23results about "Lithium hexafluorophosphate" patented technology

This invention relates to the field of lithium battery technology and discloses a method for purifying lithium hexafluorophosphate by continuous flow crystallization. The method includes: (1) adding a first organic solvent to crude lithium hexafluorophosphate to dissolve it, preparing a saturated lithium hexafluorophosphate-organic solvent solution, filtering to remove insoluble matter, and obtaining a saturated lithium hexafluorophosphate solution; (2) feeding the saturated lithium hexafluorophosphate solution and the second organic solvent into a microchannel reactor for cooling using metering pumps, filtering the precipitated crystals, washing them with a cooled third organic solvent, and then vacuum drying. The lithium hexafluorophosphate precipitated by the method of this invention has high purity and stable quality, making it very suitable for industrial promotion and application.

The application provides a purification method of lithium fluoride, high-purity lithium fluoride, lithium hexafluorophosphate, an electrolyte and a device, and the purification method of the lithium fluoride comprises the following steps: performing water washing treatment on the lithium fluoride to be purified at 0-50 DEG C to obtain a mixture containing a first solid-phase product; performing ultrasonic treatment on the mixture at 20-25 kHz to obtain a second solid-phase product through filtration; performing fluorination reaction on the second solid-phase product with electronic-grade anhydrous hydrofluoric acid to obtain a third liquid-phase product; performing ion exchange on the third liquid-phase product by using a chelating resin at 0-80 DEG C, and then performing cooling evaporation crystallization, and obtaining a fourth solid-phase product through filtration; and performing cleaning treatment on the fourth solid-phase product by using inert gas at 150-250 DEG C to obtain high-purity lithium fluoride. The high-purity lithium fluoride obtained by the purification method has low content of lithium carbonate and other impurities, and is beneficial to improving the performance and stability of subsequent products.

A method for generating / synthesising a metal hexafluorophosphate is disclosed which comprises dissolving ammonium hexafluorophosphate in tetrahydrofuran (THF) solvent, and flowing the resulting dissol

Provided herein are compositions and methods of making compositions useful in the production of battery electrolyte precursors and battery electrolytes.

The invention relates to a preparation process of high-purity lithium hexafluorophosphate, which comprises the following specific steps: S1, quantitatively adding anhydrous hydrogen fluoride into a corresponding reaction kettle body, and controlling the environment temperature in the reaction kettle body at-50 DEG C to-20 DEG C through a temperature control device; s2, maintaining the pressure in the reaction kettle body at 0.1-0.5 MPa, dispersing and adding solid phosphorus pentachloride into the reaction kettle body through a corresponding feeding device, and enabling the solid phosphorus pentachloride to react with the anhydrous hydrogen fluoride in the step S1 at the temperature of-50 DEG C to-20 DEG C to obtain phosphorus pentafluoride and gaseous hydrogen chloride, the gaseous hydrogen chloride escapes from the reaction liquid and then is discharged for recovery or absorption treatment; and S3, dispersing and adding lithium fluoride into the reaction kettle body through the feeding device, and carrying out complexing reaction on the lithium fluoride and phosphorus pentafluoride in the anhydrous hydrogen fluoride to obtain lithium hexafluorophosphate. The reaction process is high in controllability, so that the high-purity lithium hexafluorophosphate product can be stably prepared.

The application discloses a preparation method of a flame-retardant lithium hexafluorophosphate organic solution, lithium hexafluorophosphate and a lithium battery. The preparation method comprises the following steps: mixing and reacting a lithium hexafluorophosphate salt and a benign flame-retardant solvent solution containing a lithium compound to obtain a lithium hexafluorophosphate solution with a flame-retardant effect, wherein the benign flame-retardant solvent comprises at least one of a phosphate ester and a phosphite ester; removing part of the solvent in the lithium hexafluorophosphate solution with the flame-retardant effect to obtain a concentrated solution; adding a carbonate to the concentrated solution to remove impurities; and then removing the carbonate to obtain the flame-retardant lithium hexafluorophosphate organic solution. The preparation method of the flame-retardant lithium hexafluorophosphate organic solution provided by the application does not require a strict anhydrous and anaerobic reaction environment, and the reaction speed is fast. The obtained flame-retardant lithium hexafluorophosphate organic solution does not need to go through processes such as drying, crystallization and dissolution, and can be directly used in a battery and has a certain flame-retardant property. The performance of the flame-retardant lithium hexafluorophosphate organic solution is similar to that of a commercial electrolyte.

