31 results about "Lithium sulphate" patented technology

A method for producing battery-grade lithium dihydrogen phosphate using lithium-containing brine includes the following steps: (1) adding sodium hydroxide solution to lithium-containing mother liquor, adding the mixed solution to sodium dihydrogen phosphate solution, maintaining the pH of the system at 9-11, reacting, separating the solid and liquid phases to obtain lithium phosphate precipitate and mother liquor; (2) adjusting the slurry, adding concentrated sulfuric acid to react, separating the solid and liquid phases to obtain a mixed solution of liquid-phase lithium dihydrogen phosphate and lithium sulfate; (3) vacuum cooling and crystallization separation to obtain lithium dihydrogen phosphate crystals. This invention achieves efficient recovery of lithium ions from low-concentration lithium-containing brine, eliminating the need for conventional processes such as electrodialysis and MVR for further concentration of lithium-containing mother liquor. It also avoids the use of phosphoric acid in the acidification process, saving raw material costs, reducing the amount of water added in the acidification process, and reducing energy consumption in the crystallization separation process. The resulting battery-grade lithium dihydrogen phosphate is of stable quality, uniformly distributed, and bright white in color, suitable for preparing lithium-ion battery cathode materials, and has a low cost.

The application belongs to the technical field of lithium ion battery negative electrode materials, and particularly relates to a MXene two-dimensional material, a graphite negative electrode material and a preparation method of the MXene two-dimensional material, the preparation method of the MXene two-dimensional material being as follows: lithium sulfate solution is added into a MXene dispersion liquid, stirred uniformly, vacuum dried, calcined at 300-500 DEG C, and the MXene two-dimensional material is obtained; and the application can effectively improve lithium ion conductivity and improve the performance of a battery.

Capture mixtures and activated capture mixtures are provided that are useful for nucleic acid separation and purification are provided. The mixtures comprise lithium lauryl sulfate, lithium hydroxide, a zwitterionic sulfonic acid buffering agent, and optionally, proteinase K, capture probes comprising a first specific binding partner (SBP), and a second specific binding partner immobilized to a solid support. Related combinations, methods, uses, and kits, are also provided.

The application discloses a mine filling and plugging material quick-setting additive and a preparation method thereof. The water-retaining agent in the quick-setting additive is a composite water-retaining system formed by hydroxypropyl methyl cellulose and modified starch. The hydroxypropyl methyl cellulose physically wraps free water in the slurry; the modified starch adsorbs water molecules through hydrogen bonding, and the double mechanism significantly reduces the bleeding rate; the coagulation accelerator adopts a spray drying wrapping technology, and a core-shell structure composite particle is constructed, in which aluminum lithium sulfate is used as a 'quick-release core', and active calcium silicate gel slurry obtained by the reaction of nano calcium silicate and sodium silicate is used as a'slow-release wrapping layer', so that the coagulation accelerator can promote coagulation, prevent sodium silicate from being consumed too early, and realize sustained coagulation. The early strength agent adopts a gel-gelling method, so that the early strength agent can provide persistent early strength excitation and solve the problem of weak late strength growth. The interface reinforcing agent can make the interface transition zone structure more strong and tough, and improve the integrity and damage resistance after the slurry coagulation and hardening.

The application discloses a preparation and purification method of high-purity radioiodine-labeled antigen. The method comprises the following steps: pre-activating carrier-free sodium iodine[125I] solution in an orthogonal solvation sensitization buffer containing lithium sulfate, 18-crown-6 and beta-cyclodextrin; adding antigen and chloramine-T for a labeling reaction; and performing magnetic separation and purification by using a suspension containing adamantane-modified magnetic microspheres and quaternary ammonium salt-modified strong anion exchange magnetic microspheres after the reaction. The orthogonal solvation effect is used to enhance the nucleophilic activity of iodine ions, and the amount of oxidizing agent is reduced to reduce protein damage; impurities are quickly removed through the double mechanisms of electrostatic adsorption and host-guest recognition. The application has the advantages of high labeling efficiency, high radiochemical purity of the product and complete retention of biological activity.

