33 results about "Lithium sulfate" patented technology

The invention relates to a method for simultaneously preparing lithium hydroxide and sulfuric acid. The invention provides a method for simultaneously preparing lithium hydroxide and sulfuric acid, which comprises the following steps: preparing a bipolar membrane electrodialysis device which comprises a first bipolar membrane, an anion exchange membrane, a cation exchange membrane and a second bipolar membrane, and forming an acid chamber between the first bipolar membrane and the anion exchange membrane, a salt chamber is formed between the anion exchange membrane and the cation exchange membrane, and an alkali chamber is formed between the cation exchange membrane and the second bipolar membrane; a lithium sulfate aqueous solution is added into a salt chamber of the bipolar membrane electrodialysis device, a sulfuric acid aqueous solution is added into an acid chamber, and a lithium hydroxide aqueous solution is added into an alkali chamber; and discharging the desalted solution formed in the salt chamber of the bipolar membrane electrodialysis device, discharging the sulfuric acid aqueous solution formed in the acid chamber, and discharging the lithium hydroxide aqueous solution formed in the alkali chamber.

The invention discloses a method for recovering high-purity fluorine and silicon from fluorine-silicon slag and co-producing a low-alkali fluorine-free accelerator, which comprises the following steps: S1, dissolving the fluorine-silicon slag in a sodium hydroxide solution to obtain a solution A; s2, adding dilute sulphuric acid into the solution A, reacting until gel is obtained, and filtering to obtain filtrate A and high-purity silicon dioxide gel; s3, adding calcium sulfate and EDTA (Ethylene Diamine Tetraacetic Acid) into the filtrate A, stirring and reacting, and filtering after the reaction is finished to obtain calcium fluoride and filtrate B; and S4, taking clear water, heating, carrying out heat preservation, then adding aluminum sulfate, lithium sulfate, diethanol amine and the filtrate B obtained in S3, continuously stirring until the aluminum sulfate is completely dissolved, then adding hydrated magnesium silicate, continuously carrying out heat preservation stirring, and obtaining the low-alkali fluorine-free accelerator after stirring is finished. The method is simple in process and easy to implement industrially, and fluoride and silicon oxide obtained through separation are high in purity and beneficial to follow-up extension application; more importantly, high-value recycling of the fluorosilicon slag is achieved, and the problems of stockpiling waste and environmental pollution of the fluorosilicon slag are solved.

The application discloses a purification and dissolution-resisting production method of battery-grade lithium carbonate, which comprises the following steps: 1) primary purification: cooling and cold precipitation of a crude lithium sulfate solution to obtain a primary purified solution; 2) secondary purification: adjusting the pH with sodium hydroxide, adding a flocculating agent, and filtering to obtain a secondary purified solution; 3) tertiary purification: adjusting the pH with sulfuric acid, sequentially adding disodium ethylenediaminetetraacetate, oxalic acid and activated carbon, and filtering to obtain a tertiary purified solution; 4) carbonization and synthesis: determining the content of Li in the tertiary purified solution, adding solid Na2CO3 or Na2CO3 solution according to the content of Li, and reacting for 30 min; adding dodecyl primary amine and reacting for 30 min, and filtering to obtain crude lithium carbonate; 5) washing: washing twice with water, washing with ethanol, filtering and drying to obtain battery-grade lithium carbonate; and 6) mother liquor recovery. The battery-grade lithium carbonate produced has a purity higher than 99.95%, a yield higher than 99%, and a whiteness higher than 95%, and realizes safe and environment-friendly production with high purity, high yield and high whiteness.

The application relates to the technical field of lithium hydroxide production, and discloses a processing technology for preparing battery-grade lithium hydroxide, which comprises the following steps: lithium ore is crushed to a reasonable particle size and then is sent into a roasting furnace, lithium ore is destroyed through high-temperature roasting, the roasted ore clinker is sent into a reaction kettle, sulfuric acid solution is added to carry out acidification reaction, then water is added to carry out leaching, and a crude leaching solution containing lithium sulfate is obtained. The application is provided with a sealing element, the large contact area design of the L-shaped sealing strip improves the reliability of the primary sealing, the cooperation of the elastic pressing strip and the spring can effectively compensate for the slight deformation in the equipment operation process, the stability of the sealing performance is ensured, the double-sealing structure can effectively prevent the leakage of the heat exchange medium, the problems of resource waste, environmental pollution and equipment damage caused by medium leakage are avoided, the influence of cross contamination of different media on product quality is also avoided.

