CN107059100A - A kind of method of nickel button anolyte depickling - Google Patents
A kind of method of nickel button anolyte depickling Download PDFInfo
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- CN107059100A CN107059100A CN201710181916.5A CN201710181916A CN107059100A CN 107059100 A CN107059100 A CN 107059100A CN 201710181916 A CN201710181916 A CN 201710181916A CN 107059100 A CN107059100 A CN 107059100A
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- Prior art keywords
- anolyte
- depickling
- nickel button
- additive
- extraction
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/402—Mixtures of acyclic or carbocyclic compounds of different types
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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
A kind of method of nickel button anolyte depickling, non-ferrous metal technical field of wet metallurgy, methods described comprises the following steps：Prepare organic phase：N 235, additive, sulfonated kerosene are mixed, wherein the extractants of N 235 occupy the 12.5%~25% of machine phase volume, and additive occupies the 13%~25.5% of machine phase volume, and sulfonated kerosene occupies the 60%~65% of machine phase volume；Wherein additive is the mixed liquor of isooctanol, sec-octyl alcohol or isooctanol and sec-octyl alcohol；Extract depickling：The organic phase prepared and pH value are mixed for 1.5~2.5 nickel button anolyte, wherein organic phase and the volume ratio of nickel button anolyte are 0.8:1~1:2, during which with uniform stirring, incorporation time 3~5 minutes, whole process temperature control is at 25 ~ 60 DEG C, after demixing, and upper strata is that N 235 loads organic, and lower floor is the nickel button anolyte that pH value is 3.0~4.0.
Description
Technical field
The present invention relates to non-ferrous metal technical field of wet metallurgy, specifically a kind of method of nickel button anolyte depickling.
Background technology
Nickel button（Including Active Nickel Containing Sulphur button）It is the indispensable raw material of accuracy electroplate industry, in electroplating process, mainly
Anode material as basket plating industry.Compared with general electrolytic nickel, chemolysis activity is good, and the tank voltage of electroplating bath is low,
Electric energy is saved, there is very wide application prospect in electroplating industry.
Main electrodeposition reaction is as follows in nickel button production process：
Anode reaction：H2O - 2e = 2H+ + 1/2O2
Cathode reaction：Ni2+ + 2e = Ni
With the progress of above-mentioned reaction, anolyte pH value is more and more lower, and the anolyte pH value of output is 2.5 in actual production process
~1.5, substantial amounts of nertralizer nickelous carbonate need to be relied on（Or sodium carbonate）Regulation pH becomes qualified catholyte, catholyte pH value
Standard is 3.0~4.0, and 2 tons or so of nickelous carbonate need to be consumed by often producing 1 ton of nickel button, because nickelous carbonate high processing costs cause nickel button
Production cost expense is higher, therefore need to explore new anolyte deacidifying process reduction nickel button production cost.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method of nickel button anolyte depickling, have solved prior art
The problem of production cost is higher.
The present invention solve technical problem technical scheme be：A kind of method of nickel button anolyte depickling, methods described includes
Following steps：
Prepare organic phase：N-235, additive, sulfonated kerosene are mixed, wherein N-235 extractants occupy machine phase volume
12.5%~25%, additive occupies the 13%~25.5% of machine phase volume, and sulfonated kerosene occupies the 60%~65% of machine phase volume；Wherein
Additive is the mixed liquor of isooctanol, sec-octyl alcohol or isooctanol and sec-octyl alcohol；
Extract depickling：The organic phase prepared and pH value are mixed for 1.5~2.5 nickel button anolyte, wherein organic phase and nickel
The volume ratio for detaining anolyte is 0.8:1~1:2, during which with uniform stirring, incorporation time 3~5 minutes, whole process temperature control
System is at 25 ~ 60 DEG C, after demixing, and upper strata is that N-235 loads are organic, and lower floor is the nickel button anode that pH value is 3.0~4.0
Liquid.
The extraction preferred cross current solvent extraction method of depickling step.
In the extraction depickling step, 2 cross current solvent extractions are at most carried out, you can reach pH3.0~4.0 needed for catholyte.
When the additive selects the mixed liquor of isooctanol and sec-octyl alcohol, the volume ratio of isooctanol and sec-octyl alcohol maintains 1:
1。
Can be that N-235 load organic phases are stripped to waste liquid after the extraction depickling terminates, back extraction concentration is
10%~15%NaOH solution, adjoint uniform stirring, NaOH during the NaOH solution prepared is added into load organic phases during back extraction
It is organic that solution can be used for continuous several times backwash to load, until the close neutrality of backwash liquor.
The beneficial effects of the present invention are：The acid stripping method provided, technological process is simple and direct, and production cost is low, without adding
Enter other nertralizers, anolyte deacidification efficiency is high, catholyte requirement needed for electrodeposition production, and N-235 can be met by producing pH value of solution
Extraction deacidifying process belongs to domestic initiation applied to nickel button anolyte depickling.
The effect of sulfonated kerosene and advantage：Sulfonated kerosene functions as diluent, is tied with extract without chemistry
The atent solvent of conjunction, can effectively improve the physical property of extraction organic phase, reduces the viscosity of extractant, increases its mobility, change
Become the density of organic phase, expand the density contrast of it and aqueous phase, be conducive to the separating clarifying of two-phase.