This invention belongs to the field of lithium sulfide technology and discloses a method and apparatus for preparing lithium sulfide by hydrothermal reduction. The method includes: mixing and dispersing lithium sulfate with a pore-forming agent to form a composite precursor; subjecting the composite precursor to hydrothermal reduction in a hydrogen-containing reducing atmosphere, with plasma used for external field enhancement during the hydrothermal reduction process, to obtain crude lithium sulfide. This invention can improve the preparation efficiency of lithium sulfide and obtain high-purity, high-yield lithium sulfide products.

The application discloses a preparation method for synthesizing sulfide solid-state batteries by using lithium sulfide, and belongs to the technical field of sulfide solid electrolytes. High-activity lithium sulfide is prepared by carbon thermal reduction of lithium sulfate monohydrate and graphite, and then, the high-activity lithium sulfide is mixed with lithium chloride, phosphorus pentasulfide and hyperbranched amphiphilic grinding aids as raw materials to obtain high-purity Li6PS5Cl electrolyte powder through pre-mixing, high-energy ball milling and high-temperature sintering, and then, the electrolyte film is prepared by pressing and molding, and a symmetrical battery is assembled. The high-activity lithium sulfide is prepared in situ by carbon thermal reduction, the raw material conversion rate is significantly improved, the synthesis cycle is shortened, and the generation of impurities is reduced; the powder dispersion is strengthened by the hyperbranched amphiphilic grinding aids, the obtained electrolyte has high cycle stability, long service life, high raw material utilization rate and excellent electrochemical performance, the process is efficient and simple, the conditions are controllable, and the process is suitable for industrialized production of high-performance full solid-state lithium batteries.

This invention relates to the field of lithium extraction technology from lithium-containing organic wastewater, specifically to a method for preparing battery-grade lithium carbonate from lithium-containing organic wastewater. The method provided by this invention first recovers organic acids from the wastewater through esterification and hydrolysis reactions. Then, under pH 11-12 conditions, lithium is precipitated with trisodium phosphate to obtain crude lithium phosphate solid. The lithium is then enriched, dissolved in acid, and extracted to remove phosphoric acid. The raffinate is adjusted to pH 9-11 to remove impurities, yielding a lithium sulfate solution. After concentration using MVR (Medium-Volume Reduction), impurities are further removed under pH 10.5-11.5 and activated carbon adsorption conditions to obtain a pure lithium sulfate solution. The obtained pure lithium sulfate solution is mixed with a carbonate solution to obtain crude lithium carbonate. Finally, after washing, drying, crushing, and iron removal, battery-grade lithium carbonate is obtained.

The utility model relates to lithium carbonate production technical field, the utility model provides a system of reducing lithium entrainment in lithium precipitation mother liquor, it includes the lithium precipitation reaction kettle for mixing sodium carbonate solution and sodium sulfate, lithium sulfate raw material, lithium precipitation reaction kettle includes jar body, is used to accommodate reaction raw material, still includes stirring rod body, one end of stirring rod body is rotatively established at the top of jar body for being connected with rotary drive spare, the other end extends to jar body bottom, is equipped with stirring paddle no.

The utility model relates to lithium sulfate production technical field, and disclose a kind of solid-liquid separation device for lithium sulfate production, the device includes base and shell, base is annular and is provided with rotating groove in middle part;Shell is rotatably connected to the one end outside of base;Rotatably connected with separation assembly in shell interior, one end of shell near base is provided with rotary liquid inlet component, spiral vane is fixedly connected in shell interior, spiral vane continuously extends from one end of shell to its other end, separation assembly is provided with reverse osmosis cleaning assembly for cleaning separation assembly in interior.The device is sent into shell interior by rotary liquid inlet component with lithium sulfate solution, solid-liquid separation is carried out using hard metal mesh tube and filter cloth in separation assembly, and continuous efficient separation process is realized by spiral vane and gear disc drive, meanwhile, reverse osmosis cleaning assembly is equipped to prevent the blockage of filter cloth and semi-permeable membrane, ensure the automation and high efficiency of lithium sulfate production.

An all-solid-state secondary battery comprising: a positive electrode 11 which contains a lithium-containing sulfate; a negative electrode 13 containing a substance capable of lithium insertion and extraction at a potential lower than that of the positive electrode; and a chloride solid electrolyte 12 containing lithium.

