239results about "Lithium sulfates/sulfites" patented technology

The present disclosure relates to the extraction of lithium from underground reservoirs of naturally occurring brines. Described herein are systems and methods to extract lithium entrapped within reservoirs that were previously inaccessible.

The present application discloses a method for recovering battery-grade iron phosphate and lithium salts from lithium iron phosphate waste materials and its application, comprising the following steps: S100, dissolving the lithium iron phosphate waste materials with a phosphoric acid solution, filtering to obtain a waste material dissolution solution; S200, adding an acid solution and an oxidant to the waste material dissolution solution to obtain a crystallization stock solution; S300, diluting the crystallization stock solution with water until its pH value is 1.0 to 1.5, and performing high-temperature crystallization to obtain hydrated iron phosphate and a lithium-containing filtrate; S400, roasting the hydrated iron phosphate to obtain battery-grade iron phosphate; S500, removing water from the lithium-containing filtrate to obtain solution a, circulating solution a to dissolve the lithium iron phosphate waste materials, and concentrating to obtain lithium salts. The present application uses a phosphoric acid solution as the leaching solvent, does not require the use of an alkali solution subsequently and can be leached cyclically, improving the economic benefits while enabling the efficient recovery of all elements of Li, Fe, and P, and also capable of obtaining a battery-grade iron phosphate product with an iron-to-phosphorus ratio meeting the requirements.

The present disclosure relates to the extraction of lithium from liquid resources such as natural and synthetic brines, leachate solutions from clays and minerals, and recycled products.

The invention belongs to the technical field of lithium-containing waste treatment, and particularly discloses a method for preparing lithium carbonate by recycling lithium through cooperative treatment of lithium-containing waste. The method specifically comprises the following steps: mixing a lithium amide waste material, a lithium sulfide waste material and water, then mixing with a hydrogen peroxide solution and a sulfuric acid solution, and carrying out an acid dissolution reaction to obtain a lithium-containing acid solution and an insoluble substance; mixing the lithium-containing acid solution with alkali liquor, and carrying out alkalization reaction to obtain insoluble impurities and alkalized feed liquid; concentrating the alkalized feed liquid to obtain concentrated alkalized feed liquid, and mixing the concentrated alkalized feed liquid with a sodium carbonate solution for lithium precipitation reaction to obtain lithium precipitation mother liquor and lithium carbonate; extracting the lithium element in the lithium precipitation mother liquor, and evaporating and concentrating the raffinate to separate out sodium sulfate and ammonium sulfate; ammonium sulfate and the lithium iron phosphate waste are mixed and then sequentially subjected to roasting and leaching, and a leaching solution and a lithium-containing acid solution are mixed for alkalization. The method has the characteristics of high process integration level, high economic value and less environmental pollution, and conforms to the new concept of chemical green atom economy.

The invention relates to a surface-modified lithium-rich positive electrode material, a positive electrode plate as well as a preparation method and application of the surface-modified lithium-rich positive electrode material. The surface-modified lithium-rich positive electrode material comprises a lithium-rich positive electrode material matrix, a lithium salt coating layer and a spinel structure transition layer, wherein the lithium salt coating layer and the spinel structure transition layer are generated through an in-situ reaction; the spinel structure transition layer is positioned between the lithium-rich positive electrode material matrix and the lithium salt coating layer; the lithium salt coating layer is generated through an in-situ reaction of an aluminum salt and a lithium raw material; wherein the lithium raw material comprises lithium oxide and / or a material capable of generating lithium oxide through thermal decomposition, and the lithium salt coating layer is generated through in-situ reaction of lithium oxide and aluminum salt; lattices of the spinel structure transition layer and the lithium salt coating layer on the surface of the lithium-rich manganese-based positive electrode material substrate contain an element A in concentration gradient distribution, and the element A is combined with an element O to form an element A-O bond. Through surface modification, the lithium-rich positive electrode material not only has excellent lattice oxygen stability under high voltage, but also shows good lithium ion diffusivity and electrochemical performance.

