CN107634218B - Method for preparing ternary material precursor by using positive and negative electrode materials of capacitive nickel-hydrogen power battery - Google Patents

Method for preparing ternary material precursor by using positive and negative electrode materials of capacitive nickel-hydrogen power battery Download PDF

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CN107634218B
CN107634218B CN201710759924.3A CN201710759924A CN107634218B CN 107634218 B CN107634218 B CN 107634218B CN 201710759924 A CN201710759924 A CN 201710759924A CN 107634218 B CN107634218 B CN 107634218B
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nickel
cobalt
power battery
hydrogen power
negative electrode
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CN107634218A (en
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张亚莉
宫本奎
张丽鹏
楚玮
毛迦勒
蒋志军
徐旭
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Shandong University of Technology
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    • Y02E60/10—Energy storage using batteries
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention belongs to the technical field of ternary material precursor preparation, and particularly relates to a method for preparing a ternary material precursor by using a positive and negative electrode material of a capacitive nickel-hydrogen power battery. Adding the anode and cathode materials and an oxidizing sodium source of the capacitive nickel-hydrogen power battery into a sulfuric acid solution at the same time for leaching reaction, and filtering to obtain a filtrate and a filter cake; adding a cobalt source and a manganese source into the filtrate, adjusting the pH value, adding a fluoride, and filtering to obtain a filtrate; adding a precipitator into the filtrate, reacting, filtering, washing and drying to obtain the ternary material precursor. The invention takes the waste capacitive nickel-hydrogen power battery as the raw material, has low cost, high product quality and good economical efficiency, and realizes the directional circulation of nickel-cobalt resources.

Description

Method for preparing ternary material precursor by using positive and negative electrode materials of capacitive nickel-hydrogen power battery
Technical Field
The invention belongs to the technical field of ternary material precursor preparation, and particularly relates to a method for preparing a ternary material precursor by using a positive and negative electrode material of a capacitive nickel-hydrogen power battery.
Background
The ternary material has the advantages of high capacity and high voltage of lithium nickelate, high voltage and high safety of lithium manganate and good cyclicity of lithium cobaltate, overcomes the defects of difficult and unstable synthesis of lithium manganate and lithium nickelate and high cost of lithium cobaltate, and becomes the mainstream anode material at present. However, the nickel cobalt salt used as the main raw material for producing the precursors of lithium nickelate, lithium cobaltate and lithium manganate has insufficient resources, which seriously restricts the large-scale industrial production of the ternary material. Most of nickel cobalt salts for preparing ternary materials at present are analytically pure and chemically pure sulfates, most of the sulfates are prepared from ores, and the serious shortage of nickel cobalt ore resources becomes a bottleneck of the development of the ternary materials.
On the other hand, with the rapid development of new energy automobiles, the capacitive nickel-hydrogen power battery can be scrapped after being used for three to five years, and the accumulated scrapping amount exceeds 17 ten thousand tons by 2018. After the capacitive power battery is retired, if necessary recovery and treatment are not performed, not only can resources be wasted, but also the environment can be polluted, so that the contradiction between the development of the new energy automobile industry and the environment and the resources is more and more prominent. Whether the capacitive power battery can be effectively recycled or not only directly influences the sustainable development of the new energy automobile industry, but also influences the realization of the national strategies of energy conservation, emission reduction and the like. The direct preparation of the nickel-cobalt-manganese ternary material precursor from the nickel-cobalt material obtained in the recovery process of the waste capacitive power battery can break through the bottleneck of nickel-cobalt resource shortage and realize the directional circulation of the metal resource of the battery material.
The positive and negative electrode materials of the capacitive nickel-hydrogen power battery not only contain components such as nickel and cobalt, but also contain rare earth. In the recovery process, how to separate rare earth from metals such as nickel and cobalt is the most critical step. The separation effect is poor, so that rare earth is doped in the nickel-cobalt-manganese ternary material precursor, the function of the material is influenced, and the rare earth is greatly wasted.
