212results about "Phosphorus halides/oxyhalides" patented technology

The invention discloses a preparation method and a production system of phosphorus trifluoride, and belongs to the technical field of preparation of phosphorus trifluoride. Phosphorus trichloride and first mixed gas are continuously introduced into a reactor, the first mixed gas comprises anhydrous hydrogen fluoride and inert gas, phosphorus trichloride and anhydrous hydrogen fluoride in the first mixed gas are subjected to a double decomposition reaction in the reactor, and intermediate gas containing phosphorus trifluoride is generated. Collecting intermediate gas discharged from the reactor, and rectifying and purifying the intermediate gas to obtain a phosphorus trifluoride product. The inert gas carries anhydrous hydrogen fluoride and phosphorus trichloride to generate double decomposition reaction to generate phosphorus trifluoride, and the inert gas can dilute the concentration of the raw material gas anhydrous hydrogen fluoride participating in the reaction and also can take away heat generated by the reaction, so that the temperature of the reactor is more stable, and continuous production of phosphorus trifluoride is realized.

The invention discloses a purification process of phosphorus trifluoride. The purification process comprises the following steps: S1, heating liquid in a first storage tank, and pumping the heated liquid into a flash evaporator for flash evaporation; s2, introducing the flashed gas into a first rectifying tower for rectification, condensing the rectified top products phosphorus trifluoride and hydrogen chloride, and introducing the condensed top products into an intermediate first product storage tank; s3, pumping the material in the middle first product storage tank into a second rectifying tower for rectification, condensing the top gas rectified by the second rectifying tower, and introducing the condensed gas into the first product storage tank for storage; s4, a finished product in the first product storage tank is pumped into a gasifier to be gasified and enters a gas-liquid separation tank to be separated, and separated gas is discharged from the top and sequentially introduced into three phosphorus trifluoride purification devices to be purified; s5, the purified gas is introduced into a filter to be filtered, the filtered gas enters a filling system to be filled after pressure stabilization, impurities in phosphorus trifluoride can be completely removed, and the purity of phosphorus trifluoride is improved in a jumping mode.

The invention discloses a preparation method of phosphorus oxyfluoride based on reaction separation equipment, which comprises the following specific steps: S1, a heat exchange medium enters a driving pipe fitting through a heat exchange medium inlet pipe of the reaction separation equipment, is pressurized at a discharge end of the driving pipe fitting and then is sprayed out in a horizontally outward inclined manner, a heat exchange mechanism and a second filler layer of the reaction separation equipment are driven to integrally rotate, so that a circulating heat source circularly passes through the whole reaction area; s2, respectively feeding liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride when the reaction temperature of the reaction zone reaches a set value; s3, liquid industrial phosphoric acid and gaseous anhydrous hydrogen fluoride are in contact on the surface of the rotating second filler layer and react to generate phosphorus oxyfluoride gas; and S4, extracting phosphorus oxyfluoride gas generated by the reaction along the top of the reaction separation tower body. The controllability of the reaction process can be effectively ensured, and the reaction effect is obviously improved.

The utility model discloses an atomizing nozzle, a phosphorus pentachloride synthesis reactor and a phosphorus pentachloride synthesis system, which comprise a nozzle body, a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and an outlet, the second inlet and the fourth inlet are both used for introducing first gas, and the fifth inlet is used for introducing second gas; the atomizing nozzle disclosed by the utility model can strengthen gas-liquid mixing and control the size and the shape of atomized particles, and in addition, the atomizing nozzle disclosed by the utility model is arranged on the reactor body, so that the distribution uniformity of materials in the space of the reactor body is improved, and a high-temperature area in the reactor body is reduced or eliminated.

The invention discloses a phosphorus trifluoride production device and method, and belongs to the technical field of phosphorus trifluoride production, the device comprises a reaction part, a pretreatment part and a post-treatment part, the reaction part comprises a first raw material tank, a second raw material tank, a reaction kettle and a collection cold trap, the pretreatment part comprises a primary separation tower and an absorption tower, and the post-treatment part comprises a secondary separation tower and an absorption tower. The post-treatment part comprises an adsorption tower, a light component removal tower and a heavy component removal tower; the production method comprises the following steps: adding raw materials of phosphorus trichloride and hydrogen fluoride into a reaction kettle to generate phosphorus trifluoride and hydrogen chloride, collecting the phosphorus trifluoride and hydrogen chloride in a collecting cold trap, heating the collecting cold trap to vaporize the phosphorus trifluoride and hydrogen chloride, and sequentially entering a primary separation tower, a light component removal tower and a heavy component removal tower for a series of treatment, and finally, high-purity phosphorus trifluoride gas is extracted from the heavy component removal tower to a filling system. According to the method, high-purity phosphorus trifluoride with the purity larger than or equal to 99.999% can be finally produced, and the problem that in the prior art, the purity of phosphorus trifluoride is not enough is solved.

