80results about "Phosphorus halides/oxyhalides" patented technology

The invention discloses a phosphorus trichloride production reaction kettle with a defoaming structure, and relates to the technical field of reaction kettles. According to the phosphorus trichloride production reaction kettle with the defoaming structure, through cooperation of the obliquely-installed sawtooth plates and the protruding strip rings, during rotation, the sawtooth plates drive foam on the liquid level to move towards the periphery, in the movement process, the foam on the liquid level is separated from the protruding strip rings, and the foam on the liquid level is removed. The sawteeth at the top of the sawtooth plate are in contact with accumulated foam, so that part of the foam is broken, the unbroken foam outwards impacts the inner wall of the convex strip ring under the action of centrifugal force, so that the foam is in contact with the convex strips uniformly arranged on the inner wall of the inner convex ring, and compared with a smooth inner wall of a traditional reaction kettle, the contact area is reduced when the convex strips of the inner convex ring are in contact with the foam; and the pressure during impact is increased, so that the foam is broken under higher pressure, and the defoaming effect is improved.

The invention relates to the technical field of chemical equipment, in particular to reaction equipment for preparing phosphorus oxyfluoride, which comprises: a main body internally provided with a gas inlet cavity, a reaction cavity and a separation cavity in sequence from bottom to top; the gas-solid distribution mechanism is arranged in the gas inlet cavity and comprises a gas flow distribution assembly, a distribution driving assembly and a solid phase distribution pore plate, a gas flow channel is formed in the gas flow distribution assembly, and the size of the gas flow channel periodically changes along with bidirectional rotation of the gas flow distribution assembly; the guide mechanism comprises a rectification grid plate, a guide plate group and a guide driving assembly, and the guide driving assembly drives the guide plate group to rotate; the heat exchange mechanism is arranged around the outer edge of the main body corresponding to the gas inlet cavity, the reaction cavity and the separation cavity; and the separation mechanism is arranged in the separation cavity and is used for carrying out solid-gas separation on the gas flow in the separation cavity. According to the method, phosphorus oxyfluoride can be efficiently obtained at low cost through continuous solid-gas reaction, and the method has good industrial value.

The invention discloses a production method of a hexafluorophosphate product, the hexafluorophosphate product is 2-(inner-5-norbornene-2, 3-dicarboximide)-1, 1, 3, 3-tetramethylurea hexafluorophosphate, the first-step reaction of the invention comprises the following steps: preparing an intermediate from norbornene dianhydride as a raw material and a hydroxylamine compound under the action of organic alkali; in the second-step reaction, the intermediate and TCFH are subjected to a nucleophilic substitution reaction under the action of an alkaline metal catalyst to obtain a crude product, and the crude product is purified to obtain a target product; the synthesis route used in the invention is simple, special high temperature or high pressure is not needed in the reaction process, and the used catalyst is a conventional raw material which is low in price and easy to obtain; according to the method, the purity of the product can be increased to 99.8% or above, the total yield is stabilized to be 85% or above, in addition, the reaction route greatly reduces side reactions, and by-products in the product are few in variety and low in content.

The purpose of the present invention is to provide a production method for phosphorus trifluoride in which the reaction can be carried out using readily available materials at a temperature equal to or lower than atmospheric temperature, said method being suitable for use on an industrial scale.　The production method for phosphorus trifluoride involves reacting phosphorus trichloride and hydrogen fluoride in the presence of an organic solvent.

The present invention produces phosphorus trifluoride at a high yield by using readily available raw materials (phosphorus trichloride and hydrogen fluoride), and produces a high-purity phosphorus trifluoride by purifying an obtained product gas containing phosphorus trifluoride by using a method suitable for mass production.　The present invention pertains to: a method for producing phosphorus trifluoride, the method comprising (a) a step for reacting phosphorus trichloride with hydrogen fluoride to produce a product gas, and (b) a step for removing hydrogen chloride from the product gas; and a high-purity phosphorus trifluoride obtained by said method.

An integrated process for co-production of phosphorus pentafluoride (PF5) and fluorosulfonic acid (HSO3F) in high yield and purity through a single reaction step is provided. The method comprises reacting a first reagent comprising an aqueous solution of hexafluorophosphoric acid (HPF6) and hydrofluoric acid (HF) with a second reagent comprising fuming sulfuric acid (H2SO4SO3), and recovering a product mixture comprising phosphorus pentafluoride (PF5) and fluorosulfonic acid (HSO3F).