Chinese patent CN103545504A discloses a method for preparing a ternary cathode material precursor, which takes nickel hydroxide, manganese and cobalt concentrate as an intermediate product of the production of electrolytic nickel from laterite-nickel ore as a raw material, and the preparation process comprises the following process flows: acid leaching, impurity removal and recrystallization, mixed salt preparation, precipitator preparation, synthesis reaction, pH value adjustment, separation and washing, and drying for 8 steps. The patent takes nickel hydroxide, manganese and cobalt concentrate as an intermediate product of electrolytic nickel production from laterite-nickel ore as a raw material, and does not contain rare earth elements, so the patent does not relate to the separation process of metals such as nickel and cobalt and rare earth.
Chinese patent CN105633500A discloses a method for preparing a ternary cathode material precursor by using a recycled lithium ion battery material, which comprises the following steps: dissolving and recovering the lithium ion battery anode material by using sulfuric acid and hydrogen peroxide to obtain a first solution; adjusting the pH value of the first solution to 5-6.5, adding a filter aid and filtering to remove impurities to obtain a second solution; adding nickel sulfate, cobalt sulfate and/or manganese sulfate into the second solution, and adjusting the molar ratio of nickel, cobalt and manganese to be 0.4-0.6:0.1-0.3:0.2-0.4 to obtain a third solution; adding a complexing precipitant into the third solution, adjusting the pH value of the third solution to 7-9, and reacting to obtain a nickel-cobalt-manganese ternary material precursor precipitate; and washing and drying the nickel-cobalt-manganese ternary material precursor precipitate to obtain the ternary cathode material precursor. The patent takes the anode material of the lithium ion battery as the raw material and does not contain rare earth elements, so the patent does not relate to the separation process of metals such as nickel and cobalt and the like and rare earth.
Based on the above problems, a method capable of directly separating metals such as rare earth and nickel cobalt and effectively preparing a ternary material precursor is needed.
Disclosure of Invention
The invention aims to provide a method for preparing a ternary material precursor by using positive and negative electrode materials of a capacitive nickel-hydrogen power battery, which is used for directly separating rare earth, nickel, cobalt and other metals to effectively prepare the ternary material precursor.
The invention relates to a method for preparing a ternary material precursor by using positive and negative electrode materials of a capacitive nickel-hydrogen power battery, which comprises the following steps:
(1) adding the anode and cathode materials and an oxidizing sodium source of the capacitive nickel-hydrogen power battery into a sulfuric acid solution at the same time for leaching reaction, and filtering to obtain a filtrate and a filter cake;
(2) adding a cobalt source and a manganese source into the filtrate obtained in the step (1), adjusting the pH value, adding a fluoride, and filtering to obtain a filtrate;
(3) and (3) adding a precipitator into the filtrate obtained in the step (2), reacting, filtering, washing and drying to obtain the ternary material precursor.
Wherein:
in the step (1), the oxidizing sodium source is sodium hypochlorite, sodium peroxide or sodium chlorate, the mass ratio of the oxidizing sodium source to the positive and negative electrode materials of the capacitive nickel-hydrogen power battery is 150-.
In the step (1), the concentration of the sulfuric acid solution is 130-200g/L, the volume-to-mass ratio of the sulfuric acid solution to the positive and negative electrode materials of the capacitive nickel-hydrogen power battery is 4-15:1, the sulfuric acid solution is counted by L, and the positive and negative electrode materials of the capacitive nickel-hydrogen power battery are counted by kg.
In the step (1), the leaching reaction time is 60-90min, and the leaching reaction temperature is 40-70 ℃.
In the step (2), the cobalt source is one or more of metal cobalt, cobalt oxide, cobalt sulfate, cobalt oxalate, cobalt carbonate, cobalt hydroxide or cobalt chloride; the manganese source is one or more of metal manganese, manganese oxide, manganese chloride, manganese sulfate, manganese nitrate or pyrolusite.
In the step (2), before adding the cobalt source and the manganese source, the concentration of nickel in the filtrate obtained in the step (1) is adjusted to be 0.1-3.5mol/L, so that the molar ratio of nickel to cobalt to manganese is 8:1: 1.
In the step (2), an alkali source is adopted to adjust the pH value to 4.5-5.5, wherein the alkali source is one or more of sodium hydroxide, potassium hydroxide or ammonia water.
