CN111004918B - Method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries - Google Patents
Method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries Download PDFInfo
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- CN111004918B CN111004918B CN201911336969.5A CN201911336969A CN111004918B CN 111004918 B CN111004918 B CN 111004918B CN 201911336969 A CN201911336969 A CN 201911336969A CN 111004918 B CN111004918 B CN 111004918B
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- Y02P10/00—Technologies related to metal processing
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Abstract
The invention provides a method for recycling and preparing alpha spherical nickel by utilizing waste nickel-hydrogen batteries, which comprises the steps of firstly carrying out heat treatment on the waste nickel-hydrogen batteries and carbon powder, then crushing and sieving to obtain active substance powder, leaching and filtering the active substance powder to obtain a sulfate solution containing nickel, cobalt, manganese and aluminum ions, then adding a potassium permanganate solution into the sulfate solution containing the nickel, cobalt, manganese and aluminum ions to react with a sodium sulfate solution, then filtering to obtain a high-purity nickel-cobalt-aluminum sulfate mixed solution, carrying out complexation on the high-purity nickel-cobalt-aluminum sulfate mixed solution and ammonia water, then respectively dropwise adding a complexation product, a sodium hydroxide and sodium carbonate mixed solution and corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented into a reaction container with the ammonia water at 55-70 ℃ for reaction, wherein the PH value of the mixed solution in the reaction container is controlled to be 11.7-11.8, and the alpha spherical nickel is prepared after the reaction product is subjected to standing aging, filtering, washing and drying. The method has the advantages of simple and novel process, less pollution and high product purity.
Description
Technical Field
The invention relates to a method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries.
Background
Environmental pollution and petroleum energy crisis problems jointly promote the development of energy-saving and new energy automobiles. With the rapid development of domestic hybrid electric vehicles, the usage amount of the nickel-hydrogen power battery will gradually increase. However, all nickel-hydrogen power batteries have a certain service life, and need to be replaced after a period of use to generate more waste nickel-hydrogen batteries, and the waste batteries contain metal nickel, cobalt, manganese, aluminum, rare earth and the like, and these elements, if not treated, will generate great threat to the natural environment and human health, and will generate great resource waste. The traditional waste nickel-hydrogen battery is subjected to pretreatment, and then mainly aims at sorting out active substance powder for recovery treatment, and the current method mostly adopts the processes of wet leaching, chemical impurity removal, extraction and the like to respectively recover nickel, cobalt and manganese in the waste battery into nickel-cobalt-manganese salt, so that the method has long recovery process and low recovery value.
Disclosure of Invention
The invention aims to provide a method for recycling and preparing alpha spherical nickel by utilizing waste nickel-hydrogen batteries, which has the advantages of simple and novel process, high product purity and less pollution.
The invention is realized by the following scheme:
a method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries, which comprises the following steps,
(a) carrying out heat treatment on the waste nickel-metal hydride battery and carbon powder, crushing, sieving to obtain active substance powder, leaching the active substance powder with hydrogen peroxide and sulfuric acid, and filtering to obtain a sulfate solution containing nickel, cobalt, manganese and aluminum ions; generally, before sieving, iron materials are separated by magnetic separation, and then sieving is carried out, wherein oversize products mainly comprise diaphragms and plastics, and undersize products mainly comprise active substance powder, and the active substance powder mainly comprises nickel, cobalt, manganese, aluminum, rare earth and a small amount of iron; the leaching step can be used for filtering and removing carbon and a small amount of cracked organic matters to obtain a sulfate solution mainly containing nickel, cobalt, manganese and aluminum, and the leaching is carried out according to a conventional process, and specifically comprises the following steps: placing active substance powder into a mixed solution of hydrogen peroxide and sulfuric acid at the temperature of 65-70 ℃, stirring for more than 4 hours, and controlling the stirring speed to be 95-100 rpm, wherein the dosage of the mixed solution of hydrogen peroxide and sulfuric acid is calculated according to the requirement that 20g of the active substance powder needs 1L of the mixed solution of hydrogen peroxide and sulfuric acid, the dosage of hydrogen peroxide is calculated according to the requirement that 1g of the active substance powder needs 0.4ml of hydrogen peroxide, the initial molar concentration of the sulfuric acid is 1mol/L, filtering after leaching to obtain filter residue, and drying, wherein the drying temperature is generally controlled to be about 70 ℃;
(b) heating the sulfate solution containing nickel, cobalt, manganese and aluminum ions obtained in the step (a) to 80-98 ℃, adding a certain amount of potassium permanganate solution and sodium sulfate solution into the sulfate solution, controlling the pH of the reaction solution to be not more than 3.5 by adding sodium hydroxide solution or/and sodium carbonate solution, stirring and keeping the temperature (namely the temperature is 80-98 ℃) for a certain time, and filtering the reaction product to obtain a high-purity nickel-cobalt-aluminum sulfate mixed solution; the filter residues obtained by filtering in the step mainly comprise manganese dioxide residues, jarosite residues and rare earth complex salt residues;
(c) complexing the high-purity nickel-cobalt-aluminum sulfate mixed solution obtained in the step (b) with ammonia water, then respectively dropwise adding the complex product, the mixed solution of sodium hydroxide and sodium carbonate and the corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented into a reaction container which is at the temperature of 55-70 ℃ and is filled with ammonia water for reaction, wherein the pH of the mixed solution in the reaction container is controlled to be 11.7-11.8, and standing, aging, filtering, washing and drying the reaction product to obtain the alpha-spherical nickel. The mixed solution of sodium hydroxide and sodium carbonate is used for adjusting the PH of the mixed solution in the reaction vessel; wherein the processes of standing aging, filtering, washing and drying are carried out according to the standing aging, filtering, washing and drying processes in the prior alpha spherical nickel preparation.
