42results about "Tungsten halides" patented technology

Disclosed are a tungsten hexafluoride preparation method and apparatus based on photoelectric synergy. A photocatalyst and metal tungsten are sequentially filled in a discharge area of a plasma reactor in a direction of gas entry, and the discharge area of the plasma reactor is irradiated with light at the same time; the background gas generates a large amount of plasma in the discharge area, SF6 undergoes decomposition under the synergistic effect of photocatalysis and plasma, SF6 is decomposed to generate fluorine atoms and low-fluorine sulfides such as SF5 and SF4. The generated fluorine ions, SF5, SF4 and low-fluorine sulfides further react with metal tungsten to generate WF6 specialty gas, which not only realizes the utilization of fluorine resources of SF6, but also replaces highly toxic fluorine gas with non-toxic SF6 exhaust gas in the plasma reactor for reaction, thereby ensuring safe operation and low energy consumption.

The present invention provides a precursor comprising a tungsten precursor and a carbonaceous material. The precursor comprises less than 0.02% by weight of the carbonaceous material, based on the total weight of the precursor. A method for purifying a tungsten precursor may comprise at least one of the following steps: obtaining a source vessel containing a tungsten precursor and a carbonaceous material; separating the tungsten precursor from at least a first portion of the carbonaceous material; recovering the precursor in the collection container; or any combination thereof.

The invention belongs to the technical field of fluorine-containing fine chemical synthesis, and particularly relates to a device and a method for improving tungsten hexafluoride synthesis efficiency of a fluidized bed reactor. The method comprises the following steps: adding tungsten powder and nickel powder into a stirring kettle, uniformly mixing the tungsten powder and the nickel powder to obtain a mixture, feeding the mixture into a reactor by using nitrogen, heating the reactor to 240-280 DEG C, introducing feed gas NF3 with the pressure of 0.2 MPa into the reactor through a first raw material tank / a second raw material tank, and reacting to obtain crude tungsten hexafluoride, after metal impurities are separated from the product gas through the first-stage cyclone separator and the second-stage cyclone separator, the product gas enters the heat exchanger to be cooled and finally enters the collecting tank, and metal powder separated by the cyclone separators is recycled into a dust collecting system and conveyed to the stirring kettle through nitrogen pressure to be recycled. By adding the nickel powder, fluidization of the tungsten powder can be achieved, continuous circular reaction can be achieved, only the nickel powder and the tungsten powder need to be recycled regularly except for controlling the flow speed of NF3, operation is simplified, cost is reduced, and the reaction efficiency is greatly improved.

Methods for removing impurities from precursors and related systems are provided. A method comprises at least one thermal cycle. The at least one thermal cycle comprises one or more of the following steps: heating a vessel comprising a precursor and at least one impurity to a temperature for a duration sufficient to vaporize at least a portion of the at least one impurity; measuring a vapor pressure within the vessel to obtain a measured vapor pressure and comparing the measured vapor pressure to a set point vapor pressure; and when the measured vapor pressure is above or within the set point vapor pressure, removing, from the vessel, at least a portion of a vapor comprising the at least one impurity. Other methods and systems are provided herein.

The invention discloses a synthesis process of tungsten hexafluoride, and relates to the technical field of special gas synthesis. The process comprises the following steps: mixing ammonium fluoride and hydrofluoric acid to prepare an activation solution, carrying out ultrasonic activation treatment on tungsten powder to obtain pretreated tungsten powder, and reacting the pretreated tungsten powder with fluorine gas at a certain temperature and pressure to prepare a liquefied crude product tungsten hexafluoride; the preparation method comprises the following steps: by taking aluminum sec-butoxide and the like as raw materials, carrying out sol-gel and ethanol supercritical drying and calcining to prepare highly porous activated aluminum oxide; gasifying the crude tungsten hexafluoride, adsorbing with activated aluminum oxide, and rectifying to obtain purified tungsten hexafluoride liquid; and finally, dissolving in liquid sulfur dioxide, treating under illumination with the wavelength of 395nm, and carrying out distillation separation to obtain high-purity tungsten hexafluoride. According to the method, the activation pretreatment is combined with multi-stage purification, so that the purity and the synthesis efficiency of tungsten hexafluoride are remarkably improved.

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.

A tungsten hexafluoride manufacturing method of the present invention includes a reaction step of reacting tungsten containing arsenic or an arsenic compound with a gas of a fluorine element-containing compound so as to obtain a mixture containing tungsten hexafluoride and a trivalent arsenic compound, and a distillation step of distilling and purifying the mixture so as to separate and remove a fraction containing the trivalent arsenic compound and to obtain tungsten hexafluoride.

