CN104310495A - Method for producing nickel chloride solution through leaching nickel hydroxide cobalt with hydrochloric acid - Google Patents
Method for producing nickel chloride solution through leaching nickel hydroxide cobalt with hydrochloric acid Download PDFInfo
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- CN104310495A CN104310495A CN201410551517.XA CN201410551517A CN104310495A CN 104310495 A CN104310495 A CN 104310495A CN 201410551517 A CN201410551517 A CN 201410551517A CN 104310495 A CN104310495 A CN 104310495A
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- leaching
- hydrochloric acid
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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
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Abstract
The invention provides a method for producing a nickel chloride solution through leaching nickel hydroxide cobalt with hydrochloric acid. The method comprises the following steps: step one, carrying out two-stage leaching, namely, firstly adding a nickel chloride solution into a reaction kettle, then adding hydrochloric acid and one-stage leaching residue for leaching, always controlling the concentration of [H<+>] of the solution in the reaction kettle to 0.1-0.8mol/L, then filtering the solution by a filter press so as to produce a second-stage leaching liquid and second-stage leaching residue; and step two, carrying out one-stage leaching, namely, adding the second-stage leaching liquid into a one-stage leaching kettle, adding nickel hydroxide cobalt into the one-stage leaching kettle for adjusting the pH value of the solution, after the pH value reaches 3.5-4.0, carrying out filter pressing, so as to produce one-stage leaching liquid and one-stage leaching residue, and eliminating impurities of the one-stage leaching liquid so as to obtain the product nickel chloride solution. The method can effectively prevent generation and overflowing of chlorine in leaching; furthermore, the second-stage leaching residue formed in the leaching process contains little nickel, so that the method can effectively improve the leaching rate of the nickel.
Description
Technical field
The invention belongs to technical field of non-ferrous metallurgy, relate to a kind of method that Leaching in Hydrochloric Acid nickel hydroxide cobalt produces nickel chloride solution.
Background technology
In nickelous chloride products production, first nickel chloride solution will be produced, produce the method for nickel chloride solution more, the method that the method, hydrochloric acid and the nickelous carbonate that have hydrochloric acid and electrolytic nickel to react react, nickel sulfate solution extract and entirely extract-the hydrochloric acid method, the method for high sulfonium nickel ore concentrate chlorine leaching, the method etc. of Leaching in Hydrochloric Acid nickel hydroxide cobalt that make the transition.In all multi-methods, owing to being subject to the restriction of resource, resources advantage will be shown gradually by the treatment process of the nickel hydroxide cobalt of process red soil nickel ore gained.But, because the nickel hydroxide cobalt of nickel laterite ammonia leaching output contains oxidizing species (being commonly considered as potassium permanganate), in Leaching in Hydrochloric Acid process, as solution [H
+] concentration higher time can react because of salt excessive acid and with oxidizing species and cause chlorine output, great impact is caused on the environment of production scene.
Summary of the invention
The object of the invention is to for prior art Problems existing, the nickel hydroxide cobalt of nickel laterite ammonia leaching output and technical hydrochloric acid is adopted to react, by controlling the reaction conditions of leaching process, under the condition of leaching yield ensureing nickel, avoid or reduce the spillage of chlorine, output is used for the nickel chloride solution of nickelous chloride products production.
For this reason, the present invention adopts following technical scheme:
Leaching in Hydrochloric Acid nickel hydroxide cobalt produces a method for nickel chloride solution, comprises following processing step:
The first step: two sections of leachings, two sections of leaching process first add nickel chloride solution in reactor, and then add hydrochloric acid and one section of leached mud leaches, hydrochloric acid is added and nickel hydroxide cobalt leaches during initial leaching, control the add-on of hydrochloric acid and one section of leached mud or hydrochloric acid and nickel hydroxide cobalt, make [the H of solution in reactor
+] concentration controls all the time between 0.1-0.8mol/L, two sections of temperature leached control at 50-80 DEG C; After leaching, solution is through Filter Press, output two sections of leach liquors and two sections of leached muds;
Second step: one section of leaching, two sections of leach liquors are added in a leaching still, in a leaching still, add nickel hydroxide cobalt again and carry out solution ph adjustment, this process temperature controls at 60-90 DEG C, be adjusted to after 3.5-4.0 until solution ph and carry out press filtration, output one section of leach liquor and one section of leached mud, namely one section of leach liquor obtains nickel chloride solution product after removal of impurities, and one section of leached mud returns two sections of leaching process and leaches.