The application relates to a lithium sulfide production method, which comprises the following steps: a lithium sulfate preparation step, in which lithium carbonate and concentrated sulfuric acid are reacted to obtain lithium sulfate crystals; a pretreatment step, in which the lithium sulfate crystals are ball-milled with a carbon source under an inert atmosphere, so that the carbon source is wrapped around the surface of the lithium sulfate particles in the form of microparticles to obtain a ball-milling mixture; a carbon source pyrolysis step, in which the ball-milling mixture is heated at a temperature of 400-500 DEG C for 1-2 hours, so that the carbon source is pyrolyzed to form a porous carbon skeleton to obtain a pyrolysis mixture; a lithium sulfide generation step, in which the pyrolysis mixture is heated at a temperature of 675-775 DEG C for 6-9 hours, so that the lithium sulfate is reduced by the carbon to generate lithium sulfide to obtain a lithium sulfide mixture; a purification step, in which the lithium sulfide mixture is added into anhydrous ethanol, and after filtration separation and evaporation drying, pure lithium sulfide powder is obtained; and a calcination step, in which the pure lithium sulfide powder is calcined under an inert atmosphere for 1-2 hours to obtain dry lithium sulfide powder. The application can obtain high-purity lithium sulfide products.

The present disclosure discloses a method for producing lithium sulfide, the method comprising a lithium sulfide synthesis step of synthesizing lithium sulfide powder by reacting lithium sulfate powder with a reaction gas containing carbon monoxide, wherein the method further comprising before the lithium sulfide synthesis step, a lithium sulfate pulverization step for pulverizing the lithium sulfate powder into a predetermined size.

This invention discloses a method for regenerating waste lithium iron phosphate batteries into lithium manganese iron phosphate cathode material, comprising the following steps: obtaining lithium sulfate solution and iron phosphate slag by oxidative acid leaching of lithium iron phosphate battery powder; calcining a mixture of manganese oxide and phosphoric acid slag to obtain ferric oxide doped with Mn and phosphorus pentoxide gas; collecting the phosphorus pentoxide gas to obtain a phosphoric acid solution, and reacting the phosphoric acid solution with ammonia and lithium sulfate solution to obtain lithium phosphate; reacting the Mn-doped ferric oxide with sulfur dioxide to obtain ferrous sulfate doped with Mn; and reacting the lithium phosphate and ferrous sulfate doped with Mn with water to obtain lithium manganese iron phosphate cathode material. The regeneration method of this invention can effectively separate lithium / iron-phosphorus, while effectively improving the recovery rate of phosphorus and iron (phosphorus recovery rate > 99%, iron recovery rate > 99%), to directly synthesize high-purity battery-grade lithium manganese iron phosphate cathode material. This method breaks through the traditional long process of dissolution-separation-resynthesis, greatly shortening the process chain and reducing material loss and energy consumption.

This invention provides a lithium sulfate solution concentration device, comprising: a first evaporator; a first evaporator heater, the inlet end of which is connected to the first evaporator via a first pipeline, and the outlet end of which is connected back to the first evaporator; a first circulation pump located on the first pipeline; a feed pipe connected to the first pipeline; a second evaporator; a second evaporator heater, the inlet end of which is connected to the second evaporator via a second pipeline, and the outlet end of which is connected back to the second evaporator; a second circulation pump located on the second pipeline; a discharge pipe connected to the drain port of the second evaporator; the first evaporator connected to the second evaporator heater; and the drain ports of the first and second evaporators connected via a transfer pipe, wherein the connection end of the transfer pipe to the drain port of the first evaporator is higher than the other end. By setting the height difference between the two ends of the transfer pipe, the transfer pump is eliminated, avoiding problems such as easy clogging, easy wear, and difficult maintenance that exist during the use of the transfer pump, thus improving production efficiency and saving operating energy and equipment costs.