The invention discloses a preparation method of phosphorus pentafluoride, which comprises the following steps: 1) mixing fluorine-containing inorganic salt and hydrogen-containing inorganic salt, and carrying out activation process treatment; and 2) adding phosphorus pentoxide into the system in the step 1) for reaction to generate phosphorus pentafluoride gas. The method has the advantages of low reaction temperature and high product purity, does not need to use high-toxicity and high-corrosivity hydrogen fluoride, and is environment-friendly, simple in process and suitable for industrial production.

The invention discloses a method for separating phosphorus pentafluoride-hydrogen chloride mixed gas, which comprises the following steps of: introducing the phosphorus pentafluoride-hydrogen chloride mixed gas into a reaction kettle by taking a perfluoropolypropyl ether fluorinated solution as a solvent and lithium fluoride as a raw material, so that the phosphorus pentafluoride and the lithium fluoride react to generate lithium hexafluorophosphate, and hydrogen chloride is discharged in a gas phase manner; heating the generated lithium hexafluorophosphate to decompose the lithium hexafluorophosphate into phosphorus pentafluoride and lithium fluoride, discharging the phosphorus pentafluoride in a gas phase manner, and retaining the lithium fluoride in the perfluoropolypropyl ether fluorinated solution for recycling; the solvent and raw materials provided by the invention can be recycled for multiple times, the whole process flow is greatly simplified, and efficient and stable separation of HCl and phosphorus pentafluoride is realized.

The solid electrolyte contains Na, M [alpha], M [beta], and F, where M [alpha] is at least one element that is a trivalent cation, and M [beta] is at least one element that is a tetravalent or higher cation. As a result, it is possible to provide a solid electrolyte having high ion conductivity. Preferably, M [beta] is an element having a tetravalent cation, the solid electrolyte contains a component represented by the compositional formula Na3-xM [alpha] 1-xM [beta] xF6, and 0 < x < 1 is satisfied.

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

This disclosure relates to a process for preparing ultra-high-purity alkali metal hexafluorophosphate (MPF6), comprising the steps of: (a) filling a first reactor "B" with alkali metal fluoride (MF) and flowing nitrogen gas through the first reactor "B"; (b) cooling the first reactor "B" to a predetermined temperature, then filling it with anhydrous hydrogen fluoride (AHF) gas and stirring the mixture containing alkali metal fluoride (MF) dissolved in AHF within the first reactor "B"; (c) cooling the mixture containing alkali metal fluoride (MF) dissolved in AHF within the first reactor "B" to a predetermined temperature; and (d) filling a second reactor "A" with phosphorus pentachloride (PCl5) and adding AHF in lots to achieve high purity The present invention relates to a process comprising: (e) generating phosphorus pentafluoride (PF5) and hydrogen chloride (HCl) gas; (f) reacting alkali metal fluoride (MF) dissolved in AHF in a first reactor "B" with the mixture of phosphorus pentafluoride (PF5) and hydrogen chloride (HCl) gas obtained in step (d) to obtain an alkali metal hexafluorophosphate mother liquor dissolved in AHF under a PF5 gas atmosphere; and (f) cooling the first reactor "B" to a predetermined temperature, maintaining the temperature of the alkali metal hexafluorophosphate mother liquor dissolved in AHF for a predetermined time, followed by filtration and drying at a predetermined temperature to obtain an alkali metal hexafluorophosphate (MPF6) selected from NaPF6, KPF6, or CsPF6.

This solid electrolyte includes a crystal phase that has an argyrodite crystal structure, and contains elemental lithium (Li), elemental phosphorus (P), elemental sulfur (S), and elemental halogen (X). The crystallite size of the crystal phase having the argyrodite crystal structure is no more than 40 nm. In an XRD pattern, Ia / Ib is no more than 0.2 when the intensity of a peak A observed in the range 2θ = 27.0° ± 0.5° is Ia and the intensity of a peak B observed in the range 2θ = 25.5° ± 1.0° is Ib.

The invention relates to the technical field of chemical equipment, in particular to purification equipment for preparing phosphorus oxyfluoride and a purification method of the purification equipment. The purification equipment for preparing the phosphorus oxyfluoride comprises a main body, a gas inlet cavity, a purification cavity and an adsorption cavity are formed in the main body; the gas-liquid purification module is arranged in the purification cavity and comprises a corrugated disc set, a liquid distribution assembly, a driving assembly and a blocking assembly, and the driving assembly drives the liquid distribution assembly to rotate and drives the corrugated disc set to rotate at the same time, so that the purification liquid forms a uniform liquid film; a purified liquid path and an airflow path are arranged in the blocking assembly, the purified liquid path enables purified liquid on the corrugated inner disc to flow to the corrugated outer disc, and the airflow path enables airflow flowing through all the corrugated outer disc to flow back to the position below the corrugated inner disc; and the gas-solid adsorption module is used for further adsorbing the gas purified by the gas-liquid purification module and then discharging the gas out of the purification cavity. According to the purification equipment for preparing the phosphorus oxyfluoride, provided by the invention, the gas is in full contact with the purification liquid, so that the purification effect is ensured.

