CN112374548A - Method for treating high-iron material containing nickel-cobalt-manganese hydroxide - Google Patents
Method for treating high-iron material containing nickel-cobalt-manganese hydroxide Download PDFInfo
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Abstract
The invention discloses a method for treating a nickel-cobalt-manganese-containing hydroxide high-iron material, which comprises the following steps of: s1, preparing the nickel-cobalt-manganese-containing hydroxide high-iron material into slurry; s2, injecting a sulfuric acid solution to dissolve the slurry; s3, adding sodium hypochlorite; s4, adding a sodium hydroxide solution; s5, performing solid-liquid separation, and obtaining a filtrate which is the nickel-cobalt-manganese sulfate raw material. The advantages are that: 1. the method has simple and convenient process, short treatment flow and low treatment technical difficulty, has the treatment period of about 1 ton/day, and is suitable for being popularized and used by common nickel-cobalt-manganese hydroxide manufacturing enterprises. 2. The treatment facility is simple, only uses miniature PP material dissolving kettle, pressure filter and supporting acid-base storage tank can satisfy the operation requirement, and the place suitability is strong. 3. The treatment cost is about 1.2 ten thousand yuan/ton calculated by cobalt, and the treatment cost is low. 4. Oil intake is not involved, and impurities which can influence the production and quality of the ternary precursor are not introduced into the system.
Description
Technical Field
The invention relates to the field of lithium ion battery production, in particular to a nickel-cobalt-manganese ternary precursor production technology.
Background
The magnetic foreign body index of the nickel-cobalt-manganese hydroxide product mainly relates to the product safety, and the source of the magnetic foreign body index mainly has 3 approaches: raw and auxiliary materials, production equipment and an operating environment. In order to control the content of magnetic foreign matters in the product, a demagnetizing device is added in the rear end production process, and when the material passes through the demagnetizing device, the magnetic material is adsorbed and separated by the demagnetizing device. The material is mostly a normal material containing nickel-cobalt-manganese hydroxide, and secondly a magnetic material containing high iron, so that the material is called a high-iron material containing nickel-cobalt-manganese hydroxide.
With the capacity expansion of precursor materials and the stricter control requirement of magnetic foreign body indexes, the quantity of high iron materials containing nickel, cobalt and manganese hydroxides is also increasing. The prior treatment method is to utilize the nickel-cobalt-manganese-containing hydroxide high-iron material and other wastes after slurrying and dissolving, extraction, impurity removal and purification. The method has the following defects:
1. the method has the advantages of complex process, about 1 ton/week of treatment period, long treatment process and relatively high treatment technical difficulty.
2. The extraction box equipment grading system is complex, the requirement on a production site is high, and the occupied area of the equipment is generally large.
3. The treatment cost is about 4.2 ten thousand yuan/ton in comparison with cobalt, and the treatment cost is relatively high.
4. The method uses a large amount of organic processing materials, so that the processed mixed solution is mixed with oil and is not beneficial to the generation of nickel-cobalt-manganese hydroxide.
Disclosure of Invention
In order to reduce the treatment cost of the high-iron material containing the nickel-cobalt-manganese hydroxide and simplify the treatment process, the invention provides a treatment method of the high-iron material containing the nickel-cobalt-manganese hydroxide.
The technical scheme adopted by the invention is as follows: the method for treating the nickel-cobalt-manganese-containing hydroxide high-iron material comprises the following steps:
s1, preparing the nickel-cobalt-manganese-containing hydroxide high-iron material into slurry;
s2, injecting a sulfuric acid solution into the slurry to dissolve the slurry to obtain a first solution;
s3, adding sodium hypochlorite into the first solution for oxidation to obtain a second solution;
s4, adding a sodium hydroxide solution into the second solution to adjust the pH value to 3-4, and then stirring and preserving heat for more than 30min to obtain a third solution;
s5, carrying out solid-liquid separation on the third solution to obtain filter residue and filtrate, wherein the filtrate is the nickel-cobalt-manganese sulfate raw material;
and S6, using the nickel-cobalt-manganese sulfate raw material as a nickel-cobalt-manganese ternary precursor production raw material.