This invention provides a direct repair method for waste ternary lithium battery cathode materials, as well as the repaired cathode material and its applications. The direct repair method for waste ternary lithium battery cathode materials includes: S1, heat-treating the waste cathode sheet, followed by mechanical stripping and weak alkali dissolution treatment to obtain the cathode material to be repaired; S2, mixing the cathode material to be repaired, a eutectic salt, a dopant, and a co-solvent to obtain a mixture, subjecting the mixture to a first annealing treatment under a protective atmosphere, followed by a second annealing treatment under an oxygen-containing atmosphere, to obtain the repaired cathode material; wherein the eutectic salt includes lithium carbonate, lithium chloride, and lithium sulfate. The direct repair method for waste ternary lithium battery cathode materials provided by this invention can obtain repaired cathode materials with stable crystal structure, low impurity content, and good electrochemical performance recovery, balancing repair effectiveness and process economy.

This invention provides a method for synthesizing high-purity lithium sulfate and the resulting high-purity lithium sulfate. The method includes sequentially subjecting a lithium-sodium stock solution to precipitation for impurity removal, extraction, washing, and back-extraction to obtain a primary lithium sulfate solution. After degreasing the primary lithium sulfate solution, ammonium sulfate is used as a settling agent for precipitation treatment to obtain lithium sulfate precipitate. This precipitate is then dissolved, ultrafiltered, and adsorbed for deep impurity removal, followed by crystallization and secondary crystallization to obtain a high-purity lithium sulfate product with a purity ≥99.9%. The method for synthesizing high-purity lithium sulfate provided by this invention utilizes an extraction process to separate lithium and sodium, and uses ammonium sulfate as a settling agent. This allows for efficient and stable precipitation of lithium sulfate without introducing additional impurities. Furthermore, ammonium sulfate is readily available and inexpensive. Therefore, the method for synthesizing high-purity lithium sulfate provided by this invention is beneficial for thoroughly removing impurities and achieving high lithium recovery rates and purity.

The present invention relates to a method for producing lithium sulfide, the method comprising the steps of: preparing lithium sulfide containing impurities; and removing the impurities from the lithium sulfide, wherein the step of removing the impurities comprises a step of pyrolyzing at least one of lithium carbonate (Li2CO3) and lithium sulfate (Li2SO4).

Process for obtaining lithium sulfate that involves generating salts from sulfated brines to be subsequently processed and generate finished products such as lithium carbonate and / or lithium hydroxide monohydrate. The process includes optimizing the precipitation of Li2SO4*H2O in ponds, for which it includes adding magnesium chloride or calcium chloride to the natural brine, decreasing the SO4 / Mg ratio, avoiding the precipitation of other sulfated salts that later concentrate together with the lithium sulfate in a flotation stage, minimizing the performance of the collector in the plant and increasing the impurities in the final product.

The application provides a method for removing iron and aluminum from leaching solution in lithium mica waste lithium extraction process, and relates to the technical field of solid waste treatment. The method for removing iron and aluminum from leaching solution in lithium mica waste lithium extraction process comprises the following steps: step S1, leaching solution pretreatment, solid-liquid separation is performed on the leaching solution to remove insoluble substances, and a clear lithium sulfate-containing leaching solution is obtained; and component analysis is performed; step S2, metal impurities are removed in stages: step S21, iron and aluminum are removed by neutralization precipitation; step S22, aluminum is removed by deep neutralization precipitation; step S3, solid-liquid separation and washing; and step S4, washing utilization. The method has high selectivity and less loss of valuable metals: by accurately controlling pH in stages, Fe 3+ is precipitated first at a lower pH, and Al 3+ is precipitated at a higher pH, so that the precipitation pH range of lithium, rubidium and cesium ions is effectively avoided, thereby greatly reducing their coprecipitation loss and surface adsorption loss. The one-time precipitation recovery rate of lithium can be increased to more than 99%.

A dry thermal reaction-based method for producing lithium sulfate from black mass or black powder and converting same into lithium hydroxide, according to one embodiment of the present invention, can produce lithium sulfate and convert same into lithium hydroxide through water leaching and a dry thermal reaction, which uses a sulfate additive. In addition, unlike a conventional secondary battery waste resource recycling process, strong acid and alkaline solutions are not used, and thus environmental pollutants such as waste liquid and waste slurry are not generated, thereby significantly reducing environmental treatment costs. Additionally, lithium recovery efficiency is high due to the high solubility of lithium sulfate (about 27 times that of lithium carbonate). Further, a resource circulation process such as reusing metal sulfate residues, which are process by-products, as a sulfate additive without additional post-treatment, recycling process water (ultrapure water) and recycling generated dust can be implemented.

