CN106048638B - A kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity - Google Patents
A kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity Download PDFInfo
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- CN106048638B CN106048638B CN201610462149.0A CN201610462149A CN106048638B CN 106048638 B CN106048638 B CN 106048638B CN 201610462149 A CN201610462149 A CN 201610462149A CN 106048638 B CN106048638 B CN 106048638B
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Abstract
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：Metallic nickel is placed in Ni―Ti anode frame as anode, electrolyte is used as using the mixed acid solution of sulfuric acid and hydrochloric acid, cathode is used as using titanium plate, the surface area of the cathode titanium plates is less than the surface area of the metallic nickel of the anode, then leading to direct current electrolysis, pH value completes liquid making process, the metallic nickel that periodic reverse current dissolving cathode separates out to terminal.The method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity of the present invention has the characteristics that current efficiency is high, energy consumption cost is low, technique is environmentally protective and easy to operate.
Description
Technical field
The present invention relates to technical field of wet metallurgy, is specially a kind of molten metallic nickel liquid making of small cathode deposition period reverse current electricity
Method.
Background technology
Nickel sulfate is widely used in chemical industry, light industry, machinery, oil, electronics and other industrial circles.At present, both at home and abroad
Nickel sulfate mainly has two class purposes, and one kind is used to electroplate reagent, another kind of to be used for battery material.In recent years, with new material, new
The continuous renewal of the fast development of energy industry, battery material and its manufacturing technology, battery industry have obtained tremendous development.Especially
The driving being substantially improved by the new-energy automobile production amount of disappearing, have stimulated the demand to power battery and associated materials, battery in 2015
2.2 ten thousand tons of the nickel in field, amplification reaches 16%, it is contemplated that 2016-2020 average annual growth rates are expected to reach 15%.In contrast,
Being slumped by nickel valency wilfulness influences, and the higher electrolytic nickel manufacturing enterprise of home costs stops production successively, some manage electrolytic nickel mainly originally
Enterprise also begins to the underproduction and transfers to produce nickel sulfate.
The production technology of nickel sulfate is larger by the different difference of nickel bearing raw material, mainly there is metallic nickel method, smelting by-product product
Recycling, nickel compound transition are prepared, produced by being recycled in nickeliferous waste material.Wherein metallic nickel method be divided into again direct acid-soluble method and
Electrolysis, direct acid-soluble method carry out oxidation dissolution metallic nickel with the mixed acid containing nitric acid and sulfuric acid, are carried out after liquid making simple net
Condensing crystallizing can obtain refined sulfuric acid nickel product after change.The technique has the advantages that production capacity is big, but there is set at the same time
The shortcomings of standby complicated and seriously corroded, utilization rate of raw materials be not high, liquid making process environment is severe and produces toxic gas.With
The continuous improvement of people's environmental consciousness and national requirements for environmental protection, in recent years people develop successively with electrolysis original to substitute
Mixed acid liquid making technique.Compared with traditional method, electrolysis is a kind of nickel sulfate production work pollution-free, product purity is high
Skill, the process equipment is simple, and the introducing probability of impurity is low, technological process is short, and nickel utilization rate is high.But there is also electrolyte terminal acid
The problems such as degree is high, and current efficiency is low, and power consumption is high, and technical process reduces cathode precipitating metal nickel, and electricity with acidity
The insoluble problem of solution.
The content of the invention
The object of the present invention is to provide a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, there is electric current
It is efficient, energy consumption cost is low, technique is environmentally protective and it is easy to operate the characteristics of.
The present invention can be achieved through the following technical solutions：
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metallic nickel is placed in Ni―Ti anode frame as anode, using the mixed acid solution of sulfuric acid and hydrochloric acid as electrolyte, the moon is used as using titanium plate
Pole, the surface area of the cathode titanium plates are less than the surface area of the metallic nickel of the anode, then lead to direct current electrolysis pH to terminal
Value completes liquid making process, the metallic nickel that periodic reverse current dissolving cathode separates out.
Further, the metallic nickel as anode is metal nickel plate, metal nickel block or metallic nickel pillow.
Further, it is characterised in that：The total acid concentration of mixed acid solution is 2.5~4.0 mol/L.
Further, the surface area of the cathode titanium plates is the 5~20% of the anode metal nickel surface area.
Further, the process conditions of the direct current electrolysis are：Anodic current density is 200~250A/m2, electrolyte
Temperature is room temperature, and for heteropole away from for 15~25mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 10~40cm/h.
Further, the endpoint pH is 3.0~4.0.
Further, the cycle of the periodic reverse current is that the metallic nickel separated out with cathode the liquid making starting stage is completely molten
Solution.
Further, the grade of the metallic nickel is at least up to Ni9990 trades mark requirement in GB/T6516-2010.