The invention relates to reaction equipment for preparing lithium hexafluorophosphate, which comprises a reaction kettle body, and a stirring shaft is rotatably mounted in the reaction kettle body; the feeding assembly comprises a set of discharging hoppers, and fixing plug bodies are installed on the bottom sides of the discharging hoppers in a liftable mode; the dispersing and discharging assembly comprises a set of arc-shaped guide grooves formed in the lower side of the fixed plug body, and the middles of the arc-shaped guide grooves protrude upwards; when the arc-shaped material guide groove rotates to pass through the bottom side of the fixed plug body, the driving mechanism drives the fixed plug body to leave the discharging opening of the discharging hopper; the heat exchange jacket is fixedly mounted on the outer side of the reaction kettle body, corresponding fixing grooves are concavely formed in the bottom side of the reaction kettle body at intervals, and corresponding heat exchange containers are respectively mounted in the fixing grooves in a swinging manner. According to the invention, the blanking uniformity of the material can be effectively and greatly improved, and the uniformity of the reaction temperature of the material in different reaction area ranges can be effectively and obviously improved.

The application discloses a continuous preparation process and device of liquid lithium hexafluorophosphate, and comprises the following operation steps: A10), continuously feeding lithium fluoride suspension to the top of a hexafluoride reaction plate tower; continuously feeding gaseous high-purity phosphorus pentafluoride to the bottom of the hexafluoride reaction plate tower; A20), carrying out reaction in the hexafluoride reaction plate tower, and feeding the reaction product from the bottom of the hexafluoride reaction tower into a bottom tank; A30), feeding the remaining reaction product output by a circulating heat exchanger into a liquid lithium hexafluorophosphate product extraction tank in one way and into a lithium fluoride suspension preparation kettle in the other way; and A40), connecting a filter to the product extraction end of the product extraction tank to remove the excessive solid-phase material after reaction, so as to obtain the liquid lithium hexafluorophosphate, the hydrogen chloride content of which is less than 25 ppm, and the hydrogen fluoride is not detected; the application has high continuous level and stability, does not need additional deacidification treatment, and has obviously higher output efficiency, and does not have the hidden troubles of shutdown maintenance due to problems such as blockage.

The crystallizer comprises a vertical container, the vertical container is installed on a fixing support through an elastic mechanism, and a vibration unit is further installed on the vertical container; a jacket matched with the vertical container in shape is arranged outside the vertical container, a refrigerant cavity is formed between the jacket and the vertical container, and the jacket is further provided with a refrigerant inlet and a refrigerant outlet which are communicated with the refrigerant cavity; the vertical container is provided with a mother liquor feed port, a nitrogen inlet, a mother liquor outlet and a discharge port; the discharge port is positioned at the bottom of the vertical container and is used for discharging crystallized materials, and meanwhile, a discharge valve for controlling the discharge port to be opened and closed is also arranged at the discharge port; the nitrogen inlet and the mother liquor outlet are positioned at the top of the vertical container, and a mother liquor insertion pipe downwards extending into the vertical container is also arranged at the mother liquor outlet. The device is simple in structure, easy to operate and capable of prohibiting external air from making contact with materials, controlling the amount of insoluble substances of lithium hexafluorophosphate and ensuring the stability of the quality of lithium hexafluorophosphate.