Processes for treating an aqueous composition comprising lithium sulfate and sulfuric acid. The processes comprise evaporatively crystallizing the aqueous composition comprising lithium sulfate and sulfuric acid under conditions to obtain crystals of lithium sulfate monohydrate and a lithium sulfate-reduced solution; and optionally separating the crystals of the lithium sulfate monohydrate from the lithium sulfate-reduced solution. The processes optionally further comprise concentrating the lithium sulfate-reduced solution under conditions to obtain an acidic condensate and a concentrate comprising sulfuric acid.

This utility model discloses a high-efficiency lithium sulfate solution calcium removal reactor, relating to the field of lithium sulfate processing technology. It includes a reaction chamber with a lithium sulfate solution inlet and a calcium removal agent inlet mounted on its upper surface. An agitator shaft is installed inside the reaction chamber. Vertical rods are mounted above horizontal bars, and agitator blades are mounted on the agitator shaft. First scrapers are mounted on the outer sides of the horizontal bars, and second scrapers are mounted below the horizontal bars. A discharge pipe is installed at the bottom of the reaction chamber, and a conveying auger is fixedly connected to the agitator shaft. A water storage tank is installed on the left side of the reaction chamber. When cleaning the reaction chamber is required, a circulating water pump draws water from the water storage tank through a pumping pipe, and the water is sprayed through a cleaning nozzle on the discharge pipe to simply rinse the agitator blades. The agitator blades stir the cleaning solution in the reaction chamber, and together with the first and second scrapers, the interior of the reaction chamber is cleaned.

The application discloses a method for treating black powder of waste power battery. Lithium is preferentially extracted from the black powder through high-pressure leaching, and lithium sulfate solution and lithium extraction residue are generated. The lithium extraction residue is subjected to acid leaching to obtain leaching solution. The leaching solution is subjected to organic extraction containing carboxylic acid extractant, and iron, aluminum and copper are sequentially separated and recovered. The raffinate after copper separation is subjected to P204 manganese extraction, P507 cobalt extraction and C272 magnesium extraction in sequence, and manganese sulfate solution, cobalt sulfate solution, magnesium sulfate solution and nickel sulfate solution are obtained. Compared with the prior art, lithium is extracted through high-pressure leaching, SO2 tail gas is eliminated from the source, high-temperature roasting is not needed, and the method is clean and efficient. Meanwhile, iron, aluminum, copper and magnesium removed as hazardous waste in the traditional process are converted into by-products such as iron sulfate, aluminum sulfate, electrodeposited copper and magnesium sulfate through carboxylic acid extraction, and high-value resourceization of impurity elements is realized. The method has the advantages of high valuable metal yield, low cost, green environmental protection and the like, and realizes efficient resource utilization of nickel, cobalt, lithium, iron, aluminum and copper in the black powder of the waste power battery.

This application relates to the fields of chemical and new energy materials technology, and in particular to a method for preparing battery-grade lithium carbonate from lithium sulfate and battery-grade lithium carbonate powder, which includes steps such as interface control reaction, precipitation reaction, aging treatment, solid-liquid separation, washing, and drying. By optimizing the type and amount of crystallization modifier, the precipitant dropping rate, reaction conditions, and post-processing, the purity, particle size distribution uniformity, and crystal morphology regularity of lithium carbonate are significantly improved. This application also provides an apparatus and process parameter optimization method for optimizing the lithium carbonate crystallization process, which can achieve fully automated production and improve product quality consistency. The obtained battery-grade lithium carbonate powder is suitable for preparing lithium iron phosphate, ternary materials, or lithium cobalt oxide lithium battery cathode materials, and can significantly improve the energy density, cycle life, and charge / discharge efficiency of lithium batteries.

