CN106048222A - Separation and purification method for manganese ions in high-nickel solution - Google Patents

Separation and purification method for manganese ions in high-nickel solution Download PDF

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Publication number
CN106048222A
CN106048222A CN201610592443.3A CN201610592443A CN106048222A CN 106048222 A CN106048222 A CN 106048222A CN 201610592443 A CN201610592443 A CN 201610592443A CN 106048222 A CN106048222 A CN 106048222A
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CN
China
Prior art keywords
solution
nickel
manganese
reaction
nickel solution
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Pending
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CN201610592443.3A
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Chinese (zh)
Inventor
郭勇
李亦婧
郑军福
张树峰
程少逸
卢建波
朱纪念
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lanzhou Institute of Chemical Physics LICP of CAS
Jinchuan Group Co Ltd
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Lanzhou Institute of Chemical Physics LICP of CAS
Jinchuan Group Co Ltd
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Priority to CN201610592443.3A priority Critical patent/CN106048222A/en
Publication of CN106048222A publication Critical patent/CN106048222A/en
Pending legal-status Critical Current

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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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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

Abstract

The invention discloses a separation and purification method for manganese ions in a high-nickel solution. The separation and purification method for the manganese ions in the high-nickel solution comprises the specific steps that the pH value of the high-nickel solution containing the manganese ions is adjusted to range from 1.0 to 5.0 through a hydrochloric acid solution and a sodium hydroxide solution; then, heating reflux is carried out on the high-nickel solution, when the temperature reaches 60-90 DEG C, a persulfate oxidizing agent is added to the high-nickel solution, a reaction is conducted under the condition of stirring at the temperature, and a sodium carbonate solution is continuously added to the high-nickel solution in the reaction process to enable the pH value of the high-nickel solution to be kept at 1.0-5.0; and filtering is conducted after the reaction process is finished, filter residues are washed with deionized water, filter liquor is collected to a constant volume, and the content of the manganese ions in the filter liquor and the mass ratio of manganese to nickel in the filter residues are measured. The separation and purification method for the manganese ions in the high-nickel solution has the beneficial effects that the purifying depth is high, the reaction efficiency is high, the amount of nickel contained by the generated residues without manganese is small, and the operation cost is low.

