CN107815542B - A kind of synergic reagent and method for nickel selective extraction in acid solution - Google Patents
A kind of synergic reagent and method for nickel selective extraction in acid solution Download PDFInfo
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- 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
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- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
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Abstract
The invention discloses a kind of synergic reagents and method for nickel selective extraction in acid solution, synergic reagent is made of phosphate (salt) with picolinic acid ester, using the organic phase containing synergic reagent from acid solution selective extraction nickel, it can be realized efficiently separating for the foreign ions such as nickel ion and manganese ion, magnesium ion, calcium ion, load organic phases carry out the solution containing nickel that back extraction obtains high-purity using inorganic acid.This method is to nickel recovery height, and nickel and impurity good separating effect, process are short, it is easy to accomplish industrialization.
Description
Technical field
The present invention relates to a kind of synergic reagents, in particular to one kind is by picolinic acid ester and phosphate or phosphate ester salt group
At synergic reagent, and using synergic reagent selective extraction nickel from acid solution containing nickel method, belong to chemistry
Abstraction technique field.
Background technique
Nickel is important strategic rare metal, and industrially tool has been widely used.The hydrometallurgy of acid system be from
It is low-grade containing extract in nickel resources (such as nickel laterite, dead catalyst containing nickel, nickel-molybdenum ore, electroplating sludge) nickel main method it
One.The acid solution containing nickel containing impurity, such as nickel laterite can be generated in the acid system hydrometallurgy process of nickel-containing material
Sulphuric leachate, electroplating sludge sulphuric leachate, give up nickel-containing catalyst sulphuric leachate etc..In these acid solution containing nickels in addition to
Outside containing valuable metallic nickel ions, also contain a large amount of base metal cation impurity, such as iron, aluminium, manganese, magnesium, calcium, chromium.By grinding
The effort of the person's of studying carefully many years has been achieved for some achievements in terms of extraction of nickel from nickel acidic leaching solution, for example, Chinese patent
(patent No.: ZL201310332212.5) discloses a kind of synergic reagent and the selective extraction nickel from acid nickeliferous aqueous solution
Method, solve the separation problem of nickel and base metal impurity such as iron, aluminium, manganese, magnesium, calcium, chromium etc., can from nickel containing 2g/L,
(pH < 2) selectively extraction of nickel, the single-stage extraction rate of nickel in 30g/L aluminium and the ferric dead catalyst sulphuric leachate of 1g/L
Reach 96% or more, respectively up to 2524 and 4346, load organic phases are stripped with dilute sulfuric acid, inverse through 3 grades for ferronickel, nickel aluminium separation
Stream back extraction, the back extraction ratio of nickel is 99% or more.But one of synergic reagent constituent used in the patented technology " naphthalene sulphur
The synthesis technology of acid " is complex, at high cost, leads to the extraction and recovery higher cost of nickel.
Summary of the invention
For the traditional handicraft of nickel is proposed from nickeliferous acid solution there are at high cost, process is complicated, impurity separation is incomplete
The defects of and existing patent of invention (ZL201310332212.5) technology the deficiencies of there are higher costs, the purpose of the present invention
Be be to provide it is a kind of at low cost, can be from the acid solution containing nickel containing plurality of impurity ions such as manganese ion, magnesium ion, calcium ions
The synergic reagent of middle selective extraction nickel.
Another object of the present invention is to be that provide a kind of above-mentioned synergic reagent of use selects from acid solution containing nickel
The method of selecting property extraction of nickel, this method are able to achieve efficiently separating for nickel ion and manganese ion, magnesium ion, calcium ion etc., extract to nickel
Take high income, process short, at low cost, it is easy to accomplish industrial application.
In order to achieve the above technical purposes, the present invention provides a kind of collaborations for nickel selective extraction in acid solution
Extractant is made of picolinic acid ester with phosphate and/or phosphate ester salt；The picolinic acid ester has Formulas I structure；The phosphorus
Acid esters or phosphate ester salt have Formula II structure；
Wherein,
R is selected from C6~12Alkyl；
M is hydrogen ion, calcium ion, magnesium ion, ammonium ion or alkali metal ion；
N is the valence state number of M.