In the step (2), the fluoride is one or more of sodium fluoride, potassium fluoride or ammonium fluoride.
In the step (3), a precipitator is added into the filtrate obtained in the step (2) to enable the concentration of the precipitator to be 0.1-7mol/L, wherein the precipitator is one or more of sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate or ammonium bicarbonate.
In the step (3), the reaction temperature is 10-100 ℃, and the reaction time is 10-120 min.
The positive and negative electrode materials of the capacitive nickel-hydrogen power battery contain Ni, NiO, CoO, ZnO and Ni2O3、Co2O3、Mn2O3、Re2O3And the reaction equation of the leaching process is as follows:
2Ni+3NaClO+6H+＝2Ni3++3H2O+3NaCl (1)
NiO+2NaClO+4H+＝Ni3++2H2O+2NaCl (2)
CoO+2NaClO+4H+＝Co3++2H2O+2NaCl (3)
2Ni3++3H2SO4＝Ni2(SO4)3+6H+ (4)
2Co3++3H2SO4＝Co2(SO4)3+6H+ (5)
Ni2O3+3H2SO4＝Ni2(SO4)3+3H2O (6)
Co2O3+3H2SO4＝Co2(SO4)3+3H2O (7)
Mn2O3+3H2SO4＝Mn2(SO4)3+3H2O (8)
ZnO+H2SO4＝ZnSO4+H2O (9)
Re2O3+4H2SO4+2Na+＝Re2(SO4)3·Na2SO4↓+3H2O+2H+ (10)
the invention has the following beneficial effects:
the invention provides a method for preparing a ternary material precursor by comprehensively utilizing anode and cathode materials of a waste capacitive nickel-hydrogen power battery in order to overcome the current situations of insufficient nickel-cobalt resources, pollution of the waste battery and the like, wherein the anode and cathode materials of the waste capacitive nickel-hydrogen power battery and an oxidized sodium source are simultaneously added into a sulfuric acid solution for leaching reaction, so that nickel and cobalt in the solution are firstly oxidized into high valence state from low valence state; the high valence state nickel cobalt manganese zinc and other metals in the solution react with the sulfuric acid solution to generate sulfate, and the rare earth metal reacts with the sulfuric acid solution and the oxidized sodium source to generate rare earth sulfate double salt precipitate. Filtering the rare earth sulfate double salt precipitate to form a filter cake for recovering rare earth metals; and the sulfate of metals such as nickel, cobalt, manganese, zinc and the like is remained in the solution and is used for preparing the precursor of the ternary material. Therefore, the invention realizes the effective separation of metals such as nickel and cobalt and the like from the rare earth.
The invention firstly adds fluoride to remove impurities such as calcium, magnesium and the like; and adding a precipitator, and controlling the synthesis conditions to ensure that metals beneficial to the electrochemical performance of the ternary material lithium ion battery in the anode and cathode material leachate selectively enter precipitation, and metals such as calcium, magnesium and the like do not enter precipitation.
The product obtained by the method is a zinc-doped ternary material precursor, and the zinc element is uniformly distributed in ternary material precursor particles, so that the problem that the doped elements are difficult to uniformly mix is solved, and the conductivity of the material is greatly improved.
The invention directly utilizes the nickel-cobalt material obtained in the recovery process of the waste capacitive nickel-hydrogen power battery to synthesize the nickel-cobalt-manganese ternary material precursor, and is particularly suitable for providing excellent nickel source and cobalt source for the production of lithium ion battery materials. The invention takes the waste capacitive nickel-hydrogen power battery as the raw material, has low cost, high product quality and good economical efficiency, and realizes the directional circulation of nickel-cobalt resources. After the integrated new formulation of lily and radix astragali decoction is subjected to scale production, huge environmental benefits, social benefits and economic benefits can be brought.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
Adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 200mg of sodium hypochlorite into 4.5L of 190g/L sulfuric acid solution at the same time, carrying out leaching reaction at 40 ℃ for 90min, filtering to obtain filtrate and filter cake, wherein the filter cake is used for recovering rare earth, and the filtrate does not contain rare earth elements through detection;
adjusting the concentration of nickel ions in the filtrate to be 1.5mol/L by adding water, dissolving a certain amount of cobalt hydroxide and manganese oxide to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of ammonia water into the mixed solution, adjusting the pH value to be 5, and adding potassium fluoride until no precipitate is generated. Filtering to obtain filtrate, adding potassium carbonate into the filtrate to enable the concentration of the potassium carbonate to be 2mol/L, reacting for 20min in a stirring reactor at 50 ℃, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. Wherein the zinc accounts for 1 percent of the total mass of the zinc-doped nickel-cobalt-manganese ternary precursor.
