. In the production process, the increase of the copper content in the treatment raw materials can cause the concentration of copper ions in a production system to be enriched in the two-stage pressurized leaching solution, increase the copper removal pressure of subsequent procedures and influence the chemical composition of the electrodeposited nickel. It is very important to find a direct and effective method for removing copper from the two-stage pressurized leachate, reduce the copper removal pressure of the subsequent process, inhibit copper ions in the leaching tailings, and produce a copper anode plate by using the produced high-copper tailings as a raw material to enter a copper smelting system.
Wu Xinmin et al, in 1995, No. 4, have described the mechanistic research of copper removal by active nickel sulfide. The results show that: the property of the active nickel sulfide is researched, the composition of the nickel electrolysis anolyte is analyzed, and the copper of the active nickel sulfide is removed [ Cu (II) ]]The process is subjected to a dynamic experiment and an intermediate product is analyzed, and a copper removal mechanism of the active nickel sulfide is provided: the active nickel sulfide has larger specific surface area, CuCl2-4Ni formed without fast action on the surface of active nickel sulfide2+The copper removal diffusion control step can be converted from three-dimensional diffusion control to one-dimensional diffusion control through an intermediate transition state due to the existence of the active nickel sulfide pore structure.
Wangkaiyi et al, published in Hunan metallurgy 1993, fifth 9 months, study on deep purification of copper from nickel electrolyte by nickel sulfide precipitation transformation (Secrete de-Cue). The principle of copper removal by nickel sulfide precipitation conversion and the optimal process conditions for copper removal by nickel sulfide are shown.
In conclusion, how to effectively reduce the concentration of copper ions in the electrodeposition system and a method for producing high-copper tailings are not reported yet.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for removing copper ions in the nickel production process by electrodeposition, which is simple to operate, low in production cost and capable of effectively reducing the concentration of copper ions in an electrodeposition system and producing high-copper tailings.
The purpose of the invention is realized by the following technical scheme.
A method for removing copper ions in the process of producing nickel by electrodeposition is characterized in that the steps of the process for removing copper ions comprise:
(1) reacting the sodium sulfide solution with the nickel electrolyte solution to prepare nickel sulfide solution;
(2) adding the prepared nickel sulfide liquid into the pressurized leaching liquid to carry out copper removal reaction;
(3) and (3) filtering the reacted solution except copper, taking the produced filter residue as high-copper tailing and adding the filter residue to a copper smelting system for pyrometallurgy, and returning the filtrate as leaching preparation solution.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that after the sodium sulfide liquid and the nickel electrolyte liquid react to prepare nickel sulfide in the step (1), hydrazine hydrate is added to ensure the reducibility of the nickel sulfide liquid.
The invention discloses a method for removing copper ions in the process of producing nickel by electrodeposition, which is characterized in that the reaction conditions of sodium sulfide liquid and nickel electrolyte in the step (1) are as follows: the molar ratio of the concentration of nickel ions in the nickel electrolyte to the sodium sulfide solution is 1:0.8-1, the reaction temperature is 50-70 ℃, and the reaction time is 3-4 hours.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that the pressurized leachate obtained in the step (2) is a two-stage pressurized leachate.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that in the step (2), before the pressurized leachate is subjected to copper removal reaction, sodium sulfite solid is added to ensure the reaction activity in the copper removal reaction process, and then nickel sulfide liquid is added to perform copper removal reaction.
The method for removing copper ions in the process of producing nickel by electrodeposition is characterized in that the copper removal reaction conditions in the step (2) are as follows: adding sodium sulfite according to the mol ratio of Cu2+:Na2SO3Adding nickel sulfide solution according to the mol ratio of Cu to 1:0.4-0.82+NiS 1:0.4-1, wherein Cu2+The two-stage pressure leaching of copper ions is carried out at the reaction temperature of 65-75 ℃ for 30-60 min.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that in the step (3), the solution after copper removal of nickel sulfide produced in the step (2) is filtered by a filter press, the filtrate is returned to be used as a second-stage normal-pressure leaching solution, and high-copper filter residues are removed.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that in the step (1), after sodium sulfide liquid reacts with electrolyte to generate nickel sulfide liquid, hydrazine hydrate is added to ensure the reaction activity of the nickel sulfide liquid, and the amount of the hydrazine hydrate added to the nickel sulfide liquid is as follows: adding 0.1-0.5 ml of hydrazine hydrate into each liter of nickel sulfide liquid.