Synergic reagent of the invention is made of picolinic acid ester and phosphate (salt), and many experiments show that the two combines
It is had obvious synergistic function using to the nickel extraction in acid solution, phosphate (salt) or picolinic acid ester is used alone
When being used to extract nickel in acid solution as extractant, not only the extraction yield of nickel ion is low, and poor selectivity, with manganese from
The inferior separating effect of the foreign ions such as son, calcium ion and magnesium ion；It is extracted when being used as using phosphate (salt) and picolinic acid ester
It is high to the extraction yield of nickel ion when nickel in agent synergic solvent extraction acid solution, and the extraction yield of magnesium ion, calcium ion and manganese ion
Lower, therefore, picolinic acid ester and phosphate (salt) have an apparent positive coorperativity extraction to nickel ion, and to manganese ion,
Calcium ion and magnesium ion etc. have it is apparent inhibit extraction, so as to realize nickel ion and manganese ion, magnesium ion, calcium from
The extraction and separation of son etc..
The ratio between total mole number of preferred scheme, picolinic acid ester molal quantity and phosphate and phosphate ester salt is 1~6:1.
In preferred proportional region, the synergistic effect of the two can be given full play to, best effect of extracting is reached.
The method of the present invention also provides a kind of from acid solution selective extraction nickel, this method be will contain manganese ion,
The acidic aqueous solution of at least one of magnesium ion, calcium ion foreign ion and nickel ion using the organic phase containing synergic reagent into
Row single-stage or multi-stage counter current extraction, nickel ion selectively extract into organic phase, and foreign ion stays in raffinate；Load organic phases warp
After washing, single-stage is carried out using inorganic acid solution or multi-stage countercurrent is stripped, obtains pure solution containing nickel.
Preferred scheme, the acidic aqueous solution pH value are 1.2~5.0.
Preferred scheme, the organic phase are made of synergic reagent and organic diluent.
Preferred scheme, the total concentration of phosphate and phosphate ester salt is between 0.1~0.6mol/L in the organic phase.
More preferably scheme, the organic diluent be sulfonated kerosene, No. 260 solvent naphthas, aviation kerosine, Escaid110,
C8~13At least one of higher alcohols.
Preferred scheme, the inorganic acid solution are H+Sulfuric acid solution, hydrochloric acid of the concentration between 0.5~4.0mol/L are molten
At least one of liquid, nitric acid solution.
Preferred scheme, the series of the extraction are 1~10 grade.
More preferably scheme, the ratio between volume flow of organic phase and water phase is 1/5~10/1 in the extraction process.
Preferred scheme, the series of the back extraction are 1~10 grade.
More preferably scheme, during the back extraction the ratio between organic phase and the volume flow of inorganic acid solution be 1/1~
10/1。
Compared with the prior art, technical solution of the present invention bring the utility model has the advantages that
1) synergic reagent of the invention has apparent synergistic in the extraction process of acid nickel solution nickel ion
Effect, and have to foreign metal ions such as manganese ion, calcium ion, magnesium ions and inhibit extraction, it can be with more highly selective
Nickel ion is extracted from acid solution.
2) synergic reagent of the invention is commercially available conventional reagent, at low cost, advantageously reduces making for synergic reagent
Use cost.
3) method flow of the invention using nickel in synergic reagent selective extraction acid solution is short, nickel high income,
Good impurity removing effect, chemical reagent consumption is small, at low cost, it is easy to accomplish industrialization.
Specific embodiment
Following embodiment is intended to illustrate invention, rather than further limits to protection scope of the present invention.
In embodiment, distribution ratio D, separation β, extraction yield E1(%), stripping rate E2Respectively with impurities removing efficiency Y (%)
It is calculated by formula (1)~formula (5):
D=CMO/CMR (1)
βNi/M=DNi/DM (2)
E1=(CFVF-CRVR)/(CFVF) × 100% (3)
E2=Cs/(Co× R) × 100% (4)
Y=(CMF/CNiF-CMS/CNiS)/(CMF/CNiF) × 100% (5)
In formula (1), CMO,CMRRespectively indicate the concentration (g/L) of metal ions M in load organic phases and raffinate；Formula (2)
In, βNi/MIndicate the separation of Ni and impurity M, DNi,DMRespectively indicate the distribution ratio of Ni Yu impurity M；C in formula (3)F,CRRespectively
Indicate the concentration (g/L) of metal ion in feed liquid and raffinate；VF,VRRespectively indicate feed liquid and raffinate volume；In formula (4),
Cs,CoThe concentration (g/L) of metal ion in strip liquor and load organic phases is respectively indicated, R indicates organic phase and water phase volume flow
The ratio between；In formula (5), CMF, CNiFRespectively indicate the concentration (g/L) of foreign metal ion M and nickel ion in feed liquid, CMS, CNiSRespectively
Indicate the concentration (g/L) of foreign metal ion M and nickel ion in strip liquor.