The invention belongs to the technical field of chemical synthesis, and relates to a lithium battery electrolyte raw material production technology, in particular to a preparation method of phosphorus pentafluoride. The method comprises the following steps: adding phosphorus trichloride, liquid chlorine and hydrogen fluoride into a reactor in proportion, and reacting to prepare hydrogen chloride and phosphorus pentafluoride; the molar ratio of phosphorus trichloride to liquid chlorine to hydrogen fluoride is preferably 1: 1: 5, and the reactor comprises a bottom reaction section, a middle filler section and a top condensation section. The working pressure of the reactor is 0.1-3.0 MpaG, the temperature of the reaction section is 0-40 DEG C, and the temperature of the condensation section is-20 to-60 DEG C. The mixed gas of phosphorus pentafluoride and hydrogen chloride can be prepared in one step and conveyed to the rear end to be refined and separated. The method has the advantages of simple process flow, easily available raw materials, low production cost and high efficiency.

The present disclosure provides a method for producing lithium fluoride, and the like, comprising: a step 1 for preparing an aqueous solution of at least one of lithium chloride and lithium sulfate; a step 2 in which an aqueous solution of at least one of lithium chloride and lithium sulfate is mixed with an aqueous hydrofluoric acid solution; and a step 3 in which a mixed solution of an aqueous solution of at least one of lithium chloride and lithium sulfate and an aqueous solution of hydrofluoric acid is mixed with an alkali, the pH of the liquid obtained in the step 3 being 3-6.

The present invention provides a phosphorus pentafluoride preparation method, which comprises: mixing a hexafluorophosphoric acid solution and a dehydrating agent, and carrying out a dehydration reaction at a temperature of 30-160 DEG C under a pressure of 0.1-3 MPa, wherein the hexafluorophosphoric acid solution contains water and hydrogen fluoride; after the dehydration reaction is finished, the reaction system is subjected to rapid pressure relief, and mixed gas containing phosphorus pentafluoride is obtained; wherein the pressure relief rate of the rapid pressure relief is greater than or equal to 0.1 MPa / min; and carrying out purification treatment on the mixed gas containing phosphorus pentafluoride to prepare the phosphorus pentafluoride gas.

The invention discloses a system and a method for cleaning a chlorination kettle for phosphorus trichloride production, the system comprises a chlorination kettle, the chlorination kettle is provided with a chlorine feeding pipeline, a yellow phosphorus feeding pipeline and a discharging pipeline, and the discharging pipeline is connected with a feeding port of a primary filtering device through a first material pump; a liquid phase outlet of the first-stage filtering device is connected with a feeding hole of the second-stage filtering device, and a solid phase outlet of the first-stage filtering device is connected with a feeding hole of the third-stage filtering device; a liquid phase outlet of the second-stage filtering device is connected with an inlet of the first-stage buffer tank, and a solid phase outlet of the second-stage filtering device is connected with a feeding hole of the third-stage filtering device; a liquid phase outlet of the third-stage filtering device is connected with a feeding hole of the first-stage filtering device, and a solid phase outlet of the third-stage filtering device is connected with an inlet of the second-stage buffering tank; an outlet of the primary buffer tank is connected with a feeding hole of the phosphorus washing tower through a second material pump; and the discharge hole of the phosphorus washing tower is connected with the reflux inlet of the chlorination kettle through a reflux pipeline. The method avoids the risks of byproduct acid generation, hydrogen accumulation, yellow phosphorus spontaneous combustion and the like, is high in efficiency and is suitable for industrial continuous production.

