CN110607439A - Spherical nickel protoxide sectional oxidation acid leaching treatment method - Google Patents
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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
- 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
- C22B23/0423—Halogenated acids or salts thereof
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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
- 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
- C22B23/043—Sulfurated acids or salts thereof
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- 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
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- 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
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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
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- 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
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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Abstract
The invention relates to a sectional oxidation acid leaching treatment method of spherical nickel protoxide, which is characterized in that the spherical nickel protoxide is mechanically activated, and the mechanically activated nickel protoxide is subjected to two-stage countercurrent oxidation acid leaching; adding a ternary precursor waste which is easy to dissolve in acid, nickel powder, cobalt powder and other pure materials which are easy to dissolve in acid and contain nickel, cobalt, manganese and the like into the first-stage leachate, adding a proper amount of reducing agent or oxidizing agent according to the properties of the materials to consume the acid in the leachate to a pH value of more than 4.0, and obtaining a nickel leachate; the leachate after acid consumption is used for synthesizing a ternary precursor, preparing a high-purity nickel plate, nickel sulfate, nickel chloride crystals and the like. The method has the advantages of high recovery rate of nickel protoxide, short process, simplicity, easy implementation, low cost, less investment and obvious economic and social benefits.
Description
Technical Field
The invention belongs to the field of chemical industry, relates to the recycling of nickel elements in spherical nickel protoxide, and particularly relates to a sectional oxidation acid leaching treatment method for spherical nickel protoxide.
Background
Nickel is widely used in the fields of steel manufacturing such as stainless steel and alloy structural steel, electroplating, high nickel base alloy, batteries and the like, and is widely used in various military manufacturing industries such as airplanes and radars, civil machinery manufacturing industry, electroplating industry and the like. Because nickel has better performances of corrosion resistance, high temperature resistance, rust prevention and the like, the nickel is widely applied to the steel fields of stainless steel, alloy steel and the like. The consumption of nickel is the greatest in stainless steel applications, and primary nickel ores of 2/3 worldwide are all used for the production of stainless steel. The nickel-doped alloy steel can improve the strength of the alloy steel and keep good plasticity and toughness of the alloy steel, and is mainly applied to manufacturing acid-resistant towers, medical instruments and daily necessities in chemical production, and mechanical manufacturing, transportation, military industry and the like for modifying bridges, building warships and the like. The nickel-based alloy is an alloy with comprehensive properties such as high strength, certain oxidation and corrosion resistance and the like at a high temperature of 650-1000 ℃. The nickel-based alloy product is widely applied to the industrial fields of aviation, ships, chemical engineering, electronics, medicine, energy and the like. Nickel is also used in the battery field, mainly in nickel-hydrogen batteries, cadmium-nickel batteries, lithium ion batteries, and the like. Lithium ion batteries are now the best chemical batteries for rechargeable performance that have been commercialized throughout the world, and in recent years hundreds of millions of lithium ion batteries have been produced each year and have grown at a rate of over 20% year by year. The demand of nickel and cobalt which are raw materials required by the production of the lithium ion battery is rapidly increased along with the rapid development of the lithium ion battery industry, the nickel-cobalt-manganese ternary lithium ion battery becomes a mainstream product, the high-nickel lithium ion battery becomes the development direction of the lithium ion battery in the future in recent years, and the demand of metal nickel is increased along with the rapid development of the lithium ion battery industry. In addition, nickel is also used in the field of electroplating, catalysts, pigments and dyes. The nickel can also be made into novel ceramics such as nickel ferrite, nickel zinc ferrite and the like, and can be used as an iron core of a transformer, an antenna of a radio, an electromagnetic crane and the like, so that the application is very wide.
