CN107746951A - Method for separating nickel in sulfate solution - Google Patents
Method for separating nickel in sulfate solution Download PDFInfo
- Publication number
- CN107746951A CN107746951A CN201710883215.6A CN201710883215A CN107746951A CN 107746951 A CN107746951 A CN 107746951A CN 201710883215 A CN201710883215 A CN 201710883215A CN 107746951 A CN107746951 A CN 107746951A
- Authority
- CN
- China
- Prior art keywords
- nickel
- sulfate
- separation method
- organic phase
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- C22B23/0476—Separation of nickel from cobalt
- C22B23/0492—Separation of nickel from cobalt in ammoniacal type solutions
-
- 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
Abstract
The invention discloses a method for separating nickel in a sulfate solution, which comprises the following steps: adjusting the pH value of the solution after cobalt extraction to 7-10 by using a complexing neutralizer, and extracting and separating nickel by using No. 260 solvent oil as a diluent and a nickel extracting agent as an organic phase to obtain a nickel-loaded organic phase and a sulfate raffinate; and washing and back-extracting the nickel-loaded organic phase to obtain a nickel-containing back-extraction solution and an organic phase. The method can effectively separate nickel in the high-concentration sulfate solution, and has the advantages of low energy consumption, low reagent consumption, short operation flow, low equipment requirement and easy realization of continuous operation.
Description
Technical field
The present invention relates to technical field of wet metallurgy, it is related to a kind of separation method of nickel in sulfate liquor.The sulfuric acid
Salting liquid refers in particular to the sulfate liquor that cobalt intermediate products obtain after sulfuric acid leaching, extraction cobalt, and the solution mainly contains sulfuric acid
It is one or two kinds of in ammonium and sodium sulphate.
Background technology
Cobalt is a kind of important strategy metal, is the key function element of the materials such as lithium battery, hard alloy.For a long time with
Come, China's cobalt resource critical shortage, cobalt yield mostlys come from nickel, the byproduct of metallurgy of copper technique.China annual about 90%
Cobalt resource Dependent Demand import, but as cobalt resource exporting country limitation raw ore exports, the cobalt raw ore of China's import is fewer and fewer,
Therefore it is to smelt cobalt intermediate products mostly, hydrometallurgy cobalt intermediate products are important one kind therein.
Ammonia soaks in the cobalt intermediate products that the techniques such as the heavy cobalt of cobalt, ammonium sulfide, the heavy cobalt of carbon ammonium obtain, inevitably containing few
The NH of amount4 +, and the NH in subsequent leaching process4 +It can be leached into solution.Domestic generally use " sulfuric acid leaching-
P204 removal of impurities-P507 (or Cyanex272) extractions cobalt " the PROCESS FOR TREATMENT cobalt intermediate products, and had using NaOH or ammoniacal liquor saponification
Machine phase.Due to containing NH in raw material4 +, therefore contain NH in cobalt leachate4 +, no matter this cobalt leachate use when extraction carries cobalt
Which kind of saponification mode, all contain NH in solution after extracting cobalt4 +, such as：Solution is containing sulphur after the extraction cobalt obtained using NaOH saponification
The high-concentration sulfuric acid sodium solution of sour ammonium, solution is high-concentration sulfuric acid ammonium salt solution after the extraction cobalt obtained using ammoniacal liquor saponification；This height
In concentration sulphuric acid ammonium salt solution or high-concentration sulfuric acid sodium solution containing ammonium sulfate, production process can remain 1~3g/L nickel, and
Current extraction can not effectively remove it during carrying cobalt, although can be removed using vulcanized sodium or carbon ammonium precipitation method
Nickel, but both processing methods are not easy to realize continuous operation, and need to increase the devices such as stirring, filtering, produced among gained nickel
The further dissolution process of product need, operating process are cumbersome.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of separation side of nickel in sulfate liquor
Method, the nickel in high-concentration sulfuric acid salting liquid can not only be efficiently separated, and energy consumption is low, reagent consumes less, operating process is short, sets
It is standby to require that low, easy realize operates continuously.
