CN111559764B - Dezincification inducer, preparation method and application thereof, and dezincification method in nickel-cobalt-manganese sulfate solution - Google Patents
Dezincification inducer, preparation method and application thereof, and dezincification method in nickel-cobalt-manganese sulfate solution Download PDFInfo
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- CN111559764B CN111559764B CN202010677463.7A CN202010677463A CN111559764B CN 111559764 B CN111559764 B CN 111559764B CN 202010677463 A CN202010677463 A CN 202010677463A CN 111559764 B CN111559764 B CN 111559764B
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- C01—INORGANIC CHEMISTRY
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- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
Abstract
The invention provides a zinc removal inducer, a preparation method and application thereof, and a method for removing zinc from a nickel-cobalt-manganese-sulfuric acid solution. The main components of the zinc removal inducer comprise iron oxyhydroxide and aluminum hydroxide, and under the action of the zinc removal inducer, zinc is adsorbed and precipitated in the precipitation process by utilizing the adsorption effect of goethite and aluminum hydroxide, and meanwhile, coprecipitation is generated to remove zinc from the solution. The method can be carried out in a pure sulfuric acid system without adding other anions, the process operation is simple, the production flow is short, and the generated slag can be recycled.
Description
Technical Field
The invention relates to the technical field of solution purification and impurity removal, in particular to a zinc removal inducer and a method for removing zinc from a nickel-cobalt-manganese sulfate solution.
Background
The nickel-cobalt-manganese ternary lithium ion battery has the advantages of high specific capacity, good safety, good cycling stability and the like, and is widely applied to the fields of notebook computers, digital equipment, electric bicycles and the like. The nickel cobalt manganese sulfate solution is generally generated by leaching the anode of a lithium ion battery or a corresponding wet-process intermediate product, and the leachate contains a large amount of zinc, iron, aluminum, calcium, magnesium and the like, wherein the iron and the aluminum are removed by an alum forming method, the calcium and the magnesium can be removed by a sodium fluoride method, and the process method is applied and relatively mature. The zinc removing method mainly comprises a hydrogen sulfide precipitation method, an extraction method, an anion exchange method, a ferrite coprecipitation method and an alkali salt precipitation method. The method is applied to actual production, but the treatment difficulty is high, and the condition control is limited. For example, the hydrogen sulfide precipitation method has great operation difficulty and great risk because hydrogen sulfide gas is used; the extraction method generally adopts P204 for extraction, and because an organic solvent is used, the TOC content in a solution is higher, and the treatment process and the treatment difficulty are increased; the anion exchange method has high operation requirements, the treatment difficulty of the regenerated liquid is high, the capacity is limited, and the one-time investment is large; although the ferrite coprecipitation method is simple to operate, chloride ions need to be added, secondary pollution is brought to the solution, and the use of the solution is greatly limited; the basic salt precipitation method is particularly easy to carry out by using the conversion of basic salt of copper, zinc and corresponding anions can be removed from wastewater by using the conversion reaction of the basic salt, but the reaction needs to be carried out in a hydrochloride solution.
Disclosure of Invention
Aiming at the problems in the prior art, the direct research on a simple and feasible zinc removal method is a problem for the technicians in the field. The technical problem to be solved by the invention is as follows: provides an economic, practical and effective zinc removal inducer and a preparation method thereof, and provides a zinc removal method in a nickel-cobalt-manganese sulfate solution with convenient operation, simple flow and good zinc removal effect.
The solution of the invention is realized by the following steps:
the alkali used in the present invention refers to a hydroxide and/or a carbonate.
A dezincification inducer is called as No. 1 dezincification inducer for the convenience of expression, and mainly comprises iron oxyhydroxide and aluminum hydroxide, wherein the mass ratio of the aluminum hydroxide to the iron oxyhydroxide is 1: 4-14.
The preparation method of the No. 1 dezincification inducer comprises the following steps: sulfate or chloride or nitrate of aluminum and ferrous iron is mixed according to the mass ratio of 1: 3-10, heating to 85-90 ℃, adjusting the pH value of the solution to 5.5-6.5 by alkali, reacting for 1-4 hours, filtering and washing to obtain the product.