The present application relates to the technical field of chemical engineering, and provides a lithium hexafluorophosphate solution, and a preparation method therefor and a device therefor. The method comprises: performing a first contact reaction on a first phosphorus pentafluoride gas and a lithium fluoride solution to obtain a first reaction product; performing a second contact reaction on the first reaction product and a second phosphorus pentafluoride gas to obtain a second reaction product; and performing a third contact reaction on the second reaction product and a third phosphorus pentafluoride gas to obtain the lithium hexafluorophosphate solution. The phosphorus pentafluoride gas is step-fed, such that the feeding ratio of phosphorus pentafluoride to lithium fluoride can be dynamically and accurately controlled; and according to the reaction kinetic characteristics, the reaction process is optimized, and the chemical reaction speed between phosphorus pentafluoride and lithium fluoride is accelerated, so the lithium hexafluorophosphate solution can be efficiently synthesized in a short time, and the purity and the yield of the lithium hexafluorophosphate solution are improved.

A method for recovering lithium salts from a lithium battery waste mass, comprising: (a) dissolving the lithium salts in the lithium battery waste mass in a weight of water equivalent to 100 to 0.1 times the weight of the lithium battery waste mass, either in a one-time process or in a continuous process; (b) evaporating the aqueous solution to dryness; and (c) agitating the dry residue with a solvent comprising water, a carbonate, or a mixture thereof.

The present invention provides a method for producing phosphorus trifluoride and a method for producing phosphorus pentafluoride, which have high reaction efficiency, low reaction temperature and an excellent energy efficiency. The method for producing phosphorus trifluoride comprises: a step of introducing phosphorus trichloride and hydrogen fluoride into a first reactor; and a step of discharging phosphorus trifluoride from the first reactor, wherein the first reactor contains carbon material. The method for producing dichloro-phosphorus trifluoride comprises a step of introducing the phosphorus trifluoride obtained above and chlorine into a second reactor; and a step of discharging dichloro-phosphorus trifluoride from the second reactor. The method for producing phosphorus pentafluoride comprises: a step of introducing the dichloro-phosphorus trifluoride obtained above and hydrogen fluoride into a third reactor; and a step of discharging phosphorus pentafluoride from the third reactor. The method for producing lithium hexafluorophosphate comprises a step of introducing the phosphorus pentafluoride obtained above and lithium fluoride into a fourth reactor; and a step of discharging lithium hexafluorophosphate from the fourth reactor.

The application provides a preparation method and application of a sodium hexafluorophosphate concentrated solution and belongs to the field of batteries. Sodium halide and phosphorus pentachloride are reacted in a solvent (first reaction), a precursor solution generated in the reaction is reacted with hydrogen fluoride (second reaction), a sodium hexafluorophosphate solution is generated, and then degassing, filtration, concentration, dilution and resin deacidification are sequentially performed to obtain the sodium hexafluorophosphate concentrated solution. Then, impurities are removed by degassing, filtration, concentration, dilution and deacidification resin to obtain a final product. The sodium hexafluorophosphate concentrated solution product obtained by the application can be used as an electrolyte salt for a sodium ion battery electrolyte, and has the same or higher battery performance as that of a common sodium hexafluorophosphate crystal.

The application relates to a preparation method of lithium hexafluorophosphate and belongs to the field of preparation of lithium hexafluorophosphate. The preparation method comprises the following steps: carrying out high-pressure dry reaction of lithium fluoride solid and phosphorus pentafluoride gas, then continuously introducing the phosphorus pentafluoride gas to pressurize to 3.4 MPa or above and keep pressure, and cooling and decompressing to prepare lithium hexafluorophosphate; the pressure of the high pressure is 0.9-2.5 MPa, and the particle size of the lithium fluoride solid is 200-600 meshes. The reaction system is pressurized to 3.4 MPa or above and kept pressure, so that the phosphorus pentafluoride gas reaches a gas-liquid supercritical state, the fine lithium hexafluorophosphate crystal particles are rearranged and grown in the environment, and are approximately dissolved in the gas-liquid supercritical state of the phosphorus pentafluoride; in this way, the phosphorus pentafluoride can penetrate into the crystal grain and further react with the lithium fluoride, the residual lithium fluoride impurities are reduced, and the purity of the lithium hexafluorophosphate is improved.

