28results about "Zirconium halides" patented technology

The present application provides a molten salt extraction and distillation separation device for zirconium and hafnium tetrachloride, comprising a distillation tower, a reboiler, a reflux tank, a circulation tank, a sublimator, a gas preheater, and a condenser. During installation, the various components are connected in sequence to obtain a complete molten salt extraction and distillation separation device for zirconium and hafnium tetrachloride. The device has a simple structure, is easy to operate, and is convenient to connect, and is suitable for the molten salt extraction and distillation separation of zirconium and hafnium tetrachloride.

A positive electrode material 1000 in one embodiment of the present disclosure comprises a positive electrode active material 110, a coating layer 111 that includes a first solid electrolyte and covers at least part of the surface of the positive electrode active material 110, and a second solid electrolyte 100. The first solid electrolyte contains Li, M1, and F. M1 is at least one selected from the group consisting of Ti, Al, and Zr. The second solid electrolyte 100 contains Li, M2, O, and X. M2 is at least one selected from the group consisting of Ta and Nb. X is at least one selected from the group consisting of F, Cl, Br, and I.

The application relates to a modified lithium-rich manganese-based material, a preparation method thereof, a positive plate and a battery. The modified lithium-rich manganese-based material comprises a double-alkali-metal manganese-rich matrix, and the expression of the double-alkali-metal manganese-rich matrix is as follows: Li 1+x Na z Mn a Co b Ni c M 1‑a‑b‑c O 2+x+z‑y D y ; wherein, 0

This invention discloses a process for preparing chlorides by reducing chlorination with rare metal oxides, comprising the following steps: S1, in an inert atmosphere, a mixture containing rare metal oxide powder, a reducing agent, and a chloride salt is subjected to a reduction reaction at a predetermined temperature 1; S2, the temperature is lowered to a predetermined temperature 2, oxygen is introduced, and the concentration of oxygen in the mixed gas is adjusted to carry out a chlorination reaction, and the chlorinated product is condensed and collected. This invention eliminates the need for gaseous chlorinating agents such as chlorine or hydrogen chloride, avoiding the leakage risks of liquid chlorine and compressed hydrogen chloride during storage and transportation; the raw materials can be directly rare metal oxides, with a wide range of sources, good process adaptability, and significantly reduced production costs.

Provided is a solid electrolyte (11) which has a compound that contains lithium, a halogen, and one or more elements that are selected from the group consisting of Zr, Al, Y, Zn, In, Ta, Nb, Hf, La, Ce, Ba, Sr, Ca, Mg, and Ga. The fluorine concentration in a surface region (11B) is higher than that in a central region (11A), and the thickness of the surface region (11B) is 1 nm to 1,000 nm.

The utility model discloses a device for purifying crude zirconium tetrachloride, which comprises a tank body, the top of the tank body is fixedly connected with a tank cover through a bolt, the top of the tank cover is communicated with a zirconium tetrachloride exhaust pipeline, the lower part of one side of the tank body is communicated with an argon pipeline, and one side, far away from the argon pipeline, of the tank body is communicated with a hydrogen pipeline. The utility model relates to the technical field of zirconium tetrachloride purification, in particular to a device for purifying crude zirconium tetrachloride, which can be used for treating waste gas generated during purification through the matching of a tank body, a tank cover and a treatment device, and can be used for carrying out auxiliary heating and heat preservation on the tank body by utilizing waste heat of the waste gas because the temperature of the waste gas is higher when the waste gas is exhausted. The heat in the tank body is prevented from being directly and rapidly dissipated through the tank body, so that the energy-saving performance is improved, and external treatment equipment is not needed for waste gas treatment, so that the input of the equipment can be reduced, and the investment of economic cost is reduced.

Disclosed herein is the compound (NaxLi3−x)(3−y) / 3Y1−yZryCl6, where x is greater than 0 and less than 3 and where y is greater than 0 and less than 1. Where x = 1 and y = 0.75, the compound is Na0.75Li1.5Y0.25Zr0.75Cl6. The compound is usable as an effective solid electrolyte for a solid-state battery. The solid electrolyte can utilize lithium ions and / or sodium ions as charge carriers.