The key to the treatment of the high-iron material containing nickel-cobalt-manganese hydroxide is how to remove impurities therein which affect the production or performance of the precursor without introducing new impurities, and simultaneously, the feasibility on cost is considered. In contrast, the inventor provides the treatment method, and experiments prove that the method can remove impurities which mainly comprise iron ions and affect the production or performance of the precursor in the high-iron material containing the nickel-cobalt-manganese hydroxide, the impurity content of the product can completely meet the production requirement of the ternary precursor, and the treatment cost is low. Although this method requires the addition of sodium hypochlorite and sodium hydroxide to the system and thus introduces sodium ions and hypochlorite into the system. However, a large amount of sodium hydroxide alkaline precipitator is required to be added when the coprecipitation method is adopted to produce the ternary precursor, so that the introduced sodium ions cannot cause any influence on the product quality; hypochlorite is completely reduced into chloride ions in the oxidation reduction process, the chloride ions do not influence the precipitation reaction of nickel, cobalt and manganese hydroxides, and the hypochlorite ions are discharged into industrial wastewater in a washing process and do not influence the quality of downstream products. Therefore, the method introduces new impurities, but the introduced impurities are just impurities which do not influence the synthesis and quality of the ternary precursor, so the impurities can be directly utilized without retreatment, and the method is ingenious.
In the scheme, the product quality is influenced by excessive sodium hypochlorite or incomplete oxidation reaction, and for this reason, the usage amount of the sodium hypochlorite can be determined in the step S3 according to the following method: and (3) moving a proper amount of the second solution into a detection container by using a pipette, adding an iron ion detection reagent, dripping a diphenylamine sodium sulfonate reagent, stopping adding sodium hypochlorite if the solution is purple, and otherwise, continuously adding the sodium hypochlorite. In actual production, the method of detecting can be carried out through continuous sampling, so that the addition of sodium hypochlorite is stopped in time to prevent the excessive reagent and ensure the complete oxidation reaction.
The iron ion detection reagent can be prepared by the following method: after 500ml of water was added to a 2000ml beaker, 150ml of concentrated sulfuric acid was slowly added while stirring with a glass rod, and then 150ml of concentrated phosphoric acid was added thereto, and then the solution was diluted to 1000ml with water and mixed well.
The sodium diphenylamine sulfonate reagent can be prepared by the following method: 0.5g of sodium diphenylamine sulfonate is weighed and put into a 250ml beaker, 100ml of water is added for dissolving, and then 5 drops of concentrated sulfuric acid are dripped into the beaker for mixing.
As a further improvement of the present invention, the slurry of step S1 is prepared according to the following method: adding the nickel-cobalt-manganese-containing hydroxide high-iron material into hot pure water at the temperature of 70-90 ℃, and uniformly stirring.
As a further improvement of the invention, the mass concentration of the sulfuric acid solution in the step S2 is 40-45%.
As a further improvement of the invention, step S5 uses a 8000-mesh filter press to carry out filter pressing washing, so as to realize solid-liquid separation, and filter residues can be used as cement production raw materials.
The invention has the beneficial effects that: 1. the method has simple and convenient process, short treatment flow and low treatment technical difficulty, has the treatment period of about 1 ton/day, and is suitable for being popularized and used by common nickel-cobalt-manganese hydroxide manufacturing enterprises. 2. The treatment facility is simple, only uses miniature PP material dissolving kettle, pressure filter and supporting acid-base storage tank can satisfy the operation requirement, and the place suitability is strong. 3. The treatment cost is about 1.2 ten thousand yuan/ton calculated by cobalt, and the treatment cost is low. 4. Oil intake is not involved, and impurities which can influence the production and quality of the ternary precursor are not introduced into the system.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The first embodiment is as follows:
the nickel-cobalt-manganese-containing hydroxide high-iron material is treated according to the following method:
s1, confirmation of 5m3The integrity of the dissolving kettle and the accessories of the solution overflow conduit, the sulfuric acid, the pure water and the like are smooth.