The method for removing copper ions in the nickel production process by electrodeposition is characterized in that the nickel electrodeposition liquid in the step (1) is a new nickel electrodeposition liquid.
The invention relates to a method for removing copper ions in the nickel production process by electrodeposition, which comprises the steps of firstly preparing nickel sulfide liquid by reacting a new nickel electrodeposition liquid with sodium sulfide liquid, reacting the prepared nickel sulfide liquid with a second-stage pressurized leaching liquid, and restraining copper ions in the second-stage pressurized leaching liquid in slag in the form of copper sulfide. The copper ion concentration of the two-stage pressurized leaching solution is reduced, high-copper tailings with high copper content and low nickel content are produced, and the high-copper tailings are used as raw materials to enter a copper smelting system for smelting. The process is simple to operate and low in production cost.
Compared with the prior art, the method of the invention has the following advantages:
(1) compared with the traditional process, the method has the characteristics of short flow, low nickel content in tailings and the like.
(2) The original equipment is adopted for operation, the process is mature, the post operation is simple, and the post labor intensity is not increased;
(3) the method has the advantages that the copper ion concentration of the electrodeposition system is reduced, and the high-copper tailings are produced. Therefore, under the condition of not changing the existing process flow, the direct and effective method is adopted to carry out copper removal operation on the two-stage pressurized leaching solution, the copper removal pressure of the subsequent process is reduced, copper ions are inhibited in the leaching tailings, the produced two-stage pressurized leaching solution meeting the process requirements is used for the two-stage normal-pressure leaching solution preparation, and simultaneously, the produced high-copper tailings are used as raw materials to enter a copper smelting system to produce a copper anode plate.
Drawings
FIG. 1 is a process flow diagram of a method for removing copper ions in the process of producing nickel by electrodeposition according to the present invention.
Detailed Description
A method for removing copper ions in the process of producing nickel by electrodeposition comprises the following steps:
firstly, sodium sulfide liquid reacts with the new nickel electrodeposition liquid to prepare nickel sulfide liquid.
Wherein, the preparation of the nickel sulfide liquid is followed by adding hydrazine hydrate, and the reducing atmosphere in the reaction process is kept. The reaction time is 3-4 h;
adding sodium sulfite into the second-stage pressurized leaching solution through a crane according to the concentration of copper ions in the second-stage pressurized leaching solution, pumping the nickel sulfide solution prepared in the first step into a copper removing groove of the second-stage pressurized leaching solution through a solution delivery pump, and performing copper removing reaction with the second-stage pressurized leaching solution; wherein the reaction temperature is 65-75 ℃, and the reaction time is 30-60 min;
and step three, conveying the liquid after the copper is removed after the reaction in the step two to a filter press through a pipeline for filtering, taking the produced filter residue as high-copper tailing and adding the high-copper tailing to a copper smelting system for pyrometallurgy, and returning the filtrate to a second-stage normal-pressure leaching solution preparation.
In the second step, sodium sulfite is added before the copper removal reaction of the two-stage pressurized leachate to ensure the reaction activity in the copper removal reaction process.
And (3) producing high-copper tailings with nickel content of less than or equal to 5% and copper content of more than or equal to 50%, and performing pyrometallurgical smelting by using the produced high-copper tailings as raw materials for producing the copper anode plate. The filtrate is returned to the electrowinning system for atmospheric pressure leaching. The method has the advantages of simple operation, less field equipment modification, no pollution and good copper removal effect.
The method for reducing the copper ion concentration of the electrodeposition system and producing the high copper tailings is further described in detail with reference to the attached drawings.