Embodiment 1
Aqueous phase liquid: material liquid pH=2.0, each concentration of metal ions in feed liquid: Ni2+: 3.102g/L, Mn2+: 2.801g/L,
Mg2+: 1.447g/L, Ca2+: 0.487g/L.
Organic phase: three kinds that number is respectively 1,2,3 are prepared and forms different organic phases, the diluent in organic phase is sulphur
Change kerosene, No. 1 organic phase is the sulfonated kerosene solution of 1.0mol/L pyridine caprylate, the P204 that No. 2 organic phases are 0.25mol/L
Sulfonated kerosene solution, the sulfonated kerosene solution for the P204+1.0mol/L pyridine caprylate that No. 3 organic phases are 0.25mol/L.
Extraction and separation: above-mentioned 3 kinds of organic phases item that (volume ratio of organic phase and water phase) is 1/1 compared with feed liquid respectively
Carrying out single-stage extraction under part, the extraction equilibrium time is 10min, 25 DEG C of temperature.Experimental result is as shown in table 1.
The synergistic effect that 1 P204 of table and pyridine caprylate extract nickel
As it can be seen from table 1 phosphoric acid ester extractant P204 or picolinic acid ester extraction of nickel, the extraction yield of nickel is used alone
Very low (< 1%)；When phosphoric acid ester extractant P204 is used alone, the extraction yield of calcium is 7.0%；Picolinic acid ester is used alone
When, manganese, the extraction yield of calcium is respectively 7.21%, 33.41%, and magnesium-based is not originally extracted；When using phosphoric acid ester extractant P204 and
When the mixed extractant synergic solvent extraction nickel of picolinic acid ester composition, Ni2+Extraction yield reaches 53.68%, and the extraction yield of magnesium, calcium is equal
Lower than 1%.The distribution ratio of nickel, which is not only much larger than, when extracting mixed extractant is used alone phosphate or picolinic acid ester as extraction
The distribution ratio of nickel when agent, and it is much larger than sum of the two；But P204 is still even lower than used alone in the extraction yield of manganese, magnesium, calcium
Or extraction yield when picolinic acid ester, when using extracting mixed extractant, the separation of Ni/Mn, Ni/Mg and Ni/Ca are distinguished
Up to 3.62,5368 and 1789.It is indicated above that being had obviously by the mixed extractant that phosphate P204 and pyridine acid acid esters form to nickel
Positive coorperativity extraction, and then there is apparent counter-cooperative-ing extraction to act on magnesium, calcium, can be from containing Mn2+、Mg2+、Ca2+Equal impurity
Acid solution in selective extraction nickel.
Embodiment 2
Aqueous phase liquid is the same as embodiment 1.
Organic phase: six kinds that number is respectively 1,2,3,4,5,6 are prepared and forms different organic phases, the dilution in organic phase
Agent is sulfonated kerosene, and the concentration of pyridine caprylate is 1mol/L, and P204 concentration is respectively 0mol/L, 0.05mol/L, 0.15mol/
L、0.25mol/L、0.4mol/L、0.5mol/L。
Extraction and separation: above-mentioned 6 kinds of organic phases item that (volume ratio of organic phase and water phase) is 1/1 compared with feed liquid respectively
Carrying out single-stage extraction under part, the extraction equilibrium time is 30min, 25 DEG C of temperature.Experimental result is as shown in table 2.
2 extraction experiments result of table
From table 2 it can be seen that the concentration with extractant P204 increases, the separation of nickel and magnesium, calcium increases, in P204
When concentration reaches 0.5mol/L, the separation of nickel and manganese magnesium calcium is respectively 6.18,389.76,267.8.Should the result shows that,
Under the extraction system, the raising of P204 concentration is significantly increased to the separating effect of nickel and impurity especially magnesium calcium.
Embodiment 3
Aqueous phase liquid is the same as embodiment 1.