Further, in step one, two sections of leaching process adopt 3 reactor serial operations, and 3 reactors are numbered 1 respectively
#, 2
#, 3
#, 1
#first add nickel chloride solution in reactor, then add hydrochloric acid and one section of leached mud leaches, initially add hydrochloric acid when leaching and nickel hydroxide cobalt leaches, the add-on controlling hydrochloric acid and one section of leached mud or hydrochloric acid and nickel hydroxide cobalt makes 1
#[the H of solution in reactor
+] concentration controls between 0.1-0.8mol/L; 1
#the full rear slurry of reactor is through upflow tube overflow to 2
#in reactor, simultaneously to 2
#add hydrochloric acid and nickel hydroxide cobalt in reactor, the add-on controlling hydrochloric acid and nickel hydroxide cobalt makes 2
#[H in reactor
+] concentration is between 0.1-0.8mol/L; 2
#the full rear slurry of reactor is through upflow tube overflow to 3
#further ageing reaction is carried out, 3 in reactor
#after reactor is full, open pressure filter by 3
#in reactor, slurries carry out press filtration, obtain two sections of leach liquors and two sections of leached muds.
Further, leaching process of the present invention hydrochloric acid used is technical hydrochloric acid, and its mass percent concentration is 30%-36%.
Further, in step one, the nickel chloride solution volume added in advance in reactor accounts for the 60-80% of reactor volume, and the mass concentration of nickel chloride solution is 120-170g/L.
The present invention adopts two sections of leachings, and one section of object leached two sections of leach liquors is carried out the adjustment of pH value, and two sections of leachings are leached one section of leached mud and raw material, output two sections of leach liquors, so, effectively can reduce the nickel content of final leached mud, improve the leaching yield of nickel.Wherein, two sections of leaching process adopt the mode of three reactor serial operations, react compared to single still, [the H of solution
+] concentration is more easy to control and production efficiency is higher, by control hydrochloric acid and add the amount of raw material (one section of leached mud and nickel hydroxide cobalt), make [the H of solution
+] concentration is easily controlled within the scope of this low concentration of 0.1-0.8mol/L, thus decreases the generation of chlorine in leaching process.Add nickel chloride solution in a kettle. in advance during two sections of leachings, after its object is to prevent hydrochloric acid from adding, make [the H in solution
+] excessive concentration, play the effect of dilute hydrochloric acid.Two sections of extraction temperatures control at 50 DEG C-80 DEG C, are conducive to the quantity reducing foam.During one section of leaching, the object of regulator solution pH value is to make solution reach the requirement of follow-up abstraction impurity removal, make to obtain good abstraction impurity removal effect, dedoping step can adopt the purifying method of a CN104073633A(nickel hydroxide cobalt salt acid leaching liquor) disclosed in scheme.
To sum up, beneficial effect of the present invention is: generation and the spilling that effectively can suppress chlorine in leaching process, and meanwhile, two sections of leached muds that leaching process is formed are nickeliferous low, effectively can improve the leaching yield of nickel; In addition, the inventive method production efficiency is high, and processing parameter condition is easy to control.
Embodiment
The composition of the nickel hydroxide cobalt raw material that following embodiment adopts is in table 1.
Embodiment 1
The nickel hydroxide cobalt composition that leaching process adopts is in table 1.