Example 2
Adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 250mg of sodium chlorate into 15L of sulfuric acid with the concentration of 160g/L at the same time, carrying out leaching reaction at 60 ℃ for 60min, filtering to obtain filtrate and filter cake, wherein the filter cake is used for recovering rare earth, and the filtrate is detected to contain no rare earth elements;
adjusting the concentration of nickel ions in the filtrate to be 2.0mol/L by evaporation, dissolving a certain amount of cobalt sulfate and manganese chloride to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of sodium hydroxide into the mixed solution, adjusting the pH value to be 5.2, and adding sodium fluoride until no precipitate is generated. Filtering to obtain filtrate, adding sodium carbonate into the filtrate to make the concentration of the sodium carbonate be 4mol/L, reacting for 40min in a stirring reactor at 80 ℃, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. Wherein the zinc accounts for 1.5 percent of the total mass of the zinc-doped nickel-cobalt-manganese ternary precursor.
Example 3
Adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 200mg of sodium peroxide into 12L of sulfuric acid with the concentration of 150g/L at the same time, carrying out leaching reaction at 50 ℃ for 80min, filtering to obtain filtrate and filter cake, wherein the filter cake is used for recovering rare earth, and the filtrate does not contain rare earth elements through detection;
adding water to adjust the concentration of nickel ions in the filtrate to be 1.0mol/L, dissolving a certain amount of cobalt chloride and manganese sulfate to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of ammonia water into the mixed solution, adjusting the pH value to be 4.8, and adding potassium fluoride until no precipitate is generated. Filtering to obtain filtrate, adding ammonium carbonate into the filtrate to make the concentration of the ammonium carbonate be 6mol/L, reacting for 60min in a stirring reactor at 70 ℃, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. Wherein zinc accounts for 1.2 percent of the total mass of the zinc-doped nickel-cobalt-manganese ternary precursor.
Example 4
Adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 150mg of sodium hypochlorite into 6L of sulfuric acid with the concentration of 130g/L at the same time, carrying out leaching reaction at 45 ℃ for 75min, filtering to obtain filtrate and filter cake, wherein the filter cake is used for recovering rare earth, and the filtrate does not contain rare earth elements through detection;
adjusting the concentration of nickel ions in the filtrate to 0.8mol/L by adding water, dissolving a certain amount of cobalt hydroxide and manganese oxide to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of potassium hydroxide into the mixed solution, adjusting the pH value to 5.5, and adding ammonium fluoride until no precipitate is generated. Filtering to obtain a filtrate, adding potassium bicarbonate into the filtrate to enable the concentration of the potassium bicarbonate to be 5mol/L, reacting for 80min in a stirring reactor at 35 ℃, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. Wherein the zinc accounts for 1.4 percent of the total mass of the zinc-doped nickel-cobalt-manganese ternary precursor.
Example 5
Adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 300mg of sodium peroxide into 9L of sulfuric acid with the concentration of 190g/L at the same time, carrying out leaching reaction at 70 ℃ for 90min, filtering to obtain filtrate and filter cake, wherein the filter cake is used for recovering rare earth, and the filtrate does not contain rare earth elements through detection;
adjusting the concentration of nickel ions in the filtrate to be 3mol/L by evaporation, dissolving a certain amount of cobalt oxide and manganese chloride to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of ammonia water into the mixed solution, adjusting the pH value to be 4.5, and adding potassium fluoride until no precipitate is generated. Filtering to obtain filtrate, adding potassium carbonate into the filtrate to make the concentration of the potassium carbonate be 6.5mol/L, reacting in a stirring reactor at 90 ℃ for 100min, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. Wherein zinc accounts for 1.1 percent of the total mass of the zinc-doped nickel-cobalt-manganese ternary precursor.