S2, adding about 1m into the kettle3The stirring was started, and 250kg of a nickel-containing cobalt-manganese hydroxide high-iron material was slowly added from the vessel mouth to conduct slurrying.
And S3, after slurrying is finished, starting a concentrated sulfuric acid injection pump, slowly injecting concentrated sulfuric acid with the mass concentration of 45% at the speed of 200L/h, observing the boiling state of the dissolution kettle, and preventing the slurry from overflowing the dissolution kettle until the slurry is completely dissolved.
S4, after the dissolution is finished, overflowing the solution to an oxidation tank, keeping the temperature at 70-90 ℃, adding a proper amount of sodium hypochlorite, continuously transferring the proper amount of solution to a detection container by using a pipette, adding an iron ion detection reagent, and verifying whether the reaction end point is reached or not by dropping a diphenylamine sodium sulfonate reagent; the addition of sodium hypochlorite was stopped until the solution just appeared purple. The iron ion detection reagent is prepared according to the following method: after 500ml of water was added to a 2000ml beaker, 150ml of concentrated sulfuric acid having a mass concentration of 98% was slowly added while stirring with a glass rod, 150ml of concentrated phosphoric acid having a mass concentration of 85% was then added, and water was added to dilute the solution to 1000ml and mix it. The sodium diphenylamine sulfonate reagent is prepared by the following method: 0.5g of sodium diphenylamine sulfonate is weighed and put into a 250ml beaker, 100ml of water is added for dissolving, and then 5 drops of concentrated sulfuric acid with the mass concentration of 98 percent are dripped into the beaker for uniformly mixing.
S5, slowly injecting a sodium hydroxide solution with the mass concentration of 30%, adjusting the pH of the solution to 3.6, allowing a precipitate to appear, and stirring for 1 hour under heat preservation.
S6, pumping the mixed solution of nickel, cobalt and manganese sulfates containing the slag into a 8000-mesh filter press at a constant speed for filter pressing and washing, collecting the filtrate for recycling, and separately collecting the filter pressing residue which can be used as a cement raw material.
S7, detecting the components of the filtrate obtained in the step S6, and the result is shown in Table 1.
Example two:
the nickel-cobalt-manganese-containing hydroxide high-iron material is treated according to the following method:
s1, confirmation of 10m3The integrity of the dissolving kettle and the accessories of the solution overflow conduit, the sulfuric acid, the pure water and the like are smooth.
S2, adding about 3m into the kettle3The stirring is started, and 750kg of nickel-containing cobalt-manganese hydroxide high-iron material is slowly added from the kettle mouth for slurrying.
And S3, after slurrying is finished, starting a concentrated sulfuric acid injection pump, slowly injecting concentrated sulfuric acid with the mass concentration of 45% at the speed of 200L/h, observing the boiling state of the dissolution kettle, and preventing the slurry from overflowing the dissolution kettle until the slurry is completely dissolved.
S4, after the dissolution is finished, overflowing the solution to an oxidation tank, keeping the temperature at 70-90 ℃, adding a proper amount of sodium hypochlorite, continuously transferring the proper amount of solution to a detection container by using a pipette, adding an iron ion detection reagent, and verifying whether the reaction end point is reached or not by dropping a diphenylamine sodium sulfonate reagent; the addition of sodium hypochlorite was stopped until the solution just appeared purple. The iron ion detection reagent is prepared according to the following method: after 500ml of water was added to a 2000ml beaker, 150ml of concentrated sulfuric acid having a mass concentration of 98% was slowly added while stirring with a glass rod, 150ml of concentrated phosphoric acid having a mass concentration of 85% was then added, and water was added to dilute the solution to 1000ml and mix it. The sodium diphenylamine sulfonate reagent is prepared by the following method: 0.5g of sodium diphenylamine sulfonate is weighed and put into a 250ml beaker, 100ml of water is added for dissolving, and then 5 drops of concentrated sulfuric acid with the mass concentration of 98 percent are dripped into the beaker for uniformly mixing.