The invention relates to the technical field of chemical engineering, in particular to a preparation method of tungsten pentachloride, which comprises the following steps: S1, feeding tungsten hexachloride into a fluidized bed reactor through gravity and inert gas flow, continuously introducing inert gas into the fluidized bed reactor, keeping the tungsten hexachloride in the fluidized bed reactor to be fluidized, preheating and preserving heat; s2, introducing mixed gas of nitrogen or inert gas and hydrogen into the fluidized bed reactor, and reacting in the fluidized bed reactor; and S3, collecting tungsten pentachloride. The equipment and operation are simple, continuous production of high-quality tungsten pentachloride can be achieved, the technological process is simple, the operation unit is small, daily operation and maintenance are simple, and automatic control is facilitated.

High purity tungsten precursors and methods for purifying the tungsten precursors are provided. The method for purifying the precursors can include at least one of the following steps: obtaining a source container containing WCl4, WOCl4, and either WCl5 or WCl6, separating the WCl5 or WCl6 from at least a first portion of the WOCl4, separating the WCl5 or WCl6 from at least a second portion of the WOCl4, collecting the precursors in a collection container, or any combination thereof.

The present invention relates to an adsorption tower for preparing high-purity tungsten hexafluoride, and belongs to the technical field of tungsten hexafluoride preparation. The adsorption tower includes an adsorption tower body, an adsorbent, a feeding mechanism and a discharging mechanism, and may also include at least one of a stirring mechanism, a recycling mechanism and a cleaning mechanism. A baffle and a filter are sequentially arranged in the adsorption tower body from top to bottom. The baffle is filled with adsorbent particles capable of adsorbing HF. The filter is used to filter granular impurities. The feeding mechanism is used to add new adsorbent particles into the adsorption tower body. The discharging mechanism is used to discharge adsorbent particles with high utilization rate at the bottom of the adsorbent filled on the baffle, the stirring mechanism is used to stir the adsorbent particles filled on the baffle, the recycling mechanism is used to desorb the discharged adsorbent particles for recycling, and the cleaning mechanism is used to clean the filter. The adsorption tower of the present invention can greatly improve the utilization rate of the adsorbent and improve the adsorption effect through reasonable structural design.

A device which can be exposed to chemical vapors, such as a molybdenum vapor, a tungsten vapor, or any combination thereof, which has a coating covering at least a portion thereof. The coating reduces or inhibits mass change at an outer surface of the device from exposure to the vapor. In certain situations, the mass change is a mass gain, and the coating reduces or inhibits the mass gain of equal to or less than 1 x 10-5 g mm-2.

A tungsten hexafluoride manufacturing method of the present invention includes a reaction step of reacting tungsten with a gas of a fluorine element-containing compound so as to obtain a mixture that contains tungsten hexafluoride and hydrogen fluoride-containing impurities, and a discharge step of performing distillation of the mixture while performing a discharge operation at least two or more times during the distillation so as to obtain tungsten hexafluoride, the discharge operation being an operation in which a storage operation and a purge operation are alternately performed.

The invention provides a method for removing metal impurities in tungsten hexafluoride by fluorine gas, which comprises the following steps: contacting fluorine gas with crude tungsten hexafluoride, carrying out oxidation reaction on fluorine gas and the metal impurities in the crude tungsten hexafluoride to finally form a plurality of metal fluorides, and carrying out two-stage separation on tungsten hexafluoride and a mixture of residual fluorine gas and metal fluorides, residual fluorine gas, metal fluoride and high-purity tungsten hexafluoride are obtained respectively, the separated high-purity tungsten hexafluoride is collected after heat exchange, and finally removal of metal impurities in tungsten hexafluoride is completed. The invention also relates to a device for removing metal impurities in tungsten hexafluoride by using fluorine gas, which comprises a reactor, the reactor is connected with a first-stage separator, the first-stage separator is connected with a second-stage separator, the second-stage separator is connected with a heat exchanger, and the heat exchanger is connected with a collector. The purity of tungsten hexafluoride can reach 99.9%, and the limitation of the purity of crude gas is solved.

Aspects disclosed herein include a system for generating singlet oxygen in a gas, the system comprising: a substrate; and hexanuclear clusters operably immobilized on at least a portion of the substrate; wherein each hexanuclear cluster comprises a photosensitive octahedral core complex characterized by formula FX1a: M6X8 (FX1a); wherein each M is independently Mo, W, or Re; wherein each X is independently a halide anion ligand; wherein the clusters are exposed to the gas and the gas comprises O2 gas; wherein the clusters are exposed to a light; and wherein each hexanuclear cluster is a photosensitizer configured to generate the gaseous singlet oxygen when irradiated by the light in the presence of the O2 gas.

