CN106191917A - A kind of impurity removal process of nickle electrolysis anode solution - Google Patents

A kind of impurity removal process of nickle electrolysis anode solution Download PDF

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Publication number
CN106191917A
CN106191917A CN201610637509.6A CN201610637509A CN106191917A CN 106191917 A CN106191917 A CN 106191917A CN 201610637509 A CN201610637509 A CN 201610637509A CN 106191917 A CN106191917 A CN 106191917A
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anode solution
electrolysis anode
nickle electrolysis
concentration
nickle
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CN201610637509.6A
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伍廉奎
郑国渠
曹华珍
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Co Ltd Of Yiwu Scientific And Technical Research Institute Of Zhejiang Polytechnical University
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Co Ltd Of Yiwu Scientific And Technical Research Institute Of Zhejiang Polytechnical University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C25C1/08Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06Operating or servicing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

A kind of impurity removal process of nickle electrolysis anode solution, said method comprising the steps of: (1) nickle electrolysis anode solution containing ammonium chloride concentration range is 30~300g/L, nickel ion concentration scope is 0.5~100g/L, copper ion concentration scope is 0.5~10g/L, iron concentration scope is 0.01~2g/L, take nickle electrolysis anode solution, adding nickel sulfide makes its concentration range be 0.5~20g/L, control temperature 20~70 DEG C, magnetic agitation rotating speed 300~700r/min, after stirring 10~120min, filtering, filtrate is the nickle electrolysis anode solution after copper removal;(2) the nickle electrolysis anode solution addition ammonia after copper removal makes its concentration be 30~400g/L, stirs 1~20min, the nickle electrolysis anode solution after filtration, after obtaining except ferrum.This technique has the advantages such as technique is simple, raw material is simple and easy to get, flow process does not introduce other impurity, copper removal ferrum excellent effect.