The invention discloses a method for extracting lithium sulfate from high-iron spodumene concentrate, which comprises the following steps: mixing high-iron spodumene concentrate, sulfate and carbonate, and processing to obtain powder; the mass ratio of the high-iron spodumene concentrate to the sulfate to the carbonate is 1: (0.3-0.8): (0.01-0.5); the powder is subjected to brick pressing forming, a powder green brick is obtained, and the powder green brick is dried and roasted at the temperature of 900-1050 DEG C; cooling and crushing the roasted powder green brick to obtain a roasted particle material; adding water into the roasted particle material, carrying out ball milling, and leaching to obtain a leaching solution and leaching residues; and carrying out purification and concentration treatment on the leachate to obtain the lithium sulfate. By implementing the method, the interference of iron impurities can be eliminated, and the cost is reduced while the lithium recovery rate is improved.

The present invention relates to a bipolar electrodialysis apparatus for producing lithium hydroxide and sulfuric acid from a lithium sulfate solution. A bipolar electrodialysis apparatus (100) for producing lithium hydroxide and sulfuric acid from lithium sulfate comprises: a positive electrode (20) and a negative electrode (30) that face each other; a first bipolar film (40), an anion-selective dialysis film (60), a cation-selective dialysis film (70), and a second bipolar film (50) that are disposed between the positive electrode (20) and the negative electrode (30); and a porous first nickel foam (80) disposed on the plane of the positive electrode (20) to be in close contact with each other and a porous second nickel foam (90) disposed on the plane of the negative electrode (30) to be in close contact with each other, wherein the nickel foams (80, 90) have a porosity of 50-90%.

The invention discloses a method for removing fluorine from a lithium salt solution, and particularly relates to the technical field of lithium salt solution impurity removal, and the method comprises the following steps: S1, adding sodium hydroxide or lithium hydroxide into lithium salt solutions such as lithium sulfate and lithium chloride to adjust the lithium salt solutions to be alkaline, so that the lithium hydroxide solution can be directly used; s2, adding calcium hydrogen phosphate into the alkaline lithium salt solution, stirring, and filtering to obtain a low-fluorine lithium salt solution; compared with the prior art, the calcium hydrophosphate is innovatively selected as the fluorine removal agent for the lithium salt solution, the fluorine-removed lithium salt solution is obtained by adding the calcium hydrophosphate into the alkaline lithium salt solution, controlling the reaction time and filtering, the fluorine content of the fluorine-removed lithium salt solution is lower than 5 mg / L, the fluorine ion removal effect is good, and corrosion of fluorine ions to equipment is avoided.

The invention provides a method for removing impurities from a lithium sulfate strip liquor, a lithium sulfate solution, a lithium-containing compound and application. The method comprises the following steps: firstly, mixing a lithium sulfate strip liquor, a first impurity removal agent and a second impurity removal agent to obtain a mixed solution; the pH value of the mixed solution is adjusted to be acidic for the first time, a first filtrate and a first filter residue are obtained after the first reaction, the first impurity removing agent comprises a vulcanizing agent, and the second impurity removing agent comprises a calcium removing agent; the pH value of the first filtrate is adjusted to be alkaline for the second time, and second filtrate and second filter residues are obtained after the second reaction; and further treating the second filtrate to obtain a purified lithium sulfate solution. According to the impurity removal method provided by the invention, the concentration of divalent cation impurities such as copper, iron, calcium and magnesium in the lithium sulfate strip liquor can be greatly reduced, so that the purified lithium sulfate solution can meet the process requirements of a bipolar membrane system for preparing a lithium-containing product, and the large-scale production of the high-purity and high-efficiency lithium-containing product is realized.