Description

The purification method of manganese ion in a kind of high nickel solution
Technical field
The present invention relates to the purification method of manganese ion in a kind of high nickel solution.The present invention passes through oxide sulfate agent will Bivalent manganese in solution is oxidized to manganese dioxide precipitate thus reaches the purpose of manganese ion in purification separation nickel electrolyte.
Background technology
Metallic nickel accounts for critical role in national economy, is important strategic resources and purposes metal list widely Material.The a large amount of manganese ions contained in the leachate obtained by feed hydrogen nickel oxide acidleach during wet method nickel metallurgy, as without Cross demanganization to process and be directly entered electrolysis system and then the physicochemical properties of nickel electrolyte can be produced impact.Manganese during nickel electrowinning Ion carries out following redox reaction between anode and cathode:
Anode: Mn2+ + 2H2O – 2e → MnO2↓+ 4H+
Mn2+ + 4H2O – 5e → MnO4 - + 8H+；
Negative electrode: MnO4 - + 8H+ + 5e → Mn2+ + 4H2O。
So consume electric energy, and Mn at negative and positive interpolar receiving and losing electrons repeatedly2+Lose electronics at anode and be oxidized into black The manganese dioxide of brown is attached to anode surface and causes anode conductivity to reduce, and current efficiency declines, and electric energy consumption increases, and enters simultaneously The manganese dioxide slag entering solution makes solution viscosity increase, and what impact produced is normally carried out.
Summary of the invention
It is an object of the invention to provide the isolation of purified of manganese ion in a kind of high nickel solution effective and easy and simple to handle Method.
Present invention is generally directed to the purification separation of manganese ion in high nickel solution, reduce the content of impurity manganese in nickel solution, subtract Little production is consumed energy, and has the using value of reality and the biggest market potential.
The purification method of manganese ion in a kind of high nickel solution, it is characterised in that concretely comprise the following steps: with hydrochloric acid solution and The pH value of the high nickel solution containing manganese ion is regulated to 1.0 ~ 5.0 by sodium hydroxide solution, is then heated to reflux, when temperature reaches 60 When ~ 90 DEG C, adding persulfate oxidation agent in solution, stirring reaction 1 hour, is continuously added in course of reaction at this temperature Sodium carbonate liquor, makes pH value of solution be maintained at 1.0 ~ 5.0, and filtering residue is filtered and is washed with deionized in reaction after terminating, collect filtrate And constant volume, measure in this solution the mass ratio of manganese and nickel element in manganese ion content and filtering residue.
In the described high nickel solution containing manganese ion, the mass concentration of nickel ion is 60g/L, and the mass concentration of manganese ion is 5g/L.
The mass concentration of described hydrochloric acid solution is 10%, and the mass concentration of sodium hydroxide solution is 10%, sodium carbonate liquor Mass concentration is 5%.
Described persulfate oxidation agent is any one in sodium peroxydisulfate, Ammonium persulfate., potassium peroxydisulfate.
Described persulfate oxidation agent is 1.0 ~ 3.0 with the mol ratio of manganese ion in solution.
The present invention utilizes persulfate as the Mn in oxidizing high nickel solution2+MnO for indissoluble2, to reach point From the purpose of manganese, its reaction principle is as follows.
It is good that the present invention compared with prior art has the purification degree of depth, and reaction efficiency is high, and it is few that the demanganization slag of generation carries nickel amount secretly And the advantage that operating cost is low, it is suitable in nickel fibers relevant enterprise promoting.
Detailed description of the invention
Embodiment 1
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 2.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 60 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 2.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is potassium peroxydisulfate.
Persulfate oxidation agent is 1.0 with the mol ratio of manganese ion in solution.
Embodiment 2
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 2.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 60 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 2.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is sodium peroxydisulfate.
Persulfate oxidation agent is 3.0 with the mol ratio of manganese ion in solution.
Embodiment 3
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 3.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 70 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 3.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is sodium peroxydisulfate.
Persulfate oxidation agent is 1.5 with the mol ratio of manganese ion in solution.
Embodiment 4
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 4.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 80 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 4.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is Ammonium persulfate..
Persulfate oxidation agent is 2.0 with the mol ratio of manganese ion in solution.
Embodiment 5
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 5.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 90 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 5.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is Ammonium persulfate..
Persulfate oxidation agent is 3.0 with the mol ratio of manganese ion in solution.
Embodiment 6
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 4.5 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 80 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 4.5, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is potassium peroxydisulfate.
Persulfate oxidation agent is 1.2 with the mol ratio of manganese ion in solution.
Embodiment 7
Take high nickel solution 100 milliliters, regulate the pH value of high nickel solution to 5.0 with hydrochloric acid solution and sodium hydroxide solution.
The 100 milliliters of high nickel solutions adjusted are added to three neck round bottom flask, is heated and refluxed for, when temperature reaches 80 DEG C time, in solution add persulfate oxidation agent, at this temperature stirring reaction 1 hour, course of reaction is continuously added carbon Acid sodium solution, makes pH value of solution be maintained at 5.0, and reaction is filtered after terminating and washs filtering residue in three times with 90mL deionized water, collects Filtrate is also settled to 250mL.
Hydrochloric acid solution mass concentration is 10%, and sodium hydroxide solution mass concentration is 10%, and sodium carbonate liquor mass concentration is 5%。
Persulfate oxidation agent is Ammonium persulfate..
Persulfate oxidation agent is 2.0 with the mol ratio of manganese ion in solution.
Fe content in filtrate constant volume liquid after table 1 embodiment 1～7 demanganization
Manganese nickel mass ratio in filtering residue after table 2 embodiment 3～8 demanganization
。