Provided herein are compositions and methods of manufacturing compositions useful in producing battery electrolyte precursors and battery electrolytes.

The application discloses a kind of liquid lithium hexafluorophosphate degassing device and its degassing method, including scraper evaporator E201, concentrated collection tank V301 after degassing, condenser E202, solvent collection tank V303 and vacuum pump P103, wherein, the scraper evaporator E201 is connected with the delivery pipeline of liquid lithium hexafluorophosphate raw material, and the liquid lithium hexafluorophosphate raw material is under the action of heating and rotating centrifugal force of the scraper evaporator E201, part liquid produces vaporization, and the material of vaporization is transported to the condenser E202, and the liquid that is not vaporized is transported to the concentrated collection tank V301 after degassing;The output end of the condenser E202 is connected with the solvent collection tank V303, and the gas phase output end of the solvent collection tank V303 is connected with the vacuum pump P103;The application realizes high-efficiency excellent degassing effect, and finally ensures that the hydrogen chloride content of liquid lithium hexafluorophosphate after degassing treatment by the application is less than 10ppm, reliably guarantees its performance as lithium ion battery electrolyte.

The invention relates to a feeding device of reaction equipment for preparing lithium hexafluorophosphate, which comprises a group of blanking hoppers which are respectively arranged on two sides of the top of a reaction kettle body, fixed plug bodies are respectively arranged on the bottom sides of the blanking hoppers in a lifting way, and the fixed plug bodies are respectively upwards and fixedly connected with corresponding connecting rods; the connecting rods are movably connected to the discharging hopper through corresponding elastic connecting pieces. The dispersing and discharging assembly comprises a group of arc-shaped material guiding grooves formed in the lower side of the fixed plug body, the arc-shaped material guiding grooves are connected to a stirring shaft through first connecting rods, and a horizontal material dispersing assembly and a vertical material dispersing assembly are correspondingly arranged on the bottom sides of the arc-shaped material guiding grooves according to the height; and the driving mechanism comprises a traction assembly connected to the bottom side of the fixed plug body and a driving assembly connected to the top of the arc-shaped guide groove. According to the device, materials can be effectively and uniformly dispersed and discharged, so that the discharging uniformity of the materials is greatly improved.

The application discloses a Li + A preparation method of Li + Amino-functionalized mesoporous carbon adsorbent and liquid lithium hexafluorophosphate, which is suitable for an amino-functionalized impurity removal adsorbent in a hydrogen fluoride-containing system. A liquid lithium hexafluorophosphate solution is obtained by reacting a carbonate suspension of LiF with phosphorus pentafluoride, and then the solution is functionalized by an amino group, wherein the amino-functionalized agent is 3-aminopropyl dimethyl fluorosilane, which can exist stably in the impurity removal system containing hydrogen fluoride. In a conventional preparation method of the liquid lithium hexafluorophosphate, a silazane / phosphate or lithiumized molecular sieve is usually added to remove water, acid or metal ions, however, the addition of the additive will affect the performance of a battery, and the preparation process of the lithiumized molecular sieve is complex, and it is difficult to realize industrialization. The Li + The amino-functionalized mesoporous carbon adsorbent can realize deep removal of impurities in a liquid lithium hexafluorophosphate system.

Disclosed in the present invention are a continuous preparation process and device of liquid lithium hexafluorophosphate. The continuous preparation process comprises operation steps of: A10), continuously feeding a lithium fluoride suspension into the top of a hexafluorination reaction plate tower; and continuously feeding gas-phase high-purity phosphorus pentafluoride into the bottom of the hexafluorination reaction plate tower; A20), carrying out a reaction in the hexafluorination reaction plate tower, and enabling the reaction product to enter a tower bottom storage tank from the tower bottom of the hexafluorination reaction tower; A30), introducing part of the remaining reaction product output by means of a circulating heat exchanger into a liquid lithium hexafluorophosphate product extraction tank, and introducing the other part into a lithium fluoride suspension formulation kettle; and A40), connecting a filter to a product extraction end of the product extraction tank for removing redundant reacted solid-phase materials, so as to obtain liquid lithium hexafluorophosphate, wherein the hydrogen chloride content of the liquid lithium hexafluorophosphate is less than 25 ppm, and hydrogen fluoride is not detected. The present invention has a high continuous level and is stable, does not require an extra deacidification treatment, has a significantly higher output efficiency, and does not cause hidden dangers of halting production and maintenance due to problems of blocking, etc.