S5, slowly injecting a sodium hydroxide solution with the mass concentration of 30%, adjusting the pH of the solution to 3.8, allowing a precipitate to appear, and stirring for 1.5 hours under the condition of heat preservation.
S6, pumping the mixed solution of nickel, cobalt and manganese sulfates containing the slag into a 8000-mesh filter press at a constant speed for filter pressing and washing, collecting the filtrate for recycling, and separately collecting the filter pressing residue which can be used as a cement raw material.
S7, detecting the components of the filtrate obtained in the step S6, and the result is shown in Table 1.
Example three:
the nickel-cobalt-manganese-containing hydroxide high-iron material is treated according to the following method:
s1, confirmation of 10m3The integrity of the dissolving kettle and the accessories of the solution overflow conduit, the sulfuric acid, the pure water and the like are smooth.
S2, adding about 5m into the kettle3The stirring is started, and 1250kg of nickel-containing cobalt-manganese hydroxide high-iron material is slowly added from the kettle mouth for slurrying.
And S3, after slurrying is finished, starting a concentrated sulfuric acid injection pump, slowly injecting concentrated sulfuric acid with the mass concentration of 45% at the speed of 200L/h, observing the boiling state of the dissolution kettle, and preventing the slurry from overflowing the dissolution kettle until the slurry is completely dissolved.
S4, after the dissolution is finished, overflowing the solution to an oxidation tank, keeping the temperature at 70-90 ℃, adding a proper amount of sodium hypochlorite, continuously transferring the proper amount of solution to a detection container by using a pipette, adding an iron ion detection reagent, and verifying whether the reaction end point is reached or not by dropping a diphenylamine sodium sulfonate reagent; the addition of sodium hypochlorite was stopped until the solution just appeared purple. The iron ion detection reagent is prepared according to the following method: after 500ml of water was added to a 2000ml beaker, 150ml of concentrated sulfuric acid having a mass concentration of 98% was slowly added while stirring with a glass rod, 150ml of concentrated phosphoric acid having a mass concentration of 85% was then added, and water was added to dilute the solution to 1000ml and mix it. The sodium diphenylamine sulfonate reagent is prepared by the following method: 0.5g of sodium diphenylamine sulfonate is weighed and put into a 250ml beaker, 100ml of water is added for dissolving, and then 5 drops of concentrated sulfuric acid with the mass concentration of 98 percent are dripped into the beaker for uniformly mixing.
S5, slowly injecting a sodium hydroxide solution with the mass concentration of 50%, adjusting the pH of the solution to 3.6, allowing a precipitate to appear, and stirring for 2 hours under the condition of heat preservation.
S6, pumping the mixed solution of nickel, cobalt and manganese sulfates containing the slag into a 8000-mesh filter press at a constant speed for filter pressing and washing, collecting the filtrate for recycling, and separately collecting the filter pressing residue which can be used as a cement raw material.
S7, detecting the components of the filtrate obtained in the step S6, and the result is shown in Table 1.
The detection method comprises the following steps:
detecting the components of the treated filtrate
(1) The detection of the total amount of Ni, Co and Mn refers to the No. 1 chemical analysis method of nickel cobalt lithium manganate according to the colored industry standard YS/T1006.1-2014: determination of the total amount of nickel, cobalt and manganese by EDTA titration.
(2) The determination of Ni, Co and Mn components refers to the colored industry standard YS/T928.3-2013 chemical analysis method of nickel, cobalt and manganese three-element hydroxide part 3, namely the determination of the amounts of nickel, cobalt and manganese by inductively coupled plasma atomic emission spectrometry.
(3) And (4) detecting impurities Fe, Cu, Ca, Mg, Zn, Si and Al according to a colored industry standard YS/T928.4-2013 chemical analysis method for nickel, cobalt and manganese three-element hydroxides, namely a method for measuring the amounts of iron, calcium, magnesium, copper, zinc, silicon, aluminum and sodium by inductively coupled plasma atomic emission spectrometry.
(4) The impurity Pb is determined according to a non-ferrous industry standard YS/T928.5-2013 chemical analysis method for nickel, cobalt and manganese three-element hydroxide, part 5, namely, the determination of lead content by inductively coupled plasma mass spectrometry.
