50results about "Manganese compounds preparation" patented technology

A method for processing lithium ion battery scrap according to this invention includes a leaching step of leaching lithium ion battery scrap to obtain a leached solution; an aluminum removal step of neutralizing the leached solution to a pH range of from 4.0 to 6.0, then performing solid-liquid separation and removing aluminum in the leached solution to obtain a first separated solution; and an iron removal step of adding an oxidizing agent to the first separated solution and adjusting the pH in a range of from 3.0 to 5.0, then performing solid-liquid separation and removing iron in the first separated solution to obtain a second separated solution.

The invention discloses a method for preparing a high-purity manganese sulfate solution with low cost. The method comprises the following steps: (1) copper removal: obtaining copper-removed raw liquid manganese of which Cu is less than or equal to 0.2g/L; (2) pH value adjustment: adjusting the pH value of the copper-removed raw liquid manganese to be 1.5 to 5.0; (3) saponification: saponifying an extraction agent by using NaOH, Na2CO3, KOH, K2CO3 or ammonium hydroxide, so as to obtain sodium salt, potassium salt or ammonium salt containing the extraction agent; (4) manganese transforming saponification; (5) Mn and Ca extraction separation: making Ca in the raw liquid manganese enter an organic phase to be separated from Mn, and making all or most of Cu, Al, Zn and Cd enter the organic phase, so as to obtain extraction raffinate namely decalcified liquid manganese of which Ca is less than or equal to 5ppm; (6) deep purification: adding Na2S, NaHS, K2S, KHS or (NH4)2S into the decalcified liquid manganese, adjusting the pH value to be 4.0 to 6.0, and performing solid-liquid separation, so as to obtain a high-purity MnSO4 solution satisfying production of a positive precursor of a lithium ion battery.

The invention discloses a method for removing calcium ions from a manganese sulfate solution, and belongs to the technical field of hydrometallurgy. According to the method, a calcium-containing manganese sulfate solution is taken as a raw material, an extraction agent, namely bi(2,4,4trimethylamyl) phosphinic acid, with a certain concentration is taken as an organic phase, a manganese sulfate solution is taken as an aqueous phase and multistage countercurrent extraction is carried out, wherein strip liquor is a relatively-pure manganese sulfate solution with extremely-low impurity content andcan be used for directly preparing a battery grade manganese sulfate product. The organic phase is recycled after being washed and regenerated. The method has the advantages of short process flow, fast onset, low cost, low consumption of auxiliary materials and power, high labor production efficiency, clean production process, no pollution and the like.

The invention provides a preparation method of battery-grade manganese sulfate and belongs to the technical field of hydrometallurgy. The method comprises steps as follows: step one, a manganese sulfate solution is taken as a pre-extraction solution; step two, 400 g/L of sodium hydroxide is added to octocapric acid for saponification; step three, the pre-extraction solution and octocapric acid after saponification are subjected to mixed extraction; step four, 20 g/L of sulfuric acid is pumped into an extraction box to be contacted with an extracted organic phase for the extraction reaction; step five, the extracted organic phase containing manganese ions is subjected to reverse extraction with 20 g/L of sulfuric acid; step six, battery-grade manganese sulfate is obtained. According to the method, the manganese sulfate solution with higher impurity content is enabled to enter an extraction system and the purpose of removing impurities is achieved by extraction, washing and reverse extraction of the solution; the overall technological process avoids chemical purification, chemical calcium removal and chemical magnesium removal processes, so that energy and auxiliary materials are saved, besides, no negative ions such as fluoride ions are introduced, and the requirement for equipment is reduced.

The invention provides a purification treatment method of a manganese sulfate solution. The purification treatment method comprises the following steps: S1, preparing an extraction organic phase, andsaponifying the extraction organic phase to obtain a saponified organic phase; S2, extracting the manganese sulfate solution by using the saponified organic phase to obtain a manganese-rich organic phase; S3, washing the manganese-rich organic phase for the first time by adopting water to obtain a primary purified manganese-rich organic phase; S4, washing the primary purified manganese-rich organic phase for the second time by adopting a manganese-containing strong acid solution to obtain a secondary purified manganese-rich organic phase; and S5, carrying out reverse extraction on the secondary purified manganese-rich organic phase by using sulfuric acid to obtain a high-purity manganese sulfate solution and a regenerated organic phase. According to the method, pure manganese sulfate doesnot need to be adopted for carrying out manganese conversion saponification on the saponification organic phase, and the used washing liquid is cheap water and a manganese-containing strong acid solution, so that the purification treatment cost is relatively low.

