CN107338357B - A kind of nitric acid Selectively leaching method of the high iron alloy powder of low nickel - Google Patents
A kind of nitric acid Selectively leaching method of the high iron alloy powder of low nickel Download PDFInfo
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- CN107338357B CN107338357B CN201710551799.7A CN201710551799A CN107338357B CN 107338357 B CN107338357 B CN 107338357B CN 201710551799 A CN201710551799 A CN 201710551799A CN 107338357 B CN107338357 B CN 107338357B
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/065—Nitric acids or salts thereof
-
- 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
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0438—Nitric acids or salts thereof
-
- 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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
Abstract
The invention discloses a kind of nitric acid Selectively leaching methods of low high iron alloy powder of nickel, the high iron alloy powder of low nickel is used one section of concentrated nitric acid leaching by this method first, magnetic separation is carried out at the end of full leaching, magnetic concentrate return continues to leach, leached mud and leachate are obtained after remaining slurry filtration, leachate enters neutralization iron removal step；It is added in the low high iron alloy powder progress of nickel and except iron, neutralizes except iron reaction end carries out magnetic separation, magnetic concentrate returns to one section of full leaching process, obtains neutralization scum after remaining slurry filtration and select immersion liquid in leachate；Filtered neutralization scum obtains the iron extract mine producation of iron content 60%-65% by washing, dry, calcining.Nickel, cobalt are leached and remove the completion of one step of iron by the present invention, realize the Selectively leaching of nickel cobalt and iron, nickel, cobalt enter solution, iron inhibition is opened a way in slag, so that nickel cobalt is efficiently separated with iron, nickel cobalt leaching rate > 98%, the nickeliferous < 0.5% of leached mud, iron < 10%, Co < 0.02%, scum iron > 50%, nickel < 0.1% are neutralized, immersion liquid iron content < 3g/L is selected.
Description
Technical field
The invention belongs to non-ferrous metal technical field of wet metallurgy, and in particular to a kind of nitric acid choosing of the low high iron alloy powder of nickel
Selecting property leaching method.
Background technique
Lateritic nickel ore use RKEF smelting process output thick ferronickel, be the high iron alloy powder of low nickel, composition 2%-8%Ni,
50%-68%Fe、0.08%-0.3%Co、0.1%-0.6%Mn、3%-10%Mg、0.3%-1.0%Al、1.0%-2.8%Cr、3%-10%Si。
The ferronickel powder mainly directly applies to the production of stainless steel, in the process nickel can only as low-end product application, and cobalt with
Nickel enters stainless steel, causes a large amount of losses of cobalt, does not embody the value of cobalt.Each metal is mainly with simple substance in the thick ferronickel powder
Or alloy form exists, using traditional sulfuric acid leaching, nickel cobalt leaching rate 50% hereinafter, and a large amount of iron in the form of ferrous iron into
Entering solution causes the next step difficult except iron；Potassium cloride ferronickel cobalt leaching rate can reach 95% or so, but remove iron cost
It is high.
Summary of the invention
The purpose of the present invention is to solve the technical problems existing in the prior art, provide a kind of nickel, cobalt leaching rate it is high,
The nitric acid selective leaching of environmentally protective, at low cost, the sour high iron alloy powder of low nickel that consumes less and can make nickel cobalt and iron to efficiently separate
Method out.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of nitric acid of high iron alloy powder of low nickel selects
Property leaching method, method includes the following steps:
A) one section of full leaching-magnetic separation: being added concentrated nitric acid in the high iron alloy powder of low nickel, and the additional amount of concentrated nitric acid is 100-
The high iron alloy powder of the low nickel of 300ml/100g, adding diluent control liquid-solid ratio is 5-10:1, and extraction temperature is 75 DEG C -105 DEG C,
Extraction time is 4h-8h, recycles NO in leaching processx, magnetic separation is carried out at the end of full leaching, magnetic concentrate return continues to leach,
Solid-liquor separation after remaining slurry filtration, obtained leached mud are silicon slag, outlet；Leachate enters neutralization iron removal step；
B) it neutralizing and removes iron-magnetic separation: the low high iron alloy powder of nickel being added in one section of leachate, control liquid-solid ratio is 5-10:1,
Extraction temperature is 75 DEG C -105 DEG C, endpoint pH 1-3, extraction time 4h-8h, neutralizes in iron removal and recycles NOx, neutralization removes
Iron reaction terminates to carry out magnetic separation, and magnetic concentrate returns to one section of full leaching process, solid-liquor separation after remaining slurry filtration, and obtained slag is
Neutralize scum, solution be select immersion liquid based on nickel cobalt, further to select immersion liquid removal of impurities recycling nickel cobalt；
C) neutralize scum processing: filtered neutralization scum obtains iron content 60%-65%'s by washing, dry, calcining
Iron extract mine producation, wash water returns to one section of full leaching process and uses as diluent in washing process.