Description

A kind of impurity removal process of nickle electrolysis anode solution
(1) technical field
The present invention relates to the impurity removal process of a kind of nickle electrolysis anode solution, belong to technical field of wet metallurgy.
(2) background technology
In the commercial production of current electrolytic nickel, mainly carry out electrolytic nickel with sulfuric acid system, this technique changing through many decades Make and reform, the most perfect, the most ripe, but it is as the development of society, and the progress of science and technology, traditional electro-nickel process The most day by day appear its shortcoming existed.The shortcoming that traditional electrolytic nickel technique exists is as follows:
1. use acid system electric deposition nickel technique, with boric acid as buffer agent, need strictly to be controlled by pH 4.5~5.4 In the range of, the too low meeting of pH causes cathode efficiency to reduce, and the too high meeting of pH causes the formation of nickel hydroxide, the physical property of nickel and shape Looks are deteriorated.
2. acid system, in electrolytic process Anodic liquid, impurity content and kind are more, numerous in acid system remove impurity flow process Miscellaneous, process cost is higher.
Therefore, relative efficiency is green, technological process relative ease, it is possible to is suitable for automatic and mechanical and produces, increases production capacity, The ammonia complexing system electrolytic nickel method of the pH scope of expansion buffer additive has self-evident for the commercial production of electronickelling Huge meaning, and also comply with the green production policy advocated of country instantly, and using ammonium chloride system as anolyte Electrolysis, it is possible to being configured to conform to the ammonia complexing system electrolyte of negative electrode electro-deposition requirement, copper and ferrum are major impurities in anolyte, But ammonium chloride system copper removal ferrum technique study almost without.
The present invention proposes a kind of method of ammonium chloride system copper removal ferrum, has huge for ammonia complexing alkaline system electrolytic nickel Big prospect, environment and economic benefit.
(3) summary of the invention
It is an object of the invention to for ammonia complexing alkaline system electrolytic nickel copper removal ferrum research almost without problem, propose one Plant nis matte in alkaline electrolyte, leach impurity removal process, by ammonium chloride system electrolytic nickel anolyte, add nickel sulfide Copper removal, addition ammonia, except ferrum, can effectively remove impurity, be successfully obtained copper iron content and reach the electrolyte of standard, this technique There is the advantages such as technique is simple, raw material is simple and easy to get, flow process does not introduce other impurity, copper removal ferrum excellent effect.
For achieving the above object, the present invention adopts the following technical scheme that
The impurity removal process of a kind of nickle electrolysis anode solution, said method comprising the steps of:
(1) nickle electrolysis anode solution containing ammonium chloride concentration range be 30~300g/L, nickel ion concentration scope be 0.5~ 100g/L, copper ion concentration scope are 0.5~10g/L, iron concentration scope is 0.01~2g/L, take nickle electrolysis anode solution, Adding nickel sulfide makes its concentration range be 0.5~20g/L, control temperature 20~70 DEG C, magnetic agitation rotating speed 300~700r/ Min, after stirring 10~120min, filters, and filtrate is the nickle electrolysis anode solution after copper removal;
(2) the nickle electrolysis anode solution addition ammonia after copper removal makes its concentration be 30~400g/L, stirs 1~20min, mistake After filter, the nickle electrolysis anode solution after obtaining except ferrum, prepare nickel for negative electrode electro-deposition.
Further, in step (1), described ammonia chloride concentration is preferably 50~200g/L.
Further, in step (1), described nickel ion concentration is preferably 5~80g/L.
Further, in step (1), described copper ion concentration is preferably 1~5g/L.
Further, in step (1), described iron concentration is preferably 0.05~1g/L.
Further, in step (1), nickel sulfide concentration is preferably 1~10g.
Further, in step (1), temperature range is preferably 40~60 DEG C.
Further, in step (1), magnetic agitation rotating speed is preferably 400~600r/min.
Further, in step (1), mixing time is preferably 20~80min.
Further, in step (2), ammonia concn is preferably 50~250g/L.
Further, in step (2), mixing time is preferably 3~10min.
Further, described preparation is made up of step (1)~(2).
The anode that nickle electrolysis anode solution of the present invention is corresponding is converter mattes.
The invention has the beneficial effects as follows: the present invention solves nickel ammonia alkali electrolysis system Anodic liquid and removes impurity copper ferrum Problem, effect disclosure satisfy that industrial requirement.Needed raw material reusable edible of the present invention, technological process is simple, and environmental protection has Huge prospect, environment and economic benefit.
(4) accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of embodiment 3 electronickelling.
(5) detailed description of the invention
Below by specific embodiment, the present invention is further detailed, but protection scope of the present invention not only limiting In this.
Embodiment 1
Take containing ammonium chloride concentration 30g/L, nickel ion concentration is 0.5g/L, copper ion concentration is 0.5g/L, iron concentration For 0.01g/L, taking electrolyte 1L in beaker, add nickel sulfide, its quality is 0.5g, controls temperature 20 DEG C, and magnetic agitation turns Speed 700r/min, after stirring 10min, filters, and filtrate is electrolyte after copper removal.After copper removal, electrolyte addition ammonia is allowed to again Concentration is 30g/L, Glass rod stirring 1min, after filtration, obtains, except electrolyte after ferrum, preparing nickel for negative electrode electro-deposition.
Copper removal rate based on example 1 is 99.21%, except ferrum rate is 98.57%.
Nickel plating to embodiment 1 gained carries out macroscopic observation layer by layer and SEM characterizes, and nickel coating macro morphology is bright and flat Whole, the smooth densification of microscopic appearance.
Embodiment 2
Take containing ammonium chloride concentration 300g/L, nickel ion concentration is 100g/L, copper ion concentration is 10g/L, iron concentration For 2g/L, taking electrolyte 1L in beaker, add nickel sulfide, its quality is 20g, controls temperature 70 C, magnetic agitation rotating speed 300r/min, after stirring 120min, filters, and filtrate is electrolyte after copper removal.After copper removal, electrolyte adds 400g/L ammonia again Water, Glass rod stirring 20min, after filtration, obtain, except electrolyte after ferrum, preparing nickel for negative electrode electro-deposition.
Copper removal rate based on example 2 is 98.88%, except ferrum rate is 97.27%.
Nickel plating to embodiment 1 gained carries out macroscopic observation layer by layer and SEM characterizes, and nickel coating macro morphology is bright and flat Whole, the smooth densification of microscopic appearance.
Embodiment 3
Take containing ammonium chloride concentration 50g/L, nickel ion concentration is 5g/L, copper ion concentration is 1g/L, iron concentration is 0.05g/L, takes electrolyte 1L in beaker, adds nickel sulfide, and its quality is 1g, controls temperature 40 DEG C, magnetic agitation rotating speed 400r/min, after stirring 80min, filters, and filtrate is electrolyte after copper removal.After copper removal, electrolyte adds 50g/L ammonia again, Glass rod stirring 3min, after filtration, obtains, except electrolyte after ferrum, preparing nickel for negative electrode electro-deposition.
Copper removal rate based on example 3 is 99.57%, except ferrum rate is 98.65%.
The nickel coating of embodiment 3 gained being carried out macroscopic observation and SEM characterizes, nickel coating macro morphology is bright and smooth, The smooth densification of microscopic appearance.
Embodiment 4
Take containing ammonium chloride concentration 200g/L, nickel ion concentration is 80g/L, copper ion concentration is 5g/L, iron concentration is 1g/L, takes electrolyte 1L in beaker, adds nickel sulfide, and its quality is 10g, controls temperature 60 C, magnetic agitation rotating speed 600r/ Min, after stirring 20min, filters, and filtrate is electrolyte after copper removal.After copper removal, electrolyte adds 250g/L ammonia, glass again Rod stirring 10min, after filtration, obtains, except electrolyte after ferrum, preparing nickel for negative electrode electro-deposition.
Copper removal rate based on example 4 is 98.79%, except ferrum rate is 99.11%.
The nickel coating of embodiment 4 gained being carried out macroscopic observation and SEM characterizes, nickel coating macro morphology is bright and smooth, The smooth densification of microscopic appearance.
Embodiment 5
Take containing ammonium chloride concentration 125g/L, nickel ion concentration is 40g/L, copper ion concentration is 2.5g/L, iron concentration For 0.5g/L, taking electrolyte 1L in beaker, add nickel sulfide, its quality is 5g, controls temperature 50 C, magnetic agitation rotating speed 500r/min, after stirring 40min, filters, and filtrate is electrolyte after copper removal.After copper removal, electrolyte adds 120g/L ammonia again Water, Glass rod stirring 5min, after filtration, obtain, except electrolyte after ferrum, preparing nickel for negative electrode electro-deposition.
Copper removal rate based on example 5 is 99.53%, except ferrum rate is 99.32%.
The nickel coating of embodiment 5 gained being carried out macroscopic observation and SEM characterizes, nickel coating macro morphology is bright and smooth, The smooth densification of microscopic appearance.