The nickel protoxide is light green or dark green powdery solid, has good catalytic activity, ferromagnetism, heat-sensitive gas sensitivity and electroluminescent performance, and is an important inorganic functional material. At present, the domestic production of nickel protoxide powder mainly utilizes spray pyrolysis technology and chemical synthesis and then calcination technology. The nickel protoxide products are generally treated at high temperature, the recycling difficulty of the nickel protoxide after failure is high, the research on the field is few at present, and documents and patents which can be found in China are very limited.
The spherical nickel protoxide recycled in the invention is blackish green spherical particles with the diameter of about 2mm, and the raw material cannot leach nickel by using 2-9mol/L sulfuric acid solution at the temperature of 90 ℃. The raw material can be leached by high-concentration sulfuric acid and hydrochloric acid at a high temperature of more than 300 ℃ for more than 6 hours. The spherical nickel protoxide has high yield, develops an economic and reasonable industrial application method of the material, and has great economic and social benefits.
The patent with the application number of CN201711156784.7 discloses a method for preparing nickel salt by directly leaching nickel oxide under normal pressure, and discloses a method for preparing nickel sulfate or nickel chloride by leaching nickel oxide under normal pressure, which comprises the steps of mixing dilute sulfuric acid solution with nickel oxide, stirring and reacting for 1 ~ 5h at the temperature of 50 ~ 100 ℃ to gradually generate yellow-green solid, washing the yellow-green solid to weak acidity by distilled water after solid-liquid separation, dissolving by distilled water or hydrogen peroxide aqueous solution with the concentration of 1 ~ 5% to generate corresponding nickel sulfate solution, or mixing hydrochloric acid solution with nickel oxide, stirring and reacting for 1 ~ 3h at the temperature of 50 ~ 100 ℃ to gradually generate green nickel chloride solution, wherein the nickel content of the nickel salt solution prepared by the method is more than 110 g/L.
The invention discloses a method for preparing nickel sulfate by acid leaching nickel oxide under the conditions of high temperature and high pressure, which comprises the steps of placing the nickel oxide in a reaction kettle, adding 0.92 ~.68 mol/L dilute sulfuric acid solution, stirring and reacting for 0.5 ~ h under the condition of 150 ~ ℃, and carrying out suction filtration on the reaction solution to obtain a nickel sulfate solution.
At present, the granular spherical nickel protoxide with the thickness of about 2mm cannot be leached out by using a 2-9mol/L sulfuric acid solution at the temperature of 90 ℃, the raw material can be leached out by using high-concentration sulfuric acid and hydrochloric acid with the temperature of more than 300 ℃ for more than 6 hours, and the method has the advantages of large difficulty in industrial utilization, long time and low efficiency.
Disclosure of Invention
In order to solve the problems of high difficulty in industrial utilization and high treatment cost of large-particle nickel protoxide in the prior art, the invention provides a method for sectional oxidation acid leaching treatment of spherical nickel protoxide.
The technical scheme adopted by the invention is as follows: a spherical nickel protoxide subsection oxidation acid leaching treatment method comprises the following steps:
step (1), mechanical activation of spherical nickel protoxide: mechanical activation is carried out on the spherical nickel protoxide by a ball mill to control the granularity of the material below 50 mu m;
step (2), two-stage countercurrent oxidation acid leaching, namely leaching the nickel protoxide after mechanical activation at the leaching temperature of 80-100 ℃, firstly, using inorganic acid with the concentration of 1.8 ~ 3.5.5 mol/L to carry out one-stage leaching for 0.5 ~ 3h, concentrating a thickener after leaching, enabling the first-stage leaching solution to enter an acid consumption stage, enabling leaching residues to enter a second-stage leaching stage, adopting the inorganic acid with the concentration of 3.5-4.5mol/L for the second-stage leaching, enabling the leaching time to be 0.5 ~ 3h, adding a proper amount of oxidant in the two-stage leaching process, carrying out solid-liquid separation after the second-stage leaching, and returning the second-stage leaching solution to the first stage to carry out countercurrent leaching;
and (3) adding materials containing nickel, cobalt and manganese which are easy to dissolve in acid into the first-stage leachate according to the application field of the nickel protoxide leachate, consuming residual acid to a pH value of more than 4.0, and using the leachate after acid consumption to synthesize a ternary precursor and prepare high-purity nickel plates, nickel sulfate and nickel chloride crystals.