The purpose of the present invention is achieved through the following technical solutions：
The separation method of nickel, comprises the following steps in a kind of sulfate liquor：
Step A, the pH value of solution is adjusted to 7~10 after extracting cobalt using complexing nertralizer, then use with nickel extractant with
The organic extractant phase separation nickel that No. 260 oil miscible solvents are combined into, obtains nickel-loaded organic phase and sulfate raffinate；
Step B, the nickel-loaded organic phase is washed, be stripped, so as to obtain nickeliferous strip liquor and organic phase.
Preferably, the organic phase that the organic phase that step B is obtained returns in step A as extract and separate nickel is reused.
Preferably, the nickeliferous strip liquor is directly used in nickel electrowinning system or evaporative crystallization, so as to obtain nickel sulfate.
Preferably, the complexing nertralizer uses at least one of ammoniacal liquor or ammonia.
Preferably, in step, the volumetric concentration of the nickel extractant is 5~10%, and extraction phase is than O/A=0.5~1:
1, extraction series is 2~3 grades, and incorporation time is 2~5min.
Preferably, nickel extractant is using at least one of extractant LIX984, LIX984N, LIX973 or LIX84.
Preferably, in stepb, O/A=10~20 are compared in washing:1, washing series is 1~2 grade, and O/A=is compared in back extraction
1~5:1, back extraction series is 2~3 grades, and incorporation time is 5~10min.
Preferably, when the sulfate raffinate is ammonium sulfate and sodium sulphate mixed solution, to the ammonium sulfate and sulfuric acid
Sodium hydroxide is added in sodium mixed solution, and is heated, so as to reclaim NH3, then be evaporated, so as to reclaim sodium sulphate.
Preferably, when the sulfate raffinate is ammonium sulfate, directly ammonium sulfate is evaporated, so as to
Reclaim ammonium sulfate.
As seen from the above technical solution provided by the invention, in sulfate liquor provided by the present invention nickel separation
Method first adds the complexing nertralizer that can be not only complexed but also can adjust pH value into solution after extraction cobalt, thereby may be ensured that nickel not
Precipitation, then using nickel extractant extraction and recovery nickel, so as to realize that nickel is separated with ammonium sulfate (sodium sulphate) solution, then it is right
Nickel-loaded organic phase is washed, is stripped, and so as to obtain pure nickel salt solution and organic phase, and organic phase can return
It is continuing with.It can be seen that the present invention can not only efficiently separate the nickel in high-concentration sulfuric acid salting liquid, and energy consumption is low, reagent disappears
Consumption is less, operating process is short, equipment requirement is low, easy realize operates continuously.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 provides the schematic flow sheet of the separation method of nickel in sulfate liquor for the embodiment of the present invention.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The separation method of nickel in sulfate liquor provided by the present invention is described in detail below.The embodiment of the present invention
In the content that is not described in detail belong to prior art known to professional and technical personnel in the field.
The separation method of nickel, specifically may include steps of in a kind of sulfate liquor：
Step A, the pH value of solution is adjusted to 7~10 after extracting cobalt using complexing nertralizer, then use with nickel extractant with
The organic extractant phase separation nickel that No. 260 oil miscible solvents are combined into, obtains nickel-loaded organic phase and sulfate raffinate.
Specifically, solution is mainly high-concentration sulfuric acid ammonium salt solution or the high concentration sodium sulfate containing ammonium sulfate after the extraction cobalt
Solution, and sulfate concentration is 150~250g/L, and nickel ion concentration is 1~3g/L, therefore preferably with ammoniacal liquor or ammonia
At least one the pH value of solution after extraction cobalt is adjusted as complexing nertralizer；The addition of ammonia makes nickel with [Ni (NH3)1~4]
SO4Form is present, it ensure that nickel not hydrolytic precipitation.And the pH value for extracting solution after cobalt can make nickel extractant straight in 7~10
Connect and combined with the nickel in solution after extraction cobalt, the equation of extractive reaction is：2R-H+[Ni(NH3)1~4]SO4=R-Ni-R+H2SO4+(1
~4) NH3.In actual applications, the volumetric concentration of nickel extractant is preferably 5~10%, and extraction phase is preferably 0.5~1 than O/A:
1, extraction series is preferably 2~3 grades, and incorporation time is preferably 2~5min.The nickel extractant can use extractant
LIX984, LIX984N, LIX973 or LIX84 etc., can also use in the prior art other can extract the extraction of nickel, copper, zinc
Agent.When sulfate raffinate is ammonium sulfate, directly ammonium sulfate is evaporated, so as to reclaim ammonium sulfate.Work as sulphur
When hydrochlorate raffinate is ammonium sulfate and sodium sulphate mixed solution, hydroxide is added into the ammonium sulfate and sodium sulphate mixed solution
Sodium, and heated, so as to reclaim NH3, then be evaporated, so as to reclaim sodium sulphate.