Further, the granularity of the low high iron alloy powder of nickel is 20 mesh or less in the step a).
Further, calcination temperature is 200 DEG C -400 DEG C when calcining in the step c), time 1h-3h.
The present invention has the advantages that the nitric acid selectivity of the high iron alloy powder of low nickel of the invention compared with the prior art
The high iron alloy powder of low nickel is used one section of concentrated nitric acid leaching by leaching method first, carries out magnetic separation at the end of full leaching, magnetic concentrate returns
It returns and continues to leach, leached mud and leachate are obtained after remaining slurry filtration, leachate enters neutralization iron removal step；In leachate
The low high iron alloy powder of nickel is added neutralize except iron, neutralizes except iron reaction terminates to carry out magnetic separation, magnetic concentrate returns to one section of full leaching
Process obtains after remaining slurry filtration neutralizing scum and selects immersion liquid；Filtered neutralization scum is obtained by washing, dry, calcining
To the iron extract mine producation of iron content 60%-65%.The present invention leaches nickel, cobalt with except one step of iron is completed, and realizes the choosing of nickel cobalt and iron
Selecting property leaches, and nickel, cobalt enter solution, and iron inhibition is opened a way in slag, so that nickel cobalt is efficiently separated with iron, nickel cobalt leaching rate > 98%,
The nickeliferous < 0.5% of leached mud, iron < 10%, Co < 0.02% neutralize scum iron > 50%, nickel < 0.1%, select immersion liquid iron content < 3g/L.
In addition, the leaching solution of the low high iron alloy powder of nickel of the present invention remains as ferronickel powder except iron material, any impurity is not introduced,
And continue to leach ferronickel using the acid for removing iron generation is neutralized, the 50%-60% of nitric acid consumption when saving complete soak；Before being greatly saved
Phase leach production cost and it is subsequent remove iron cost.The present invention carries out magnetic separation, magnetic separation essence after removing iron to one section of leaching and neutralization simultaneously
Mine return continues to leach, and can separate the metalliferous material not reacted completely, returns and leaches process, ensure that valuable metal
Leaching rate, while ensure that nickel cobalt content is sufficiently low in leached mud and neutralization scum, has been effectively ensured the rate of recovery of nickel, cobalt, iron.
The present invention not only saves sour consumption, greatly reduces subsequent except iron cost, leaches and neutralize the nitrogen oxidation released in iron removal
Object also recoverable is that one is green, environmental protection, inexpensive New Metallurgical Technologies.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples.
Embodiment 1
The low high iron alloy powder composition of nickel is as shown in Table 1.
Table one: the low high iron alloy powder composition (%) of nickel
The nitric acid Selectively leaching method of the low high iron alloy powder of nickel the following steps are included:
A) one section of full leaching-magnetic separation: being added concentrated nitric acid in the high iron alloy powder of low nickel, and the additional amount of concentrated nitric acid is 100ml/
The high iron alloy powder of the low nickel of 100g, adding diluent control liquid-solid ratio is 5:1, and extraction temperature is 105 DEG C, extraction time 4h,
NO is recycled in leaching processx(mixture of NO and NO2) carries out magnetic separation at the end of full leaching, magnetic concentrate return continues to leach,
Solid-liquor separation after remaining slurry filtration, obtained leached mud are silicon slag, outlet；Leachate enters neutralization iron removal step.It soaks after measured
The ingredient slagged tap are as follows: 0.34 7.78 0.012 21.57 0.32 % of %, Mn of %, Si of %, Co of %, Fe of Ni.