In the step (2), the inorganic acid is sulfuric acid, hydrochloric acid or nitric acid.
In the step (2), when the second-stage leaching solution enters the first-stage reaction kettle, water is added to dilute the second-stage leaching solution into the first-stage required acid
And (4) concentration.
In the step (2), the oxidant is hydrogen peroxide, potassium permanganate, sodium chlorate and sodium persulfate or pure oxygen or ozone is introduced.
In the step (2), if a small amount of unleached nickel protoxide exists in the second-stage leaching, returning to the step (1)
Leaching is continued after mechanical activation.
In the step (3), different raw materials are selected for acid consumption according to the application field of the leachate, if the leachate is used for synthesizing a ternary precursor, materials containing nickel, cobalt, manganese and the like, such as the ternary precursor or ternary waste, nickel powder, cobalt powder, electrolytic manganese, metal manganese powder and the like, are added; if the method is applied to the preparation of products such as nickel sulfate crystals, nickel chloride crystals, electrodeposited nickel plates and the like, purer materials such as nickel carbonate, nickel hydroxide, nickel buttons, nickel powder and the like are selected for acid consumption; adding proper reducing agent or oxidant, such as hydrogen peroxide, sodium sulfite, etc. according to the characteristics of acid-consuming material. The oxidant is sodium persulfate, hydrogen peroxide, oxygen, sodium chlorate, potassium permanganate, etc.
The nickel protoxide is spherical particles with the granularity of about 2mm, and has the advantages of high hardness, low activity, high nickel main grade and low impurity content.
The invention has the beneficial effects that:
the method comprises the steps of mechanically activating spherical nickel protoxide to a particle size of below 50 mu m, then carrying out two-stage oxidation acid leaching, wherein one stage adopts low-acidity leaching, the other stage adopts high-acidity leaching, the first-stage leaching solution is diluted and then consumes acid for utilization, the first-stage leaching residue enters a second-stage leaching, and the second-stage leaching solution enters a first-stage reaction kettle; the acidity of the leachate is reduced as much as possible through the first-stage low-acidity leaching, the leaching rate of the nickel protoxide is ensured through the second-stage high-acidity leaching, and the leachate keeps proper concentration according to the application field of the solution and the nickel decomposition degree, such as the nickel concentration of a sulfuric acid system is below 100g/L, and the nickel concentration of nickel chloride is below 200g/L, so that the solution and a pipeline are prevented from crystallizing.
The leached solution can be directly used for synthesizing a ternary precursor, producing nickel sulfate, nickel chloride, electrolytic nickel plates and the like after consuming acid by using ternary waste materials and the like; the invention is a simple and high-efficiency industrial application method of nickel protoxide, the nickel protoxide is through two-section oxidation acid leaching after mechanical activation, the nickel solution that is got can be applied to many kinds of fields, the technological process of this method is short, simple, high-efficient, easy industrialization, the nickel protoxide is high to reclaim the rate, with low costs, with little investment, the economic social benefit is apparent.
In the leaching process, a proper oxidant such as hydrogen peroxide, potassium permanganate, sodium chlorate and sodium persulfate is added or pure oxygen, ozone and the like are introduced to improve the reaction speed, leaching residues are almost not generated after the second-stage leaching, and if a small amount of leaching residues exist, the mechanical activation is returned to continue the leaching; diluting the first-stage leachate to a nickel concentration of about 90g/L according to the use requirement for later use;
drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the specific drawings;
the spherical nickel protoxide is spherical or ellipsoidal with the granularity of about 2mm, and has high hardness, low activity and high purity.