Table 1 embodiment 1 nickel hydroxide cobalt composition/%
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | H 2O |
| 42.27 | 0.72 | 0.01 | 0.07 | 0.14 | 0.86 | 0.08 | 0.77 | 0.022 | 51.00 |
The first step: two sections of leachings, adopt 3 reactor serial operations, 3 reactors are numbered 1 respectively
#, 2
#, 3
#, 1
#first add nickel chloride solution in reactor, then add hydrochloric acid and one section of leached mud leaches, initially add hydrochloric acid when leaching and nickel hydroxide cobalt leaches, leaching process monitoring solution [H
+] concentration is 0.47mol/L, 1
#the full rear slurry of reactor flow to 2 through upflow tube
#in reactor, simultaneously 2
#reactor adds hydrochloric acid and nickel hydroxide cobalt, records 2
#reactor [H
+] concentration is 0.68 mol/L; 2
#the full rear slurry of reactor is through upflow tube overflow to 3
#reactor, records 3
#solution [H in reactor
+] concentration is 0.42 mol/L, 3
#after reactor is full, open filter pressing pump by 3
#in reactor, slurries filter, and obtain two sections of leach liquors and two sections of leached muds, and two sections of leach liquors enter two immersion liquid Lower tanks, at two immersion liquid Lower tank sampling analysis, record [the H of two sections of leach liquors
+] concentration is 0.38mol/L, outer row after two sections of leached muds washings; Chlorine is not produced in two sections of leaching process.1 is recorded in leaching process
#, 2
#, 3
#the temperature of reactor is respectively 53 DEG C, 68 DEG C, 60 DEG C, and in operating process, in reactor, bubble amt is less and do not affect reinforced process, and the excessive phenomenon of foam does not occur.
Second step: one section of leaching.Two sections of leach liquors are added in a leaching still, add nickel hydroxide cobalt and carry out pH value adjustment, the pH regulating terminal to record solution is 3.5, temperature is 73 DEG C, pH value has regulated rear unlatching filter pressing pump to filter solution in a leaching still, and obtain one section of leach liquor and one section of leached mud, namely one section of leach liquor obtains nickel chloride solution product after removal of impurities, its composition is as shown in table 2, and filter residue adds two sections and leaches 1
#proceed in reactor to leach, in a dipped journey, do not produce chlorine.
Table 2 embodiment 1 one sections of leach liquor composition/g/L
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | SO 4 2 |
| 168.93 | 4.49 | 0.17 | 0.0099 | 1.11 | 4.31 | 0.18 | 5.29 | 0.27 | 46.19 |
Embodiment 2
The nickel hydroxide cobalt composition that leaching process adopts is in table 3.
Table 3 embodiment 2 nickel hydroxide cobalt composition/%
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | H 2O |
| 43.40 | 0.75 | 0.018 | 0.09 | 0.16 | 0.83 | 0.012 | 1.01 | 0.016 | 49.00 |
The first step: two sections of leachings.Concrete operations with embodiment 1,1
#reactor leaching process solution [H
+] concentration is 0.69mol/L, 2
#reactor [H
+] concentration is 0.72 mol/L; 3
#solution [H in reactor
+] concentration is 0.51 mol/L.At two immersion liquid Lower tank sampling analysis, [the H of two sections of leach liquors
+] concentration is 0.58mol/L, do not produce chlorine in two sections of leaching process.1 is recorded in leaching process
#, 2
#, 3
#the temperature of reactor is respectively 50 DEG C, 62 DEG C, 57 DEG C, and in operating process, in still, bubble amt does not affect reinforced process, and the excessive phenomenon of foam does not occur.
Second step: one section of leaching.Added in a leaching still by two sections of leach liquors, add nickel hydroxide cobalt and carry out pH value adjustment, the pH value regulating terminal solution is 4.0, and temperature is 60 DEG C, does not produce chlorine in a dipped journey, and one section of leach liquor composition is in table 4.
Table 4 embodiment 2 one sections of leach liquor composition/g/L
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | SO 4 2 |
| 174.60 | 3.27 | 0.22 | 0.0026 | 0.99 | 5.17 | 0.16 | 8.68 | 0.38 | 35.72 |
Embodiment 3
The nickel hydroxide cobalt composition that leaching process adopts is in table 5.