Comparative example 1
The sodium hypochlorite in example 1 was changed to hydrogen peroxide to react under otherwise unchanged conditions. The method comprises the following specific steps:
adding 1kg of positive and negative electrode materials of the capacitive nickel-hydrogen power battery and 200mg of hydrogen peroxide into 4.5L of 190g/L sulfuric acid at the same time, carrying out leaching reaction at 40 ℃ for 90min, filtering to obtain a filtrate and a filter cake, wherein the filter cake is used for recovering rare earth, and detecting that the filtrate contains rare earth elements;
adjusting the concentration of nickel ions in the filtrate to be 1.5mol/L by adding water, dissolving a certain amount of cobalt hydroxide and manganese oxide to ensure that the molar ratio of nickel, cobalt and manganese is 8:1:1, adding a proper amount of ammonia water into the mixed solution, adjusting the pH value to be 5, and adding potassium fluoride until no precipitate is generated. Filtering to obtain a filtrate, adding potassium carbonate into the filtrate to enable the concentration of the potassium carbonate to be 2mol/L, reacting for 20min in a stirring reactor at 50 ℃, filtering, washing and drying to obtain the zinc-doped nickel-cobalt-manganese ternary precursor. And detecting to obtain the nickel-cobalt-manganese ternary precursor containing rare earth elements.

Claims (7)

1. A method for preparing a ternary material precursor by using positive and negative electrode materials of a capacitive nickel-hydrogen power battery is characterized by comprising the following steps:
(1) adding the anode and cathode materials and an oxidizing sodium source of the capacitive nickel-hydrogen power battery into a sulfuric acid solution at the same time for leaching reaction, and filtering to obtain a filtrate and a filter cake; the oxidizing sodium source is sodium hypochlorite, sodium peroxide or sodium chlorate;
(2) adding a cobalt source and a manganese source into the filtrate obtained in the step (1), adjusting the pH value, adding a fluoride, and filtering to obtain a filtrate;
(3) adding a precipitator into the filtrate obtained in the step (2), reacting, filtering, washing and drying to obtain a ternary material precursor;
in the step (1), the mass ratio of the oxidizing sodium source to the positive and negative electrode materials of the capacitive nickel-hydrogen power battery is 150-;
in the step (1), the concentration of the sulfuric acid solution is 130-200g/L, the volume mass ratio of the sulfuric acid solution to the positive and negative electrode materials of the capacitive nickel-hydrogen power battery is 4-15:1, the sulfuric acid solution is counted by L, and the positive and negative electrode materials of the capacitive nickel-hydrogen power battery are counted by kg;
in the step (2), before adding the cobalt source and the manganese source, the concentration of nickel in the filtrate obtained in the step (1) is adjusted to be 0.1-3.5mol/L, so that the molar ratio of nickel to cobalt to manganese is 8:1: 1.
2. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (1), the leaching reaction time is 60-90min, and the leaching reaction temperature is 40-70 ℃.
3. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (2), the cobalt source is one or more of metal cobalt, cobalt oxide, cobalt sulfate, cobalt oxalate, cobalt carbonate, cobalt hydroxide or cobalt chloride; the manganese source is one or more of metal manganese, manganese oxide, manganese chloride, manganese sulfate, manganese nitrate or pyrolusite.
4. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (2), an alkali source is adopted to adjust the pH value to 4.5-5.5, wherein the alkali source is one or more of sodium hydroxide, potassium hydroxide or ammonia water.
5. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (2), the fluoride is one or more of sodium fluoride, potassium fluoride or ammonium fluoride.
6. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (3), a precipitator is added into the filtrate obtained in the step (2) to enable the concentration of the precipitator to be 0.1-7mol/L, wherein the precipitator is one or more of sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate or ammonium bicarbonate.
7. The method for preparing the ternary material precursor by using the positive and negative electrode materials of the capacitive nickel-hydrogen power battery according to claim 1, wherein the method comprises the following steps: in the step (3), the reaction temperature is 10-100 ℃, and the reaction time is 10-120 min.
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