The invention discloses a method for separating and recycling phosphorus, iron and lithium in battery black powder, and relates to the technical field of battery recycling. The method comprises the following steps: carrying out acid leaching on battery black powder to obtain a battery black powder leaching solution and filter residues; an oxidizing agent is added into the battery black powder leaching solution, the pH of the solution is adjusted to 1.8-2.5, solid-liquid separation is conducted after the reaction is completed, and iron phosphate sediment and a lithium-containing solution are obtained; adjusting the pH value of the lithium-containing solution to 10-12, and carrying out solid-liquid separation after the reaction is completed to obtain a metal precipitate and a lithium sulfate solution; dissolving the iron phosphate precipitate in a sulfuric acid solution, adding a reducing agent to reduce ferric iron into ferrous iron, separating out ferrous sulfate by adopting an alcohol precipitation method or an ammonium sulfate crystallization method, and performing solid-liquid separation after the reaction is completed to obtain ferrous sulfate precipitate or ammonium ferrous sulfate crystals and mother liquor; and evaporating and concentrating the mother liquor, and extracting to obtain a phosphoric acid solution. According to the method, the three elements of phosphorus, iron and lithium in the battery black powder can be recycled, and the environmental problem caused by stacking of the lithium extraction slag can be avoided.

The invention discloses a method for preparing high-purity lithium sulfide from a lithium sulfate mother liquor, which comprises the following steps: preparing a lithium sulfate concentrated liquor: adding 98% concentrated sulfuric acid into the lithium sulfate mother liquor to adjust the pH value, adjusting the pH value to 6-7, carrying out precise filtration to filter out possible impurities to obtain a filtrate, introducing the filtrate into an MVR evaporation system, and concentrating the mother liquor to obtain a concentrated liquor, performing freezing crystallization on the concentrated solution by using a cooling crystallizer, and then performing centrifugal separation under the action of a centrifugal machine to obtain solid slag which is mirabilite and a solution which is lithium sulfate concentrated solution; and preparing crude lithium sulfide: performing evaporative crystallization on the obtained lithium sulfate concentrated solution, adding pure water for slurrying, and performing centrifugal filtration and cleaning for 2-3 times. The impurity content is effectively controlled through a multi-stage purification process, the Li2S product with the purity larger than or equal to 99.95% is finally obtained, the key technical problem of direct conversion from a liquid battery recycling material to a solid battery positive electrode raw material is solved, and core material support is provided for lithium battery industry closed loop and industrial product iteration.

The invention discloses a device and a method for extracting lithium sulfate in salt lake brine, and relates to the field of lithium sulfate production process, the device comprises a treatment tank, an upper cover for sealing is arranged at the top of the treatment tank, a supporting frame for supporting is arranged outside the treatment tank, and the device further comprises a filtering part for filtering a solvent, a filter plate is cleaned through an upper scraping assembly and an ejection assembly in the cleaning mechanism, filtered materials are discharged into a collecting barrel through a feeding port to be discharged, the filter plate is rotated into the cleaning mechanism, the situation that the filtered materials penetrate through the filter plate due to scraping of the filtered materials in the cleaning and filtering process is avoided, and the purity of filtered liquid is guaranteed; and in the cleaning process, filtering is not affected, and equipment does not need to be paused for cleaning.

A process (1000) for producing a lithium salt (190) by treating a particulate lithium containing material containing lithium bearing minerals comprising pressure leaching (20) the lithium containing material with concentrated sulphuric acid to form a pregnant solution (22) containing lithium sulphate as a source of lithium for a selected lithium salt for production (190) and impurities; removing the impurities in a series of steps (30, 40, 50, 60, 70) including removal (70) of at least one sulphate compound contained in the pregnant solution, said at least one sulphate compound containing at least one of potassium and sodium; and producing the selected lithium salt (190) following impurity removal (30, 40, 50, 60, 70).

The invention discloses a green roasting method for recycling desulfurized gypsum, and belongs to the technical field of solid waste recycling. According to the process disclosed by the invention, the desulfurized gypsum solid waste rich in calcium sulfate is used for replacing part or all of sulfate to be mixed with lepidolite for roasting reaction, and components such as calcium carbonate and calcium sulfite contained in the desulfurized gypsum are utilized by controlling the step-by-step heating rate and the roasting temperature; under specific roasting process conditions, calcium oxide and calcium sulfide generated through self-reaction serve as purifying agents and react with fluorine and thallium to form stable calcium fluoride and thallium sulfide precipitates, fluorine and thallium are fixed in the high-temperature roasting stage, the pressure of follow-up flue gas treatment and wastewater treatment is effectively reduced through self-purification, and environmental pollution is reduced.