Table 5 embodiment 3 nickel hydroxide cobalt composition/%
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | H 2O |
| 44.06 | 0.82 | 0.013 | 0.11 | 0.13 | 0.74 | 0.013 | 0.99 | 0.019 | 52.00 |
The first step: two sections of leachings.Concrete operations with embodiment 1,1
#reactor leaching process solution [H
+] concentration is 0.35mol/L, 2
#reactor [H
+] concentration is 0.41 mol/L; 3
#solution [H in reactor
+] concentration is 0.29 mol/L.At two immersion liquid Lower tank sampling analysis, [the H of two sections of leach liquors
+] concentration is 0.15mol/L, do not produce chlorine in two sections of leaching process.1 is recorded in leaching process
#, 2
#, 3
#the temperature of reactor is respectively 56 DEG C, 71 DEG C, 66 DEG C, and in operating process, in still, bubble amt does not affect reinforced process, and the excessive phenomenon of foam does not occur.
Second step: one section of leaching.Added in a leaching still by two sections of leach liquors, add nickel hydroxide cobalt and carry out pH value adjustment, the pH value regulating terminal solution is 3.7, and temperature is 90 DEG C, does not produce chlorine in one section of leaching process, and one section of leach liquor composition is in table 6.
Table 6 embodiment 3 one sections of leach liquor composition/g/L
| Ni | Co | Cu | Fe | Zn | Mn | Ca | Mg | Na | SO 4 2 |
| 188.46 | 5.01 | 0.16 | 0.0021 | 1.15 | 5.56 | 0.17 | 7.31 | 0.33 | 40.53 |
Claims (4)
1. Leaching in Hydrochloric Acid nickel hydroxide cobalt produces a method for nickel chloride solution, it is characterized in that, comprises following processing step:
The first step: two sections of leachings, two sections of leaching process first add nickel chloride solution in reactor, and then add hydrochloric acid and one section of leached mud leaches, hydrochloric acid is added and nickel hydroxide cobalt leaches during initial leaching, control the add-on of hydrochloric acid and one section of leached mud or hydrochloric acid and nickel hydroxide cobalt, make [the H of solution in reactor
+] concentration controls all the time between 0.1-0.8mol/L, two sections of temperature leached control at 50-80 DEG C; After leaching, solution is through Filter Press, output two sections of leach liquors and two sections of leached muds;
Second step: one section of leaching, two sections of leach liquors are added in a leaching still, in a leaching still, add nickel hydroxide cobalt again and carry out solution ph adjustment, this process temperature controls at 60-90 DEG C, be adjusted to after 3.5-4.0 until solution ph and carry out press filtration, output one section of leach liquor and one section of leached mud, namely one section of leach liquor obtains nickel chloride solution product after removal of impurities, and one section of leached mud returns two sections of leaching process and leaches.
2. a kind of Leaching in Hydrochloric Acid nickel hydroxide cobalt according to claim 1 produces the method for nickel chloride solution, and it is characterized in that, two sections of leaching process adopt 3 reactor serial operations, and 3 reactors are numbered 1 respectively
#, 2
#, 3
#, 1
#first add nickel chloride solution in reactor, then add hydrochloric acid and one section of leached mud leaches, initially add hydrochloric acid when leaching and nickel hydroxide cobalt leaches, the add-on controlling hydrochloric acid and one section of leached mud or hydrochloric acid and nickel hydroxide cobalt makes 1
#[the H of solution in reactor
+] concentration controls between 0.1-0.8mol/L; 1
#the full rear slurry of reactor is through upflow tube overflow to 2
#in reactor, simultaneously to 2
#add hydrochloric acid and nickel hydroxide cobalt in reactor, the add-on controlling hydrochloric acid and nickel hydroxide cobalt makes 2
#[H in reactor
+] concentration is between 0.1-0.8mol/L; 2
#the full rear slurry of reactor is through upflow tube overflow to 3
#react further in reactor, 3
#after reactor is full, open pressure filter by 3
#in reactor, slurries carry out press filtration, obtain two sections of leach liquors and two sections of leached muds.