The invention discloses a method for extracting lithium sulfate from spodumene concentrate, which comprises the following steps: mixing spodumene concentrate and auxiliary materials, and processing to obtain powder; the auxiliary materials comprise a first auxiliary material and a second auxiliary material, the first auxiliary material is lithium-containing tail mud, and the second auxiliary material is sulfate and / or carbonate; the powder is subjected to brick pressing forming, a powder green brick is obtained, and the powder green brick is dried and roasted at the temperature of 900-1050 DEG C; the roasted powder green bricks are crushed, and roasted particle materials are obtained; adding water into the roasted particle material, carrying out ball milling, and leaching to obtain a leaching solution and leaching residues; and carrying out purification and concentration treatment on the leachate to obtain the lithium sulfate. By implementing the method, base plate-free direct roasting can be realized, and the cost is reduced while the lithium recovery rate is improved.

Provided is a method for purifying a lithium sulfate solution, comprising the steps of: leaching a lithium-containing ore with sulfuric acid to obtain a lithium sulfate solution mixed with a leach residue; adding an alkaline supplementary material to the lithium sulfate solution mixed with the leach residue to form a magnesium precipitate; and removing the magnesium precipitate and the leach residue by solid-liquid separation, wherein the step of forming the magnesium precipitate is performed at a pH higher than the isoelectric point of the magnesium precipitate and lower than the isoelectric point of the leach residue.

The present invention provides an optimized method for recovering high-purity lithium sulfate from a lithium-containing composite oxide deposited on an eroded surface of a waste sagger discarded. Therefore, when the method for producing high-purity lithium sulfate from a waste sagger of the present invention is used, it is expected not only to be able to produce high-purity lithium sulfate that can be used for manufacturing lithium secondary batteries by recycling a discarded waste sagger, but also to be able to recycle a positive electrode active material, iron oxide, alumina, silicate, and calcium carbonate obtained as by-products during the production process of the lithium sulfate.

Embodiments provides a process of extracting lithium from spodumene. The process comprises providing a lithium sulfate solution (12) formed from leaching spodumene with sulfuric acid, and adding calcium chloride to the lithium sulfate solution to form a lithium chloride solution and to precipitate gypsum, for example in a conversion unit (14). The lithium chloride solution may then be subject to a sorbent process to selectively adsorb lithium ions to a sorbent, for example in a sorbent unit (16), and form a lithium-depleted solution (20). The process also includes desorbing the lithium ions from the sorbent to produce a lithium-rich solution (24).

The application discloses a method for recycling battery powder in an integrated whole chain, which comprises the following steps: firstly, the content of copper and aluminum in the subsequent separation process is reduced as much as possible by using the method of centrifugal gravity separation, so as to reduce the cost of impurity removal; and secondly, the battery powder is subjected to aerobic roasting, so that the battery powder reacts with iron sulfate, H2O2 and sulfuric acid. On the one hand, the long-chain organic matters such as the binder and the carbon-coated film attached to the surface of the lithium iron phosphate positive active material are removed, so that the hydrophilicity of the positive active material is restored, and the separation effect between the positive and negative active materials is enhanced. On the other hand, the aerobic roasting can make the battery powder react with iron sulfate, H2O2 and sulfuric acid to generate roasting products such as lithium sulfate. The lithium in the products after the aerobic roasting can be extracted by using water, and no reagent other than water is needed in the lithium extraction step, so that the lithium extraction efficiency is further improved.

The invention discloses a method for preparing lithium carbonate or lithium hydroxide through lithium sulfate desulfurization, and relates to the technical field of lithium compound preparation. According to the method, sulfate ions in a lithium sulfate solution are removed through a precipitation method or an extraction method, metal ion impurities such as Fe, Al and Mg existing in the solution are removed in a hydroxide precipitation mode in the mode of adjusting the pH of the solution, finally lithium carbonate is generated through a lithium precipitation method, lithium hydroxide is generated through a cooling crystallization precipitation mode, and the lithium sulfate solution is obtained. Therefore, the purity of the product is obviously improved; after sulfate ions are removed by utilizing an extraction method, the alkalinity of the aqueous-phase lithium-containing solution is remarkably improved, so that the dosage of alkaline substances during subsequent lithium precipitation and pH adjustment is reduced, and the cost of raw materials is greatly reduced; the method for preparing lithium carbonate or lithium hydroxide through lithium sulfate desulfurization is simple in reaction, easy and convenient to operate, easy to implement and suitable for large-scale industrial production of lithium carbonate and lithium hydroxide.