The invention relates to the technical field of chemical preparation, in particular to a preparation method of phosphorus trifluoride, which comprises the following steps: step 1, preparing reactants: preparing phosphorus pentoxide and pure fluorine gas; 2, mixing reactants: in a proper reaction container, mixing phosphorus pentoxide with pure fluorine gas; step 3, controlling the reaction conditions of reactants: ensuring that the reaction is carried out at proper temperature and pressure so as to promote the smooth proceeding of the reaction; and 4, separating the product to obtain phosphorus trifluoride. The method comprises the following steps: putting phosphorus pentoxide into a dry container, preparing a storage tank filled with fluorine gas, putting the prepared phosphorus pentoxide into a reaction container, introducing the dry fluorine gas from the storage tank, carrying out a reaction at high temperature and high pressure, and after the reaction is completed, adding the fluorine gas into the reaction container, phosphorus trifluoride and a byproduct oxyfluoride are separated through a physical method (distillation or condensation), so that the process is simple, and the reaction conversion rate is high.

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 discloses a preparation method of phosphorus trifluoride. The preparation method comprises the following steps: S1, respectively adding phosphorus trichloride and anhydrous hydrogen fluoride into a uniform-temperature material changing structure of a reaction kettle; s2, condensing the crude phosphorus trifluoride gas, introducing the condensed crude phosphorus trifluoride gas into a first storage tank for storage, heating liquid in the first storage tank, and pumping the heated liquid into a flash evaporator for flash evaporation; s3, introducing the gas subjected to flash evaporation into a first rectifying tower for rectification, and introducing a product into an intermediate first product storage tank; s4, rectifying the material in the middle first product storage tank, condensing the rectified gas, and introducing the condensed gas into the first product storage tank for storage; s5, gasifying the finished product in the first product storage tank, enabling the gasified finished product to enter a gas-liquid separation tank for separation, discharging separated gas from the top, and sequentially introducing the separated gas into three phosphorus trifluoride purification devices for purification; s6, the purified gas is introduced into a filter to be filtered, the filtered gas enters a filling system to be filled after the pressure of the filtered gas is stabilized, and the stability of the product and the safety of equipment are guaranteed.

The invention discloses a continuous preparation method of high-purity phosphorus oxyfluoride and a device thereof, and relates to the technical field of production for phosphorus oxyfluoride preparation.According to the continuous preparation method of the high-purity phosphorus oxyfluoride, by conducting preheating treatment on a preheating head tank of polyphosphoric acid, the polyphosphoric acid is preheated from liquid in a viscous state to obtain liquid easy to convey, and the liquid is controlled through an electromagnetic valve; polyphosphoric acid is conveyed into a constant-temperature kettle through a high-level-difference pipeline, the polyphosphoric acid is further heated and stirred to keep constant temperature through the constant-temperature kettle, the polyphosphoric acid and anhydrous hydrogen fluoride are subjected to gas-liquid two-phase exchange contact in a preparation tower to realize reaction and separation, and prepared phosphorus oxyfluoride gas is separated from the top of the preparation tower; after further drying is achieved through the spray drying tower, the phosphorus oxyfluoride product with the purity reaching 99.6%-99.8% is prepared through the condenser and the gas-liquid separator, the reaction yield is 95%-96%, the purity of phosphorus oxyfluoride is high, few side reactions exist in the production process, and the reaction yield is high.

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.

