CN109762992A - A kind of preparation process separating nickel cobalt from high cobalt nickel material containing zinc - Google Patents
A kind of preparation process separating nickel cobalt from high cobalt nickel material containing zinc Download PDFInfo
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- CN109762992A CN109762992A CN201910104723.9A CN201910104723A CN109762992A CN 109762992 A CN109762992 A CN 109762992A CN 201910104723 A CN201910104723 A CN 201910104723A CN 109762992 A CN109762992 A CN 109762992A
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- nickel
- sulfuric acid
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Abstract
The present invention relates to metal smelt slag recovery technology fields, and in particular to a kind of preparation process that nickel cobalt is separated from high cobalt nickel material containing zinc.For the present invention the following steps are included: high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1 by (1), the ratio of the mole of cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc is 1.2:1~1.5:1；(2) Chloride Solution is added in Xiang Shangshu suspension A1, makes 0.5g/L≤Cl‑≤ 2g/L obtains mixed liquor A 2；(3) mixed liquor A 2 is added to the anode region of electrolysis installation, while injects the mixed solution of sulfuric acid solution or sulfuric acid and zinc sulfate to cathodic region；(4) temperature of the electrolytic cell of electrolysis installation is controlled at 55~85 DEG C, 60~240min of duration is reacted, to which nickel cobalt sediment after reaction, is obtained by filtration.The present invention with anode replace oxidant oxidation, have many advantages, such as it is high-efficient, at low cost, do not introduce new impurity.
Description
Technical field
The present invention relates to metal smelt slag recovery technology fields, specially a kind of to separate nickel cobalt from high cobalt nickel material containing zinc
Preparation process.
Background technique
For traditional handicraft when handling the nickel cobalt material containing zinc, there are mainly three types of the technical methods of use: 1), extracting
Method；2), displacement method；3) oxidizing method.
The defect of currently used method is as follows: 1) extraction uses a large amount of organic extractant phase agent, and at high cost, step is more,
Aqueous solution will also be handled after being polluted by organic phase by activated carbon adsorption.2) displacement method generally uses excessive zinc powder pair
Nickel cobalt ion is replaced, and in industrial practice, zinc powder often will excessively arrive 150-250 times of stoichiometric ratio, can be only achieved foot
It is odd high that enough high clean-up effects, so operation lead to cost, and obtained cobalt nickel materials (being industrially referred to as purification slag) are still
It is nickel cobalt zinc mixture, utility value is low.3) oxidizing method is to be aoxidized using strong oxidizer to this material, often
Oxidant generally has: persulfate, chlorine or chlorate, ozone etc., and often price is higher for these strong oxidizers, or itself
It is unstable, and other foreign ions can be introduced into solution, industrial application is also seldom at present, still rests on experiment rank
Section.4) the cathodic reduction separating technology in currently studying, since nickel cobalt belongs to the low overvoltage metal of hydrogen, when it is in cathode
When surface is precipitated, hydrogen can be reduced in the overpotential on its surface, hydrogen is caused to be precipitated, current efficiency is rapidly reduced to level off to 0.
Summary of the invention
For above-mentioned problem, the purpose of the present invention is to provide a kind of from high cobalt nickel material containing zinc separates the system of nickel cobalt
Standby technique, it is more with impurity in the cobalt nickel that solves the problems, such as current traditional handicraft higher cost, isolate.
To solve the above problems, technical scheme is as follows:
A kind of preparation process separating nickel cobalt from high cobalt nickel material containing zinc, comprising the following steps:
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, the cobalt nickel zinc in high cobalt nickel material containing zinc is total
The ratio of mole and the mole of dilute sulfuric acid is 1.2:1~1.5:1.
(2) Chloride Solution is added in Xiang Shangshu suspension A1, makes 0.5g/L≤Cl-≤ 2g/L obtains mixed liquor A 2.
(3) mixed liquor A 2 is added to the anode region of electrolysis installation, at the same to cathodic region inject sulfuric acid solution or sulfuric acid with
The mixed solution of zinc sulfate.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 55~85 DEG C, 60~240min of duration is reacted, to the end of reacting
Afterwards, nickel cobalt sediment is obtained by filtration.