The invention relates to the technical field of metallurgy, in particular to a method for improving the leaching rate of clinker lithium. According to the leaching method, water washing is adopted in the immersion cleaning stage, acid washing is adopted in the leaching stage, under the condition that most lithium sulfate in the clinker can be leached out by water, insoluble lithium potassium sulfate double salt in the clinker is further dissolved through sulfuric acid leaching, and therefore the leaching rate of clinker lithium is increased. Wherein the dosage of the sulfuric acid can be determined according to an experimental formula, namely the total molar dosage of the sulfuric acid is 0.2 * molar weight of lithium in the clinker + 0.2 * molar weight of potassium in the clinker + 0.03 molar weight of sodium in the clinker. 10% dilute sulfuric acid is prepared according to the total molar weight of sulfuric acid to serve as leaching acid liquor, experiments confirm that the filtering performance of a filter cake is not obviously influenced when 10% acid is adopted as washing liquor, a good washing effect can be guaranteed, leaching liquor and the washing liquor are separated and purified respectively, and the treatment cost and loss of lithium in the solution can be reduced.

The application discloses a kind of 3D printing desert sand concrete mortar, printing method and application, and wherein, 3D printing desert sand concrete mortar is made of including the following weight parts of raw materials: fast hard sulphoaluminate cement 200-300 parts;Modified desert sand 100-200 parts;Silica fume 20-50 parts;Viscosity modifier 0.1-0.5 parts;Retarder 0.5-1.5 parts;Early strength agent 1-2 parts;Water 100-150 parts;Wherein, the modified desert sand is pickled and washed to neutral after drying desert sand, and its particle size range is 0.075-0.3mm.The viscosity modifier is warm wheel glue or xanthan gum, the retarder is sodium citrate or tartaric acid, the early strength agent is lithium sulfate or lithium carbonate, and water-cement ratio is 0.40-0.50.The application is optimized by raw material formula, desert sand modification treatment and printing process synergistic innovation, which solves the performance contradiction problem of 3D printing material and the technical problem of desert sand application, realizes resource local material and green low-carbon construction, and has significant practical value and broad popularization prospect in the field of 3D printing of desert area building.

The invention discloses a surfactant for an electrolyte determination reagent and a preparation method of the surfactant. The surfactant comprises alkyl glycoside, lithium dodecyl sulfate, lauroyl diethanolamide and a polyoxyethylene polyoxypropylene block copolymer, the mass ratio of the alkyl glycoside to the lithium dodecyl sulfate to the lauric acid diethanolamide to the polyoxyethylene polyoxypropylene block copolymer is 1: (0.1-5): (0.1-5): (0.1-5). The surfactant is stable in property, low in price, easy to obtain and environmentally friendly. The alkyl glycoside provides basic micelle construction, can reduce the initial surface tension of the system, and has low interference risk on electrolyte determination; the lithium dodecyl sulfate can enhance the dispersion stability, and the lithium salt avoids interference on sodium ion detection; lauroyl diethanolamide can provide a synergistic solubilizing effect, so that the dispersing capacity on lipid interferents is improved; the polyoxyethylene-polyoxypropylene block copolymer can resist high salt precipitation and inhibit hemolysis of a sample during testing. The components have a synergistic effect, so that the stability of the electrolyte determination reagent is improved.

A method of concentrating lithium containing solutions includes inputting a feed brine solution to an initial separation stage, the feed brine solution including lithium sulfate and one or more of sodium sulfate, potassium sulfate, calcium sulfate, and sodium chloride dissolved in water. In the initial separation stage, the feed brine solution is introduced to a pre-treatment membrane at a pressure that is less than the osmotic pressure of the feed brine solution. An initial permeate that passes through the pre-treatment membrane becomes the feed to a final separation stage, and an initial retentate that does not pass through the pre-treatment membrane includes a precipitate of at least one of the salts other than lithium sulfate. In the final separation stage, the initial permeate is introduced to a nanofiltration membrane at a pressure that is less than the osmotic pressure of the initial permeate. A final retentate that does not pass through the nanofiltration membrane is combined with the initial retentate to obtain a product solution having a higher concentration of dissolved lithium sulfate than the feed brine solution.

The process for obtaining potassium chloride (KCI) consists of a sequence of unit stages to obtain a commercial grade product, which is a KCI obtained from low grade sources. The process starts with the salts from the potassium carnallite precipitation pits and the tails from the lithium sulfate process. These then pass through a classification and grinding circuit, then a reverse flotation stage for sodium chloride removal, followed by a leaching stage and finally washing and filtering.