The invention relates to a preparation method of phosphorus pentafluoride, which comprises the following steps: mixing a fluorocarbon compound with a phosphorus oxide compound and an oxidizing agent, reacting in a dry closed environment at high temperature and high pressure, collecting gas, and purifying to obtain the phosphorus pentafluoride. The invention also discloses a preparation method of lithium hexafluorophosphate, which comprises the following step: carrying out gas-solid reaction on the obtained phosphorus pentafluoride and lithium fluoride in a fluidized bed to prepare the lithium hexafluorophosphate. The method solves the problems of low purity of lithium hexafluorophosphate, difficulty in treatment of byproducts, low production efficiency and the like in the prior art.

The invention discloses reaction separation equipment for preparing phosphorus oxyfluoride, which comprises a reaction separation tower body, the lower end of the reaction separation tower body is sequentially provided with a feeding zone, a plurality of reaction zones and a separation zone from top to bottom, the feeding zone and the separation zone are fixedly filled with first filler layers, and the reaction zones are filled with second filler layers; the heat exchange mechanism comprises a heat exchange medium inlet container and a heat exchange medium outlet container, a plurality of heat exchange guide pipes are evenly distributed on the periphery of the heat exchange medium inlet container and the periphery of the heat exchange medium outlet container respectively, and heat exchange medium circulation pipes pre-buried in the second packing layer are longitudinally connected between the heat exchange guide pipes respectively; corresponding driving pipe fittings are upwards and rotationally mounted at the feeding ends of the heat exchange medium inlet pipes respectively; and a plurality of heat exchange medium discharge pipes. According to the invention, the reaction temperature uniformity in each reaction zone can be effectively improved, and the sufficient uniform distribution effect is ensured when materials slowly flow through the reaction zones.

The present invention belongs to the technical field of phosphorus pentafluoride preparation, and specifically relates to a method for synthesizing phosphorus pentafluoride by using yellow phosphorus and fluorine gas. The synthesis method comprises the steps of dissolving yellow phosphorus in an inert solvent to prepare a yellow phosphorus solution, then passing the yellow phosphorus solution and fluorine gas into a microchannel reactor for mixed reaction, and separating and purifying the generated gaseous product through a pressurized condensation system to obtain phosphorus pentafluoride. The synthesis method of the present invention utilizes a specific inert solvent to dissolve highly reactive yellow phosphorus, and then continuously synthesizes phosphorus pentafluoride by reacting the yellow phosphorus solution with fluorine gas in a microchannel reactor through a gas-liquid phase reaction. The method has the advantages of low reaction temperature, high reaction efficiency, few reaction by-products, and high product yield.

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.

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

The invention belongs to the technical field of fluorine chemical material preparation, and particularly relates to a method for continuously preparing phosphorus trifluoride based on liquid-liquid microfluidics. The method comprises the following steps: mixing AHF liquid with an excessive PC13 liquid material in a spherical liquid drop form, introducing the mixture into a spiral tube microreactor, controlling the pressure in the spiral tube microreactor to be 1.0-2.5 MPa and the temperature to be 60-140 DEG C, carrying out reaction, carrying out reduced pressure gas-liquid separation on the reacted material, and separating and purifying a gas-phase component to obtain phosphorus trifluoride, and the liquid-phase component enters the spiral tube microreactor as a PC13 liquid feed cycle to participate in the reaction. According to the invention, efficient, safe and continuous preparation of phosphorus trifluoride is realized through an innovative liquid-liquid microfluidic technology.

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.

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The present invention belongs to the technical field of phosphorus pentafluoride preparation, and in particular to a method for efficiently synthesizing phosphorus pentafluoride using phosphoric acid and hydrogen fluoride. The synthesis method comprises the following steps: adding phosphoric acid and anhydrous hydrogen fluoride into a reactor at a temperature of 20°C to 10°C and mixing them uniformly, then passing SF4 into a mixed reaction, introducing the reaction mixture into a thermal decomposition kettle for thermal decomposition, and performing rectification and separation on the gas phase product obtained by decomposition to obtain high-purity phosphorus pentafluoride; wherein the molar ratio of the phosphoric acid and anhydrous hydrogen fluoride added is 1:1~2; the molar ratio of the SF4 to phosphoric acid is 2~2.5:1. The present invention uses phosphoric acid and anhydrous hydrogen fluoride as raw materials, and by adding SF4 as a dehydrating agent and an auxiliary fluorinating agent, the efficiency of the fluorination reaction can be significantly improved, and the product quality and yield can be improved. The synthesis method of the present invention has the advantages of mild conditions, simple process, low equipment requirements, and environmental protection and high efficiency.