Isooctanol, the effect of sec-octyl alcohol and advantage：N-235 extractants solubility in diluent sulfonated kerosene is smaller, easily
There is third phase（Third phase is that not miscible second formed in solvent extraction process between organic phase and aqueous phase is organic
Phase）, additive must be added to eliminate the third phase formed in extraction process, therefore add additive sec-octyl alcohol or isooctanol.Cause
Isooctanol and sec-octyl alcohol easily regenerate, and chemical stability is good, so being used for eliminating the 3rd produced in extraction process as additive
Phase.
The advantage of cross current solvent extraction：Feed liquid and raffinate at different levels are all in contact with fresh extractant, and extraction yield is higher, extraction
Time is short, few compared to counter-current extraction extraction series, is more suitably applied to the quick deacidifying process of nickel button anolyte.
N-235 extracts depickling principle：N-235 is tertiary amine compounds, and its chemical name is trialkylamine, and N-235 belongs to
Basic extractant, occurs following reaction in sulfuric acid solution with sulfuric acid：2R3N+H2SO4=(R3NH) 2SO4, when in solution
When acidity is very high, neutral organic sulfate (R3NH) 2SO4 and the sulfuric acid in solution of generation react again：(R3NH)2·
SO4+H2SO4=2 (R3NH) HSO4, reacts the organic disulfate generated and is transferred in load organic phases, so as to reach electrodeposition sun
The purpose of pole liquid depickling.
Illustrate why this technological process back extraction can obtain the N-235 of high-quality：N-235 load organic phases are stripped with NaOH solution
Reacted when taking：(R3NH) HSO4+2NaOH=R3N+Na2SO4+2H2O, is regenerated load organic phases N-235, therefore
As long as strict control backwash liquor NaOH solution concentration, N-235 organic phases can be achieved on recycling, and extraction acidity can be not
It can decline with the increase of access times.
Why technological process can discharge Na influence：This technological process Na will not be loaded with phase into N-235,
Na is stayed in backwash liquor all the time, and backwash liquor is metabisulfite solution, builds up to finite concentration, available for production sodium sulphate.
Embodiment
The present invention will be further described with reference to embodiments.
Embodiment 1.
A kind of method of nickel button anolyte depickling, methods described comprises the following steps：
Prepare organic phase：N-235, additive, sulfonated kerosene are mixed, wherein N-235 extractants occupy machine phase volume
12.5%, additive occupies the 13% of machine phase volume, and remaining is sulfonated kerosene.Wherein additive is isooctanol.
Organic phase dilution：The organic phase prepared is mixed with water conjunction, the wherein volume ratio of organic phase and aqueous phase is 0.8:
1。
Extract depickling：Nickel button anolyte is mixed with the organic phase prepared, during which with uniform stirring, during mixing
Between 3~5 minutes, whole process temperature maintains 25 ~ 60 degrees Celsius, after demixing, remove waste, the extraction
The preferred cross current solvent extraction method of depickling step.
Back extraction：Can be that load organic phases are stripped to waste liquid after extraction depickling terminates, back extraction concentration is 10%
~15%NaOH solution；Adjoint uniform stirring during NaOH solution is added into load organic phases during back extraction, NaOH solution can be used for connecting
Continuous multiple backwash load is organic, until the close neutrality of washing lotion.
Embodiment 2.
A kind of method of nickel button anolyte depickling, methods described comprises the following steps：
Prepare organic phase：N-235, additive, sulfonated kerosene are mixed, wherein N-235 extractants occupy machine phase volume
25%, additive occupies the 25.5% of machine phase volume, and remaining is sulfonated kerosene, and wherein additive is sec-octyl alcohol.
Organic phase dilution：The organic phase prepared is mixed with water conjunction, the wherein volume ratio of organic phase and aqueous phase is 1:2.
Extract depickling：Nickel button anolyte is mixed with the organic phase after dilution, during which with uniform stirring, during mixing
Between 3~5 minutes, whole process temperature maintains 25 ~ 60 degrees Celsius, after demixing, removes waste i.e., and the extraction is de-
The sour preferred cross current solvent extraction method of step.
Back extraction：Can be that load organic phases are stripped to waste liquid after extraction depickling terminates, back extraction concentration is 10%
~15%NaOH solution；Adjoint uniform stirring during NaOH solution is added into load organic phases during back extraction, NaOH solution can be used for connecting
Continuous multiple backwash load is organic, until the close neutrality of washing lotion.
Embodiment 3.
A kind of method of nickel button anolyte depickling, methods described comprises the following steps：
Prepare organic phase：N-235, additive, sulfonated kerosene are mixed, wherein N-235 extractants occupy machine phase volume
20%, additive occupies the 18% of machine phase volume, and sulfonated kerosene occupies the 62% of machine phase volume；Wherein additive be isooctanol with it is secondary
The mixed liquor of octanol；The volume ratio of isooctanol and sec-octyl alcohol maintains 1:1.