Organic phase: six kinds that number is respectively 1,2,3,4,5,6 are prepared and forms different organic phases, the dilution in organic phase
Agent is sulfonated kerosene, and P204 concentration is 0.25mol/L, pyridine octanoic acid ester concentration be respectively 0,0.25mol/L, 0.55mol/L,
0.75mol/L、1mol/L、1.25mol/L。
Extraction and separation: above-mentioned 6 kinds of organic phases item that (volume ratio of organic phase and water phase) is 1/1 compared with feed liquid respectively
Carrying out single-stage extraction under part, the extraction equilibrium time is 30min, 25 DEG C of temperature.Experimental result is as shown in table 3.
3 extraction test result of table
From table 3 it is observed that the extraction yield of nickel constantly rises as extractant pyridine octanoic acid ester concentration increases, work as pyrrole
When pyridine octanoic acid ester concentration is 1.25mol/L, in the case where not adjusting pH, the extraction yield of nickel reaches 57.9%.Increase extraction simultaneously
Agent pyridine octanoic acid ester concentration is taken, the separating effect of nickel and other metals is preferable.In addition, increasing the concentration of pyridine caprylate, split-phase
Time does not change substantially.Should the result shows that, under the extraction system, pyridine octanoic acid ester concentration it is appropriate increase to nickel and impurity
The separating effect of manganese magnesium calcium is significantly increased.
Embodiment 4
Aqueous phase liquid is the same as embodiment 1.
Organic phase: five kinds that number is respectively 1,2,3,4,5 are prepared and forms different organic phases, the diluent in organic phase
For sulfonated kerosene, the concentration of pyridine caprylate is 1.25mol/L, and P204 concentration is 0.25mol/L, using sodium hydroxide to 5 parts
Organic phase saponification, saponification rate is respectively 0%, 10%, 20%, 30%, 40%.Extraction and separation: above-mentioned 5 kinds of organic phases respectively with material
Liquid carries out single-stage extraction under conditions of being 1/1 compared to (volume ratio of organic phase and water phase), and the extraction equilibrium time is 30min,
25 DEG C of temperature.Experimental result is as shown in table 4.
4 extraction test result of table
As can be seen from Table 4, in extraction process, with the increase of saponification rate, the extraction yield of nickel and manganese all obviously rises,
Wherein the extraction yield variation of nickel is especially significant, rises to 78% from 59%.The separation of nickel and magnesium with saponification rate increase
First reduce and remain unchanged afterwards, nickel increases with the increase of saponification rate with the separation of manganese and calcium.It is 40% in saponification rate
When, the separation of nickel and manganese magnesium calcium is respectively 9.67,108.31,41.31.The result shows that under the extraction system, organic soap
The raising of rate is significantly improved to the separating effect of nickel and impurity manganese, calcium.
Embodiment 5
Aqueous phase liquid is the same as embodiment 1.
Organic phase: P204 concentration is 0.25mol/L in organic phase, and the concentration of 4PC is 1.25mol/L；Organic phase saponification rate
It is 40%.
Cascade extraction: carrying out 5 stage countercurrent extractions to feed liquid using above-mentioned organic phase, and the extraction equilibrium time is 10min,
25 DEG C of temperature.Experimental result is as shown in table 5.
5 extraction test result of table
As can be seen from Table 5, it being extracted by 5 stage countercurrents, the extraction yield of nickel reaches 98.7%, and other impurities metal
Extraction yield is substantially all 5% hereinafter, lower than respective single-stage extraction rate.Should the result shows that, under the extraction system, pass through 5
Stage countercurrent extraction, the rate of recovery of nickel greatly improve, and the separating effect of nickel and other foreign metals is significant.
Embodiment 6
Stripping agent: 0.5mol/L dilute sulfuric acid
Nickel concentration is 2.85g/L in load organic phases
Extraction and separation: single-stage extraction, extraction equilibrium are carried out under conditions of comparing 1/1 to load organic phases using stripping agent
Time is respectively 1min, 3min, 5min, 8min, 10min, 15min；25 DEG C of temperature.Experimental result is as shown in table 6.
6 extraction test result of table
As can be seen from Table 6, after Stripping times reach 3min, back extraction ratio maintains essentially in 91% or so, shows
Back extraction has reached balance when 3min or so, and strip kinetics are very fast.
Claims (10)
1. a kind of synergic reagent for nickel selective extraction in acid solution, it is characterised in that: by picolinic acid ester and phosphorus
Acid esters and/or phosphate ester salt composition；The picolinic acid ester has Formulas I structure；The phosphate or phosphate ester salt have Formula II
Structure；
Wherein,
R is selected from C6~12Alkyl；
M is hydrogen ion, calcium ion, magnesium ion, ammonium ion or alkali metal ion；
N is the valence state number of M.