In the step (c), the ammonia water complexed with the high-purity nickel cobalt aluminum sulfate mixed solution and Ni in the high-purity nickel cobalt aluminum sulfate mixed solution2+、Co2+Adding Al3+The molar ratio of (A) to (B) is 2-3: 1, i.e. mol [ NH ]3H2O]：mol[Ni2++Co2++Al3+]2-3: 1, Ni in the mixed solution of ammonia water and high-purity nickel-cobalt-aluminum sulfate in a reaction vessel2+、Co2+Adding Al3+In a molar ratio of 0.5 to 1: 1, i.e. mol [ NH ]3H2O]：mol[Ni2++Co2++Al3+]0.5-1: 1, the molar concentrations of ammonia water complexed with a high-purity nickel-cobalt-aluminum sulfate mixed solution and ammonia water filled in a reaction container are both 0.3-2 mol/L; the amount of the corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented is determined according to the mol [ Al ] of the mixed solution in the reaction vessel3++Co2+]/mol[Al3++Co2++Ni2+]Calculated as 15-20%.
In the step (c), the preparation process of the mixed solution of sodium hydroxide and sodium carbonate comprises the following specific steps: adding 2-6 g of sodium carbonate solid into 100ml of 1-3 mol/L sodium hydroxide solution, and uniformly mixing to obtain a sodium hydroxide and sodium carbonate mixed solution.
In the step (a), the effective carbon content of the carbon powder is more than 80%, and the using amount of the carbon powder is 5-10% of the weight of the waste nickel-hydrogen battery.
In the step (b), Mn is contained in potassium permanganate and sulfate solution containing nickel, cobalt, manganese and aluminum ions2+Adding Fe2+The molar ratio of the sodium sulfate to the sulfate solution containing nickel, cobalt, manganese and aluminum ions is 13:15, and Re is contained in the sulfate solution2+The molar ratio of (1) to (3) is controlled to be 2:3, and the heat preservation time is controlled to be 1-4 h.
In the step (a), the heat treatment process specifically comprises the following steps: and (3) placing the waste nickel-metal hydride battery and the carbon powder in heat treatment equipment at 400-600 ℃ for 2-6 h. The step can prevent iron elements and the like from being oxidized, and avoid influencing the subsequent physical magnetic separation of iron.
The invention relates to a method for recycling and preparing alpha spherical nickel by utilizing waste nickel-hydrogen batteries, which comprises the steps of directly carrying out iron removal, manganese removal and rare earth impurity removal on active substance powder leachate obtained by recycling through a potassium permanganate solution and a sodium sulfate solution to obtain a high-purity nickel-cobalt-aluminum sulfate mixed solution, then placing the high-purity nickel-cobalt-aluminum sulfate mixed solution into a reaction container after complexing with ammonia water, and adjusting the proportion of nickel, cobalt and aluminum by supplementing corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution according to requirements to finally prepare the alpha spherical nickel. The method for recycling and preparing the alpha spherical nickel by utilizing the waste nickel-hydrogen battery has the advantages of simple and novel process, high product purity, high safety and little pollution.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the description of the examples.