The reaction principle is as follows:
Fe2++O2+H2O→FeOOH↓+H+
H++OH-→H2O
H++CO3 2-→CO2↑+H2O
Al3++OH-→Al(OH)3↓
based on the same inventive concept, the invention also provides a zinc removal inducer, which is called as No. 2 zinc removal inducer for convenient expression and mainly comprises iron oxyhydroxide, aluminum hydroxide, hydroxide of nickel, cobalt or manganese and/or carbonate; the No. 2 dezincification inducer comprises the following components in percentage by mass: aluminum hydroxide: hydroxide and/or carbonate of nickel, cobalt or manganese ═ 1: 0.1-0.4: 1.5-5.5. The preparation method comprises the following steps: the preparation method comprises the following steps of (1) mixing ferrous iron, aluminum, and sulfate or chloride or nitrate of nickel or cobalt or manganese in a mass ratio of 1: 0.1-0.3: 1-3, heating to 85-90 ℃, adjusting the pH value of the solution to 7.5-8.5 by alkali, reacting for 1-4 hours, filtering and washing to obtain the product.
The reaction principle is as follows:
Fe2++O2+H2O→FeOOH↓+H+
H++OH-→H2O
H++CO3 2-→CO2↑+H2O
Al3++OH-→Al(OH)3↓
Ni2++OH-→Ni(OH)2↓
Ni2++CO3 2-→NiCO3↓
based on the same inventive concept, the zinc removal inducer is used for removing zinc in the nickel-cobalt-manganese sulfate solution.
In addition, the invention provides a method for removing zinc from a nickel-cobalt-manganese sulfate solution, which uses the zinc removal inducer, and specifically comprises the following steps:
step S1, ferrous sulfate is supplemented to the nickel-cobalt-manganese sulfate solution to ensure that the concentration of ferrous ions in the solution is 100-500 mg/L;
step S2, on the basis of the step S1, the temperature of the nickel-cobalt-manganese sulfate solution is raised to 75-100 ℃, and then the temperature is increased by every 1m3Adding 5-30kg No. 2 dezincification inducer into the solution, and reacting for 1-3 hours;
the main chemical reactions taking place in step S2 are as follows:
Ni(OH)2+H+→Ni2++H2O
NiCO3+H+→Ni2++CO2↑+H2O
Al(OH)3+H+→Al3++H2O
Fe2++O2+H2O→FeOOH↓+H+
step S3, keeping the temperature of the solution at 85-95 deg.C, adjusting the pH of the solution to 4.5-5.5 with alkali, and adding water at a ratio of 1m3Adding 5-15kg No. 1 dezincification inducer into the solution, and reacting for 1-3 hours;
the main chemical reaction in step S3 is as follows:
H++OH-→H2O
H++CO3 2-→CO2↑+H2O
Al3++OH-→Al(OH)3↓
Ni2++OH-→Ni(OH)2↓
Ni2++CO3 2-→NiCO3↓
Zn2++OH-→Zn(OH)2↓
Zn2++CO3 2-→ZnCO3↓
step S4, keeping the temperature of the solution at 85-95 deg.C, adjusting the pH value of the solution to 5.5-6.5 with alkali, and measuring the volume of the solution to 1m3Adding No. 1 dezincification inducer 1-5kg, reacting for 1-3 hours;
the main chemical reaction in step S4 is as follows:
H++OH-→H2O
H++CO3 2-→CO2↑+H2O
Al3++OH-→Al(OH)3↓
Ni2++OH-→Ni(OH)2↓
Ni2++CO3 2-→NiCO3↓
Zn2++OH-→Zn(OH)2↓
Zn2++CO3 2-→ZnCO3↓
and step S5, performing filter pressing and washing to obtain the zinc-removed nickel-cobalt-manganese sulfuric acid solution.