2. a kind of synergic reagent for nickel selective extraction in acid solution according to claim 1, feature exist
In: the ratio between total mole number of picolinic acid ester molal quantity and phosphate and phosphate ester salt is 1~6:1.
3. a kind of method of the selective extraction nickel from acid solution, it is characterised in that: manganese ion, magnesium ion, calcium ion will be contained
At least one of the acidic aqueous solution of foreign ion and nickel ion use containing the organic of as claimed in claim 1 or 22 synergic reagents
It mutually carries out single-stage or multi-stage counter current extraction, nickel ion selectively extracts into organic phase, foreign ion stays in raffinate；It loads organic
After mutually washed, single-stage is carried out using inorganic acid solution or multi-stage countercurrent is stripped, obtains pure solution containing nickel.
4. the method for the selective extraction nickel according to claim 3 from acid solution, it is characterised in that: the acid water
Solution ph is 1.2~5.0.
5. the method for the selective extraction nickel according to claim 3 from acid solution, it is characterised in that:
The organic phase is made of synergic reagent and organic diluent；
The total concentration of phosphate and phosphate ester salt is between 0.1~0.6mol/L in the organic phase；
The organic diluent is sulfonated kerosene, No. 260 solvent naphthas, aviation kerosine, Escaid110, C8~13Higher alcohols in extremely
Few one kind.
6. the method for the selective extraction nickel according to claim 3 from acid solution, it is characterised in that: the inorganic acid
Solution is H+At least one of sulfuric acid solution of the concentration between 0.5~4.0mol/L, hydrochloric acid solution, nitric acid solution.
7. according to the method for the described in any item selective extraction nickel from acid solution of claim 3~6, it is characterised in that:
The series of the extraction is 1~10 grade.
8. the method for the selective extraction nickel according to claim 7 from acid solution, it is characterised in that: described to extract
The ratio between volume flow of organic phase and water phase is 1/5~10/1 in journey.
9. according to the method for the described in any item selective extraction nickel from acid solution of claim 3~6, it is characterised in that:
The series of the back extraction is 1~10 grade.
10. the method for the selective extraction nickel according to claim 9 from acid solution, it is characterised in that: the back extraction
The ratio between organic phase and the volume flow of inorganic acid solution are 1/1~10/1 during taking.
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| CN108642283B (en) * | 2018-05-25 | 2019-09-27 | 中南大学 | A kind of nickel cobalt synergic reagent and its method separated for nickel cobalt with impurity extraction |
| CN109097599B (en) * | 2018-09-27 | 2021-06-04 | 中南大学 | Method for separating manganese, calcium and magnesium by synergistic extraction |
| CN111533174B (en) * | 2020-04-10 | 2022-12-13 | 吉林吉恩镍业股份有限公司 | Method for removing zinc, calcium and magnesium ions in manganese sulfate solution by synergistic extraction method |
| CN114134341B (en) * | 2020-09-04 | 2023-01-13 | 苏州博萃循环科技有限公司 | Method for recovering nickel, cobalt and manganese in feed liquid containing nickel, cobalt and manganese |
| CN112442605A (en) * | 2020-11-24 | 2021-03-05 | 北京博萃循环科技有限公司 | Method for separating nickel and magnesium and application thereof |
| CN112430733A (en) * | 2020-11-30 | 2021-03-02 | 北京博萃循环科技有限公司 | Method for treating laterite-nickel ore |
| CN112607813B (en) * | 2021-01-04 | 2022-08-19 | 南昌航空大学 | Method for synergistically extracting nickel from nickel plating wastewater |
| GB202108372D0 (en) * | 2021-06-11 | 2021-07-28 | Johnson Matthey Plc | A recycling method for battery and catalyst materials |
| CN113481367B (en) * | 2021-06-30 | 2022-08-26 | 中南大学 | Method for selectively extracting and separating nickel and lithium |
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| CN104073638B (en) * | 2014-06-23 | 2016-05-25 | 先进储能材料国家工程研究中心有限责任公司 | A kind of method that adopts used Ni-MH battery to prepare ball-shape nickel hydroxide |
| CN105695740A (en) * | 2016-02-02 | 2016-06-22 | 中南大学 | Method capable of improving acid resistance during reverse extraction of extraction agent containing pyridine carboxylic ester and dinonylnaphthalene sulfonic acid and application of method |
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