The present invention describes a solid-state material having ionic conductivity for lithium ions, a composite comprising said solid-state material and a positive electrode active material, a method for preparing said solid-state material, the use of said solid-state material as a solid electrolyte in an electrochemical cell, a solid structure selected from the group consisting of a positive electrode (cathode), a negative electrode (anode) and a separator of an electrochemical cell comprising said solid-state material, and an electrochemical cell comprising such a solid-state structure.

This invention relates to the field of non-ferrous metal metallurgy, and particularly to a zirconium tetrachloride purification system and method. The zirconium tetrachloride purification system includes a purification furnace; a vacuum collection tank connected to the furnace via a first pipeline, on which an exhaust valve is installed, and a discharge port at the bottom of the vacuum collection tank; a circulating cooling water system connected to the vacuum collection tank; a filter connected to the vacuum collection tank via a second pipeline, on which a first pneumatic valve is installed; a tail gas spray tower connected to the filter via a third pipeline; and a control system electrically connected to the exhaust valve and the first pneumatic valve. This zirconium tetrachloride purification system and method solves the problems of low control accuracy and inherent dangers in existing zirconium tetrachloride purification methods.

[ 89 Zr][Zr(oxalate)4] 4- From salt 89 A method for synthesizing ZrCl4 is provided. 89 Zr]ZrCl4 is reacted with a biomarker targeting agent, 89 Zr-labeled radiopharmaceuticals can be produced. 89 Zr-labeled radiopharmaceuticals are used, for example, in non-invasive molecular imaging.

The invention discloses a multi-anion doped chlorine-based solid electrolyte as well as a preparation method and application thereof. The chemical formula of the polyanion doped chlorine-based solid electrolyte is ZrCl4.xLi3PO4.yLinA.zLiA '(0.2 < = x < = 0.7, 0.05 < = y < = 0.6, 0 < = z < = 1; linA is Li2S and / or Li3N, and LiA'is one or more of LiF, LiCl, LiBr and LiI). By introducing various anions, the multi-anion doped chloride solid electrolyte with high ionic conductivity is prepared. By adjusting the variety and proportion of anions, the electrochemical stability window of the chloride solid electrolyte can be broadened, and the chloride solid electrolyte can stably operate at the high voltage of 4.5 V when matched with a high-voltage positive electrode. In addition, the all-solid-state battery using the polyanion doped chloride solid electrolyte has excellent fast charging performance and cycling stability.

The application belongs to the technical field of sponge zirconium production and relates to a method for preparing and producing refined zirconium tetrachloride, which comprises the following steps: S1, boiling chlorination, a carbon powder filtering settler is connected to the gas outlet of a chlorination furnace, the gas outlet of the carbon powder filtering settler is connected to a hydrogen charging iron remover, the cavity temperature in the carbon powder filtering settler and the hydrogen charging iron remover is respectively controlled to be 400±10 DEG C, and hydrogen is introduced into the hydrogen charging iron remover; S2, condensation, the gas outlet of the hydrogen charging iron remover is sequentially connected with a first-stage condenser, a second-stage condenser and a third-stage condenser, the cavity temperature in the first-stage condenser is controlled to be 280±10 DEG C, the cavity temperature in the second-stage condenser is controlled to be 240±10 DEG C, the cavity temperature in the third-stage condenser is controlled to be 220±10 DEG C, and the condensed materials at the outlets of the condensers are all refined zirconium tetrachloride. The method can completely cancel the purification process of the traditional refined zirconium tetrachloride preparation process, and greatly saves energy, manpower and other costs.

The application provides a molten salt extraction rectification separation method of zirconium hafnium tetrachloride, and is particularly suitable for a molten salt extraction rectification separation device. In the molten salt extraction rectification separation, main components such as a rectification tower, a sublimer, a reflux tank, a condenser, a reboiler and a circulating tank are connected first, then zirconium hafnium chloride raw materials to be separated and chloride salt for rectification are filled, and finally the device is started to realize the separation of zirconium hafnium chloride under rectification conditions. The separation device and method have good usability and process adaptability, and the prepared zirconium tetrachloride and hafnium tetrachloride meet the use requirements in the fields of atomic energy, aerospace, high-power laser and integrated circuit, and provide reference and guidance for the research and development and application of the molten salt rectification separation technology and equipment of zirconium hafnium tetrachloride.