The principle that cobalt nickel is separated with zinc in the present invention is as follows:
Due to Zn2+It does not appraise at the current rate, not oxidized, sulfate is soluble easily in water, and Co (OH)3With Ni (OH)3In
Property under conditions of be the precipitating more stable and hard to tolerate in water, therefore can by be separated by solid-liquid separation be isolated out.
Pass through after mixing high cobalt nickel material containing zinc by certain stoichiometric ratio with dilute sulfuric acid according to above-mentioned reaction principle
The electroxidation of anode acts on, can be by the Co of dissolution2+、Ni2+It is oxidized to trivalent, and is hydrolyzed into precipitating and is removed.
Further, be hydrochloric acid in Chloride Solution, sodium chloride solution, calcium chloride solution, Klorvess Liquid, zinc chloride it is molten
Liquid.
Further, the anode of electrolysis installation is moving electrode, and the revolving speed of moving electrode is 35~200r/min, the table of moving electrode
80~280A/m of surface current density2。
Further, the moving electrode is iridium tantalum coated electrode, lead dioxide electrode or the lead electrode of titanium substrate.
Further, the negative electricity machine of the electrolysis installation is fixed electrode, and fixed electrode is reticular structure, fixed electrode
Material is nickel-clad copper, copper, any one in titanium, and fixed electrode is the contact area that reticular structure can increase cathode and solution,
To reduce the overpotential of hydrogen, power consumption is reduced.
Further, the amberplex is that cation exchange is touched, filter cloth, asbestos diaphragm or anion exchange are touched.
Compared with prior art, beneficial effects of the present invention are as follows:
(1) present invention is by the way of anodic oxidation to the Co dissolved in mixed solution2+、Ni2+It is oxidized to trivalent, and is being connect
Co (OH) is hydrolyzed under conditions of weakly acidic pH3With Ni (OH)3Precipitating, to be separated with the zinc hydroxide in solution, to realize
Separation between cobalt nickel ion and zinc ion, compared with the existing technology in using organic extractant phase or zinc dust precipitation processing side
Cost is relatively low for formula, separating effect is more preferable, will not also introduce corresponding foreign ion, be applicable to industrial mass production.
(2) contact frequency that anode and solution and suspended matter can be effectively increased in the present invention using anode as moving electrode, from
And the oxidation efficiency of anode is improved, fixed electrode is that reticular structure can increase the contact area of cathode and solution, to reduce hydrogen
The overpotential of gas reduces power consumption.
Detailed description of the invention:
The present invention is described in further detail with reference to the accompanying drawings and examples.
Fig. 1 is the structural schematic diagram of electrolysis installation provided by the invention.
Appended drawing reference: 1- anode, 2- cathode, 3- amberplex, 10- electro-catalysis area, the cathodic region 20-.
Specific embodiment
The present invention is further explained combined with specific embodiments below.It will be appreciated that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.It should also be understood that be, after reading the content taught by the present invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within range defined herein.
Embodiment 1
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 44%, Co content 1.1%, nickel content 0.4%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.2:1.
(2) dilute hydrochloric acid solution is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 0.5g/L, obtain mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the iridium tantalum coating electricity of titanium substrate
Pole, the revolving speed of moving electrode are 50r/min, the surface current density 100A/m of moving electrode2；The material of fixed electrode, that is, cathode 2 is
Nickel-clad copper；The amberplex 3 of electrolysis installation is cation-exchange membrane.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 60 DEG C, reacts duration 220min, to after reaction, filter
Obtain nickel cobalt sediment.
For above-mentioned electrolysis installation it should be noted that the moving electrode of electrolysis installation is agitating shaft and paddle, wherein stirring
The motor for mixing axis and outside is attached, so that moving electrode be driven to be rotated, furthermore paddle can for screw, helical-ribbon type,
Turbine type, paddle push type etc., so that electrolyte has higher oxidation efficiency under the action of the stirring of moving electrode, electrolysis.
Embodiment 2
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 44%, Co content 1.1%, nickel content 0.4%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.3:1.