Example 1
A process for treating spherical nickel protoxide by staged oxidizing and acid leaching includes mechanical activation of spherical granular nickel protoxide by ball mill until the granularity of material is about 20 microns (10 m)3Leaching in two stages in a reaction kettle, wherein 4.5mol/L sulfuric acid is added in the second stage, 2.0mol/L sulfuric acid is added in the first stage, the temperature is raised to 100 ℃, the mechanically activated nickel protoxide is added in the first stage reaction kettle at the flow rate of 2.3t/h, acid is added in the second stage, and the flow rate of the sulfuric acid is 1.62m3Flow rate of pure water of 4.92 m/h3H, only adding water without adding acid at the first stage, wherein the water flow is 8.2m3The acidity of the leaching solution is kept unchanged, the leaching is carried out for 0.5h, sodium persulfate is added in the two leaching processes, and the flow rates of 20 percent of sodium persulfate are respectively 1.1m3And h, after the first-stage leaching is concentrated by a thickener, the supernatant liquid enters an acid consumption section, leaching slag enters a second-stage reaction kettle for leaching, the thickener is concentrated, the supernatant liquid enters a first-stage reaction kettle for two-stage countercurrent leaching, the leaching liquid consumes acid by using nickel carbonate, the nickel carbonate is added with solids, the adding flow is 0.24t/h, the acid consumption temperature is 50 ℃, the pH value of the solution is adjusted to be 5.2, and the leaching liquid is diluted to the nickel concentration of about 100g/L for later use.
Example 2
A process for treating spherical nickel protoxide by staged oxidizing and acid leaching includes mechanical activation of spherical granular nickel protoxide by ball mill until the granularity of material is about 30 microns (10 m)3Leaching in two stages in a reaction kettle, wherein 3.5mol/L sulfuric acid is added in the second stage, 2.5mol/L sulfuric acid is added in the first stage, the temperature is raised to 90 ℃, the mechanically activated nickel protoxide is added in the first stage reaction kettle, the flow rate is 0.72t/h, acid is added in the second stage, and the flow rate of the sulfuric acid is 0.51m3Flow rate of pure water is 1.87m3H, only adding water without adding acid at the first stage, wherein the water flow is 1.87m3H, keeping the acidity of the leaching solution, leaching for 2h, adding hydrogen peroxide in the two leaching processes, wherein the flow rates of 30 percent sodium persulfate are respectively 0.35m3H, adding in a first-stage reaction kettleAdding mechanically activated nickel protoxide, thickening with a thickener, allowing supernatant liquid to enter an acid consumption section, allowing leaching residues to enter a second-stage reaction kettle for leaching, adding a proper amount of hydrogen peroxide in the two-stage leaching process, thickening with the thickener, allowing supernatant liquid to enter a first-stage reaction kettle for two-stage countercurrent leaching, adding a proper amount of waste ternary positive electrode precursor into the leaching liquid, adjusting the flow rate to 72kg/h and the acid consumption temperature to 60 ℃, adjusting the pH value of the solution to 4.6, diluting the leaching liquid to the nickel concentration of about 90g/L for later use, and adding a proper amount of cobalt sulfate, manganese sulfate and the like for synthesizing the ternary precursor.