Example 1
A method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries, which comprises the following steps,
(a) placing the waste nickel-metal hydride battery and carbon powder with the weight of 5 percent of the weight of the waste nickel-metal hydride battery and the effective carbon content of 80 percent in heat treatment equipment with the temperature of 400 ℃ for 3 hours, taking out the carbon powder and cooling the carbon powder, then crushing the carbon powder, firstly separating iron materials by magnetic separation, and then sieving the iron materials, wherein oversize products mainly comprise diaphragms and plastics, and undersize products mainly comprise active substance powder which mainly comprises nickel, cobalt, manganese, aluminum, rare earth and a small amount of iron; leaching active substance powder by hydrogen peroxide and sulfuric acid, wherein the leaching is carried out according to a conventional process, and the specific steps are as follows: placing active substance powder into a mixed solution of hydrogen peroxide and sulfuric acid at the temperature of 65 ℃ and stirring for 4 hours, wherein the stirring speed is controlled to be 95rpm, wherein 20g of the active substance powder needs 1L of the mixed solution of hydrogen peroxide and sulfuric acid, the using amount of the hydrogen peroxide is calculated according to the requirement of 1g of the active substance powder on 0.4ml of hydrogen peroxide, and the initial molar concentration of the sulfuric acid is 1mol/L, then filtering the mixture to obtain filter residue and a sulfate solution containing nickel, cobalt, manganese and aluminum ions, wherein the filter residue is dried, and the drying temperature is generally controlled to be about 70 ℃;
(b) sulfate containing nickel, cobalt, manganese and aluminum ions obtained in the step (a)Heating the solution to 95 ℃, adding a certain amount of potassium permanganate solution and sodium sulfate solution into the solution, and controlling the pH of the reaction solution to be not more than 3.5 by adding sodium hydroxide solution and sodium carbonate solution, wherein Mn in the potassium permanganate solution and the sulfate solution containing nickel, cobalt, manganese and aluminum ions2+Adding Fe2+The molar ratio of the sodium sulfate to the sulfate solution containing nickel, cobalt, manganese and aluminum ions is 13:15, and Re is contained in the sulfate solution2+The molar ratio of the nickel sulfate to the aluminum sulfate is 2:3, stirring and heat preservation (namely the temperature is 95 ℃) are carried out for 1.5 hours, and then a reaction product is filtered to obtain a high-purity nickel-cobalt-aluminum sulfate mixed solution;
(c) complexing the high-purity nickel cobalt aluminum sulfate mixed solution obtained in the step (b) with ammonia water with the molar concentration of 2mol/L, and complexing the ammonia water with the high-purity nickel cobalt aluminum sulfate mixed solution with Ni in the high-purity nickel cobalt aluminum sulfate mixed solution2+、Co2+Adding Al3+In a molar ratio of 2: 1, dripping the complex product, the mixed solution of sodium hydroxide and sodium carbonate and corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented into a reaction container with the temperature of 70 ℃ and the molar concentration of 2mol/L ammonia water for reaction, and adding Ni in the mixed solution of the ammonia water and the high-purity nickel cobalt aluminum sulfate in the reaction container2+、Co2+Adding Al3+In a molar ratio of 1: 1, controlling the pH value of the mixed solution in the reaction vessel to be 11.7, and adding the corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution according to the mol [ Al ] of the mixed solution in the reaction vessel3++Co2+]/mol[Al3++Co2++Ni2+]And (3) calculating the content of the alpha-spherical nickel to be 15 percent, and preparing the alpha-spherical nickel by standing, aging, filtering, washing and drying the reaction product, wherein the standing, aging, filtering, washing and drying processes are carried out according to the standing, aging, filtering, washing and drying processes in the existing preparation of the alpha-spherical nickel.
In the step (c), a mixed solution of sodium hydroxide and sodium carbonate is prepared in advance, and the preparation process comprises the following specific steps: adding 3g of sodium carbonate solid into 100ml of 1mol/L sodium hydroxide solution, and uniformly mixing to obtain the sodium hydroxide and sodium carbonate mixed solution.
Example 2
The steps of the method for preparing the alpha spherical nickel by recycling the waste nickel-metal hydride batteries are basically the same as the steps of the method for preparing the alpha spherical nickel by recycling the waste nickel-metal hydride batteries in the embodiment 1, and the difference is that:
1. in the step (a), the weight of the carbon powder is 10% of the weight of the waste nickel-hydrogen battery, the temperature of the heat treatment equipment is 600 ℃, and the heat treatment time is controlled to be 6 hours;
2. in the step (b), the sulfate solution containing nickel, cobalt, manganese and aluminum ions obtained in the step (a) is heated to 80 ℃, and the heat preservation time is controlled to be 4 hours;
3. in the step (c), the ammonia water complexed with the high-purity nickel cobalt aluminum sulfate mixed solution and Ni in the high-purity nickel cobalt aluminum sulfate mixed solution2+、Co2+Adding Al3+In a molar ratio of 3:1, Ni in the mixed solution of ammonia water and high-purity nickel-cobalt-aluminum sulfate in a reaction vessel2+、Co2+Adding Al3+In a molar ratio of 0.5: 1, the molar concentrations of ammonia water complexed with a high-purity nickel-cobalt-aluminum sulfate mixed solution and ammonia water filled in a reaction container are both 0.5 mol/L; the amount of the corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented is determined according to the mol [ Al ] of the mixed solution in the reaction vessel3++Co2+]/mol[Al3++Co2++Ni2+]The temperature of the reaction vessel is 55 ℃ and the PH of the mixed solution in the reaction vessel is controlled to be 11.8 when the concentration is 20 percent; the preparation process of the mixed solution of sodium hydroxide and sodium carbonate comprises the following specific steps: adding 6g of sodium carbonate solid into 100ml of 3mol/L sodium hydroxide solution, and uniformly mixing to obtain the sodium hydroxide and sodium carbonate mixed solution.