3. a kind of Leaching in Hydrochloric Acid nickel hydroxide cobalt according to claim 1 produces the method for nickel chloride solution, and it is characterized in that, leaching process hydrochloric acid used is technical hydrochloric acid, and its mass percent concentration is 30%-36%.
4. a kind of Leaching in Hydrochloric Acid nickel hydroxide cobalt according to claim 1 produces the method for nickel chloride solution, it is characterized in that, in step one, the nickel chloride solution volume added in advance in reactor accounts for the 60-80% of reactor volume, and the mass concentration of nickel chloride solution is 120-170g/L.
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| CN201410551517.XA CN104310495B (en) | 2014-10-17 | 2014-10-17 | A kind of Leaching in Hydrochloric Acid nickel hydroxide cobalt is produced the method for nickel chloride solution |
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| CN201410551517.XA CN104310495B (en) | 2014-10-17 | 2014-10-17 | A kind of Leaching in Hydrochloric Acid nickel hydroxide cobalt is produced the method for nickel chloride solution |
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| CN104310495B CN104310495B (en) | 2016-05-04 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365212A (en) * | 2016-08-29 | 2017-02-01 | 金川集团股份有限公司 | Method for inhibiting chlorine from being generated when coarse nickel hydroxide is leached with concentrated hydrochloric acid |
| CN107419295A (en) * | 2017-03-24 | 2017-12-01 | 金川集团股份有限公司 | The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate |
| CN110104694A (en) * | 2019-04-23 | 2019-08-09 | 金川集团股份有限公司 | A method of nickel chloride solution is prepared using nickel oxide |
| CN110468289A (en) * | 2019-09-12 | 2019-11-19 | 金川集团股份有限公司 | A kind of method that three sections of counter current acid leachings recycle after spherical shape nickel protoxide mechanical activation |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| CN112095005A (en) * | 2020-08-12 | 2020-12-18 | 矿冶科技集团有限公司 | Method for leaching nickel and cobalt from rough nickel and cobalt hydroxide in two stages |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352119A (en) * | 2013-06-25 | 2013-10-16 | 工信华鑫科技有限公司 | Novel leaching-extracting process for wet slag of mixed nickel cobalt hydroxide |
| CN104073633A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Purification method of cobalt nickel hydroxide hydrochloric acid leaching solution |
-
2014
- 2014-10-17 CN CN201410551517.XA patent/CN104310495B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352119A (en) * | 2013-06-25 | 2013-10-16 | 工信华鑫科技有限公司 | Novel leaching-extracting process for wet slag of mixed nickel cobalt hydroxide |
| CN104073633A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Purification method of cobalt nickel hydroxide hydrochloric acid leaching solution |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365212A (en) * | 2016-08-29 | 2017-02-01 | 金川集团股份有限公司 | Method for inhibiting chlorine from being generated when coarse nickel hydroxide is leached with concentrated hydrochloric acid |
| CN107419295A (en) * | 2017-03-24 | 2017-12-01 | 金川集团股份有限公司 | The Electrolysis Extraction Method of manganese ion in a kind of nickel hydroxide hydrochloric acid leachate |
| CN110104694A (en) * | 2019-04-23 | 2019-08-09 | 金川集团股份有限公司 | A method of nickel chloride solution is prepared using nickel oxide |
| CN110468289A (en) * | 2019-09-12 | 2019-11-19 | 金川集团股份有限公司 | A kind of method that three sections of counter current acid leachings recycle after spherical shape nickel protoxide mechanical activation |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| CN112095005A (en) * | 2020-08-12 | 2020-12-18 | 矿冶科技集团有限公司 | Method for leaching nickel and cobalt from rough nickel and cobalt hydroxide in two stages |
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|---|---|
| CN104310495B (en) | 2016-05-04 |
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Effective date of registration: 20200715 Address after: No.7101 Jinchang Road, Lanzhou, Gansu Province Patentee after: Jinchuan Group Nickel Salt Co.,Ltd. Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. |