Methods for removing impurities from precursors and related systems are provided. A method comprises at least one thermal cycle. The at least one thermal cycle comprises one or more of the following steps: heating a vessel comprising a precursor and at least one impurity to a temperature for a duration sufficient to vaporize at least a portion of the at least one impurity; measuring a vapor pressure within the vessel to obtain a measured vapor pressure and comparing the measured vapor pressure to a set point vapor pressure; and when the measured vapor pressure is above or within the set point vapor pressure, removing, from the vessel, at least a portion of a vapor comprising the at least one impurity. Other methods and systems are provided herein.

The invention relates to the technical field of sodium ion batteries, in particular to a positive electrode material and a preparation method thereof, a positive plate, a sodium ion battery and electric equipment. The structural formula of the positive electrode material is Na < x > MO < 2-y > A-z < F >, naxMO2 is a layered oxide matrix material, and M is a transition metal element; a is a metal coating element, the positive electrode material contains an oxide corresponding to the element A, the oxide corresponding to the element A is located on the surface and inside the layered oxide matrix material, A comprises at least one of Al, Zr, Mg and W, and y is the ratio of the molar weight of the element A to the molar weight of the layered oxide matrix material; the positive electrode material contains metal fluoride, the metal fluoride is located on the surface of the layered oxide matrix material, and z is the ratio of the molar weight of the F element to the molar weight of the layered oxide matrix material. According to the invention, the dissolution phenomenon of transition metal elements in the material circulation process can be effectively improved, so that the circulation capacity retention rate is increased.

A method for removing fluorine gas from a fluorine-containing gas containing fluorine gas and a fluorine-containing compound gas is provided. A method for removing fluorine gas from a fluorine-containing gas containing fluorine gas and a fluorine-containing compound gas includes a removal step in which the fluorine-containing gas is brought into contact with at least one metal salt selected from the group consisting of metal chlorides, metal bromides, and metal iodides.

High purity tungsten precursors and methods of purifying tungsten precursors are provided. The method of purifying a precursor may comprise at least one of the following steps: obtaining a source vessel containing WCl4, WOCl4, and one of WCl5 or WCl6; separating the WCl5 or the WCl6 from at least a first portion of the WOCl4; separating the WCl5 or the WCl6 from at least a second portion of the WOCl4; recovering the precursor in the collection container; or any combination thereof.

Disclosed are a tungsten hexafluoride preparation method and apparatus based on photoelectric synergy. A photocatalyst and metal tungsten are sequentially filled in a discharge area of a plasma reactor in a direction of gas entry, and the discharge area of the plasma reactor is irradiated with light at the same time; the background gas generates a large amount of plasma in the discharge area, SF6 undergoes decomposition under the synergistic effect of photocatalysis and plasma, SF6 is decomposed to generate fluorine atoms and low-fluorine sulfides such as SF5 and SF4. The generated fluorine ions, SF5, SF4 and low-fluorine sulfides further react with metal tungsten to generate WF6 specialty gas, which not only realizes the utilization of fluorine resources of SF6, but also replaces highly toxic fluorine gas with non-toxic SF6 exhaust gas in the plasma reactor for reaction, thereby ensuring safe operation and low energy consumption.

The precursor includes a tungsten precursor and a carbon-containing material. The precursor includes less than 0.02 wt.% of the carbon-containing material, based on the total weight of the precursor. A method for purifying a tungsten precursor can include at least one of obtaining a source container including the tungsten precursor and the carbon-containing material, separating the tungsten precursor from at least a first portion of the carbon-containing material, recovering the precursor in a collection container, or any combination thereof.

A device which can be exposed to chemical vapors, such as a molybdenum vapor, a tungsten vapor, or any combination thereof, which has a coating covering at least a portion thereof. The coating reduces or inhibits mass change at an outer surface of the device from exposure to the vapor. In certain situations, the mass change is a mass gain, and the coating reduces or inhibits the mass gain of equal to or less than 1 x 10-5 g mm-2.

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.

The utility model relates to the technical field of tungsten hexafluoride production, and discloses intelligent production equipment for electronic-grade tungsten hexafluoride, which comprises a cooling box body, material guide pipes are arranged on the left side and the right side of the cooling box body in a penetrating manner, and cooling pipes are wound outside the material guide pipes; the water adding pipe is arranged on the left side of the cooling box body in a penetrating manner; the temperature sensor is arranged on the right side of the inner surface of the cooling box body; and the display screen is arranged on the outer surface of the cooling box body. According to the intelligent production equipment for the electronic-grade tungsten hexafluoride, a material guide pipe and a partition plate are arranged to be of a detachable structure, cleaning liquid can be injected into the material guide pipe for shaking cleaning after the material guide pipe is detached, the interior of the cooling box body can be fully cleaned, it is avoided that much water scale adheres to the interior of the cooling box body and the interior of the material guide pipe, and the service life of the cooling box body is prolonged. And the conveyed tungsten hexafluoride can be scattered and conveyed through the first baffle plate and the second baffle plate, so that sufficient heat dissipation of the tungsten hexafluoride is guaranteed.