Claims (6)

1. an impurity removal process for nickle electrolysis anode solution, said method comprising the steps of:
(1) nickle electrolysis anode solution containing ammonium chloride concentration range be 30~300g/L, nickel ion concentration scope be 0.5~100g/L, Copper ion concentration scope is 0.5~10g/L, iron concentration scope is 0.01~2g/L, takes nickle electrolysis anode solution, adds sulfuration Nickel makes its concentration range be 0.5~20g/L, control temperature 20~70 DEG C, and magnetic agitation rotating speed 300~700r/min stirs 10 ~after 120min, filter, filtrate is the nickle electrolysis anode solution after copper removal;
(2) the nickle electrolysis anode solution addition ammonia after copper removal makes its concentration be 30~400g/L, stirs 1~20min, filters After, the nickle electrolysis anode solution after obtaining except ferrum.
2. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: in step (1), described ammonia chloride Concentration is 50~200g/L, and nickel ion concentration is 5~80g/L, and copper ion concentration is 1~5g/L, iron concentration be 0.05~ 1g/L, nickel sulfide concentration is 1~10g.
3. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1 or 2, it is characterised in that: in step (1), temperature model Enclosing is 40~60 DEG C, and magnetic agitation rotating speed is 400~600r/min, and mixing time is 20~80min.
4. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: in step (2), ammonia concn is 50~250g/L.
5. the impurity removal process of the nickle electrolysis anode solution as described in claim 1 or 4, it is characterised in that: in step (2), during stirring Between be 3~10min.
6. the impurity removal process of nickle electrolysis anode solution as claimed in claim 1, it is characterised in that: described technique by step (1)~ (2) composition.
CN201610637509.6A 2016-08-04 2016-08-04 A kind of impurity removal process of nickle electrolysis anode solution Pending CN106191917A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112658059A (en) * 2019-10-16 2021-04-16 丹阳市俊晧金属科技有限公司 Efficient preparation process of pure nickel wire
CN114517309A (en) * 2022-03-15 2022-05-20 金川镍钴研究设计院有限责任公司 Method for supplementing nickel and removing copper in nickel electrolysis production system

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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
CN103320811A (en) * 2013-06-05 2013-09-25 中南大学 Method for removing impurities from nickel electrolysis anolyte
CN104099637A (en) * 2013-04-07 2014-10-15 中国科学院过程工程研究所 Gradual depth method for removing metal ion impurity from nickel anode electrolyte
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

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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
CN104099637A (en) * 2013-04-07 2014-10-15 中国科学院过程工程研究所 Gradual depth method for removing metal ion impurity from nickel anode electrolyte
CN103320811A (en) * 2013-06-05 2013-09-25 中南大学 Method for removing impurities from nickel electrolysis anolyte
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

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112658059A (en) * 2019-10-16 2021-04-16 丹阳市俊晧金属科技有限公司 Efficient preparation process of pure nickel wire
CN114517309A (en) * 2022-03-15 2022-05-20 金川镍钴研究设计院有限责任公司 Method for supplementing nickel and removing copper in nickel electrolysis production system
CN114517309B (en) * 2022-03-15 2023-09-26 金川镍钴研究设计院有限责任公司 Nickel supplementing and decoppering method in nickel electrolysis production system

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