Claims (5)

1. the purification method of manganese ion in a high nickel solution, it is characterised in that concretely comprise the following steps: with hydrochloric acid solution and hydrogen The pH value of the high nickel solution containing manganese ion is regulated to 1.0 ~ 5.0 by sodium hydroxide solution, is then heated to reflux, when temperature reach 60 ~ When 90 DEG C, adding persulfate oxidation agent in solution, stirring reaction 1 hour, is continuously added in course of reaction at this temperature Sodium carbonate liquor, makes pH value of solution be maintained at 1.0 ~ 5.0, and filtering residue is filtered and is washed with deionized in reaction after terminating, collect filtrate And constant volume, measure in this solution the mass ratio of manganese and nickel element in manganese ion content and filtering residue.
2. the method for claim 1, it is characterised in that in the described high nickel solution containing manganese ion, the quality of nickel ion is dense Degree is 60g/L, and the mass concentration of manganese ion is 5g/L.
3. the method for claim 1, it is characterised in that the mass concentration of described hydrochloric acid solution is 10%, and sodium hydroxide is molten The mass concentration of liquid is 10%, and the mass concentration of sodium carbonate liquor is 5%.
4. the method for claim 1, it is characterised in that described persulfate oxidation agent be sodium peroxydisulfate, Ammonium persulfate., Any one in potassium peroxydisulfate.
5. the method as described in claim 1 or 4, it is characterised in that described persulfate oxidation agent and the rubbing of manganese ion in solution Your ratio is 1.0 ~ 3.0.
CN201610592443.3A 2016-07-26 2016-07-26 Separation and purification method for manganese ions in high-nickel solution Pending CN106048222A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107419295A (en) * 2017-03-24 2017-12-01 金川集团股份有限公司 The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002241856A (en) * 2001-02-21 2002-08-28 Sumitomo Metal Mining Co Ltd Method for recovering valuable metal from used nickel- hydrogen secondary battery
CN1502710A (en) * 2002-11-26 2004-06-09 中南大学 Deep purification method of manganese sulfate solution
CN102041381A (en) * 2011-01-17 2011-05-04 河南永通镍业有限公司 Method for recovering nickel, cobalt, iron, manganese and magnesium from oxidized nickel ore
CN102776374A (en) * 2011-05-09 2012-11-14 深圳市格林美高新技术股份有限公司 Treatment method of nickel-cadmium slag
CN103088215A (en) * 2012-10-16 2013-05-08 赣州市豪鹏科技有限公司 Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio
CN104617349A (en) * 2014-12-09 2015-05-13 张国英 Method for preparing nickel sulfate by utilizing waste Ni-NH battery cathode material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002241856A (en) * 2001-02-21 2002-08-28 Sumitomo Metal Mining Co Ltd Method for recovering valuable metal from used nickel- hydrogen secondary battery
CN1502710A (en) * 2002-11-26 2004-06-09 中南大学 Deep purification method of manganese sulfate solution
CN102041381A (en) * 2011-01-17 2011-05-04 河南永通镍业有限公司 Method for recovering nickel, cobalt, iron, manganese and magnesium from oxidized nickel ore
CN102776374A (en) * 2011-05-09 2012-11-14 深圳市格林美高新技术股份有限公司 Treatment method of nickel-cadmium slag
CN103088215A (en) * 2012-10-16 2013-05-08 赣州市豪鹏科技有限公司 Method for separating nickel-cobalt and manganese in nickel-cobalt-manganese material with high manganese-cobalt ratio
CN104617349A (en) * 2014-12-09 2015-05-13 张国英 Method for preparing nickel sulfate by utilizing waste Ni-NH battery cathode material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107419295A (en) * 2017-03-24 2017-12-01 金川集团股份有限公司 The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate

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