Example 3
A process for treating spherical nickel protoxide by staged oxidizing and acid leaching includes mechanical activation of spherical granular nickel protoxide by ball mill until the granularity of material is about 50 microns (10 m)3Leaching in two stages in a reaction kettle, wherein 4.5mol/L sulfuric acid is added in the second stage, 3.5mol/L sulfuric acid is added in the first stage, the temperature is raised to 85 ℃, the mechanically activated nickel protoxide is added in the first stage reaction kettle, the flow rate is 0.67t/h, acid is added in the second stage, and the flow rate of the sulfuric acid is 0.48m3Flow rate of pure water is 1.44m3H, only adding water without adding acid at the first stage, wherein the water flow is 0.59m3H, keeping the acidity of the leaching solution, adding hydrogen peroxide in the two-stage leaching process, and adding 30 percent sodium persulfate with the flow of 0.67m3Leaching for 3h, after thickening with a thickener, feeding the supernatant into an acid consumption section, feeding the leaching residue into a two-section reaction kettle for leaching, and feeding pure oxygen into the two-section leaching process, wherein the oxygen flow is 0.5m3About/h, thickening by a second-stage thickener, feeding the supernatant into a first-stage reaction kettle for two-stage countercurrent leaching, consuming acid by using nickel hydroxide for the leachate, adding solid nickel hydroxide into the leachate, adjusting the pH value of the solution to 6.0 at the adding speed of 0.67kg/h, and diluting the leachate to the nickel concentration of about 100g/L for later use.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (6)
1. A spherical nickel protoxide subsection oxidation acid leaching processing method is characterized in that: the method comprises the following steps:
step (1), mechanical activation of spherical nickel protoxide: mechanical activation is carried out on the spherical nickel protoxide by a ball mill to control the granularity of the material below 50 mu m;
step (2), two-stage countercurrent oxidation acid leaching, namely leaching the nickel protoxide after mechanical activation at the leaching temperature of 80-100 ℃, firstly, using inorganic acid with the concentration of 1.8 ~ 3.5.5 mol/L to carry out one-stage leaching for 0.5 ~ 3h, concentrating a thickener after leaching, enabling the first-stage leaching solution to enter an acid consumption stage, enabling leaching residues to enter a second-stage leaching stage, adopting the inorganic acid with the concentration of 3.5-4.5mol/L for the second-stage leaching, enabling the leaching time to be 0.5 ~ 3h, adding a proper amount of oxidant in the two-stage leaching process, carrying out solid-liquid separation after the second-stage leaching, and returning the second-stage leaching solution to the first stage to carry out countercurrent leaching;
and (3) adding materials containing nickel, cobalt and manganese which are easy to dissolve in acid into the first-stage leachate according to the application field of the nickel protoxide leachate, consuming residual acid to a pH value of more than 4.0, and using the leachate after acid consumption to synthesize a ternary precursor and prepare high-purity nickel plates, nickel sulfate and nickel chloride crystals.
2. The staged oxidation acid leaching treatment method for spherical nickel protoxide according to claim 1, characterized in that: in the step (2), the inorganic acid is sulfuric acid, hydrochloric acid or nitric acid.
3. The staged oxidation acid leaching treatment method for spherical nickel protoxide according to claim 1 or 2, characterized in that: in the step (2), water is added to dilute the second-stage leachate into the first-stage reaction kettle to obtain the first-stage required acid concentration.
4. The staged oxidation acid leaching treatment method for spherical nickel protoxide according to claim 3, characterized in that: in the step (2), the oxidant is hydrogen peroxide, potassium permanganate, sodium chlorate and sodium persulfate or pure oxygen or ozone is introduced.
5. The staged oxidation acid leaching treatment method for spherical nickel protoxide according to claim 1, 2 or 4, characterized in that: in the step (2), if a small amount of nickel protoxide is not leached in the second-stage leaching, returning to the step (1) for mechanical activation and continuing leaching.
6. The staged oxidation acid leaching treatment method for spherical nickel protoxide according to claim 5, characterized in that: in the step (3), when the leachate is used for synthesizing a ternary precursor, adding ternary waste or other materials containing nickel, cobalt, manganese and the like; for producing products such as nickel sulfate crystal, nickel chloride crystal, electrodeposition nickel board, then add purer nickeliferous material: nickel carbonate, nickel hydroxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115353160A (en) * | 2022-09-22 | 2022-11-18 | 福建常青新能源科技有限公司 | Preparation method of battery-grade nickel-cobalt-manganese ternary sulfate solution |
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Application publication date: 20191224 |