The invention discloses a phosphorus oxychloride preparation method based on a flat-plate membrane reactor, and belongs to the technical field of chemical processes and reactors. The reactor comprises a plurality of liquid chamber-gas chamber-liquid chamber functional units which are arranged repeatedly and heat exchange units located between the adjacent functional units, gas-liquid micro-interface contact is achieved through a porous hydrophobic membrane, and oxygen reacts with phosphorus trichloride in a molecular diffusion mode. According to the method, the reaction temperature is controlled to be 70-95 DEG C, the oxygen pressure is controlled to be 0.01-0.05 MPa, and the heat exchange medium is combined for circulating heat transfer, so that efficient utilization of oxygen is realized, and the reaction process is mild and controllable. The continuous operation of 3-5 reactors connected in series is supported, the oxygen utilization rate can be remarkably improved, the raw material consumption is reduced, the product purity is improved, continuous production is supported, and the method is suitable for large-scale synthesis of phosphorus oxychloride.

This disclosure provides a vessel and methods for handling high-purity phosphorus fluoride compounds. The vessel can include a phosphorus fluoride component including a phosphorus fluoride compound with a purity of at least 99.9%, as measured by gas chromatography and / or infrared spectroscopy. Also disclosed is a method which includes obtaining a solid component containing a metal fluorophosphate compound and water, heating the solid component to remove water, and further heating to form a phosphorus fluoride compound with a purity of at least 99.9%, as measured by gas chromatography and / or infrared spectroscopy.

This invention belongs to the field of solid-state battery material preparation technology, and particularly relates to a method for preparing a sulfide solid electrolyte, comprising at least the following steps: mixing the raw materials and molten medium required for the sulfide solid electrolyte under an inert atmosphere, and placing the mixture in a sealed ball mill jar; mechanically grinding and simultaneously heating the ball mill jar in a heated ball milling system to obtain a molten suspension of the sulfide solid electrolyte; further heating the molten suspension of the sulfide solid electrolyte under an inert atmosphere or vacuum, causing the molten medium to boil or sublimate and separate from the sulfide solid electrolyte; and cooling to room temperature to obtain the sulfide solid electrolyte. Compared with the prior art, this invention uses molten medium-assisted heating mechanical ball milling to prepare the sulfide solid electrolyte, which can obtain a stable, high-purity, low-carbon-residue sulfide solid electrolyte with an ionic conductivity of 10.7 mS / cm, a carbon residue of <0.01 wt%, and a processing time of <2 h.

An apparatus for purifying high-purity phosphorus trifluoride according to one embodiment of the present invention comprises: a phosphorus trifluoride production unit including a reactor in which a phosphorus chloride compound solution and a metal fluoride salt react, and a purge device for vacuum-purging the reactor; a first freezing unit for cooling a phosphorus trifluoride mixed gas obtained from the phosphorus trifluoride production unit to remove unreacted materials contained in the phosphorus trifluoride mixed gas; and a second freezing unit for cooling the phosphorus trifluoride mixed gas obtained from the first freezing unit with liquid nitrogen to remove purge gas and hydrogen chloride (HCl).

The invention provides a purification system of phosphorus oxyfluoride. The purification system is a purification system for preparing phosphorus oxyfluoride based on a phosphorus pentoxide one-step method. The device specifically comprises a filtering unit, a CaF2 adsorption bed and a rectifying tower which are connected in sequence, the filtering unit comprises a tank body with a top opening, and the tank body comprises a liquid inlet and a liquid pumping pipeline arranged at the top of the tank body; the cover body is matched with the top of the tank body, an air compression pipeline and a pressure sensor are arranged at the top of the cover body, and the air compression pipeline is connected with an air compressor; the top of the candle stick is communicated with the liquid pumping pipeline; the waste liquid tank is communicated with the bottom of the tank body through a pneumatic valve; the liquid pumping pipeline and the nitrogen backflushing pipeline are communicated with the liquid pumping pipeline, and the backflushing pressure is 0.3-0.5 MPa. The particle size of bed layer particles of the CaF2 adsorption bed is 1-5 mm, the height of the CaF2 adsorption bed is 300-800 mm, a shell is made of 316L stainless steel lining PTFE with the thickness of 3 mm, 316L stainless steel balls with the thickness of 5 mm are evenly distributed on the upper section and the lower section of the axial fixed bed, and an electromagnetic heating coil is arranged on the periphery of the shell of the axial fixed bed.

The invention provides a preparation method and device of phosphorus pentafluoride, and the preparation method comprises the following steps: 1) carrying out atomization treatment on a mixed acid solution comprising a hexafluorophosphoric acid solution and a sulfuric acid solution to obtain atomized mixed acid; and 2) carrying out a thermal cracking reaction on the atomized mixed acid to obtain phosphorus pentafluoride. The preparation method of phosphorus pentafluoride provided by the invention can improve the purity of the prepared phosphorus pentafluoride, and has the advantages of high reaction efficiency, simple process and the like.