(2) sodium chloride solution is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 1g/L, obtain mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the iridium tantalum coating electricity of titanium substrate
Pole, the revolving speed of moving electrode are 150r/min, the surface current density 120A/m of moving electrode2；The material of fixed electrode, that is, negative electrode
For nickel-clad copper；The amberplex 3 of electrolysis installation is cation-exchange membrane.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 60 DEG C, reacts duration 180min, to after reaction, filter
Obtain nickel cobalt sediment.
Embodiment 3
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 44%, Co content 1.1%, nickel content 0.4%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.4:1.
(2) Klorvess Liquid is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 1.5g/L, obtain mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the iridium tantalum coating electricity of titanium substrate
Pole, the revolving speed of moving electrode are 150r/min, the surface current density 210A/m of moving electrode2；The material of fixed electrode, that is, cathode 2 is
Nickel-clad copper；The amberplex 3 of electrolysis installation is cation-exchange membrane.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 80 DEG C, reacts duration 120min, to after reaction, filter
Obtain nickel cobalt sediment.
Embodiment 4
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 52%, Co content 0.9%, nickel content 0.1%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.5:1.
(2) Klorvess Liquid is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 1.7g/L, obtain mixed liquor A 2.
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the brown lead oxide electricity of titanium substrate
Pole, the revolving speed of moving electrode are 150r/min, the surface current density 200A/m of moving electrode2；The material of fixed electrode, that is, cathode 2 is
Copper；The amberplex 3 of electrolysis installation is filter cloth.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 80 DEG C, duration 60min is reacted, to after reaction, filter
To nickel cobalt sediment.
Embodiment 5
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 52%, Co content 0.9%, nickel content 1.1%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.2:1.
(2) calcium chloride solution is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 2g/L, obtain mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the iridium tantalum coating electricity of titanium substrate
Pole, the revolving speed of moving electrode are 150r/min, the surface current density 200A/m of moving electrode2；The material of fixed electrode, that is, negative electrode
For nickel-clad copper；The amberplex 3 of electrolysis installation is asbestos diaphragm.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 80 DEG C, reacts duration 120min, to after reaction, filter
Obtain nickel cobalt sediment.
Embodiment 6
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, wherein zinc contains in the high cobalt nickel material containing zinc
Measure 38%, Co content 2.7%, nickel content 0.6%, cobalt nickel zinc integral molar quantity and dilute sulfuric acid in high cobalt nickel material containing zinc rub
The ratio of your amount is 1.4:1.
(2) Klorvess Liquid is added in Xiang Shangshu suspension A1, makes chlorine ion concentration 1.5g/L, obtain mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation 10, while injects sulfuric acid solution or sulphur to cathodic region 20
The mixed solution of acid and zinc sulfate.The anode 1 of electrolysis installation is moving electrode, and the material of moving electrode is the lead electrode of titanium substrate, is moved
The revolving speed of electrode is 150r/min, the surface current density 260A/m of moving electrode2；The material of fixed electrode, that is, cathode 2 is titanium；Electricity
The amberplex 3 for solving equipment is Ag ion exchange film.
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 85 DEG C, reacts duration 240min, to after reaction, filter
Obtain nickel cobalt sediment.
It is now that interpretation is as follows in order to which the electrolysis effectiveness to the various embodiments described above is analyzed:
Operating parameter in each embodiment of table 1
To above-mentioned sample, 200 grams are respectively taken to be tested respectively according to the operating parameter in embodiment, as a result shown in table 2 such as
Under:
The processing result of each embodiment of table 2
Composition detection situation of the filter residue of 3 section Example of table after pickling
| Embodiment | Zn | Co | Ni |
| 2 | 1.2 | 19 | 4.8 |
| 5 | 1.1 | 20.45 | 2.2 |
| 6 | 0.75 | 28 | 7.3 |
Comparative example
Ammonium persulfate oxidation is carried out to high cobalt nickel material containing zinc used in embodiment 1, embodiment 4 and embodiment 6 respectively
Method is handled, and corresponding comparative example 1, comparative example 2 and comparative example 3 are obtained.Wherein ammonium persulfate dosage and high cobalt nickel contain zinc
The stoichiometric ratio of cobalt nickel zinc in material is 4.5:1, and processing result is shown in Table 4.