The present invention relates to a secondary battery electrolyte, which includes a composite electrolyte salt; the composite electrolyte salt comprises lithium hexafluorophosphate, lithium difluorosulfonate, and lithium sulfide salts; the lithium sulfide salts include substituted sulfates (R1—SO3—Li) and / or sulfonate structure lithium salts (R2—O—SO3—Li). The present invention employs a combination of LiPF6, lithium sulfide salts, and LiFSI, where LiFSI exhibits better hydrolysis stability, superior thermal stability, and higher lithium migration capability, significantly enhancing the battery's kinetics and high-temperature performance. Lithium sulfates and sulfonate structure lithium salts also possess high lithium migration capabilities. Moreover, their anion groups rich in S and O form films that improve the composition of the SEI film and reduce membrane impedance, thereby enhancing the battery's kinetic and high-temperature performance.

The application discloses a mesoporous Al2O3-TiO2 sulfonated electrodialysis ion exchange membrane and a preparation method and application thereof, and belongs to the technical field of ion exchange membranes and resource recovery. The method innovatively adopts hydrothermal compounding to construct gradient mAl2O3-mTiO2 composite inorganic materials, and combines with an alkalinization-grafting-sulfonation modification process to prepare mAl2O3-mTiO2 / PVDF-g-PSSA composite ion exchange membranes. By adjusting the mass fraction of mAl2O3 (10% to 40%) and the doping ratio of the composite material (0.5% to 2.0%), the precise regulation of the membrane structure and performance is realized. The application has controllable process, and raw materials are easy to obtain. The obtained membrane material has wide adaptability and excellent comprehensive performance, and realizes efficient resourceization and closed-loop recovery of lithium sulfate waste liquid.

The disclosure provides a preparation method of high-purity lithium sulfide and a sulfide solid-state electrolyte, and a solid-state battery. The preparation method of the high-purity lithium sulfide comprises the following steps: adding lithium sulfate, a high-reactivity carbon source and sulfur powder into water to perform wet ball milling treatment to obtain a homogeneous slurry; performing spray drying treatment on the homogeneous slurry to obtain microsphere precursors; performing reduction calcination treatment on the microsphere precursors to obtain coarse lithium sulfide; dissolving the coarse lithium sulfide in water, filtering and evaporating and concentrating to obtain crystalline lithium sulfide; and performing calcination and crushing on the crystalline lithium sulfide to obtain high-purity lithium sulfide. The introduction of the sulfur powder into the lithium sulfate and the high-reactivity carbon source promotes the deep reduction of sulfate ions, inhibits the generation of side reactions and Li2O, reduces the oxygen content and carbon residues, and obtains lithium sulfide with less oxygen impurities and high purity. Through the combination of wet ball milling and spray drying, the microsphere precursors with uniform composition are obtained, which is beneficial to the subsequent high-temperature solid-phase reaction.

The present invention relates to a method for producing lithium hydroxide. The method for producing lithium hydroxide according to the present invention comprises: step (a), preparing lithium sulfate and sodium hydroxide; step (b), preparing a mixed solution by adding a solvent containing an alcohol to the lithium sulfate and sodium hydroxide; step (c), separating sodium sulfate decahydrate precipitated in the mixed solution to obtain a remaining lithium hydroxide solution; and step (d), obtaining lithium hydroxide from the lithium hydroxide solution, whereby lithium hydroxide usable for an energy storage device can be produced with less energy and cost compared to the prior art.

The utility model relates to lithium sulfate production technical field, aiming at the problem that the silicon content in lithium sulfate purification liquid is too high or the silicon content in purification liquid is unstable in the industrial production of lithium salt at present, specifically discloses a kind of lithium sulfate purification system, along the direction of lithium sulfate purification liquid flow, including the main filter system and secondary filter system of sequential intercommunication, the feed end of main filter system is also equipped with lithium hydraulic filter press, the discharge end of secondary filter system is also connected with leaching solution tank;The main filter system includes the main filter tank and filter primary filter press of sequential intercommunication, and the feed end of main filter tank is provided with lime feed pipe, by the improvement of purification system, can reduce artificial intervention dependence, improve production continuity, effectively control the silicon content in purification liquid always keep low and stable level, and convenient operation, high working efficiency.