The invention discloses a method for recycling a waste lithium battery and preparing a ternary precursor. The method comprises the following steps of pretreating the waste lithium battery to obtain battery powder and aluminum slag, roasting the battery powder, adding water into the roasted battery powder to prepare slurry, adding metal chloride to carry out leaching reaction, and carrying out solid-liquid separation to obtain nickel-cobalt-manganese slag and a lithium chloride solution; adding sulfuric acid into nickel-cobalt-manganese slag for acid leaching, adding aluminum slag into an acid leaching solution to remove copper, adjusting the pH value of the acid leaching solution to remove aluminum, mixing the aluminum-removed solution with a compound extraction agent, extracting to obtain a manganese-containing organic phase and a nickel-cobalt-containing raffinate, wherein the organic phase can be used for preparing manganese sulfate, and the raffinate can be used for preparing a high-purity nickel-cobalt sulfate mixed crystal through crystallization; and after the obtained battery-grade manganese sulfate and nickel-cobalt sulfate mixed crystal is dissolved in water, a certain amount of nickel-cobalt-manganese sulfate is supplemented to prepare a ternary precursor. The recovery process route provided by the invention has the advantages of simplicity in operation, low production cost, stability and reliability.

The invention discloses a method for recovering soluble manganese and ammonium from electrolytic manganese slag. The method comprises the following steps: washing the electrolytic manganese slag withwater to obtain water washing liquid and water washing slag; extracting manganese ions from the water washing liquid by adopting an organic phase containing an extracting agent to obtain raffinate anda loaded organic phase, and performing reverse extraction on the loaded organic phase by adopting an acidic solution to obtain an organic phase containing the extracting agent and reverse extractionliquid; stripping ammonia gas from the raffinate through alkalinity, absorbing part of the ammonia gas by adopting an organic phase containing an extracting agent for saponification of the extractingagent, and absorbing a part of the ammonia gas by adopting strip liquor to obtain a solution containing ammonium ions and manganese ions for electrolyzing manganese, wherein the water washing residueis used as a cement retarder or roadbed backfill. According to the method, extraction and enrichment of soluble manganese and ammonium in the electrolytic manganese residues can be achieved to obtainthe manganese electrolyte, and the washed residues can be used for building materials or road pavement to be digested, so that a present problem that the electrolytic manganese residues are piled up for a long time is thoroughly avoided.

A method is for treating a lithium ion secondary battery positive electrode active substance waste product that contains cobalt, nickel, manganese and lithium, and involves: a carbon mixing step in which a powder-form positive electrode active substance waste product is mixed with carbon to obtain a mixture in which the ratio of the mass of the carbon is 10-30% of the total mass of the positive electrode active substance waste product and the carbon; a roasting step for roasting the mixture at a temperature of 600-800 DEG C to obtain a roasted powder; a lithium dissolving step which involves a first dissolving process for dissolving the lithium in the roasted powder in water or a lithium-containing solution and a second dissolving process for dissolving the lithium in the residue obtained in the first dissolving process in water; and an acid leaching step in which the residue obtained in the lithium dissolving step is leached with acid.

The invention discloses a production process of manganese sulfate. The process comprises the following steps of 1) extracting by-products of cobalt after smelting by using Lix series organic extractant to remove copper, and stripping copper liquid into a copper electrodeposition system, and extracting remaining liquid as a first intermediate mixed solution; 2) adding sodium hypochlorite to the above extracting remaining liquid, stirring for reaction, standing to precipitate, and separating the precipitate to obtain a second intermediate mixture; 3) using a P507 organic extractant to extract the second intermediate mixture to collect an oil phase to obtain a manganese-loaded organic phase; 4) stripping the manganese-loaded organic phase with sulfuric acid, and collecting an aqueous phase toobtain a manganese sulfate solution; 5) making the manganese sulfate solution subjected to evaporative crystallization, centrifugal dehydration and drying to obtain a manganese sulfate product. The process adopts the copper extractant to extract copper in a high chloride ion solution, adopts a sodium hypochlorite calcium removing method, and removes calcium by using the poor solubility of calciumhypochlorite, thereby replacing the method of removing the calcium by using environmentally polluting fluoride in the prior art, and reducing the pollution to the environment.

