133results 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 utility model relates to the technical field of phosphorus trichloride recovery equipment, and discloses a phosphorus trichloride gaseous cooling recovery device, which comprises a main body, a water inlet is fixedly connected below the front side of the main body, a water outlet is arranged below the water inlet, and the water inlet and the water outlet are convenient to supplement and discharge water for a water tank. And the lower surface of the main body is fixedly connected with four supports, and the number of the supports is four. Compared with the prior art, the cooling device has the following advantages and effects that through the arrangement of the first cooling pipe, the fins and the spraying mechanism, gaseous phosphorus trichloride is introduced by a worker and then cooled through the first cooling pipe, and then flows into the cooling branch pipes, the fins provide heat dissipation, and the spraying mechanism sprays water onto the fins to improve the heat dissipation effect; the wind power port blows air into the device, the water evaporation efficiency is improved, the heat dissipation effect of the fins is improved again, and the effect of improving the recovery efficiency is achieved through multiple-combination heat dissipation cooling.

Provided in the present application is a method for treating a heavy bis(fluorosulfonyl)imide residue, comprising the following step: causing a starting material system comprising the heavy bis(fluorosulfonyl)imide residue and an acidic aqueous solution to react to obtain a fluorine-containing acid solution and a crude sulfamic acid product, wherein the fluorine-containing acid solution can be used as a by-product acid, thereby saving treatment costs; and the crude sulfamic acid product can also be directly sold as a product, thereby reducing treatment costs, bringing economic benefits, and achieving resource recycling of the heavy bis(fluorosulfonyl)imide residue.

The invention discloses a production method and a production system of high-purity phosphorus trifluoride and hydrogen chloride, and belongs to the field of preparation of phosphorus trifluoride and hydrogen chloride. The production method comprises the following steps: reacting phosphorus trichloride with anhydrous hydrogen fluoride to generate phosphorus trifluoride and hydrogen chloride, condensing at-20 DEG C to 0 DEG C, refluxing phosphorus trichloride and hydrogen fluoride raw materials, and outputting mixed gas of phosphorus trifluoride and hydrogen chloride; preliminarily rectifying the mixed gas to obtain a phosphorus trifluoride crude product and a hydrogen chloride crude product; the method comprises the following steps: carrying out primary rectification on a phosphorus trifluoride crude product in a phosphorus trifluoride rectification heavy component removal tower and carrying out secondary rectification in a phosphorus trifluoride rectification light component removal tower in sequence to obtain high-purity phosphorus trifluoride gas; the crude hydrogen chloride is subjected to primary rectification in a hydrogen chloride rectification heavy component removal tower and secondary rectification in a hydrogen chloride rectification light component removal tower in sequence, and high-purity hydrogen chloride gas is obtained. According to the production method, high-purity phosphorus trifluoride and high-purity hydrogen chloride can be continuously produced and obtained, meanwhile, the raw material utilization rate can be increased, the product yield can be increased, meanwhile, little waste gas is generated, the waste gas can be completely absorbed, and the requirement for environmental protection is met.

The invention provides a method for treating bis (fluorosulfonyl) imide heavy slag, which comprises the following steps: reacting a raw material system comprising bis (fluorosulfonyl) imide heavy slag and an acidic aqueous solution to obtain a fluorine-containing acid solution and a sulfamic acid crude product; wherein the fluorine-containing acid liquid can be used as a byproduct acid, so that the treatment cost is saved; and the sulfamic acid crude product can also be directly sold as a product, so that the treatment cost is reduced, economic benefits are brought, and resource recycling of the bis (fluorosulfonyl) imide heavy slag is realized.

The utility model discloses a phosphorus pentafluoride generating system for a lithium hexafluorophosphate generator. The phosphorus pentafluoride generating system comprises a phosphorus pentafluoride generator, a phosphorus pentachloride feeding valve, a phosphorus pentafluoride reaction valve, a phosphorus pentafluoride feeding valve and a feeding emptying valve, one end of the phosphorus pentachloride feeding valve is connected to a phosphorus pentachloride positive pressure sending tank through a pipeline, the other end of the phosphorus pentachloride feeding valve is connected to one end of the phosphorus pentafluoride reaction valve through a pipeline, and the other end of the phosphorus pentafluoride reaction valve is connected to a feeding port of the phosphorus pentafluoride generator; a discharge port of the phosphorus pentafluoride generator is respectively connected to one end of the phosphorus pentafluoride feeding valve and one end of the feeding emptying valve through pipelines, the other end of the phosphorus pentafluoride feeding valve is connected to the lithium hexafluorophosphate generator through a gas filter, and the other end of the feeding emptying valve is connected to a tail gas collecting device through a pipeline. According to the utility model, the feeding misoperation can be eliminated, the feeding safety is ensured, and the feeding can be controlled to be correct.

