CN105087960A - Method for extracting and separating nickel and cobalt by microemulsion - Google Patents
Method for extracting and separating nickel and cobalt by microemulsion Download PDFInfo
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- CN105087960A CN105087960A CN201510529400.6A CN201510529400A CN105087960A CN 105087960 A CN105087960 A CN 105087960A CN 201510529400 A CN201510529400 A CN 201510529400A CN 105087960 A CN105087960 A CN 105087960A
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- extraction
- cobalt
- microemulsion
- nickel
- extracting
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 38
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 33
- 239000010941 cobalt Substances 0.000 title claims abstract description 33
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003350 kerosene Substances 0.000 claims abstract description 9
- 239000001593 sorbitan monooleate Substances 0.000 claims abstract description 9
- 229940035049 sorbitan monooleate Drugs 0.000 claims abstract description 9
- 235000011069 sorbitan monooleate Nutrition 0.000 claims abstract description 9
- 239000012074 organic phase Substances 0.000 claims abstract description 8
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 15
- 238000007127 saponification reaction Methods 0.000 claims description 11
- -1 2-ethyl Chemical group 0.000 claims description 10
- JJJOZVFVARQUJV-UHFFFAOYSA-N 2-ethylhexylphosphonic acid Chemical class CCCCC(CC)CP(O)(O)=O JJJOZVFVARQUJV-UHFFFAOYSA-N 0.000 claims description 10
- 239000013543 active substance Substances 0.000 claims description 10
- 150000002148 esters Chemical class 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 7
- 238000013517 stratification Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 abstract description 9
- 239000012071 phase Substances 0.000 abstract description 9
- 229910001429 cobalt ion Inorganic materials 0.000 abstract description 8
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 abstract description 7
- 229910001453 nickel ion Inorganic materials 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 2
- ZDFBXXSHBTVQMB-UHFFFAOYSA-N 2-ethylhexoxy(2-ethylhexyl)phosphinic acid Chemical compound CCCCC(CC)COP(O)(=O)CC(CC)CCCC ZDFBXXSHBTVQMB-UHFFFAOYSA-N 0.000 abstract 1
- 239000011550 stock solution Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 12
- 238000004448 titration Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- FIHFWXNMOWDPBM-UHFFFAOYSA-N 2,4,4-trimethylpentylphosphonic acid Chemical class CC(C)(C)CC(C)CP(O)(O)=O FIHFWXNMOWDPBM-UHFFFAOYSA-N 0.000 description 1
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for extracting and separating nickel and cobalt by microemulsion, and belongs to the technical field of wet metallurgy. Firstly, surfactant sorbitan monooleate, 2-ethylhexylphosphonic acid mono 2-ethylhexyl ester and kerosene are mixed by a volume ratio of (5-20): (10-30): (85-50); sodium hydroxide solution is used for saponifying to obtain the microemulsion; the obtained microemulsion and extraction stock solution containing nickel and cobalt ions are mixed by a volume ratio of 1: 1-1: 10 for extraction; and the mixed extracted solution is stood and layered to obtain an extraction organic phase containing nickel and an extraction remained water phase containing cobalt. The method is a new method and a new process for extracting and separating the nickel and cobalt ions by a microemulsion system with low cost and high efficiency, and generates no emulsion phenomenon in the extraction process.
Description
Technical field
The present invention relates to a kind of method of microemulsion extracting and separating nickel cobalt, belong to technical field of wet metallurgy.
Background technology
The extracting and separating of microemulsion is the different Microphase Structure utilizing extraction system, improves it to the selectivity and the high efficiency that are extracted separating substances.Microemulsion is by spontaneous a kind of Thermodynamically stable, appearance transparent or the translucent dispersion system formed under suitable ratio such as water, oil, tensio-active agent under normal circumstances, likely overcome the defect of emulsion liquid film instability and breakdown of emulsion difficulty, microemulsion particle is little, thus there is larger mass transfer area, can mass-transfer efficiency be improved.