B) it neutralizes and removes iron-magnetic separation: the low high iron alloy powder of nickel being added in one section of leachate, control liquid-solid ratio is 5:1, leaching
Temperature is 105 DEG C out, endpoint pH 1, and extraction time 4h is neutralized in iron removal and recycled NOx(mixture of NO and NO2),
It neutralizes except iron reaction terminates to carry out magnetic separation, magnetic concentrate returns to one section of full leaching process, and solid-liquor separation after remaining slurry filtration obtains
Slag be neutralize scum, solution be select immersion liquid based on nickel cobalt, after measured neutralize scum ingredient are as follows: Ni 0.06 %, Fe
51.18%, Cr 0.21%, Al 0.078%, select the ingredient of immersion liquid are as follows: 6.23 0.30 0.98 g/L of g/L, Fe of g/L, Co of Ni,
1.22 0.07 0.11 g/L of g/L, Mn of g/L, Al of Cr, further to selecting the immersion liquid removal of impurities recycling nickel cobalt can to produce electric nickel, electric cobalt
Or nickel salt, cobalt salt.
C) neutralize scum processing: filtered neutralization scum obtains the iron essence of iron content 60% by washing, dry, calcining
Mineral products, calcination temperature is 200 DEG C when calcining, time 3h.Wash water returns to one section of full leaching process as dilution in washing process
Agent uses.
Embodiment 2
The low high iron alloy powder composition of nickel is as shown in Table 2.
Table two: the low high iron alloy powder composition (%) of nickel
The nitric acid Selectively leaching method of the low high iron alloy powder of nickel the following steps are included:
A) one section of full leaching-magnetic separation: being added concentrated nitric acid in the high iron alloy powder of low nickel, and the additional amount of concentrated nitric acid is 200ml/
The high iron alloy powder of the low nickel of 100g, adding diluent control liquid-solid ratio is 10:1, and extraction temperature is 75 DEG C, extraction time 8h,
NO is recycled in leaching processx(mixture of NO and NO2) carries out magnetic separation at the end of full leaching, magnetic concentrate return continues to leach,
Solid-liquor separation after remaining slurry filtration, obtained leached mud are silicon slag, outlet；Leachate enters neutralization iron removal step.It soaks after measured
The ingredient slagged tap are as follows: 0.36 8.25 %, Co 0.016% of %, Fe of Ni, Si 20.69%, Mn 0.28%.
B) it neutralizes and removes iron-magnetic separation: the low high iron alloy powder of nickel being added in one section of leachate, control liquid-solid ratio is 10:1, leaching
Temperature is 75 DEG C out, endpoint pH 2, and extraction time 8h is neutralized in iron removal and recycled NOx(mixture of NO and NO2), in
With except iron reaction terminates to carry out magnetic separation, magnetic concentrate returns to one section of full leaching process, and solid-liquor separation after remaining slurry filtration obtains
Slag is to neutralize scum, and solution is to select immersion liquid based on nickel cobalt, neutralizes the ingredient of scum after measured are as follows: Ni 0.08 %, Fe
52.87 0.25 0.082 % of %, Al of %, Cr, select the ingredient of immersion liquid are as follows: 5.24 0.31 0.75 g/L of g/L, Fe of g/L, Co,
1.30 0.09 0.13 g/L of g/L, Mn of g/L, Al of Cr, further to selecting the immersion liquid removal of impurities recycling nickel cobalt can to produce electric nickel, electric cobalt
Or nickel salt, cobalt salt.
C) neutralize scum processing: filtered neutralization scum obtains the iron of iron content 62.8% by washing, dry, calcining
Concentrate product, calcination temperature is 300 DEG C when calcining, time 2h.Wash water returns to one section of full leaching process as dilute in washing process
Release agent use.
Embodiment 3
The low high iron alloy powder composition of nickel is as shown in Table 3.
Table three: the low high iron alloy powder composition (%) of nickel
The nitric acid Selectively leaching method of the low high iron alloy powder of nickel the following steps are included:
A) one section of full leaching-magnetic separation: being added concentrated nitric acid in the high iron alloy powder of low nickel, and the additional amount of concentrated nitric acid is 300ml/
The high iron alloy powder of the low nickel of 100g, adding diluent control liquid-solid ratio is 8:1, and extraction temperature is 90 DEG C, extraction time 6h, leaching
NO is recycled during outx(mixture of NO and NO2) carries out magnetic separation at the end of full leaching, magnetic concentrate return continues to leach, remaining
Solid-liquor separation after slurry filtration, obtained leached mud are silicon slag, outlet；Leachate enters neutralization iron removal step.It leaches after measured
The ingredient of slag are as follows: Ni0.38%, Fe7.52%, Co0.017%, Si21.56%, Mn0.31%.