TABLE 1 ingredient test results Table (g/L)
Total amount of NiCoMn | Ni | Co | Mn | Cu | Fe | |
Example one filtrate | 142.37 | 90.75 | 22.60 | 31.18 | ND | 0.0032 |
EXAMPLE two filtrates | 107.73 | 59.78 | 18.69 | 30.52 | ND | 0.0042 |
EXAMPLE three filtrates | 123.34 | 69.64 | 21.35 | 33.58 | ND | 0.0029 |
Ca | Mg | Zn | Si | Al | Pb | |
Example one filtrate | 0.0043 | 0.0050 | ND | 0.0005 | 0.0008 | ND |
EXAMPLE two filtrates | 0.0035 | 0.0019 | ND | 0.0009 | 0.0035 | ND |
EXAMPLE three filtrates | 0.0028 | 0.0033 | ND | 0.0007 | 0.0022 | ND |
Claims (8)
1. The method for treating the nickel-cobalt-manganese-containing hydroxide high-iron material comprises the following steps:
s1, preparing the nickel-cobalt-manganese-containing hydroxide high-iron material into slurry;
s2, injecting a sulfuric acid solution into the slurry to dissolve the slurry to obtain a first solution;
s3, adding sodium hypochlorite into the first solution for oxidation to obtain a second solution;
s4, adding a sodium hydroxide solution into the second solution to adjust the pH value to 3-4, and then stirring and preserving heat for more than 30min to obtain a third solution;
s5, carrying out solid-liquid separation on the third solution to obtain filter residue and filtrate, wherein the filtrate is the nickel-cobalt-manganese sulfate raw material;
and S6, using the nickel-cobalt-manganese sulfate raw material as a nickel-cobalt-manganese ternary precursor production raw material.
2. The method for treating a nickel-cobalt-manganese-containing hydroxide high-iron material according to claim 1, wherein the amount of sodium hypochlorite used in step S3 is determined as follows: and (3) moving a proper amount of the second solution into a detection container by using a pipette, adding an iron ion detection reagent, dripping a diphenylamine sodium sulfonate reagent, stopping adding sodium hypochlorite if the solution is purple, and otherwise, continuously adding the sodium hypochlorite.
3. The method for treating the nickel-containing cobalt manganese hydroxide high-iron material according to claim 2, wherein the iron ion detection reagent is prepared according to the following method: after 500ml of water was added to a 2000ml beaker, 150ml of concentrated sulfuric acid was slowly added while stirring with a glass rod, and then 150ml of concentrated phosphoric acid was added thereto, and then the solution was diluted to 1000ml with water and mixed well.
4. The method for treating the nickel-cobalt-manganese-containing hydroxide high-iron material according to claim 2, wherein the sodium diphenylamine sulfonate reagent is prepared according to the following method: 0.5g of sodium diphenylamine sulfonate is weighed and put into a 250ml beaker, 100ml of water is added for dissolving, and then 5 drops of concentrated sulfuric acid are dripped into the beaker for mixing.
5. The method for treating the nickel-containing cobalt manganese hydroxide high-iron material according to any one of claims 1 to 4, wherein the slurry in step S1 is prepared according to the following method: adding the nickel-cobalt-manganese-containing hydroxide high-iron material into hot pure water at the temperature of 70-90 ℃, and uniformly stirring.
6. The method for treating a nickel-cobalt-manganese-containing hydroxide high-iron material according to any one of claims 1 to 4, characterized in that: the mass concentration of the sulfuric acid solution in the step S2 is 40-45%.
7. The method for treating a nickel-cobalt-manganese-containing hydroxide high-iron material according to any one of claims 1 to 4, characterized in that: and step S5, performing filter pressing and washing by using a 8000-mesh filter press to realize solid-liquid separation.
8. The method for treating a nickel-cobalt-manganese-containing hydroxide high-iron material according to any one of claims 1 to 4, characterized in that: and taking the filter residue as a cement production raw material.
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