Claims (3)
1. A method for preparing alpha spherical nickel by recycling waste nickel-hydrogen batteries is characterized by comprising the following steps: the method comprises the following steps of (1),
(a) carrying out heat treatment on the waste nickel-metal hydride battery and carbon powder, crushing, sieving to obtain active substance powder, leaching the active substance powder with hydrogen peroxide and sulfuric acid, and filtering to obtain a sulfate solution containing nickel, cobalt, manganese and aluminum ions; the effective carbon content of the carbon powder is more than 80%, and the using amount of the carbon powder is 5-10% of the weight of the waste nickel-hydrogen battery;
(b) heating the sulfate solution containing nickel, cobalt, manganese and aluminum ions obtained in the step (a) to 80-98 ℃, adding a potassium permanganate solution and a sodium sulfate solution into the sulfate solution, controlling the pH value of the reaction solution to be not more than 3.5 by adding a sodium hydroxide solution or/and a sodium carbonate solution, stirring and preserving heat, and filtering the reaction product to obtain a high-purity nickel-cobalt-aluminum sulfate mixed solution; mn in potassium permanganate and sulfate solution containing nickel, cobalt, manganese and aluminum ions2+Adding Fe2+The molar ratio of the sodium sulfate to the sulfate solution containing nickel, cobalt, manganese and aluminum ions is 13:15, and Re is contained in the sulfate solution2+The molar ratio of (1) to (3) is controlled to be 2:3, and the heat preservation time is controlled to be 1-4 h;
(c) complexing the high-purity nickel-cobalt-aluminum sulfate mixed solution obtained in the step (b) with ammonia water, then respectively dropwise adding the complex product, the mixed solution of sodium hydroxide and sodium carbonate and corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented into a reaction container which is at the temperature of 55-70 ℃ and is filled with ammonia water for reaction, wherein the pH value of the mixed solution in the reaction container is controlled to be 11.7-11.8, and standing, aging, filtering, washing and drying the reaction product to obtain alpha spherical nickel;
in the step (c), the ammonia water complexed with the high-purity nickel cobalt aluminum sulfate mixed solution and Ni in the high-purity nickel cobalt aluminum sulfate mixed solution2+、Co2+Adding Al3+The molar ratio of (A) to (B) is 2-3: 1, Ni in the mixed solution of ammonia water and high-purity nickel-cobalt-aluminum sulfate in a reaction vessel2+、Co2+Adding Al3+In a molar ratio of 0.5 to 1: 1, the molar concentrations of ammonia water complexed with a high-purity nickel-cobalt-aluminum sulfate mixed solution and ammonia water filled in a reaction container are both 0.3-2 mol/L; the amount of the corresponding nickel sulfate, cobalt sulfate or/and aluminum sulfate solution to be supplemented is determined according to the mol [ Al ] of the mixed solution in the reaction vessel3++Co2+]/mol[Al3++Co2++Ni2+]Calculated as 15-20%.
2. The method for preparing alpha spherical nickel by recycling waste nickel-metal hydride batteries as claimed in claim 1, wherein the method comprises the following steps: in the step (c), the preparation process of the mixed solution of sodium hydroxide and sodium carbonate comprises the following specific steps: adding 2-6 g of sodium carbonate solid into 100ml of 1-3 mol/L sodium hydroxide solution, and uniformly mixing to obtain a sodium hydroxide and sodium carbonate mixed solution.
3. The method for preparing alpha spherical nickel by recycling waste nickel-metal hydride batteries as claimed in claim 1 or 2, wherein the method comprises the following steps: in the step (a), the heat treatment process specifically comprises the following steps: and (3) placing the waste nickel-metal hydride battery and the carbon powder in heat treatment equipment at 400-600 ℃ for 2-6 h.
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| CN113789447B (en) * | 2021-08-31 | 2022-11-15 | 广东邦普循环科技有限公司 | Method for recovering nickel in iron-aluminum slag obtained by leaching battery powder |
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| CN103288145B (en) * | 2013-05-30 | 2015-02-25 | 先进储能材料国家工程研究中心有限责任公司 | Method for preparing spherical alpha-nickel hydroxide |
| JP6287970B2 (en) * | 2014-10-30 | 2018-03-07 | 住友金属鉱山株式会社 | Nickel composite hydroxide and production method thereof |
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