A molybdenum oxychloride or a tungsten oxychloride, wherein the molybdenum oxychloride or the tungsten oxychloride has a moisture content of less than 1 wt %. A method of producing a molybdenum oxychloride or a tungsten oxychloride, wherein a molybdenum oxide or a tungsten oxide as a raw material is subject to dehydration treatment at 400° C. or higher and 800° C. or less, and the raw material that underwent dehydration treatment is thereafter reacted with a chlorine gas to synthesize a molybdenum oxychloride or a tungsten oxychloride. A molybdenum oxychloride or a tungsten oxychloride is thereby provided having a low moisture content, and a production method thereof is provided.

Compositions are provided. A composition comprises a tungsten pentachloride compound. The tungsten pentachloride compound has an orthorhombic crystal structure as determined using Single-Crystal X-ray Diffraction. A method comprises obtaining a precursor, vaporizing the precursor to obtain a vaporized precursor, and exposing, under vapor deposition conditions, a substrate to the vaporized precursor. The precursor comprises a tungsten pentachloride compound having an orthorhombic crystal structure as determined by Single-Crystal X-Ray Diffraction. Related precursors and related methods are also provided, among other things.

The present application relates to a kind of hydrogen removal nonmetallic impurities in tungsten hexafluoride system, including primary light removal tower, the primary light removal tower outlet is communicated secondary light removal tower, the primary light removal tower and secondary light removal tower top outlet is communicated light component tank, the secondary light removal tower outlet is communicated column tube heat exchanger, the column tube heat exchanger is communicated collector;The present application also relates to a kind of hydrogen removal nonmetallic impurities in tungsten hexafluoride method, from the bottom of primary light removal tower, crude tungsten hexafluoride with hydrogen is introduced, and it is carried out under high temperature, catalyst condition oxidation reduction;After oxidation reduction, into secondary light removal tower, it is further reduced under higher temperature, form mixed gas, unreacted hydrogen and light component from the top of secondary light removal tower into light component tank;Mixed gas is collected after heat exchange, finally complete the removal of nonmetallic impurities in tungsten hexafluoride.The present application realizes the continuous operation of tungsten hexafluoride purification, process operation is simple, and reaction efficiency is high.

A molybdenum oxychloride or a tungsten oxychloride, wherein the molybdenum oxychloride or the tungsten oxychloride has a moisture content of less than 1 wt %. A method of producing a molybdenum oxychloride or a tungsten oxychloride, wherein a molybdenum oxide or a tungsten oxide as a raw material is subject to dehydration treatment at 400° C. or higher and 800° C. or less, and the raw material that underwent dehydration treatment is thereafter reacted with a chlorine gas to synthesize a molybdenum oxychloride or a tungsten oxychloride. An object of the present invention is to provide a molybdenum oxychloride or a tungsten oxychloride having a low moisture content, as well as a production method thereof.

The present invention relates to a process for the co-production of tungsten halides and carbon tetrafluoride. Tungsten carbide or a mixture of tungsten carbide and carbon is added to a reactor, chlorine trifluoride gas is introduced into the reactor, the reactor temperature is controlled at 340-400°C, the reaction pressure is 0.01-0.15 MPa, and a reaction is carried out to obtain a mixture comprising tungsten hexachloride, tungsten pentachloride, tungsten hexafluoride, and carbon tetrafluoride. After the reaction is completed, the reaction products are sequentially collected through a four-stage cold trap, with the first stage collecting tungsten hexachloride, the second stage collecting tungsten pentachloride, the third stage collecting tungsten hexafluoride, and the fourth stage collecting carbon tetrafluoride. The present invention has relatively mild reaction conditions, a reaction temperature below 400°C, higher safety, low raw material cost, high atom economy, higher safety, lower energy consumption, no by-products, and great economic benefits and development prospects. It meets the production requirements of chemical enterprises for safety, environmental protection, high efficiency, and circular economy.

Compositions are provided. A composition comprises a tungsten pentachloride compound. The tungsten pentachloride compound has an orthorhombic crystal structure as determined using Single-Crystal X-ray Diffraction. A method comprises obtaining a precursor, vaporizing the precursor to obtain a vaporized precursor, and exposing, under vapor deposition conditions, a substrate to the vaporized precursor. The precursor comprises a tungsten pentachloride compound having an orthorhombic crystal structure as determined by Single-Crystal X-Ray Diffraction. Related precursors and related methods are also provided, among other things.

Methods for synthesizing and / or purifying molybdenum compounds are provided. A method comprises obtaining a reagent; obtaining a metal trioxide compound; and contacting the reagent and the metal trioxide compound sufficient to form a reaction product comprising a molybdenum compound. Related compositions, related systems, and other related methods are provided, among other things.