The utility model discloses a device for recovering and separating potassium and sodium salts generated in the process of extracting lithium from ore, which is characterized in that an outlet of a salt dissolving tank is connected with a freezing buffer tank, an outlet of the freezing buffer tank is connected with a freezing crystallizer, a freezing crystal slurry outlet is connected with a freezing thickener, and an outlet of the freezing thickener is connected with a freezing centrifuge; a refrigerated centrifugal solid phase outlet is connected with a hot melting tank, a bottom outlet of the hot melting tank is connected with an anhydrous sodium sulphate crystallizer, an anhydrous sodium sulphate crystal slurry outlet is connected with an anhydrous sodium sulphate thickener and an anhydrous sodium sulphate centrifuge, and a centrifugal solid phase outlet is connected with an anhydrous sodium sulphate discharge pipe; the centrifugal liquid phase outlet is connected with an anhydrous sodium sulphate mother liquor tank; a liquid phase outlet of the freezing centrifuge is connected with a freezing mother liquor tank, freezing mother liquor flows back and enters the potassium sulfate crystallizer, a potassium sulfate crystallization magma outlet is connected with the potassium sulfate thickener and the potassium sulfate centrifuge, and a potassium sulfate centrifugal solid phase outlet is connected with a potassium sulfate salt discharge pipe. The device can be used for separating the mixed salt into sodium sulfate with extremely high purity and potassium sulfate with relatively high purity, so that the product yield is improved.

Pairing of Li2ZrCl6 (LZC) and Li6PS5Cl (LPSC) solid electrolytes, which increases the effective electrochemical and chemical stability window of the electrolyte of lithium-based solid-state batteries, and enables stable cycling with a high voltage cathode and a metallic anode, with the potential to greatly enhance solid-state battery energy density.

The invention discloses a method for efficiently recovering valuable metals from a waste ternary positive electrode material step by step. According to the method, the layered structure of the ternary positive electrode material is successfully destroyed through a sodium thiosulfate and glucose composite salt reduction roasting method, lithium is converted into soluble sulfate, and transition metal is converted into water-insoluble metal oxide, so that preconditions are provided for selective lithium extraction; and meanwhile, the generated metal oxide is more beneficial to subsequent roasting compared with a metal phase. According to the method, sodium thiosulfate and glucose composite salt are adopted for carbon-sulfur combined roasting, so that the reaction limit is reduced, and the reaction temperature and the reaction time are successfully reduced. And roasting can be performed in air, so that the whole process operation is facilitated. According to the method, the loss rate of lithium in the whole process can be reduced through two times of roasting and cyclic utilization of the leachate, the extremely high extraction rate of lithium is achieved, and a new thought is provided for recycling of the waste ternary positive electrode material.

Embodiments relate to methods and processes for purification of lithium containing brines by selectively separating boron containing compounds. The method includes passing a feed brine including lithium and at least one boron compound through at least one semi-permeable membrane in which the boron compounds are separated from the lithium by preferentially passing the boron compounds through the membrane stage(s). At least one environmental condition of the feed brine and / or membrane stage(s) may be modified to allow boron compounds to be preferentially passed through the membrane stage(s). The lithium-rich concentrate stream may be further purified and / or converted into lithium products, while the resultant boron-rich permeate stream (including the separated boron containing compounds) may be further processed.

A mobile phase including a lithium salt flows through a stationary phase including an oxygenated metal compound with affinity to the lithium salt through a Lewis acid-Lewis base interaction so that the oxygenated metal compound captures the lithium salt through the Lewis acid-Lewis base interaction. An eluent flows through the stationary phase to release the lithium salt captured by the oxygenated metal compound into the eluent. The eluent includes a Lewis base or a Lewis acid that disrupts the Lewis acid-Lewis base interaction between the lithium salt and the oxygenated metal compound. The eluent including the released lithium salt is collected after the eluent flows through the stationary phase.

The utility model relates to the technical field of coating devices, and discloses separation equipment for lithium sulfate solution production, which comprises a separation equipment body and a feed port fixedly connected to the top of the separation equipment body, and further comprises a discharge pipe fixedly connected to the bottom of the separation equipment body, a control chamber is fixedly connected to the bottom of the reaction chamber and communicates with the feeding port, a sealing plate is fixedly connected to the interior of the control chamber, and a quantity control mechanism is further arranged in the separation equipment body. Through the arrangement of the reaction chamber, the control chamber and the sealing plate, the effect of conveniently controlling the quantity of a lithium sulfate solution by a worker is achieved, the subsequent separation effect is improved, and the problem that in the using process of existing separation equipment, the lithium sulfate solution is often directly poured into a separation net at a time, and the separation efficiency is affected is solved. And the problem that the separation effect is poor due to the fact that too much liquid is poured at a time is possibly solved.