In conventional extraction, require suitable comparing, stirring velocity, mixing time etc.When there is extraction, if compare improper, or stirring velocity is improper, can reduce the percentage extraction of nickel cobalt.Kerosene, 2-ethylhexyl phosphonic acids single 2-ethyl base ester (P507), NaOH can make microemulsion, but this microemulsion percentage extraction is not that separation factor that is very high, cobalt nickel is low, needs multistage extraction, washing, stripping process, and process is complicated; And system is unstable, easy breakdown of emulsion; Organic system easily easily mixes with aqueous phase system and is mingled with, and causes the entrainment loss of organic reagent and raffinate to need complicated oil removing operation.When adding tensio-active agent sorbitan monooleate (class 80 of department) and being prepared into microemulsion, reduce the surface tension of system, greatly reduce the possibility of breakdown of emulsion, add the percentage extraction of cobalt, water, oil content are easy mutually, do not have emulsification and carry phenomenon secretly to occur.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides a kind of method of microemulsion extracting and separating nickel cobalt.The method is novel method and the novel process that a kind of inexpensive, efficient microemulsion system carries out nickel cobalt ion extracting and separating, and occurs without emulsion in extraction process, and the present invention is achieved through the following technical solutions.
A method for microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) be first (5 ~ 20) by volume by tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene: (10 ~ 30): (85 ~ 50) mix, and obtain microemulsion with sodium hydroxide solution saponification;
(2) the extraction stoste of microemulsion step (1) obtained and nickel and cobalt containing ion is that 1:1 ~ 1:4 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtains nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt.
In described step (1), sodium hydroxide solution is 0 ~ 12mol/l.
In the extraction stoste of the middle nickel and cobalt containing ion of described step (2), the mass ratio of Ni, Co is 1 ~ 100:1.
The invention has the beneficial effects as follows: base ester (P507) is domestic in sulfuric acid system extracting and separating nickel cobalt at present for the extraction agent 2-ethylhexyl phosphonic acids single 2-ethyl that the present invention adopts, the extraction agent of widespread use has 2-ethylhexyl phosphoric acid (D2EHPA or P204), 2-ethylhexyl phosphonic acids single 2-ethyl base ester (P507) and (2,4,4-tri-methyl-amyl) phosphonic acids (Cyanex272), and these three kinds of extraction agent acidity weaken successively and extracting and separating nickel, cobalt ability successively strengthen.Although the successful of Cyanex272 extracting and separating cobalt is better than P507, extraction progression can be reduced, save consumption, but price is very expensive, the producer of most domestic adopts P507 to carry out the separating-purifying of nickel and cobalt as extraction agent, and P204 is used for the degree of depth removing of the trace impurities such as Fe, Zn, Mn, Cu before Separation of nickel and cobalt, Be very effective.Use P507 to carry out the extracting and separating of nickel and cobalt, technique is comparatively ripe, can reach the object of separation.But use P507 low as its single-stage extraction efficiency comparison during extraction agent, the common extraction phenomenon of nickel is relatively more serious, needs multi-stage solvent extraction, washing, operation is comparatively complicated, and Solvent quantity is larger, and emulsion used is many, extraction time is long, sometimes also can produce serious emulsion.But experimental program of the present invention, the tensio-active agent added can reduce surface tension greatly, the percentage extraction improving cobalt (adopts the percentage extraction <80% of P507 cobalt in conventional extraction, and the percentage extraction of cobalt of the present invention is 87.93%), the common extraction phenomenon greatly reducing nickel (adopts the common extraction >10% of P507 nickel in conventional extraction, and the equal <5% of common extraction of nickel of the present invention), decrease the consumption (consumption of extraction agent reduces more than 10%) of extraction agent, reduce the consumption of emulsion, decrease extraction time, and reduce the possibility of emulsification.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The method of this microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) first by 20ml tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene be 5:15:80 mixing by volume, be that the saponification of 3mol/l sodium hydroxide solution obtains microemulsion (detailed process of saponification is stirred with the speed of 1000r/min by mixed oil phase by concentration, then using 3mol/NaOH titration, is titration end point when oil phase becomes limpid by muddiness);
(2) the extraction stoste of 50ml microemulsion step (1) obtained and nickeliferous (62.5g/l), cobalt (2.3g/l) ion is that 1:2 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtain nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt; Wherein the extraction stoste pH of nickel and cobalt containing ion is 4, and in raffinate aqueous phase, Co content is 0.45g/l, Ni content is that 61.14g/l(Ni, Co concentration is equal-volume conversion).