The invention discloses a method for removing zinc, calcium and magnesium ions in a manganese sulfate solution by a synergistic extraction method and belongs to the technical field of hydrometallurgy.The method comprises the following steps of: mixing di(2-ethylhexyl) phosphate, tributyl phosphate and dinonyl naphthalene sulfonic acid according to a certain ratio to prepare an extraction agent, and adding sulfonated kerosene to prepare an organic phase; saponifying the organic phase, and extracting and purifying zinc, calcium and magnesium ions in the manganese sulfate solution so as to prepare high-purity battery-grade manganese sulfate. According to the method, a byproduct, namely a manganese sulfate solution with relatively high impurity content, produced from production of nickel sulfate and cobalt sulfate is used as a water phase; an extraction agent prepared in proportion is used as an organic phase; after multi-stage counter-current extraction, a liquid from a water-phase outlet is a pure manganese sulfate solution; the organic phase is recycled after being subjected to segmented pickling for regeneration; and a water phase produced from the regenerative section is a zinc sulfate product. The method has the advantages that the raw material cost is low, the alkali consumption is greatly reduced, the process is simple, the flow is short, the production efficiency is high,the production process is clean, no waste water is discharged and the like.

The invention provides a treatment system and a treatment method for reducing the content of impurities in a soluble manganese salt solution. The impurities comprise calcium ions and magnesium ions, the treatment system comprises an extraction unit and an evaporative crystallization device or a precipitation unit, the extraction unit is used for removing the magnesium ions, and the extraction unitis provided with a soluble manganese salt solution inlet, an extraction agent inlet and a primary purified product outlet; the evaporative crystallization device is provided with a primary purified product inlet, and the primary purified product inlet is communicated with the primary purified product outlet through a primary purified product conveying pipeline; the precipitation unit is providedwith a primary purification product inlet and a precipitant inlet, and the primary purification product inlet is communicated with the primary purification product outlet through a primary purification product conveying pipeline. By adopting the treatment system, the impurity content in the soluble manganese salt solution can be greatly reduced. The treatment system and a treatment method for reducing the content of impurities in a soluble manganese salt solution have the advantages of being simple in structure, small in solid slag and hazardous waste discharge amount and the like, and therefore good environmental friendliness is achieved.

The invention discloses a preparation method of a battery-grade Ni-Co-Mn mixed solution and a battery-grade Mn solution. The preparation method comprises the following steps: acid dissolution, alkalization and impurity removal, calcium-magnesium-lithium synchronous precipitation, deep aging and impurity removal, collaborative extraction and refined extraction. The deep aging impurity removal and synergistic extraction step comprises the following steps: carrying out deep aging on filtrate obtained after the calcium-magnesium-lithium synchronous precipitation step, and performing filtering to remove impurities, so as to obtain aged filtrate; and extracting the aged filtrate by using P204 to obtain a loaded organic phase, and carrying out graded reverse extraction on the loaded organic phaseto obtain a battery-grade Ni-Co-Mn mixed solution and a Mn-containing solution. Through cooperation of multiple process steps of calcium-magnesium-lithium synchronous precipitation, deep aging impurity removal and synergistic extraction, the impurity content of the obtained battery-grade Ni-Co-Mn mixed solution is remarkably reduced, and the battery-grade Ni-Co-Mn mixed solution can be directly applied to preparation of a lithium battery ternary precursor material; and meanwhile, a battery-grade Mn solution can be obtained, large-scale application of the process is facilitated, and economic benefits are improved.

The invention discloses a method for recovering valuable elements from chlorination-process titanium dioxide waste acid through sectional extraction. The method comprises the following steps: S1, adding a first organic phase into the chlorination-process titanium dioxide waste acid to obtain a first extraction raffinate and an iron load, and carrying out back extraction on the iron load to obtaina ferric chloride solution; S2, adding a second organic phase into the first extraction raffinate to obtain second extraction raffinate and a scandium-titanium-zirconium-niobium load; S3, carrying outback extraction on the scandium load to obtain a scandium-titanium-zirconium-niobium enriched product; S4, adjusting the pH value of the second extraction raffinate to prepare a liquid; S5, adding athird organic phase after liquid preparation to obtain a vanadium-aluminum load and a third extraction raffinate; S6, carrying out back extraction on the vanadium-aluminum load to obtain a vanadium-aluminum mixed solution; S7, adjusting the pH value of the third extraction raffinate to prepare a liquid; S8, after liquid preparation, adding a fourth organic phase into manganese extraction feed liquid to obtain a manganese load and a fourth extraction raffinate, and carrying out back extraction on the manganese load to obtain a manganese-containing solution; and S9, neutralizing the fourth extraction raffinate, carrying out filtering, then performing concentrating and crystallizing to obtain NaCl edible salt and water, and recycling the NaCl edible salt and water.