The application belongs to the technical field of lithium purification, and relates to a method for comprehensive development and utilization of magnesium sulfate sub-type salt lake resources, which comprises the following steps: adjusting the SO4 2‑ concentration and the molar ratio of Mg 2+ , SO4 2‑ in the composition of brine to be treated to preferentially precipitate K + and realize concentration and enrichment of lithium and boron elements in the salt lake brine. The application can make the brine directly precipitate potassium salt during concentration by controlling the SO4 2‑ concentration and the molar ratio of Mg 2+ , SO4 2‑ , realize separation of potassium element from the brine, and avoid precipitation of lithium element in the form of lithium sulfate by controlling the SO4 2‑ concentration in the composition of the salt lake brine, thereby improving the purity of potassium salt and the subsequent lithium element yield, solving the problem of loss of lithium in the form of lithium sulfate precipitate when the brine with a molar ratio of Mg 2+ , SO4 2‑ <4 is collected in the prior art, and the process does not need to remove magnesium, so that the loss of boron element is small, and effective recovery of boron element is realized.

The invention discloses a method for obtaining lithium sulfate by low-temperature sulfating roasting of waste lithium batteries, which comprises the following steps: mixing concentrated sulfuric acid with water, adding ammonium sulfate and sodium sulfate for dissolving, and stirring to obtain a composite sulfate solution; atomizing and spraying the composite sulfate solution to the surface of the positive electrode material of the waste lithium battery, and drying to obtain homogeneous microsphere particles; mixing the homogeneous microsphere particles with vinasse, and roasting in a protective atmosphere to obtain a roasted product; grinding the roasted product, and mixing and stirring the ground roasted product with water to obtain slurry; and adding a pH regulator into the slurry, and taking liquid after solid-liquid separation to obtain a lithium sulfate solution. According to the method, low-temperature sulfating roasting treatment is adopted, operation is easy, safety and reliability are achieved, the acid consumption is small, the production cost is low, efficient and low-carbon recycling of lithium resources in the waste lithium batteries is achieved on the industrial scale, and a subversive solution is provided for building a full-life-cycle green closed loop of the batteries.

The present invention provides an optimized method for recovering high-purity lithium sulfate from a lithium-containing composite oxide deposited on the eroded surface of a waste refractory crucible to be discarded. Therefore, by using the method for producing high-purity lithium sulfate from the waste refractory crucible of the present invention, not only can the discarded waste refractory crucible be reused to produce high-purity lithium sulfate that can be used in the production of lithium secondary batteries, but it is also expected that the positive electrode active material, iron oxide, alumina, silicate, and calcium carbonate obtained incidentally in the production process can be reused.

The invention discloses a method for extracting lithium from electrolytic aluminum overhaul slag combined with high-aluminum-content battery powder, and relates to the technical field of solid waste comprehensive recycling. The method comprises the following steps: firstly, premixing overhaul slag powder and lithium iron phosphate battery powder to obtain powder A, wherein the fineness of the powder is greater than 150 meshes; adding sulfate, and continuously mixing for 0.5-2 hours to obtain powder B; the powder B is fed into a rotary furnace to be calcined for 2-5 h, and powder C is obtained, wherein the calcination temperature is 500-800 DEG C; the powder C is added into clear water to be stirred and leached for 1-3 h, the solid-to-liquid ratio is 1: (2-5), and the leaching temperature is 30-80 DEG C; filtering and washing to obtain leached tailings and leachate, wherein the tailings are used as raw materials of the environment-friendly brick; the lixivium is a lithium sulfate solution with the lithium concentration of 4-8 g / L, adding caustic soda flakes to remove impurities, enabling the filtrate to enter an MVR concentration system, and separating to obtain sodium sulfate salt and a lithium sulfate solution with the lithium concentration of 10-15 g / L; adding a certain amount of sodium carbonate into the lithium sulfate solution, stirring and precipitating lithium, filtering to obtain a lithium carbonate product and a lithium-containing sodium sulfate solution, and returning the lithium-containing sodium sulfate solution to the MVR for further concentration.