The utility model discloses a zirconium tetrachloride purification furnace cooler, which relates to the technical field of zirconium tetrachloride production, and comprises a sorting assembly, the sorting assembly comprises a hanging barrel, a condenser, an auxiliary heating pipe, a gas collecting chamber, an exhaust valve and a cooling pipeline, the condenser is sleeved outside the hanging barrel, the auxiliary heating pipe is inserted in the middle of the hanging barrel, and the air collecting chamber is sleeved outside the auxiliary heating pipe. The two sides of the hanging barrel are communicated with air collecting chambers, exhaust valves are arranged at the top ends of the air collecting chambers, cooling pipelines are communicated between the adjacent exhaust valves, and pipelines used for introducing air and cooling water for cooling are laid on the inner side of the condenser. The zirconium tetrachloride purification furnace cooler provided by the utility model has the characteristics that low-boiling-point impurities such as silicon tetrachloride, titanium tetrachloride and aluminum trichloride are enriched in the gas collection chamber and are intensively and automatically discharged, so that the loss amount of zirconium tetrachloride during exhaust is reduced, the impurity removal effect and the purity of refined zirconium tetrachloride are improved, the recovery rate of zirconium is improved, and the production cost is reduced. The working time consumption is short; the production efficiency is higher.

The invention discloses a solid electrolyte material as well as a preparation method and application thereof, and relates to the technical field of batteries. The chemical formula of the solid electrolyte material is Na < x > (OCN) < x > (ZrCl4) < y > and / or Na < x > (SCN) < x > (ZrCl4) < y >, x is larger than or equal to 1.5 and smaller than or equal to 2.5, and y is equal to 1. The invention also discloses a preparation method of the solid electrolyte material, which comprises the following steps: uniformly mixing sodium salt and zirconium chloride, and then carrying out sintering reaction in an inert atmosphere to obtain the solid electrolyte material. The solid electrolyte material has the advantages of excellent ionic conductivity, stable electrochemical performance and the like, and can be applied to the field of solid sodium-ion batteries.

The application discloses a preparation method of rare metal chloride, which comprises the following steps: in an inert atmosphere, a mixture containing rare metal powder, a chlorine salt and an auxiliary material is heated to a predetermined temperature, oxygen is introduced, the concentration of oxygen in the mixed gas is adjusted, a chlorination reaction is carried out, and a chlorination product is condensed and collected to obtain the rare metal chloride. The application avoids the safety production risk caused by the use of chlorine or hydrogen chloride in the traditional production, and the production process avoids the leakage risk of liquid chlorine and compressed hydrogen chloride in the storage and transportation process. Since the reaction process is a double decomposition reaction, the reaction rate is controllable, the reaction does not have obvious heat release, and is safe and reliable. The chlorine content in the production tail gas is extremely low, and the environmental pollution problem caused by a large amount of chlorine-containing tail gas in the traditional chlorination process is avoided.

A compound containing lithium, a tetravalent metal element M, chlorine and a dopant element X and having a reflection peak in each of 2θ angle ranges of 15° to 17°, 31° to 32.5°, 41° to 42.5°, 48.5° to 50° and 53° to 55° in an X-ray diffraction chart measured using a CuKa ray at 25°C, in which a half width of a reflection peak having a largest peak height in the 15° to 17° range is 0.35° to 3.00°.

The invention provides a zirconium-hafnium molten salt rectification separation system. The system comprises a rectification unit and a steam stripping unit, the rectification unit comprises a rectification tower, a reboiler and a reflux tank; the steam stripping unit comprises a steam stripping column, a fused salt extrusion tank and a gas preheater; the reboiler is respectively connected with the rectifying tower and the steam stripping column; the steam stripping column is respectively connected with the fused salt extrusion tank and the gas preheater; the reflux tank is respectively connected with the rectifying tower and the fused salt extrusion tank; the fused salt extrusion tank is also connected with a gas preheater; after the fused salt enriched by zirconium tetrachloride in the reboiler is subjected to steam stripping treatment by a steam stripping column, zirconium tetrachloride enters a steam stripping medium to be separated from the fused salt; the fused salt subjected to steam stripping further enters a rectifying tower to participate in a rectifying reaction, so that heat transfer and mass transfer balance in the rectifying tower is prevented from being damaged due to relatively high zirconium and hafnium chloride content in the fused salt; according to the method, the gas-liquid contact area is increased in a manner of separating zirconium tetrachloride by virtue of sieve plate bubbling and steam stripping, and the mass transfer rate of zirconium tetrachloride from a liquid phase to a gas phase can be remarkably improved at a relatively low temperature, so that the separation efficiency is improved.