After extraction, the percentage extraction of cobalt ion is 80.23%, and the percentage extraction of nickel ion is 2.18%.
Embodiment 2
The method of this microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) first by 20ml tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene be 10:20:70 mixing by volume, be that the saponification of 3mol/l sodium hydroxide solution obtains microemulsion (detailed process of saponification is stirred with the speed of 1000r/min by mixed oil phase by concentration, then using 3mol/NaOH titration, is titration end point when oil phase becomes limpid by muddiness);
(2) the extraction stoste of 50ml microemulsion step (1) obtained and nickeliferous (70g/l), cobalt (1.5g/l) ion is that 1:1 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtain nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt; Wherein the extraction stoste pH of nickel and cobalt containing ion is 4, Co content, and to be 0.18g/l, Ni content be that 66.93g/l(Ni, Co concentration is equal-volume converts).
After extraction, the percentage extraction of cobalt ion is 87.93%, and the percentage extraction of nickel ion is 4.38%.
Embodiment 3
The method of this microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) first by 20ml tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene be 20:15:65 mixing by volume, be that the saponification of 3mol/l sodium hydroxide solution obtains microemulsion (detailed process of saponification is stirred with the speed of 1000r/min by mixed oil phase by concentration, then using 3mol/NaOH titration, is titration end point when oil phase becomes limpid by muddiness);
(2) the extraction stoste of 50ml microemulsion step (1) obtained and nickeliferous (50g/l), cobalt (0.5g/l) ion is that 1:1 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtain nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt; Wherein the extraction stoste pH of nickel and cobalt containing ion is 4, Co content, and to be 0.07g/l, Ni content be that 49.34g/l(Ni, Co concentration is equal-volume converts).
After extraction, the percentage extraction of cobalt ion is 86.27%, and the percentage extraction of nickel ion is 1.32%.
Embodiment 4
The method of this microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) first by 20ml tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene be 5:10:85 mixing by volume, be that the saponification of 12mol/l sodium hydroxide solution obtains microemulsion (detailed process of saponification is stirred with the speed of 1000r/min by mixed oil phase by concentration, then using 12mol/lNaOH titration, is titration end point when oil phase becomes limpid by muddiness);
(2) the extraction stoste of 50ml microemulsion step (1) obtained and nickeliferous (65g/l), cobalt (2.5g/l) ion is that 1:3 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtain nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt; Wherein the extraction stoste pH of nickel and cobalt containing ion is 4, Co content, and to be 0.64g/l, Ni content be that 63.10g/l(Ni, Co concentration is equal-volume converts).
After extraction, the percentage extraction of cobalt ion is 74.31%, and the percentage extraction of nickel ion is 2.92%.
Embodiment 5
The method of this microemulsion extracting and separating nickel cobalt, its concrete steps are as follows:
(1) first by 20ml tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene by volume for 20:30:50 is mixed to get microemulsion (without saponification process);
(2) the extraction stoste of 50ml microemulsion step (1) obtained and nickeliferous (2.5g/l), cobalt (2.5g/l) ion is that 1:4 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtain nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt; Wherein the extraction stoste pH of nickel and cobalt containing ion is 4, Co content, and to be 1.04g/l, Ni content be that 2.47g/l(Ni, Co concentration is equal-volume converts).