According to the technical scheme, other anions are not added in the nickel-cobalt-manganese sulfate solution, under the action of the zinc removal inducer, the zinc is adsorbed and precipitated in the precipitation process by utilizing the adsorption effect of goethite and aluminum hydroxide, and the zinc is removed from the solution by coprecipitation. The zinc-removing inducer has the function of generating a certain amount of seed crystals in the solution to promote the coprecipitation reaction, and the nickel (or cobalt, manganese) compound in the inducer can be neutralized in the opposite directionH evolved in reaction+No additional alkali is required.
The method can be carried out in a pure sulfuric acid system without adding other anions, the process operation is simple, the production flow is short, and the zinc in the purified solution is less than 5 mg/L.
Detailed Description
Example 1:
(1) preparation of zinc removal inducer
No. 1 dezincification inducer: 10kg of aluminum sulfate and 20kg of ferrous sulfate are added into a reaction tank with stirring, and pure water is added and stirred until the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 6.3, and reacting for 2 hours under the condition of heat preservation. The zinc removal inducer 22.42kg is obtained after filtration and washing.
No. 2 dezincification inducer: 15kg of nickel sulfate, 4.5kg of aluminum sulfate and 15kg of ferrous sulfate are added into a reaction tank with a stirrer, and pure water is added and stirred until the nickel sulfate, the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 8.3, and reacting for 2 hours under the condition of heat preservation. After filtration and washing, 20.34kg of the dezincification inducer is obtained.
(2) Dezincing operation
S1, 1m3The solution of nickel, cobalt and manganese in sulfuric acid, supplemented with 0.2kg of ferrous sulfate, was measured to have the following impurities:
Fe2+:137.2mg/L、Al：2.1 mg/L、Zn:293.4 mg/L。
s2, heating the solution to 90 ℃, adding 18kg of No. 2 dezincification inducer, and reacting for 2 hours.
S3, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 5.0 by alkali, adding 15kg of No. 1 dezincification inducer, and reacting for 2 hours.
S4, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 6.1 by alkali, adding 5kg of No. 1 dezincification inducer, and reacting for 2 hours.
S5, and performing filter pressing washing.
(3) Sampling and measuring the impurities of the solution after zinc removal as follows:
Fe:2.2mg/L、Al：3.5 mg/L、Zn:4.4 mg/L。
example 2:
(1) preparation of zinc removal inducer
No. 1 dezincification inducer: 10kg of aluminum sulfate and 20kg of ferrous sulfate are added into a reaction tank with stirring, and pure water is added and stirred until the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 5.9, and reacting for 2 hours under the condition of heat preservation. After filtration and washing, 21.27kg of the dezincification inducer is obtained.
No. 2 dezincification inducer: 15kg of nickel sulfate, 4.5kg of aluminum sulfate and 15kg of ferrous sulfate are added into a reaction tank with a stirrer, and pure water is added and stirred until the nickel sulfate, the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 8.8, and reacting for 2 hours under the condition of heat preservation. After filtration and washing, 21.05kg of the dezincification inducer is obtained.
(2) Dezincing operation
S1, 1m3The solution of nickel, cobalt and manganese in sulfuric acid, supplemented with 0.2kg of ferrous sulfate, was measured to have the following impurities:
Fe2+:173.7mg/L、Al：5.7 mg/L、Zn:144.3 mg/L。
s2, heating the solution to 90 ℃, adding 20kg of No. 2 dezincification inducer, and reacting for 2 hours.
S3, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 4.5 by alkali, adding 15kg of No. 1 dezincification inducer, and reacting for 2 hours.
S4, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 6.3 by alkali, adding 5kg of No. 1 dezincification inducer, and reacting for 2 hours.
S5, and performing filter pressing washing.
(3) Sampling and measuring the impurities of the solution after zinc removal as follows:
Fe:3.2mg/L、Al：1.5 mg/L、Zn:3.1 mg/L。
example 3:
(1) preparation of zinc removal inducer
No. 1 dezincification inducer: 10kg of aluminum sulfate and 20kg of ferrous sulfate are added into a reaction tank with stirring, and pure water is added and stirred until the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 5.9, and reacting for 2 hours under the condition of heat preservation. After filtration and washing, 21.27kg of the dezincification inducer is obtained.