As shown in figure 1, the sodium sulfide liquid is firstly transported to a production site by a tank truck, 300g/L of the sodium sulfide liquid is pumped into a filter residue slurrying tank by a solution delivery pump, and is diluted to 110g/L by using fresh water. The preparation of the nickel sulfide adopts single-tank operation, firstly, nickel electrodeposition new liquid is pumped into a slurrying tank according to metallurgical calculation, then, diluted sodium sulfide liquid is pumped into the slurrying tank, and the stirring is carried out for 3-4 hours to prepare the nickel sulfide liquid. Then adding hydrazine hydrate according to the proportion of 0.1-0.5 ml per liter of nickel sulfide liquid.
According to the copper ion concentration of the two-stage pressurized leaching solution and the molar ratio of Cu2+:Na2SO3Sodium sulfite is added into the two-stage pressurized leaching solution according to the proportion of 1: 0.4-0.8. Then the prepared nickel sulfide solution is mixed with Cu according to the mol ratio2+NiS is 1:0.4-1 and slowly pumped into a copper removing groove at a fixed flow rate to perform copper removing reaction with the two-stage pressurized leaching solution. Wherein the reaction time is 30min-60min at 65-75 ℃. And after the reaction is finished, pumping the solution into a filter press for filtering, washing the filtered filter residue, and then externally feeding the filter residue to a copper smelting system for smelting. The filtrate returns to the two-stage normal pressure leaching tank for liquid preparation.
Example 1
Referring to the attached figure 1, 2165mL of sodium sulfide solution and 2500mL of new electrodeposition solution are subjected to chemical reaction for 3h to prepare nickel sulfide solution. Then 0.5ml of hydrazine hydrate is added into the nickel sulfide liquid to ensure the reducibility. Then according to two-stage pressure leaching liquor copper separationIn the case of the sub-concentration, according to Cu2+:Na2SO3Sodium sulfite was added to the two-stage pressure leach liquor at a molar ratio of 1: 0.4. Then the prepared nickel sulfide liquid is mixed with Cu2+Adding NiS into the two-stage pressurized leaching solution in a ratio of 1:0.4, reacting for 30min, and filtering to obtain filter residue containing 3.32% of nickel and 66.45% of copper. The copper ion concentration of the two-stage pressure leaching liquid is reduced from 38.13g/L to 21.01 g/L.
Example 2
Referring to the attached figure 1, 2165mL of sodium sulfide solution and 2500mL of new electrodeposition solution are subjected to chemical reaction for 4 hours to prepare nickel sulfide solution. Then 0.8ml of hydrazine hydrate is added into the nickel sulfide liquid to ensure the reducibility. According to the copper ion concentration condition of the two-stage pressurized leaching solution, according to Cu2+:Na2SO3Sodium sulfite was added to the two-stage pressure leach liquor at a molar ratio of 1: 0.8. Then the prepared nickel sulfide liquid is mixed with Cu2+Adding NiS into the two-stage pressurized leaching solution in a ratio of 1:0.6, reacting for 30min, and filtering to obtain filter residue containing 4.08% of nickel and 55.89% of copper. The copper ion concentration of the two-stage pressure leaching liquid is reduced from 38.13g/L to 25.3 g/L.
Claims (9)
1. A method for removing copper ions in the process of producing nickel by electrodeposition is characterized in that the steps of the process for removing copper ions comprise:
(1) reacting the sodium sulfide solution with the nickel electrolyte solution to prepare nickel sulfide solution;
(2) adding the prepared nickel sulfide solution into the pressurized leaching solution for copper removal reaction;
(3) and (3) filtering the reacted solution except copper, taking the produced filter residue as high-copper tailing and adding the filter residue to a copper smelting system for pyrometallurgy, and returning the filtrate as leaching preparation solution.
2. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein hydrazine hydrate is added after the sodium sulfide solution reacts with the nickel electrodeposition solution in step (1).
3. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein the reaction conditions of the sodium sulfide solution and the nickel electrodeposition solution in the step (1) are as follows: the molar ratio of the nickel ion concentration in the nickel electrolyte to the sodium sulfide solution is 1:0.8-1, the reaction temperature is 50-70 ℃, and the reaction time is 3-4 h.