The utility model discloses an evaporation and concentration system suitable for lithium sulfate purification, which is characterized in that an outlet of a raw material tank is sequentially connected with a cold side of a condensate water preheater and a cold side of a non-condensable steam preheater through an outlet of a feeding pump, and then is connected with a tube pass inlet of a heater together with an outlet pipeline of a material circulating pump; a tube pass outlet of the heater is connected with a material inlet of the integrated separator, and a material outlet of the separator is connected with an inlet of the material circulating pump; a secondary steam outlet of the integrated separator is connected with an inlet of a steam compressor through a scrubber tower, and a compressed steam pipe is connected with a shell pass steam inlet of a heater; a shell pass condensed water outlet of the heater is connected with an inlet of a condensed water tank; an outlet of the condensed water tank is connected with a hot side of the condensed water preheater through a condensed water pump; a shell pass extraction opening of the heater is connected with the hot side of the non-condensable steam preheater through a non-condensable gas conveying pipe, and a hot side outlet of the condenser is connected with a vacuumizing system. The system is high in evaporation efficiency and low in operation cost and equipment investment.

Embodiments herein relate to recycling of used lithium battery materials. In some aspects, a method may include suspending a lithium source in a solvent containing an oxidizing agent to extract lithium, forming an extracted lithium solution, separating the extracted lithium solution from residual solids of the lithium source, purifying the extracted lithium solution by precipitating and filtering impurities, and precipitating lithium in the purified lithium solution to produce lithium carbonate (Li2CO3). In some embodiments, the method may also include pre-treating the lithium source to improve the kinetics of the lithium extraction. In some embodiments, the pretreatment may include a cutting or comminution step to reduce the size of the lithium source. In some embodiments, the lithium source may include lithium ion battery waste. In some embodiments, the oxidizing agent may include sodium persulfate (Na2S2O8), potassium persulfate ((NH4) 2S2O8), ammonium persulfate (NH4) 2S2O8, hydrogen peroxide (H2O2), ozone (O3), and / or nitrous oxide (N2O).

Embodiments described herein relate to recycling of spent lithium battery material. In some aspects, a method can include suspending a lithium source in a solvent containing an oxidation reagent to extract lithium, forming an extracted lithium solution, separating the extracted lithium solution from residual solids of a lithium source, purifying the extracted lithium solution by precipitating and filtering impurities, and precipitating the lithium in the purified lithium solution to generate lithium carbonate (Li2CO3). In some embodiments, the method can further include preprocessing the lithium source to improve kinetics of the lithium extraction. In some embodiments, the preprocessing can include a cutting or shredding step to downsize the lithium source. In some embodiments, the lithium source can include lithium-ion battery waste. In some embodiments, the oxidation reagent can include sodium persulfate (Na2S2O8), potassium persulfate (K2S2O8), ammonium persulfate (NH4)2S2O8, hydrogen peroxide (H2O2), ozone (O3), and / or nitrous oxide (N2O).

The invention discloses a method for recovering metal from electronic waste or leach residue thereof, the electronic waste or leach residue comprising copper element and one or more lithium compounds, the method comprising: leaching the electronic waste or leach residue with a leaching solution comprising ammonium sulfate in the presence of an oxidizing agent, a leaching solution containing copper ions and lithium ions and solid residues are provided; and separating the leachate and the solid residue.

The present invention relates to the technical field of batteries, and specifically to a cathode material and a preparation method therefor and use thereof. A cathode material, including a cathode bulk and a coating layer coated on at least part of a surface of the cathode bulk, where a chemical formula of the cathode bulk is LiaNixCoyMnzMbO2, where 0.97≤a≤1.1, 0.5≤x<1.0, 0<y≤0.1, 0<z≤0.1, and x+y+z+b=1, and an ion M in the cathode bulk is at least one selected from Sb5+, Ti4+, Zr4+, V5+, Nb5+, W6+ and Mo6+; and the coating layer includes Li2SO4. The cathode material in the present invention has low residual alkali on a surface and good structural stability, and can improve cycle performance and safety performance of batteries.

The invention provides a method for recovering ternary black powder to prepare lithium salt, which comprises the following steps: S1, adding a reducing agent into the ternary black powder for roasting treatment to obtain roasted black powder; s2, adding water into the roasted black powder for water leaching treatment, and filtering to obtain a saturated lithium carbonate aqueous solution and an insoluble solid; s3, inorganic acid is added into the saturated lithium carbonate aqueous solution until the pH is 6.5-7, and a lithium salt aqueous solution is obtained; s4, the lithium elution rate n of the step S2 is obtained, and according to the lithium elution rate n, it is determined that insoluble solids are subjected to washing treatment, or it is determined that the insoluble solids are continuously subjected to water immersion treatment; and S5, the saturation S of the lithium salt in the lithium salt aqueous solution in the step S3 is obtained, and according to the saturation S and the lithium elution rate n, the lithium salt aqueous solution is determined to be subjected to purification treatment, or the lithium salt aqueous solution is determined to serve as water in the step S2 to be used for water immersion treatment. According to the method, a lithium salt product with relatively high purity can be obtained.