The utility model discloses a zirconium tetrachloride purification automatic deflation device which comprises a furnace body, a pressure detector is assembled on the inner wall of the furnace body in a penetrating mode, the side end of a dust collection tank is fixedly communicated with a smoke exhaust pipe, the lower end of the dust collection tank is fixedly communicated with a drainage structure, and the temperature and pressure in the furnace are monitored through the pressure detector; a first electromagnetic valve is automatically controlled to be opened for exhausting, gas enters a dust collection tank through a flue, the amount of collected gas is guaranteed, meanwhile, by adjusting the proportion of argon introduced in the exhausting process, waste gas is injected into the flue through an argon injection structure, the waste gas is mixed, and the condition that the waste gas is condensed in a pipeline is reduced; according to the flue gas treatment device, flue gas can be effectively treated, water is used for absorbing the flue gas, the flue gas is discharged through the flue gas discharge pipe, environmental pollution is reduced, the discharged water is effectively filtered through the effect of the water drainage structure, reuse of the water is guaranteed, and the flue gas treatment device is convenient to use and high in practicability.

The application relates to a composite halide solid electrolyte and a preparation method thereof, and belongs to the technical field of solid electrolytes. The preparation method comprises the following steps: S1, under a protective atmosphere, uniformly ball-milling a lithium source, a zirconium source, an M source and an ammonium halide, and then sintering, and obtaining a nitrogen-rich halide through cooling; S2, under a protective atmosphere, transferring the nitrogen-rich halide into a reaction chamber of a fluidized bed vapor deposition reactor, then circulating and sequentially introducing a metal / metalloid source compound, water and a lithium source into the reaction chamber to carry out deposition, forming a conductive interface layer on the surface of the nitrogen-rich halide, and obtaining a composite halide; and S3, circulating and sequentially introducing an aluminum source and water into the reaction chamber to carry out deposition, forming a protective layer on the surface of the composite halide, and obtaining a composite halide solid electrolyte. The material can effectively adapt to cyclic stress, avoid cracking and peeling, and ensure the durability and reliability of the protection effect of the battery in the whole service life.

Processes for the synthesis of [89Zr]ZrCl4 from [89Zr][Zr(oxalate)4]4− salt are provided. The [89Zr]ZrCl4 can be reacted with biomarker targeting agents to produce 89Zr labelled radiopharmaceuticals. The 89Zr labelled radiopharmaceuticals find use in, for example, non-invasive molecular imaging.

The utility model discloses a chlorination furnace for sponge zirconium production, which comprises a chlorination furnace main body, the outer wall of the chlorination furnace main body is fixedly sleeved with a cooling structure, and the upper end of the side wall of the chlorination furnace main body is fixedly communicated with an air exhaust structure. The chlorination furnace main body can be effectively cooled, a cooling system is added, the temperature in the furnace is reduced, the corrosion effect of chlorine is reduced, the furnace body design is optimized, the contact area between chlorine and the metal surface is reduced, the flow of chlorine is accurately controlled, too high temperature and too high chlorine concentration are avoided, corrosion to the chlorination furnace is reduced, and the service life of the chlorination furnace is prolonged. The practicability is high.

The invention discloses an unqualified sponge zirconium closed-loop recovery method, and relates to the technical field of nuclear fuel circulation and materials.The method comprises the following steps that S1, irregular and porous unqualified sponge zirconium is converted into zirconium oxide blocks or particles with stable chemical components and uniform physical forms through a high-temperature oxidation reaction; s2, processing zirconium oxide blocks or particles obtained after oxidation into powder meeting the feeding requirement of a chlorination process through a ball milling process; and S3, mixing the qualified zirconium oxide powder subjected to ball milling with a carbon-containing reducing agent according to a set proportion, putting the mixed material into a reaction device for chlorination reaction, and condensing a product to realize efficient recovery of ZrCl4. According to the method provided by the invention, the treatment problem caused by the porous and irregular physical properties of the unqualified sponge zirconium can be solved, the high purity and the quality consistency of a final product are ensured, and the method can be directly embedded into a recovery process of an existing production process, so that the high-valued recycling of the unqualified sponge zirconium is realized.