Step B, the nickel-loaded organic phase is washed, be stripped, so as to obtain nickeliferous strip liquor and organic phase, this can
To realize the separation of nickel.
Specifically, washing is preferably 10~20 compared to O/A:1, washing series is preferably 1~2 grade, and back extraction is best compared to O/A
For 1~5:1, back extraction series is preferably 2~3 grades, and sulfuric acid concentration is preferably 150~250g/L, and incorporation time is preferably 5~
10min.In actual applications, nickeliferous strip liquor is used directly for nickel electrowinning system or evaporative crystallization, so as to obtain sulfuric acid
Nickel；And the organic phase that the organic phase that step B is obtained can return in step A as extract and separate nickel is reused.
Further, the separation method of nickel at least has following excellent in the sulfate liquor that the embodiment of the present invention is provided
Point：
(1) not only nickel separation is thorough for the separation method of nickel in the sulfate liquor that the embodiment of the present invention is provided, can be direct
High-purity solution containing nickel is obtained, and can further be recycled.
(2) separation method of nickel need to only be further added by extraction tank equipment in the sulfate liquor that the embodiment of the present invention is provided,
Other equipment need not be increased, it is low for equipment requirements, it is good with existing process connecting, it is easy to accomplish continuous production.
(3) its nickel extractant of the separation method of nickel can be circulated and made in the sulfate liquor that the embodiment of the present invention is provided
With reagent consumption is few, and operating cost is low.
(4) in the sulfate liquor that the embodiment of the present invention is provided the separation method of nickel without arranging outside waste liquid, production process without
Secondary environmental pollution, easily realize work continuously compared with the conventional method, the recovery separation nickel suitable for the solution after extraction cobalt.
(5) separation method of nickel is not only suitable for from solution after extraction cobalt in the sulfate liquor that the embodiment of the present invention is provided
Recovery separation nickel, while it is also suitable for recovery separation of Zinc, copper from solution after extraction cobalt.
As fully visible, the embodiment of the present invention can not only efficiently separate the nickel in high-concentration sulfuric acid salting liquid, and energy consumption
Low, reagent consumption is less, operating process is short, equipment requirement is low, easy realize operates continuously.
In order to more clearly from show technical scheme provided by the present invention and caused technique effect, below with tool
The separation method of nickel is described in detail in the sulfate liquor that body embodiment is provided the embodiment of the present invention.
Embodiment 1
As shown in figure 1, in a kind of sulfate liquor nickel separation method, for certain extraction cobalt after solution handle, should
Extract after cobalt ammonium sulfate concentrations in solution be 200g/L, nickel ion concentration 2.5g/L, the separation method may include steps of：
Step a1, the pH value of solution after extraction cobalt is adjusted to 9~10 using ammoniacal liquor, then using No. 260 solvent naphthas as dilute
Release agent, nickel as organic extractant phase is separated using nickel extractant LIX984, nickel extractant LIX984 volumetric concentration is 10%, extraction
Take and compare O/A=1:1, extraction series is 3 grades, incorporation time 3min, so as to obtain nickel-loaded organic phase and nickeliferous 0.9mg/L
Ammonium sulfate raffinate.
Step b1, the nickel-loaded organic phase is washed, be stripped, O/A=15 is compared in washing:1, washing series is 2
O/A=3 is compared in level, back extraction:1, back extraction series is 3 grades, sulfuric acid concentration 200g/L, and incorporation time is 5~10min, so as to
To nickeliferous strip liquor and organic phase, this can realize the separation of nickel, and nickel back extraction ratio is up to 97.6%.