The invention provides a phosphorus trifluoride production system and a preparation method thereof, and belongs to the technical field of phosphorus trifluoride manufacturing. The phosphorus trifluoride production system comprises a static reactor, a gaseous fluorine source, a liquid phosphorus source, a condenser and a collector. The static reactor comprises a static mixer and a jacket type shell wrapping the static mixer, the static mixer is used for mixing reaction raw materials and providing a reaction place, and a heat exchange cavity used for containing a heat exchange medium is formed in the jacket type shell; when the production system is used for preparing phosphorus trifluoride, the problems that the mass transfer effect between a gaseous fluorine source and a liquid phosphorus source is poor and the material distribution uniformity is poor can be effectively solved, and meanwhile, the whole material system can have better temperature consistency, so that the reaction raw materials can react more efficiently and thoroughly to form phosphorus trifluoride.

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 concerns a method for the generation of a tertiary phosphine, a tertiary phosphite ester, or a hexafluorophosphate, wherein the method comprises the following steps: a) providing an elemental phosphorus, an organic disulfide, a solvent and either a compound R1-X1 and an organic base, a compound R2-O-X2 and an organic base, or a fluoride anion and b) mixing the elemental phosphorus, the organic disulfide and either the compound R1-X1 and the organic base, the compound R2-O-X2 and the organic base, or the fluoride anion in the solvent for obtaining a solution or a suspension in which the tertiary phosphine, the tertiary phosphite ester, or the hexafluorophosphate is formed.

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 application belongs to the field of organic phosphorus chemistry and phosphorus chemical industry, and particularly relates to a preparation method of phosphorus trifluoride, comprising the following steps: under the protection of inert gas, reacting phosphorus trichloride with an ionic liquid to obtain phosphorus trifluoride. The application uses the ionic liquid as a fluorine source, avoids using dangerous raw materials such as hydrogen fluoride and metal fluoride, and the ionic liquid can not only be used as a fluorine source, but also as a reaction solvent, so that the reaction activity of phosphorus trichloride and the ionic liquid is greatly improved. The application has mild reaction conditions, low reaction temperature, short reaction time, and the reaction system does not produce other byproduct gases, the post-processing operation is simple, and the reaction yield and purity are high.

The invention discloses a preparation method for continuous production of phosphorus trifluoride, and belongs to the technical field of chemical synthesis, and the key point of the technical scheme is that the preparation method for continuous production of phosphorus trifluoride comprises the following preparation steps: S1, adding phosphorus trichloride into the upper part of a rectifying tower, adding anhydrous hydrogen fluoride gas into the lower part of the rectifying tower, and stirring; contacting the two raw materials on the surface of the rectifying tower filler to complete reaction; s2, a product obtained through reaction is discharged from the top of the rectifying tower and enters a purification system, and phosphorus trifluoride is obtained.When phosphorus trifluoride is prepared through the rectifying method, the reaction process is stable, the temperature is easy to control, the gas-liquid contact area is large, the reaction is complete, the reaction speed is high, and large-batch production is facilitated.

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.

The present invention discloses a filter for preparing phosphorus trifluoride, comprising: a fixed cylinder with closed ends, one end of the fixed cylinder being upwardly provided with a feed pipe and the other end being downwardly connected to a discharge pipe; a filtering mechanism comprising a first sealed bearing and a second sealed bearing fixedly connected to the fixed cylinder, the first sealed bearing and the second sealed bearing being respectively fixedly connected to corresponding fixed ring plates, a baffle being sealed and fixedly connected to the fixed ring plate mounted on the first sealed bearing, and corresponding filter plates being fixedly connected in a serrated shape between the fixed ring plates; a dust removal mechanism comprising a dust removal notch, the bottom of the fixed cylinder outside the dust removal notch being downwardly connected to a dust removal pipe, the outer end of the filter plate being fixedly connected to a spiral dust removal plate; and a driving mechanism for driving the baffle to rotate. The present invention can effectively discharge and collect filtered particulate matter without disassembling the filter, and can effectively improve the overall structural stability of the filtering mechanism.

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.

The present invention provides a method for preparing phosphorus trifluoride, comprising the steps of mixing a phosphorus triiodide organic solution with a metal fluoride salt, and reacting until no bubbles are generated to obtain phosphorus trifluoride; the metal fluoride salt comprises any one of sodium fluoride, potassium fluoride, or aluminum fluoride, or a combination of at least two. The method is simple to operate and, by selecting a suitable metal fluoride salt, produces a phosphorus trifluoride product with stable quality, high purity, and low impurities, making it suitable for industrial production of high-purity phosphorus trifluoride.