B) it neutralizes and removes iron-magnetic separation: the low high iron alloy powder of nickel being added in one section of leachate, control liquid-solid ratio is 8:1, leaching
Temperature is 90 DEG C out, endpoint pH 2, and extraction time 6h is neutralized in iron removal and recycled NOx(mixture of NO and NO2), in
With except iron reaction terminates to carry out magnetic separation, magnetic concentrate returns to one section of full leaching process, and solid-liquor separation after remaining slurry filtration obtains
Slag is to neutralize scum, and solution is to select immersion liquid based on nickel cobalt, neutralizes the ingredient of scum after measured are as follows: Ni 0.10 %, Fe
55.23 0.22 0.075 % of %, Al of %, Cr, select the ingredient of immersion liquid are as follows: 3.26 0.25 g/L, Fe 1.50 of g/L, Co of Ni
1.25 0.12 0.15 g/L of g/L, Mn of g/L, Al of g/L, Cr, further to select immersion liquid removal of impurities recycling nickel cobalt can produce electric nickel,
Electric cobalt or nickel salt, cobalt salt.
C) neutralize scum processing: filtered neutralization scum obtains the iron essence of iron content 65% by washing, dry, calcining
Mineral products, calcination temperature is 400 DEG C when calcining, time 1h.Wash water returns to one section of full leaching process as dilution in washing process
Agent uses.
Claims (3)
1. a kind of nitric acid Selectively leaching method of the high iron alloy powder of low nickel, it is characterised in that method includes the following steps:
A) one section of full leaching-magnetic separation: being added concentrated nitric acid in the high iron alloy powder of low nickel, the low high iron alloy powder composition of nickel be 2%-8%Ni,
50%-68%Fe, 0.08%-0.3%Co, 0.1%-0.6%Mn, 3%-10%Mg, 0.3%-1.0%Al, 1.0%-2.8%Cr, 3%-10%Si,
The additional amount of concentrated nitric acid is the high iron alloy powder of the low nickel of 100-300ml/100g, and adding diluent control liquid-solid ratio is 5-10:1,
Extraction temperature is 75 DEG C -105 DEG C, extraction time 4h-8h, recycles NO in leaching processx, magnetic separation, magnetic are carried out at the end of full leaching
Concentrate selection return continues to leach, solid-liquor separation after remaining slurry filtration, and obtained leached mud is silicon slag, outlet；Leachate enters
Neutralize iron removal step；
B) it neutralizes and removes iron-magnetic separation: the low high iron alloy powder of nickel being added in one section of leachate, control liquid-solid ratio is 5-10:1, is leached
Temperature is 75 DEG C -105 DEG C, endpoint pH 1-3, extraction time 4h-8h, neutralizes in iron removal and recycles NOx, neutralize except iron is anti-
It should terminate to carry out magnetic separation, magnetic concentrate returns to one section of full leaching process, and solid-liquor separation after remaining slurry filtration, obtained slag is to neutralize
Scum, solution be select immersion liquid based on nickel cobalt, further to select immersion liquid removal of impurities recycling nickel cobalt；
C) neutralize scum processing: filtered neutralization scum obtains the iron essence of iron content 60%-65% by washing, dry, calcining
Mineral products, wash water returns to one section of full leaching process and uses as diluent in washing process.
2. a kind of nitric acid Selectively leaching method of low high iron alloy powder of nickel according to claim 1, it is characterised in that: institute
The granularity for stating the low high iron alloy powder of nickel in step a) is 20 mesh or less.
3. a kind of nitric acid Selectively leaching method of low high iron alloy powder of nickel according to claim 1, it is characterised in that: institute
Calcination temperature is 200 DEG C -400 DEG C when stating calcining in step c), time 1h-3h.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109628738A (en) * | 2019-02-26 | 2019-04-16 | 中钢集团南京新材料研究院有限公司 | A kind of method of the sulfuric acid Selectively leaching of ferronickel concentrate |
| CN111187922B (en) * | 2020-02-18 | 2022-05-06 | 云南锡业研究院有限公司 | Method for selectively leaching nickel from high-nickel copper matte under normal pressure |
| CN112481502A (en) * | 2020-11-20 | 2021-03-12 | 湖南金鑫新材料股份有限公司 | Method for leaching iron-based nickel-cobalt alloy by NO catalytic oxidation method |
| CN113637848B (en) * | 2021-07-20 | 2023-08-11 | 四川顺应动力电池材料有限公司 | Method for recycling valuable metals in nickel-cobalt alloy waste by acid leaching method |
| CN114645140A (en) * | 2022-04-02 | 2022-06-21 | 宁波容百新能源科技股份有限公司 | Method for preparing nickel intermediate product |
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