4. The method according to claim 1, wherein the pressure leachate of step (2) is a two-stage pressure leachate.
5. The method according to claim 1, wherein in the step (2), before the pressurized leachate is subjected to the copper removal reaction, sodium sulfite solid is added to ensure the reactivity during the copper removal reaction, and then nickel sulfide solution is added to perform the copper removal reaction.
6. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein the copper removal reaction conditions in step (2) are as follows: adding sodium sulfite according to the mol ratio of Cu2+:Na2SO3Adding nickel sulfide solution according to the mol ratio of Cu to 1:0.4-0.82+NiS 1:0.4-1, wherein Cu2+The two-stage pressure leaching of copper ions is carried out at the reaction temperature of 65-75 ℃ for 30-60 min.
7. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein the filtrate obtained in step (3) is returned to be used as a second-stage atmospheric leaching solution.
8. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein in step (1), before the sodium sulfide solution reacts with the electrolyte solution to generate nickel sulfide, sodium sulfite solid is added to ensure the reducibility in the reaction process; after the preparation of the nickel sulfide liquid is finished, adding hydrazine hydrate to ensure the reaction activity of the nickel sulfide liquid, wherein the amount of the nickel electrolyte added with the hydrazine hydrate is as follows: 0.1-0.5 ml of hydrazine hydrate is added into each liter of the new electro-winning solution.
9. The method for removing copper ions in the process of producing nickel by electrodeposition as claimed in claim 1, wherein the nickel electrodeposition liquid in the step (1) is a new nickel electrodeposition liquid.
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| CN202110289090.0A CN113151863A (en) | 2021-03-18 | 2021-03-18 | Method for removing copper ions in nickel production process by electrodeposition |
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| CN202110289090.0A CN113151863A (en) | 2021-03-18 | 2021-03-18 | Method for removing copper ions in nickel production process by electrodeposition |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100153A (en) * | 1994-06-29 | 1995-03-15 | 北京有色冶金设计研究总院 | Method for removal of copper from electrolytic nickel anodic liquid |
| CN103820809A (en) * | 2014-02-28 | 2014-05-28 | 金川集团股份有限公司 | Copper removal method |
| CN103864157A (en) * | 2014-02-28 | 2014-06-18 | 金川集团股份有限公司 | Preparation method of amorphous nickel sulfide |
| CN105018964A (en) * | 2015-07-24 | 2015-11-04 | 金川集团股份有限公司 | Method for activating copper ions in nickel electrolysis anodic solution |
| CN209923448U (en) * | 2019-03-20 | 2020-01-10 | 金川集团股份有限公司 | Device of liquid air stirring desorption copper sediment is made in nickel electrolysis |
| CN112280978A (en) * | 2020-11-19 | 2021-01-29 | 金川集团股份有限公司 | Method for pressure leaching of high-sulfur low-copper-nickel material |
-
2021
- 2021-03-18 CN CN202110289090.0A patent/CN113151863A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100153A (en) * | 1994-06-29 | 1995-03-15 | 北京有色冶金设计研究总院 | Method for removal of copper from electrolytic nickel anodic liquid |
| CN103820809A (en) * | 2014-02-28 | 2014-05-28 | 金川集团股份有限公司 | Copper removal method |
| CN103864157A (en) * | 2014-02-28 | 2014-06-18 | 金川集团股份有限公司 | Preparation method of amorphous nickel sulfide |
| CN105018964A (en) * | 2015-07-24 | 2015-11-04 | 金川集团股份有限公司 | Method for activating copper ions in nickel electrolysis anodic solution |
| CN209923448U (en) * | 2019-03-20 | 2020-01-10 | 金川集团股份有限公司 | Device of liquid air stirring desorption copper sediment is made in nickel electrolysis |
| CN112280978A (en) * | 2020-11-19 | 2021-01-29 | 金川集团股份有限公司 | Method for pressure leaching of high-sulfur low-copper-nickel material |
Non-Patent Citations (1)
| Title |
|---|
| 王得祥 等: ""基于硫化镍除铜反应的化学添加剂对电解镍质量影响研究"", 《材料导报》 * |
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