The present invention has following beneficial effect：Use reduction cathode area and electrochemistry is molten in a manner of periodic reverse current
The method for solving metallic nickel, by reducing cathode area, increases cathode-current density, improves electrolysis mode, is improving electrolyte pH
Solve the problems, such as that cathode analyses nickel while value, effectively increase current efficiency, reduce power consumption, current efficiency exists
More than 90%, power consumption is 1200~1500Kw h/t-Ni, and gained electrolyte need not adjust acid purification to can be directly used for being co-precipitated
Battery material, effectively reduces the production cost of battery material.
Embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, product of the present invention is made below into
One step is described in detail.
Embodiment 1
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metal nickel plate metallic nickel pillow is placed in Ni―Ti anode frame as anode, using the mixed acid solution of sulfuric acid and hydrochloric acid as electrolyte, control
It is 4.0 mol/L to make total acid concentration, and using titanium plate as cathode, the surface area of the cathode titanium plates is the anode metal nickel
The 12% of plate surface product, then leading to direct current electrolysis, pH value 3.0 completes liquid making process, periodic reverse current dissolving cathode to terminal
The metallic nickel of precipitation.
In the present embodiment, the process conditions of the direct current electrolysis are：Anodic current density is 250A/m2, electrolyte
Temperature is room temperature, and for heteropole away from for 20mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 10cm/h.The cycle
The cycle of reverse current is completely dissolved for the liquid making starting stage with the metallic nickel that cathode separates out.The grade of the metallic nickel is at least up to
The Ni9990 trades mark requirement into GB/T6516-2010.
Embodiment 2
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metal nickel block is placed in Ni―Ti anode frame as anode, using the mixed acid solution of sulfuric acid and hydrochloric acid as electrolyte, control total acid is dense
Spend for 3.2 mol/L, using titanium plate as cathode, the surface area of the cathode titanium plates is the anode metal nickel block surface area
5%, then lead to direct current electrolysis to terminal pH value 4.0 complete liquid making process, periodic reverse current dissolving cathode separate out metal
Nickel.
In the present embodiment, the process conditions of the direct current electrolysis are：Anodic current density is 225/m2, it is electrolysed liquid temperature
Spend for room temperature, for heteropole away from for 15mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 40cm/h.The cycle is anti-
It is completely dissolved to the cycle of electric current for the liquid making starting stage with the metallic nickel that cathode separates out.The grade of the metallic nickel is at least up to
Ni9990 trades mark requirement in GB/T6516-2010.
Embodiment 3
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metallic nickel pillow is placed in Ni―Ti anode frame as anode, using the mixed acid solution of sulfuric acid and hydrochloric acid as electrolyte, control total acid is dense
Spend for 2.5 mol/L, using titanium plate as cathode, the surface area of the cathode titanium plates rests the head on surface area for the anode metal nickel
20%, then lead to direct current electrolysis to terminal pH value 3.5 complete liquid making process, periodic reverse current dissolving cathode separate out gold
Belong to nickel.
In the present embodiment, the process conditions of the direct current electrolysis are：Anodic current density is 200A/m2, electrolyte
Temperature is room temperature, and for heteropole away from for 25mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 25cm/h.The cycle
The cycle of reverse current is completely dissolved for the liquid making starting stage with the metallic nickel that cathode separates out.The grade of the metallic nickel is at least up to
The Ni9990 trades mark requirement into GB/T6516-2010.
Embodiment 4
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metal nickel plate, metal nickel block or metallic nickel are rested the head on and are placed in Ni―Ti anode frame as anode as metallic nickel, with sulfuric acid and hydrochloric acid
For mixed acid solution as electrolyte, it is 3.5mol/L to control total acid concentration, using titanium plate as cathode, the surface area of the cathode titanium plates
Rest the head on surface area for the anode metal nickel plate, metal nickel block or metallic nickel 15%, then leads to direct current electrolysis pH to terminal
Value 3.2 completes liquid making process, the metallic nickel that periodic reverse current dissolving cathode separates out.
In the present embodiment, the process conditions of the direct current electrolysis are：Anodic current density is 220A/m2, electrolyte
Temperature is room temperature, and for heteropole away from for 18mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 23cm/h.The cycle
The cycle of reverse current is completely dissolved for the liquid making starting stage with the metallic nickel that cathode separates out.The grade of the metallic nickel is at least up to
The Ni9990 trades mark requirement into GB/T6516-2010.
Embodiment 5
The invention discloses a kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity, comprise the following steps：
Metal nickel plate, metal nickel block or metallic nickel are rested the head on and are placed in Ni―Ti anode frame as anode as metallic nickel, with sulfuric acid and hydrochloric acid
For mixed acid solution as electrolyte, it is 3.5 mol/L to control total acid concentration, using titanium plate as cathode, the surface of the cathode titanium plates
Product is the anode metal nickel plate, metal nickel block or metallic nickel rest the head on the 10% of surface area, then leads to direct current electrolysis to terminal
PH value 3.8 completes liquid making process, the metallic nickel that periodic reverse current dissolving cathode separates out.