The experimental result of each comparative example of table 4
Composition detection situation of the filter residue of each comparative example of table 5 after pickling
| Comparative example | Zn | Co | Ni |
| 1 | 3.6 | 12.4 | 4.1 |
| 2 | 3.7 | 11.85 | 1.4 |
| 3 | 2.1 | 15.6 | 3.6 |
The above, only presently preferred embodiments of the present invention, are not intended to limit the invention, patent protection model of the invention
It encloses and is subject to claims, it is all to change with equivalent structure made by description of the invention, similarly should all include
Within the scope of the present invention.
Claims (6)
1. a kind of preparation process for separating nickel cobalt from high cobalt nickel material containing zinc, which comprises the following steps:
(1) high cobalt nickel material containing zinc and dilute sulfuric acid are mixed into suspension A1, the cobalt nickel zinc in the high cobalt nickel material containing zinc is total
The ratio of mole and the mole of dilute sulfuric acid is 1.2:1~1.5:1；
(2) Chloride Solution is added in Xiang Shangshu suspension A1, makes 0.5g/L≤Cl-≤ 2g/L obtains mixed liquor A 2；
(3) mixed liquor A 2 is added to the anode region of electrolysis installation, while injects sulfuric acid solution or sulfuric acid and sulfuric acid to cathodic region
The mixed solution of zinc；
(4) temperature of the electrolytic cell of electrolysis installation is controlled at 55~85 DEG C, reacts 60~240min of duration, to after reaction,
Nickel cobalt sediment is obtained by filtration.
2. preparation process according to claim 1, which is characterized in that be hydrochloric acid, sodium chloride solution, chlorine in the Chloride Solution
Change calcium solution, Klorvess Liquid, liquor zinci chloridi.
3. preparation process according to claim 1, which is characterized in that the anode of the electrolysis installation is moving electrode, the dynamic electricity
The revolving speed of pole is 35~200r/min, 80~280A/m of surface current density of the moving electrode2。
4. preparation process according to claim 3, which is characterized in that the moving electrode is the iridium tantalum coated electrode of titanium substrate, two
Lead dioxide electrode or lead electrode.
5. preparation process according to claim 1, which is characterized in that the negative electricity machine of the electrolysis installation is fixed electrode, described
Fixed electrode is reticular structure, and the material of the fixed electrode is nickel-clad copper, copper, any one in titanium.
6. preparation process according to claim 1, which is characterized in that the amberplex be cation exchange touch, filter cloth, stone
Cotton diaphragm or anion exchange are touched.
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| CN201910104723.9A CN109762992A (en) | 2019-02-01 | 2019-02-01 | A kind of preparation process separating nickel cobalt from high cobalt nickel material containing zinc |
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| CN201910104723.9A CN109762992A (en) | 2019-02-01 | 2019-02-01 | A kind of preparation process separating nickel cobalt from high cobalt nickel material containing zinc |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2530957Y (en) * | 2002-03-29 | 2003-01-15 | 上海欣晨新技术有限公司 | Electrolytic bath with multi-layer vibration screen electrode |
| CN103014346A (en) * | 2012-12-03 | 2013-04-03 | 河池市津泰资源再生有限公司 | Process method for separating zinc, iron and cobalt and nickel ore concentrates from cobalt and nickel slag |
-
2019
- 2019-02-01 CN CN201910104723.9A patent/CN109762992A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2530957Y (en) * | 2002-03-29 | 2003-01-15 | 上海欣晨新技术有限公司 | Electrolytic bath with multi-layer vibration screen electrode |
| CN103014346A (en) * | 2012-12-03 | 2013-04-03 | 河池市津泰资源再生有限公司 | Process method for separating zinc, iron and cobalt and nickel ore concentrates from cobalt and nickel slag |
Non-Patent Citations (1)
| Title |
|---|
| 代海宁 主编: "《电化学基本原理及应用》", 31 March 2014, 冶金工业出版社 * |
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Application publication date: 20190517 |