The invention belongs to the field of smelting, and particularly relates to a method for preparing battery-grade manganese sulfate from manganese oxide ore, which comprises the following steps of: (1) leaching: carrying out first-stage leaching on manganese oxide ore, biomass and sulfuric acid, roasting leaching slag, mixing the roasted material and first-stage leaching liquid, carrying out second-stage leaching, and separating to obtain leaching liquid; (2) first-stage impurity removal: adding ferric sulfate, a manganese oxidizing agent and sulfide into the leachate to obtain first-stage impurity removal liquid; (3) second-stage impurity removal: carrying out manganese precipitation treatment on the first-stage impurity removal liquid to obtain a manganese hydroxide precipitate, dispersing the precipitate and a compound shown in the formula 1 in a solvent to obtain slurry, introducing carbon dioxide into the slurry, and carrying out second-stage impurity removal and solid-liquid separation to obtain impurity-removed manganese hydroxide; and (3) third-stage impurity removal: dissolving the impurity-removed manganese hydroxide with sulfuric acid, and then adding BaS and BaF2 to obtain a battery-grade manganese sulfate solution. The method disclosed by the invention is high in recovery rate and can be used for preparing high-quality battery-grade manganese sulfate.

The Mn3O4/NiMn2O4 composite structure and the pure substance NiMn2O4 are prepared to serve as the supercapacitor electrode, the two structures serve as the electrode, the electrochemical performance is greatly improved, and the cost of the electrode material can be greatly reduced; the preparation technology of NiMn2O4 is mainly a high-temperature solid-phase reaction or solvothermal combined subsequent calcination oxidation method. The application of the electrochemical ion exchange technology or the electrochemical ion exchange technology in the aspect is rarely reported, the Mn3O4/NiMn2O4 composite structure and the pure substance NiMn2O4 are prepared by using electrochemical ion exchange, the time is short, the temperature is low, the operation is simple and pollution is avoided.

Provided is a method for inhibiting extractant degradation in the DSX process through the manganese extraction control, the method comprising: (a) stirring DSX solvent and DSX feed solution, which is a solution containing a valuable metal from which iron has been removed in an agitator, in which soda ash (Na₂CO₃) is further added to maintain a constant pH; and (b) scrubbing the manganese from the DSX solvent, extracted in step (a).

The invention discloses a method for recycling purified terephthalic acid wastewater. The method comprises the following steps: providing purified terephthalic acid wastewater, adjusting the temperature of the purified terephthalic acid wastewater to 30-45 DEG C, adjusting the pH value of the purified terephthalic acid wastewater to 2.5-4.5, and filtering the purified terephthalic acid wastewater to obtain a filtrate and a first solid which contains aromatic carboxylic acid; feeding the filtrate into an extraction system for extraction treatment to obtain an extraction phase and a raffinate phase; feeding the extraction phase into a rectifying tower, performing regeneration treatment to obtain a second solid matter containing aromatic carboxylic acid, feeding the raffinate phase into an ion exchange system, and performing ion exchange treatment; and carrying out desorption treatment on ion exchange resin in the ion exchange system to obtain cobalt and manganese ions. According to the method provided by the invention, recovery treatment of organic carboxylic acid and metal ions in the PTA wastewater is comprehensively considered, and the treatment load of a downstream section is remarkably reduced while effective recycling of resources is realized.

Provided is a method for inhibiting extractant degradation comprising preparing step, extracting step and scrubbing step, the method including: (a) the preparing step of a DSX solvent by adjusting the extractant concentration of the DSX solvent to a specific range; (b) the extracting step of metal included in the feed solution by adjusting the ratio of the organic (solvent) and an aqueous (solution) as a feed solution; (c) the scrubbing step of adjusting the zinc concentration of the solution using zinc sulfate; and (d) stripping step.