In the present embodiment, the process conditions of the direct current electrolysis are：Anodic current density is 240A/m2, electrolyte
Temperature is room temperature, and for heteropole away from for 21mm, electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 30cm/h.The cycle
The cycle of reverse current is completely dissolved for the liquid making starting stage with the metallic nickel that cathode separates out.The grade of the metallic nickel is at least up to
The Ni9990 trades mark requirement into GB/T6516-2010.
The foregoing is only a preferred embodiment of the present invention, not makees limitation in any form to the present invention；It is all
The those of ordinary skill of the industry can be shown in by specification and described above and swimmingly implement the present invention；It is but all familiar
Professional and technical personnel without departing from the scope of the present invention, makes using disclosed above technology contents
A little variation, modification and evolution equivalent variations, be the present invention equivalent embodiment；Meanwhile all realities according to the present invention
Variation, modification and evolution of any equivalent variations that matter technology makees above example etc., still fall within the technology of the present invention
Within the protection domain of scheme.
Claims (3)
1. the method for the molten metallic nickel liquid making of a kind of small cathode deposition period reverse current electricity, it is characterised in that comprise the following steps：By gold
Category nickel, which is placed in Ni―Ti anode frame, is used as anode, using the mixed acid solution of sulfuric acid and hydrochloric acid as electrolyte, using titanium plate as cathode, and institute
Surface area of the surface area less than the metallic nickel of the anode of cathode titanium plates is stated, then leading to direct current electrolysis, pH value is completed to terminal
Liquid making process, the metallic nickel that periodic reverse current dissolving cathode separates out；
The metallic nickel as anode is metal nickel plate, metal nickel block or metallic nickel are rested the head on；
The total acid concentration of mixed acid solution is 2.5~4.0 mol/L；
The surface area of the cathode titanium plates is the 5~20% of the anode metal nickel surface area；
The process conditions of direct current electrolysis are：Anodic current density is 200~250A/m2, electrolyte temperature is room temperature, different
Pole span is 15~25mm, and electrolyte circular flow and the ratio of electrolytic cell cross-sectional area are 10~40cm/h.
2. the method for the molten metallic nickel liquid making of small cathode deposition period reverse current electricity according to claim 1, it is characterised in that：It is described
Endpoint pH is 3.0~4.0.
3. the method for the molten metallic nickel liquid making of small cathode deposition period reverse current electricity according to claim 1, it is characterised in that：It is described
The cycle of periodic reverse current is completely dissolved for the liquid making starting stage with the metallic nickel that cathode separates out.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610462149.0A CN106048638B (en) | 2016-06-23 | 2016-06-23 | A kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity |
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| CN201610462149.0A CN106048638B (en) | 2016-06-23 | 2016-06-23 | A kind of method of the molten metallic nickel liquid making of small cathode deposition period reverse current electricity |
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| CN106048638A CN106048638A (en) | 2016-10-26 |
| CN106048638B true CN106048638B (en) | 2018-05-04 |
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| JP7275629B2 (en) * | 2018-05-16 | 2023-05-18 | 住友金属鉱山株式会社 | Method for producing sulfuric acid solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG51885A1 (en) * | 1992-08-18 | 1993-10-15 | Valkov | Method for the producing of nickel sulphate |
| CN101960046A (en) * | 2008-03-12 | 2011-01-26 | 麦克德米德股份有限公司 | In electrolytic mode nickel is dissolved in method in the chemical nickel-plating liquid |
| CN105543891A (en) * | 2016-02-05 | 2016-05-04 | 江西瑞林稀贵金属科技有限公司 | Method for preparing copper and nickel sulfate |
-
2016
- 2016-06-23 CN CN201610462149.0A patent/CN106048638B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG51885A1 (en) * | 1992-08-18 | 1993-10-15 | Valkov | Method for the producing of nickel sulphate |
| CN101960046A (en) * | 2008-03-12 | 2011-01-26 | 麦克德米德股份有限公司 | In electrolytic mode nickel is dissolved in method in the chemical nickel-plating liquid |
| CN105543891A (en) * | 2016-02-05 | 2016-05-04 | 江西瑞林稀贵金属科技有限公司 | Method for preparing copper and nickel sulfate |
Non-Patent Citations (1)
| Title |
|---|
| "电解法制备硫酸镍工艺研究";李大平;《河南化工》;19990815(第8期);第10-12页 * |
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Inventor after: Chen Liang Inventor after: Qin Ruyong Inventor after: Dai Yun Inventor after: Fu Haikuo Inventor after: He Yuxian Inventor before: Chen Liang Inventor before: Qin Ruyong Inventor before: Fu Haikuo Inventor before: Dai Yun Inventor before: He Yuxian |
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Effective date of registration: 20210510 Address after: 513000 Qingtang Town, Yingde City, Qingyuan City, Guangdong Province Patentee after: GUANGDONG JIANA ENERGY TECHNOLOGY Co.,Ltd. Address before: 511500 Qingtang Town, Yingde, Qingyuan City, Guangdong Province Patentee before: GUANGDONG JIANA ENERGY TECHNOLOGY Co.,Ltd. Patentee before: HUNAN JIANA ENERGY TECHNOLOGY Co.,Ltd. |
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