After extraction, the percentage extraction of cobalt ion is 58.33%, and the percentage extraction of nickel ion is 1.08%.
Above the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (3)
1. a method for microemulsion extracting and separating nickel cobalt, is characterized in that concrete steps are as follows:
(1) be first (5 ~ 20) by volume by tensio-active agent sorbitan monooleate, 2-ethylhexyl phosphonic acids single 2-ethyl base ester and kerosene: (10 ~ 30): (85 ~ 50) mix, and obtain microemulsion with sodium hydroxide solution saponification;
(2) the extraction stoste of microemulsion step (1) obtained and nickel and cobalt containing ion is that 1:1 ~ 1:4 mixes and extracts according to volume ratio, by liquid stratification after the extraction of mixing, obtains nickeliferous extracted organic phase and the raffinate aqueous phase containing cobalt.
2. the method for microemulsion extracting and separating nickel cobalt according to claim 1, is characterized in that: in described step (1), sodium hydroxide solution is 0 ~ 12mol/l.
3. the method for microemulsion extracting and separating nickel cobalt according to claim 1, is characterized in that: in the extraction stoste of the middle nickel and cobalt containing ion of described step (2), the mass ratio of Ni, Co is 1 ~ 100:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510529400.6A CN105087960A (en) | 2015-08-26 | 2015-08-26 | Method for extracting and separating nickel and cobalt by microemulsion |
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| CN201510529400.6A CN105087960A (en) | 2015-08-26 | 2015-08-26 | Method for extracting and separating nickel and cobalt by microemulsion |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177294A (en) * | 2015-07-28 | 2015-12-23 | 滨州学院 | Microemulsion system and method for extracting and separating nickel and lithium |
| CN105803483A (en) * | 2016-04-06 | 2016-07-27 | 王贺 | Preparation method for electro-deposited nickel and cobalt |
| CN111115595A (en) * | 2019-12-31 | 2020-05-08 | 四川大学 | Method for purifying raffinate acid |
| CN114015901A (en) * | 2021-11-15 | 2022-02-08 | 山东大学 | O/W emulsion and preparation method and application thereof |
| CN115961149A (en) * | 2021-10-12 | 2023-04-14 | 中国科学院过程工程研究所 | Method for separating nickel and cobalt ions by organic acid non-saponification extraction and application |
| CN116855759A (en) * | 2023-08-31 | 2023-10-10 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
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| CN103173616A (en) * | 2011-12-23 | 2013-06-26 | 北京石油化工学院 | Method for extracting and separating copper and cobalt in waste lithium ion battery leach solution with microemulsion |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177294A (en) * | 2015-07-28 | 2015-12-23 | 滨州学院 | Microemulsion system and method for extracting and separating nickel and lithium |
| CN105177294B (en) * | 2015-07-28 | 2018-06-29 | 滨州学院 | The microemulsion system and method for a kind of extraction and separation nickel and lithium |
| CN105803483A (en) * | 2016-04-06 | 2016-07-27 | 王贺 | Preparation method for electro-deposited nickel and cobalt |
| CN111115595A (en) * | 2019-12-31 | 2020-05-08 | 四川大学 | Method for purifying raffinate acid |
| CN111115595B (en) * | 2019-12-31 | 2022-11-04 | 四川大学 | Method for purifying raffinate acid |
| CN115961149A (en) * | 2021-10-12 | 2023-04-14 | 中国科学院过程工程研究所 | Method for separating nickel and cobalt ions by organic acid non-saponification extraction and application |
| CN114015901A (en) * | 2021-11-15 | 2022-02-08 | 山东大学 | O/W emulsion and preparation method and application thereof |
| CN116855759A (en) * | 2023-08-31 | 2023-10-10 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
| CN116855759B (en) * | 2023-08-31 | 2023-11-17 | 赣州吉锐新能源科技股份有限公司 | High-nickel low-cobalt feed liquid deep cobalt removal process for retired battery |
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Application publication date: 20151125 |