The invention relates to a method for recovering the performance of a halide solid electrolyte. More specifically, when a halide-based solid electrolyte is heat-treated after exposure to air, the reduced ionic conductivity of the halide-based solid electrolyte due to exposure to air is restored to a level similar to that before exposure to air.

The invention provides a composite adsorbent as well as a preparation method and application thereof. The composite adsorbent comprises a rare earth element doped zeolite molecular sieve and a metal organic framework material, and can be used in a purification method for removing fluorine ions and fluorine-containing organic compounds from an acidic aqueous solution. The purification method comprises the following steps: a pretreatment step: filtering a to-be-treated acidic aqueous solution containing fluorine ions and fluorine-containing organic compounds; an adsorption step: performing adsorption treatment on the acidic aqueous solution by using the composite adsorbent, and removing fluorine-containing organic compounds from the acidic aqueous solution; and a coordination precipitation step: adding a zirconium / phosphate mixed solution into the adsorbed acidic aqueous solution to form a fluorine-containing precipitate. The technology provided by the invention can realize removal and purification of fluorine ions and fluorine-containing organic compounds in the acidic aqueous solution in a simple, efficient, cost-saving, no dangerous waste generation and high production capacity mode.

The utility model relates to the technical field of fluidizing chlorination furnace feeding, and discloses a spiral feeding device for a fluidizing chlorination furnace, which comprises a chlorination furnace feeding bin, the top of the chlorination furnace feeding bin is fixedly connected with a first feeding hopper, and the top of the chlorination furnace feeding bin is fixedly connected with a second feeding hopper. When the rotating disc rotates for a circle, the material baffle plate is not contacted with the discharging port of the first feeding hopper and the discharging port of the second feeding hopper any more, so that the discharging port of the first feeding hopper and the discharging port of the second feeding hopper are opened, materials fall into the feeding bin of the chlorination furnace, meanwhile, after the rotating disc rotates for a circle, the material baffle plate is reset, the cycle is repeated, and the material baffle plate moves in a reciprocating mode. Therefore, a large amount of materials are prevented from falling into the feeding bin of the chlorination furnace at a time, accumulation of a large amount of materials is avoided in the follow-up stirring process, the situation that the materials cannot be fully mixed is avoided, and the follow-up reaction effect is prevented from being affected.

The invention discloses a chlorination purification method for separating and recovering chromium, nickel and manganese impurities in a zirconium material, and relates to the technical field of nuclear fuel circulation and materials.The method comprises the following steps that S1, the impurity-containing zirconium material and a carbon-containing reducing agent are evenly mixed in proportion, the mixed material is placed in a reaction device, chlorine is introduced at the set temperature for a chlorination reaction, and a reaction product is obtained; a coarse ZrCl4 gaseous mixture is generated; s2, conveying a coarse ZrCl4 gaseous mixture generated by reaction into a gas phase conveying pipeline of a precondenser for precooling, so that main impurity chloride is preferentially condensed and separated out; and S3, introducing the pre-cooled gas-phase product into a main condenser for fractional condensation, thereby realizing efficient and stable removal of impurities and directional recovery of high-purity ZrCl4. According to the method provided by the invention, separation is realized by utilizing the obvious difference of volatilization temperatures of ZrCl4 and impurity chlorides such as Cr, Ni and Mn, the method can be directly embedded into an existing sponge zirconium chlorination production line, directional removal of impurity elements is realized, and the zirconium recovery rate is not lower than 90%.

The invention belongs to the technical field of solid electrochemistry and energy storage materials, and discloses a sulfite-based oxyhalide solid electrolyte material and a preparation method and application thereof. The sulfite-based oxyhalide solid electrolyte material is of an amorphous structure, and the chemical formula of the sulfite-based oxyhalide solid electrolyte material is (Na2SO3) xZrCl4, wherein x is more than or equal to 0.1 and less than or equal to 0.7. Compared with a traditional halide electrolyte, the sulfite-based oxygen halide solid electrolyte material has the advantages that the ionic conductivity is improved by one to two orders of magnitude, and an all-solid-state sodium ion battery assembled based on the material shows high efficiency, long cycle life, wide electrochemical stability window and excellent mechanical property; and the method has huge application potential in actual solid-state sodium ion battery devices.