A method for producing phosphorus trifluoride by reacting a metal fluoride, a phosphorus chloride compound, and a solvent according to the present invention uses a continuous production device including a screw reactor to produce phosphorus trifluoride, and thus can continuously mass-produce high-purity phosphorus trifluoride, has excellent selectivity for phosphorus trifluoride, and can reduce production costs and energy, thus being economical.

The application discloses a compact stable sulfide solid electrolyte and a preparation method and application thereof. The method adopts a liquid phase assisted process to prepare a homogeneous precursor, and then two-step temperature field sintering technology is adopted, that is, low temperature heat treatment is carried out at 250-350 DEG C to induce uniform nucleation, and then high temperature densification sintering is carried out at 450-550 DEG C under the condition of applying 5-20 MPa pressure. The method breaks through the limitation of traditional solid phase method or secondary normal pressure sintering, realizes accurate control of the microstructure of the electrolyte, and the electrolyte has the advantages of few grain boundary pores, compact structure, low humidity sensitivity and the like, is suitable for building full solid state lithium batteries with high energy density and long cycle life, and the process is stable and suitable for large-scale production.

The embodiment of the utility model provides a phosphorus diffusion tail gas treatment system, which relates to the technical field of environmental protection and comprises a mixed cooling box, an exhaust pipe, a spraying mechanism and a water storage tank. The mixed cooling box is provided with a first air inlet, a second air inlet and a first air outlet. The first air inlet is used for communicating with an exhaust port of the diffusion furnace, the second air inlet is used for guiding external air into the mixed cooling box, and the first air outlet is communicated with the exhaust pipe. The spraying mechanism is installed on the exhaust pipe, and a water outlet of the spraying mechanism is located above the position, communicated with the first air outlet, of the exhaust pipe. The water storage tank communicates with the bottom end of the exhaust pipe. The treatment system can effectively treat tail gas containing phosphorus oxychloride generated in the phosphorus diffusion process, the discharged gas is not prone to polluting the environment or corroding diffusion furnace equipment, and the production efficiency and the product quality are not prone to being affected.

A method for manufacturing phosphorus pentafluoride includes a dehydration step of dehydrating hexafluorophosphate hydrate using sulfuric acid containing less than 5% by mass of sulfur trioxide. Preferably, it also includes steps a) and b). a) a step of concentrating the sulfuric acid after the dehydration step. b) a step of reusing the sulfuric acid concentrated in step a) for the dehydration of hexafluorophosphate hydrate, and then using the sulfuric acid for the manufacture of phosphorus pentafluoride. Preferably, the dehydration step is carried out in the presence of hydrogen fluoride, and step c) is included before step a). c) a step of recovering the hydrogen fluoride after the dehydration step.

The method for preparing phosphorous trifluoride according to the present invention comprises the steps of: controlling the particle size (D50) of NaF to 67 μm to 137 μm; and reacting the particle size-controlled NaF, PCl3, and a solvent to prepare phosphorus trifluoride. By maximizing reactivity through control of the NaF particle size, the conversion rate of NaF can be increased, thereby suppressing the generation of unreacted NaF. Further, the selectivity for phosphorus trifluoride is excellent, and the preparation cost can be reduced.

The invention relates to a process for the recovery of phosphorus and iron compounds from iron phosphate-containing materials, characterized in that i) an iron phosphate-containing material is reacted with chlorine gas in the presence of a carbon source at a temperature of 300 to 900°C and ii) the chlorophosphorus compounds formed, in particular phosphorus oxychloride and optionally phosphorus trichloride and iron chloride, are discharged in the exhaust gas stream, and iii) the iron chloride and iv) the chlorophosphorus compounds are separated from the exhaust gas stream.

The invention discloses a membrane reaction system for preparing phosphorus oxychloride, and belongs to the technical field of chemical processes. The system comprises a phosphorus trichloride tank, an oxygen tank, at least one membrane reactor, a heat exchanger and a finished product tank, at least one group of membrane elements and heat exchange elements are arranged in the membrane reactor, each membrane element is composed of an active layer and a supporting layer, oxygen penetrates through the membrane elements in a molecular state to be in contact reaction with phosphorus trichloride on the surface of the membrane, and the heat exchange elements are used for timely removing reaction heat. The gas-liquid contact area and the mass transfer efficiency are greatly improved through membrane type mass transfer, and efficient dispersion and utilization of oxygen are achieved; the system supports multi-stage series continuous production, is accurate and controllable in reaction temperature, and has the advantages of high production efficiency, low energy consumption, safety in operation, high product purity and the like.