Embodiment 2
As shown in figure 1, in a kind of sulfate liquor nickel separation method, for certain extraction cobalt after solution handle, should
Extract after cobalt ammonium sulfate concentrations in solution be 20g/L, sodium sulfate concentration 150g/L, nickel ion concentration 1.5g/L, the separation method
It may include steps of：
Step a2, the pH value of solution after extraction cobalt is adjusted to 9~10 using ammoniacal liquor, then using No. 260 solvent naphthas as dilute
Release agent, nickel as organic extractant phase is separated using nickel extractant LIX984, nickel extractant LIX984 volumetric concentration is 10%, extraction
Take and compare O/A=2:1, extraction series is 3 grades, incorporation time 3min, so as to obtain nickel-loaded organic phase and nickeliferous 0.7mg/L
Ammonium sulfate raffinate.
Step b2, the nickel-loaded organic phase is washed, be stripped, O/A=15 is compared in washing:1, washing series is 2
O/A=3 is compared in level, back extraction:1, back extraction series is 3 grades, sulfuric acid concentration 200g/L, and incorporation time is 5~10min, so as to
To nickeliferous strip liquor and organic phase, this can realize the separation of nickel, and nickel back extraction ratio is up to 97.1%.
As fully visible, the embodiment of the present invention can not only efficiently separate the nickel in high-concentration sulfuric acid salting liquid, and energy consumption
Low, reagent consumption is less, operating process is short, equipment requirement is low, easy realize operates continuously.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can readily occur in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (9)
1. the separation method of nickel in a kind of sulfate liquor, it is characterised in that comprise the following steps：
Step A, the pH value of solution after extraction cobalt is adjusted to 7~10 using complexing nertralizer, then used with nickel extractant and No. 260
The organic extractant phase separation nickel that oil miscible solvent is combined into, obtains nickel-loaded organic phase and sulfate raffinate；
Step B, the nickel-loaded organic phase is washed, be stripped, so as to obtain nickeliferous strip liquor and organic phase.
2. the separation method of nickel in sulfate liquor according to claim 1, it is characterised in that step B is obtained organic
The organic phase in step A as extract and separate nickel is mutually returned to reuse.
3. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that the nickeliferous back extraction
Liquid is directly used in nickel electrowinning system or evaporative crystallization, so as to obtain nickel sulfate.
4. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that the complexing neutralizes
Agent uses at least one of ammoniacal liquor or ammonia.
5. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that in step, institute
The volumetric concentration for stating nickel extractant is 5~10%, and extraction phase is than O/A=0.5~1:1, extraction series is 2~3 grades, incorporation time
For 2~5min.
6. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that the nickel extractant
Using at least one of extractant LIX984, LIX984N, LIX973 or LIX84.
7. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that in stepb, wash
Wash and compare O/A=10~20:1, washing series is 1~2 grade, and O/A=1~5 are compared in back extraction:1, back extraction series is 2~3 grades, is mixed
The conjunction time is 5~10min.
8. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that when the sulfate
When raffinate is ammonium sulfate and sodium sulphate mixed solution, sodium hydroxide is added into the ammonium sulfate and sodium sulphate mixed solution, and
Heated, so as to reclaim NH3, then be evaporated, so as to reclaim sodium sulphate.
9. the separation method of nickel in sulfate liquor according to claim 1 or 2, it is characterised in that when the sulfate
When raffinate is ammonium sulfate, directly ammonium sulfate is evaporated, so as to reclaim ammonium sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710883215.6A CN107746951A (en) | 2017-09-26 | 2017-09-26 | Method for separating nickel in sulfate solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710883215.6A CN107746951A (en) | 2017-09-26 | 2017-09-26 | Method for separating nickel in sulfate solution |
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| CN201710883215.6A Pending CN107746951A (en) | 2017-09-26 | 2017-09-26 | Method for separating nickel in sulfate solution |
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Cited By (2)
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| CN115216643A (en) * | 2022-08-18 | 2022-10-21 | 科立鑫(珠海)新能源有限公司 | Purification and recovery process of nickel in high-ammonium-salt wastewater |
| CN115231631A (en) * | 2022-08-10 | 2022-10-25 | 李晓清 | Continuous production process for preparing nickel sulfate by ammonia leaching based on ammonia circulation |
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|---|---|---|---|---|
| CN115231631A (en) * | 2022-08-10 | 2022-10-25 | 李晓清 | Continuous production process for preparing nickel sulfate by ammonia leaching based on ammonia circulation |
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Application publication date: 20180302 |