The application belongs to the technical field of electrolyte material preparation, and particularly relates to a method for continuously preparing lithium hexafluorophosphate. The preparation method comprises the following steps: uniformly mixing excess liquid PF5 and solid LiF in a beater, feeding the mixture into a continuous reactor, controlling the temperature in the reactor to be greater than 18.95 DEG C and the pressure to be greater than 3.39 MPa so that the PF5 is in a supercritical state and is stirred to react, and feeding the reaction material into a spray drying tower for solid-gas separation under reduced pressure, wherein the solid-phase product is lithium hexafluorophosphate, and the gaseous component is PF5 which is recycled as a reaction raw material after being compressed and condensed. In the preparation method, the supercritical PF5 is used as a reaction raw material and a heat and mass transfer carrier at the same time, the reaction efficiency can be significantly improved, and no other solvent or gaseous component is introduced, so that the lithium hexafluorophosphate can be efficiently and continuously prepared in high quality.

The application discloses a method for recycling and utilizing waste lithium battery electrolyte resources, and comprises the following steps: freezing and cutting the waste lithium battery, and then putting the waste lithium battery into an organic solvent for leaching; performing solid-liquid separation to obtain first filtrate and first filter residue; performing distillation on the first filtrate to obtain mother liquor and organic distillate; adding a complexing solvent into the mother liquor for reaction, and then performing filtration to obtain second filtrate and second filter residue; heating the second filter residue to obtain lithium hexafluorophosphate solid; adding an amine compound into the second filtrate, and then performing filtration to obtain third filter residue; and heating the third filter residue to obtain lithium bisfluorosulfonylimide solid. The method realizes extraction and recovery of lithium hexafluorophosphate and carbonate solvents in the electrolyte, and can extract pure lithium bisfluorosulfonylimide from lithium hexafluorophosphate crystallization mother liquor.

The present disclosure relates to a process for preparing high purity Lithium Hexafluorophosphate (LiPF6), comprising the steps of: (a) reacting high purified anhydrous hydrogen fluoride (AHF) gas with solid phosphorous pentachloride to produce a mixture of pure phosphorous pentafluoride and hydrogen chloride gas, (b) reacting highly purified lithium fluoride dissolved in AHF solution with phosphorous pentafluoride and hydrogen chloride gas mixture obtained in step (a) to obtain LiPF6 mother liquor, which is LiPF6 dissolved in AHF; crystallizing the LiPF6 from the mother liquor in static crystallizer, separating the mother liquor, drying the product to remove HF; followed by drying and crushing of the crystals of LiPF6 to obtain LiPF6 powder.

The invention relates to the technical field of lithium ion batteries, in particular to a preparation and purification method of lithium hexafluorophosphate. The invention overcomes the problems of low purity and low yield of lithium hexafluorophosphate prepared by the existing process. By adopting lithium fluoride with high specific surface area to cooperate with low-temperature gradient feeding, side reaction is inhibited from the source; the problem of solubility is solved by introducing a cooling crystallization step, and anhydrous hydrogen fluoride is efficiently separated and removed by cooperating with inert gas positive pressure difference filtration and pulse purging; by adopting a precooled solvent to cooperate with ultrasonic washing, high-selectivity deacidification and high yield are realized; a composite adsorption bed prepared from modified activated aluminum oxide and lithium fluoride powder is used for deeply removing moisture and hydrolysate; two-stage vacuum drying is cooperated with trace hot argon purging, so that thermal decomposition of lithium hexafluorophosphate at high temperature is inhibited.