No. 2 dezincification inducer: 15kg of nickel sulfate, 4.5kg of aluminum sulfate and 15kg of ferrous sulfate are added into a reaction tank with a stirrer, and pure water is added and stirred until the nickel sulfate, the aluminum sulfate and the ferrous sulfate are completely dissolved. Heating to 90 ℃, adding a mixture of sodium hydroxide and sodium carbonate to adjust the pH value to 8.8, and reacting for 2 hours under the condition of heat preservation. After filtration and washing, 21.05kg of the dezincification inducer is obtained.
(2) Dezincing operation
S1, 1m3The solution of nickel, cobalt and manganese is supplemented with 0.2kg of ferrous sulfate, and the impurities of the solution are measured as follows:
Fe2+:203.7mg/L、Al：1.7 mg/L、Zn:324.3 mg/L。
s2, heating the solution to 90 ℃, adding 18kg of No. 2 dezincification inducer, and reacting for 2 hours.
S3, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 4.5 by alkali, adding 15kg of No. 1 dezincification inducer, and reacting for 2 hours.
S4, keeping the temperature at 90 ℃, adjusting the pH value of the solution to 6.5 by alkali, adding 5kg of No. 1 dezincification inducer, and reacting for 2 hours.
S5, and performing filter pressing washing.
(3) Sampling and measuring the impurities of the solution after zinc removal as follows:
Fe:0.7mg/L、Al：0.3 mg/L、Zn:1.1 mg/L。
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The dezincification inducer applied to dezincification of a nickel-cobalt-manganese sulfate solution is characterized by consisting of iron oxyhydroxide and aluminum hydroxide, wherein the mass ratio of the aluminum hydroxide to the iron oxyhydroxide is 1: 4-14.
2. The dezincification inducer applied to dezincification of nickel-cobalt-manganese sulfate solution is characterized by consisting of iron oxyhydroxide, aluminum hydroxide and/or carbonate of nickel, cobalt or manganese, and the mass ratio of the components in the dezincification inducer is as follows: aluminum hydroxide: hydroxide and/or carbonate of nickel, cobalt or manganese ═ 1: 0.1-0.4: 1.5-5.5.
3. A method of preparing the dezincification inducer of claim 1, comprising the steps of: sulfate or chloride or nitrate of aluminum and ferrous iron is mixed according to the mass ratio of 1: 3-10, heating to 85-90 ℃, adjusting the pH value of the solution to 5.5-6.5, reacting for 1-4 hours, and then filtering and washing.
4. A method of preparing the dezincification inducer of claim 2, comprising the steps of: sulfate or chloride or nitrate of ferrous iron, aluminum, nickel, cobalt or manganese and the mass ratio of 1: 0.1-0.3: 1-3, dissolving in water, heating to 85-90 deg.C, regulating pH value to 7.5-8.5, reacting for 1-4 hr, filtering and washing.
5. A method for removing zinc from a nickel-cobalt-manganese sulfate solution is characterized by comprising the following steps:
step S1, ferrous sulfate is supplemented into the nickel-cobalt-manganese sulfate solution, so that the concentration of ferrous ions in the solution is 100-500 mg/L;
step S2, on the basis of the step S1, the temperature of the nickel-cobalt-manganese sulfate solution is raised to 75-100 ℃, and the temperature is raised to 1m per step3Adding 5-30kg of the dezincification inducer as defined in claim 2 into the solution, and reacting for 1-3 hours;
step S3, on the basis of step S2, continuously keeping the temperature of the nickel cobalt manganese sulfate solution at 85-95 ℃, and adjusting the pH value of the solution to 4.5-5.5, every 1m3Adding 5-15kg of the dezincification inducer as defined in claim 1 into the solution, and reacting for 1-3 hours;
step S4, based on the step S3, continuously maintaining the temperature of the solution at 85-95 ℃, adjusting the pH value of the solution to 5.5-6.5, and then adding 1m of solution according to the volume of the solution3Adding 1-5kg of the dezincification inducer as defined in claim 1, and reacting for 1-3 hours;
and step S5, performing filter pressing and washing to obtain the nickel-cobalt-manganese sulfate solution and filter residue after zinc removal.
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