The present invention discloses a phosphorus trifluoride purification device, comprising an adsorption tower body, an upper cover, a plurality of air inlet ends, and an air outlet end, and further comprising: a double-position sliding molecular sieve structure, comprising a first molecular sieve adsorption cylinder and a second molecular sieve adsorption cylinder; a pressure variable diameter adjustment structure arranged between the first molecular sieve adsorption cylinder and the second molecular sieve adsorption cylinder, the pressure variable diameter adjustment structure comprising an elastic adjustment component arranged on the inner wall of the adsorption tower body, the upper and lower ends of the elastic adjustment component being respectively connected to the first molecular sieve adsorption cylinder and the second molecular sieve adsorption cylinder, a pressure adjustment disk being connected to the middle part of the elastic adjustment component, the pressure adjustment disk being provided with a plurality of holes for phosphorus trifluoride to pass through, the holes being provided with internal barrier structures, and a top bone component being fixedly provided on the top of the first molecular sieve adsorption cylinder. The present invention maximizes the extension of the service life of the adsorption structure while ensuring adsorption efficiency.

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 present invention relates to a comprehensive treatment method for the process tail gas of lithium hexafluorophosphate, comprising the following steps: 1) absorbing the tail gas containing phosphorus fluoride and phosphorus chloride with water to obtain a mixed acid containing hydrogen chloride, hydrogen fluoride and phosphoric acid; 2) electrolyzing the mixed acid obtained in step 1) until the hydrogen chloride in the mixed acid is completely electrolyzed to obtain a solution; 3) heating the solution obtained in step 2) to cause the water and hydrofluoric acid to escape by heat, and then obtaining hydrofluoric acid after cooling. Through electrolysis and phosphorus removal treatment, fluorine, chlorine and phosphorus in the process tail gas of lithium hexafluorophosphate are fully separated, and hydrofluoric acid and chlorine are respectively prepared. The chlorine can be recycled for the preparation of phosphorus pentachloride in the production of lithium hexafluorophosphate, realizing the recycling of chlorine. At the same time, industrial-grade hydrofluoric acid can be obtained, and the added value of the product is high.

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 device and method for producing phosphorus oxychloride using phosphorus trichloride. The device comprises a refining kettle, wherein a stirring and mixing assembly is provided in the refining kettle. The stirring and mixing assembly comprises a dual-shaft motor, a driving component, and two stirring rods. The driving component is transmission-connected to an output shaft at the bottom of the dual-shaft motor, and the two stirring rods are both transmission-connected to the driving component. A spiral cooling channel is provided in the inner wall of the refining kettle. In the invention, the stirring rods can both rotate along corresponding rotation axes and revolve around the transmission shafts, thereby fully mixing a mixture in the refining kettle and improving the yield and utilization rate of phosphorus trichloride. The rapid cooling assembly can automatically control the temperature in the refining kettle, thereby maintaining a stable reaction temperature and maintaining the production temperature of the crude phosphorus trichloride product within an appropriate range. This not only prevents the temperature in the refining kettle from being too high and causing danger, but also improves the yield of phosphorus oxychloride.

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 present invention belongs to the field of phosphorus pentachloride production, and specifically relates to a continuous phosphorus pentachloride preparation device, which includes a machine base and a housing assembly. The housing assembly includes a double-layer jacketed double-helix cylinder and a reaction port cylinder vertically fixed thereto. A hollow left helix assembly and a right helix assembly are provided inside the double-helix cylinder. The front ends of the two rotating main shafts are provided with heat transfer medium cavity inlets, and the rear ends are connected to solid transmission shafts. The top of the reaction port cylinder is provided with an upper end cover, and the upper end cover is provided with a phosphorus trichloride spray port and a chlorine inlet. A phosphorus trichloride spray nozzle is provided inside the reaction port cylinder. A phosphorus pentachloride discharge port is provided below the front end of the double-helix cylinder. The structure design of the fully enclosed, continuous reaction, crystallization, stirring, and pulverization integration completely changes the traditional production method of batch feeding and discharging and pouring and pulverizing. The material reaction is more sufficient, the discharge blockage is avoided, the leakage risk is reduced, the equipment has strong corrosion resistance, and the temperature and pressure regulation are more timely and accurate.