Organic phase dilution：The organic phase prepared is mixed with water conjunction, the wherein volume ratio of organic phase and aqueous phase is 1:
1.7。
Extract depickling：Nickel button anolyte is mixed with the organic phase after dilution, during which with uniform stirring, incorporation time
3~5 minutes, whole process temperature maintained 25 ~ 60 degrees Celsius, after demixing, removed waste, extraction depickling step
Rapid preferably cross current solvent extraction method.
Back extraction：It can be that N-235 load organic phases are stripped to waste liquid after extraction depickling terminates, be stripped concentration
For 10%~15%NaOH solution, N-235 load organic phases are 1 with NaOH solution volume ratio：1, NaOH solution is added during back extraction
With uniform stirring during load organic phases, temperature control is at 25 ~ 60 DEG C, mixed phase time 5min, 2 minutes can split-phase completely,
It is organic that NaOH solution can be used for continuous several times backwash to load, until the close neutrality of washing lotion.
Claims (5)
1. a kind of method of nickel button anolyte depickling, it is characterised in that：Methods described comprises the following steps：
Prepare organic phase：
N-235, additive, sulfonated kerosene are mixed, wherein N-235 extractants occupy the 12.5%~25% of machine phase volume,
Additive occupies the 13%~25.5% of machine phase volume, and sulfonated kerosene occupies the 60%~65% of machine phase volume；Wherein additive is different
The mixed liquor of octanol, sec-octyl alcohol or isooctanol and sec-octyl alcohol；
Extract depickling：The organic phase prepared and pH value are mixed for 1.5~2.5 nickel button anolyte, wherein organic phase and nickel
The volume ratio for detaining anolyte is 0.8:1~1:2, during which with uniform stirring, incorporation time 3~5 minutes, whole process temperature control
System is at 25 ~ 60 DEG C, after demixing, and upper strata is that N-235 loads are organic, and lower floor is the nickel button anode that pH value is 3.0~4.0
Liquid.
2. a kind of method of nickel button anolyte depickling according to claim 1, it is characterised in that：The extraction depickling step
It is preferred that cross current solvent extraction method.
3. a kind of method of nickel button anolyte depickling according to claim 2, it is characterised in that：The extraction depickling step
In, at most carry out 2 cross current solvent extractions, you can reach pH3.0~4.0 needed for catholyte.
4. a kind of method of nickel button anolyte depickling according to claim 1, it is characterised in that：The additive is from different
During the mixed liquor of octanol and sec-octyl alcohol, the volume ratio of isooctanol and sec-octyl alcohol maintains 1:1.
5. a kind of method of nickel button anolyte depickling according to claim 1, it is characterised in that：The extraction depickling terminates
Afterwards, can be that N-235 load organic phases are stripped to waste liquid, back extraction concentration is 10%~15%NaOH solution, during back extraction
Born during the NaOH solution prepared is added into load organic phases with uniform stirring, NaOH solution available for continuous several times backwash
Machine is loaded with, until the close neutrality of backwash liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710181916.5A CN107059100A (en) | 2017-03-24 | 2017-03-24 | A kind of method of nickel button anolyte depickling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710181916.5A CN107059100A (en) | 2017-03-24 | 2017-03-24 | A kind of method of nickel button anolyte depickling |
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| Publication Number | Publication Date |
|---|---|
| CN107059100A true CN107059100A (en) | 2017-08-18 |
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| CN201710181916.5A Pending CN107059100A (en) | 2017-03-24 | 2017-03-24 | A kind of method of nickel button anolyte depickling |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1225807A1 (en) * | 1984-10-25 | 1986-04-23 | Государственный научно-исследовательский и проектно-конструкторский институт гидрометаллургии цветных металлов | Method of extracting sulfuric acid |
| CN101265589A (en) * | 2007-03-12 | 2008-09-17 | 张建玲 | Method for producing electrolytic nickel using various nickel-containing raw material |
| CN103421952A (en) * | 2013-08-01 | 2013-12-04 | 中南大学 | Synergic extraction agent and method for selectively extracting nickel in acidic nickeliferous solution through synergic extraction agent |
| CN103667697A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Method for extracting zinc from low-concentration zinc sulfate solution |
-
2017
- 2017-03-24 CN CN201710181916.5A patent/CN107059100A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1225807A1 (en) * | 1984-10-25 | 1986-04-23 | Государственный научно-исследовательский и проектно-конструкторский институт гидрометаллургии цветных металлов | Method of extracting sulfuric acid |
| CN101265589A (en) * | 2007-03-12 | 2008-09-17 | 张建玲 | Method for producing electrolytic nickel using various nickel-containing raw material |
| CN103421952A (en) * | 2013-08-01 | 2013-12-04 | 中南大学 | Synergic extraction agent and method for selectively extracting nickel in acidic nickeliferous solution through synergic extraction agent |
| CN103667697A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Method for extracting zinc from low-concentration zinc sulfate solution |
Non-Patent Citations (1)
| Title |
|---|
| 王炯: ""铜电解液萃取净化工艺探索试验"", 《南方冶金学院学报》 * |
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Application publication date: 20170818 |
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