The invention provides a method for preparing high-purity lithium sulfate from a lithium-sodium mixed solution. The method comprises the following steps: providing a lithium-sodium mixed sulfate solution; the method comprises the following steps: based on a Li2SO4-Na2SO4-H2O ternary system phase diagram, evaporating and concentrating a lithium-sodium mixed sulfate solution to be saturated, and then freezing and denitrifying to obtain a denitrified solution; evaporating the denitrated solution to a co-saturation point of lithium-sodium mixed sulfate, carrying out lithium precipitation, and separating to obtain a lithium precipitation mother solution and a lithium sulfate monohydrate crude product; purifying the lithium sulfate monohydrate crude product to obtain a high-purity lithium sulfate product; freezing and crystallizing the lithium precipitation mother solution, and separating to obtain a lithium-sodium mixed sulfate hydrate and a frozen solution; the lithium-sodium mixed sulfate hydrate is returned to the lithium-sodium mixed sulfate solution, and the frozen liquid is returned to the denitrated liquid. According to the method, the process is simplified, the lithium recovery rate is increased, cost reduction and efficiency improvement are achieved, material recycling can be achieved in the whole process, and the development prospect is good.

The present invention discloses a refined lithium sulfate and its production process, belonging to the technical field of producing refined lithium sulfate. The production process of the refined lithium sulfate of the present invention includes high-temperature roasting, acidification, low-temperature roasting, leaching with water, stepwise adjusting the pH value, adding a impurity remover, solid-liquid separation and pressure filtration, and finally obtaining refined lithium sulfate, wherein the impurity remover is cellulose nanocrystal composite non-ionic PAM. By setting different pH values step by step and combining with the action of the impurity remover, the zonal flocculation and sedimentation removal of impurity particles can be realized, thereby improving the removal efficiency of impurity ions and helping the complete removal of impurity ions. The non-ionic PAM uses cellulose nanocrystals as a carrier, which can improve the mechanical strength and structural stability of the impurity remover, enhance the attraction and capture ability of the impurity remover for impurity particles, optimize the pH adaptability of the impurity remover, and efficiently remove impurity particles.

The invention provides an optimized method for recovering high-purity lithium sulfate from a lithium-containing composite oxide deposited on an erosion surface of a waste sagger. Therefore, it is expected that by means of the method for preparing the high-purity lithium sulfate from the waste saggar, the high-purity lithium sulfate capable of being used for preparing the lithium secondary battery can be prepared by recycling the waste saggar; and moreover, positive active materials, iron oxide, aluminum oxide, silicate and calcium carbonate which are additionally obtained in the preparation process can be recycled.

The positive electrode active material for a lithium secondary battery according to the present invention comprises active material particles, the active material particles comprising: an active material core comprising a lithium metal oxide; and a sulfur-containing coating layer and a metal-containing coating layer, the sulfur-containing coating layer and the metal-containing coating layer being formed on the active material core. The charge transfer resistance (Rct) of the active material particles measured at a depth of discharge (DOD) of 50% by individual contact of the measurement probe is 60 [Omega] / cm2 or less. Provided is a lithium secondary battery including a positive electrode active material having both improved conductivity and ionic conductivity.

The present specification provides a method for preparing a solid electrolyte for a secondary battery, comprising the steps of: (S1) preparing a material composition comprising phosphorus (P) sulfide, a lithium halide and lithium sulfide; (S2) mechanically milling the material composition in a milling container; and (S3) calcining a compound obtained after the milling step, wherein the calcination step (S3) performs purging using gas.

A process (100) for treating aqueous impurity containing streams containing lithium cations and impurities within a lithium extraction process comprises: (a) contacting the impurity containing stream with a soluble phosphate to produce a precipitate containing lithium phosphate and a soluble impurity containing stream; and (b) treating the precipitate containing lithium phosphate with an aqueous reagent to produce the soluble phosphate for re-use in step (a) and a lithium salt recyclable to the lithium extraction process (100). Lithium recovery from the impurity containing stream may be 80% or greater.