The application provides a dilute acid concentration process of a metal ion leaching process, relates to the technical field of lithium extraction from spodumene, and comprises the following steps: S1: purifying leaching solution generated in a metal ion leaching process to obtain purified lithium sulfate solution; S2: the purified lithium sulfate solution enters a bipolar membrane electrolysis device to be electrolyzed to obtain acid liquor; S3: the acid liquor generated by the bipolar membrane electrolysis is delivered to a buffer tank; S4: the acid liquor in the buffer tank is delivered to an evaporation concentration device to be evaporated and concentrated; and S5: the acid liquor after evaporation and concentration is concentrated again by a secondary concentration device. The leaching solution is purified to obtain low-impurity purified lithium sulfate solution, and acid / base separation is realized through bipolar membrane electrolysis, so that 10% low-impurity dilute sulfuric acid is generated, the dilute sulfuric acid generated by electrolysis can be directly used for metal leaching after concentration, the acid consumption cost of the leaching process is reduced, the environmental protection risk of waste acid discharge is eliminated at the source, and the loss of lithium metal is avoided.

The application relates to the technical field of lithium ion battery recycling and lithium salt preparation, and specifically discloses a preparation method for preparing battery-grade lithium carbonate by using lithium sulfate solution purified from waste lithium batteries as a lithium source, which comprises four steps of primary lithium precipitation, secondary lithium precipitation, MVR evaporation concentration and centrifugal washing; in the secondary lithium precipitation process, MVR concentrated solution is used as a precipitant to precipitate lithium in supernatant of the primary precipitation and centrifugal mother liquor; part of sodium sulfate is removed from the MVR concentrated solution, not only reducing the introduction of sodium ion impurities, realizing resource recycling, but also avoiding the introduction of too high sodium ion concentration, thereby avoiding the exceeding of sodium impurities in the final product, simplifying the washing process of lithium carbonate crystals, only adopting reslurry washing and pure water washing processes, reducing lithium dissolution loss, improving the lithium recovery rate, saving the washing time, the sodium carbonate consumption during lithium precipitation and the consumption of sulfuric acid and liquid alkali during decarburization, and reducing the input cost.

The invention discloses a comprehensive utilization method of electrolytic aluminum overhaul slag combined with ardealite, and relates to the technical field of comprehensive recovery of solid wastes. The method comprises the following steps: mixing overhaul slag powder, ardealite powder and calcium oxide powder to obtain powder A, wherein the fineness of the powder is greater than 150 meshes; the powder A is fed into a rotary furnace to be calcined for 2-5 h, and powder B is obtained, wherein the calcination temperature is 500-800 DEG C; the powder B is added into clear water to be stirred and leached for 1-3 h, the solid-to-liquid ratio is 1: (2-5), the leaching temperature is 30-80 DEG C, and leaching tailings and leaching liquid are obtained through filtering and washing; washing residual salt in the tailings, and drying the tailings to serve as a fluoroaluminate cement raw material; the lixivium is a lithium sulfate solution, and the lithium concentration is 2-4g / L; the lithium sulfate solution directly enters an MVR concentration system, and sodium sulfate and the lithium sulfate solution with the lithium concentration being 8-12 g / L are obtained through separation; adding a certain amount of sodium carbonate into the lithium sulfate solution, stirring and precipitating lithium, filtering to obtain a lithium carbonate product and a lithium-containing sodium sulfate solution, and returning the lithium-containing sodium sulfate solution to the MVR for further concentration.

The application discloses a lithium ion battery electrolyte and a lithium ion battery thereof, which comprises a lithium salt, an organic solvent and an additive; the additive comprises a phosphoric acid siloxane compound A with a structure of formula I, and / or a lithium sulfate salt compound B with a structure of formula II, and / or a triisocyanate compound C with a structure of formula III, and / or a film-forming additive D; in the formula I, R1 and R2 are selected from alkyl, alkenyl and alkynyl with 1-5 carbon atoms, and R3, R4, R5, R6, R7 and R8 are selected from alkyl, alkenyl, alkynyl with 1-5 carbon atoms, or trifluoromethyl and fluorine atoms; in the formula II, X is selected from alkenyl, alkynyl with 1-5 carbon atoms, or alkyl substituted by fluorine atoms; and in the formula III, Y is selected from alkyl with 1-10 carbon atoms, or alkyl with 1-10 carbon atoms substituted by fluorine atoms.