163 results about "Phosphorus trichloride" 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 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 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 hydrolysis-resistant liquid phosphite ester and a preparation method and application thereof.The hydrolysis-resistant liquid phosphite ester is prepared by the steps that 2, 2, 4-trimethyl-1, 3-pentanediol and phosphorus trichloride or phosphite triester serve as raw materials, a cyclization reaction is conducted firstly, and then the hydrolysis-resistant liquid phosphite ester is obtained; and then carrying out nucleophilic substitution on Cl or aryl and alkyl on the cyclized intermediate by using higher saturated monohydric alcohol with more than C8, wherein the molecular structure is as shown in formula I in the specification. The liquid phosphite ester is novel liquid phosphite ester, the main body of the liquid phosphite ester is of a six-membered ring structure, the basic structure of the phosphite ester is reserved to the maximum extent, and the anti-oxidation effect of the phosphite ester is guaranteed; hydrophobic aliphatic chain structures on phosphorus atoms and branched chains of the phosphorus atoms prevent water molecules from approaching P-O bonds, so that the phosphorus atoms and the branched chains are prevented from being attacked by the water molecules, and the hydrolysis resistance is improved under the conditions that any additional amine hydrolysis-resistant agent is not used and any steric hindrance group is not introduced; good practical value, economic value and market prospect are realized.

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 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 provides a preparation method of a phosphoramidite compound. The preparation method comprises the following steps: (1) mixing a nitrogen-containing compound and an acid-binding agent with a first solvent to obtain a first mixed solution; mixing phosphorus trichloride with a second solvent to obtain a second mixed solution; mixing aromatic diphenol with a third solvent to obtain a third mixed solution; (2) pumping the first mixed solution and the second mixed solution obtained in the step (1) into a first micro-mixer, and then enabling the first mixed solution and the second mixed solution to enter a first micro-channel reactor for reaction to obtain a reaction solution containing monochlorophosphoramidite; (3) enabling the reaction solution containing the monochlorophosphoramidite obtained in the step (2) and the third mixed solution obtained in the step (1) to enter a second micro-mixer, and then enabling the mixture to enter a second micro-channel reactor for reaction to obtain a phosphoramidite compound; the acid-binding agent is a polyether tertiary amine compound. The preparation method is short in reaction time and high in product yield.

The invention discloses a novel method for synthesizing a ferrocenyl phosphine ligand compound, which comprises the following steps of: reacting a ferrocene compound serving as a starting material with a Grignard reagent and phosphorus trichloride under the action of tert-butyl lithium to generate a ferrocene phosphine ligand, and synthesizing a ferrocene diphosphine ligand in one step. The method is stable and high in practicability, and a novel method for synthesizing the ferrocene ligand compound is provided.

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 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 present invention discloses a high-performance water reducer of organosilicon condensate type and a preparation method thereof. Liquid ammonia and ethylene oxide undergo a ring-opening reaction to obtain an N-hydroxyethylamine compound. The N-hydroxyethylamine compound is condensed with formaldehyde to obtain an N-hydroxyethyl-N-hydroxymethylamine intermediate. The N-hydroxyethyl-N-hydroxymethylamine intermediate undergoes an esterification reaction with phosphorus trichloride to obtain an amino alcohol intermediate containing a phosphate ester group. The amino alcohol intermediate containing a phosphate ester group is polymerized with a dihydrogen-terminated polydimethylsiloxane oligomer to obtain an organosilane-modified oligomer containing amino and phosphate ester groups, and then a high-performance water reducer is obtained through high-temperature dehydration. The phosphate ester group, siloxane group, and amino group connected to the high-performance water reducer of the present invention reduce the liquid-solid interfacial energy and improve the dispersing ability, dispersion stability, and anti-sludge ability of the high-performance water reducer to cement particles. The water reducer of the present invention has a protective effect on the steel bars in reinforced concrete, the preparation process is simple, the product has good uniformity, realizes low cost, green environmental protection, and multifunctionalization, and has good application prospects.

The invention relates to a synthesis method of triphenylphosphine, which belongs to the technical field of organic synthesis, and comprises the following steps: Step 1: adding a solvent, magnesium chips and an initiator into a reaction bottle, and heating to 50-60 DEG C; 2, dropwise adding a mixed solution of benzene halide and phosphorus trichloride, and after addition is completed, carrying out a heat preservation reaction; 3, after the reaction is finished, the temperature is reduced to the room temperature, water is added for washing and layering, an organic phase is concentrated, the solvent is recycled, and triphenylphosphine is obtained. According to the method, benzene halide and phosphorus trichloride are used as raw materials and react with magnesium chips through a one-pot method in a solvent to directly synthesize triphenylphosphine, compared with a traditional synthesis method, a Grignard reagent does not need to be prepared step by step, high energy consumption caused by low-temperature reaction conditions during subsequent Grignard reagent addition is not needed, the process is safer and more efficient, energy consumption can be effectively reduced, and the method is suitable for industrial production. Compared with a traditional synthesis method, the method has the advantages of no high risk of a sodium method process, safety and environmental protection pressure relief, simple overall process, high yield and suitability for industrial large-scale production.

This invention discloses a tail gas treatment absorption tower for phosphorus trichloride production. The invention relates to the technical field of tail gas treatment absorption towers and includes a shell. An annular plate is fixedly connected to the inner wall of the shell near the inlet pipe. The annular plate has a trapezoidal cross-section and multiple through holes in its center. Multiple elastic plates are symmetrically arranged inside each through hole, with two elastic plates forming a group. Within each group, two elastic plates are symmetrically arranged inside the through hole, and the elastic plates are inclined, forming a V-shape. In this phosphorus trichloride tail gas treatment absorption tower, the inlet pipe is tangentially oriented. This tangential inlet causes the tail gas to form a spiral upward airflow along the inner wall of the tower. The gas is further diverted through the evenly distributed through holes on the annular plate, thereby improving the uniformity of the gas flow velocity entering the bottom of the packing layer, ensuring no dead zones in gas-liquid contact, and extending the gas flow path within the tower.

The invention discloses a preparation method of an antioxidant GP, and belongs to the technical field of antioxidants, the key point of the technical scheme is that the preparation method of the antioxidant GP comprises the following preparation steps: dissolving 3, 3 ', 5, 5'-tetra-tert-butyl-2, 2 '-biphenol in a solvent, then adding an acid-binding agent, stirring uniformly, then dropwise adding a phosphorus trichloride solution, and stirring uniformly to obtain a solution A; the preparation method comprises the following steps: dropwise adding 2-(tert-butyl)-4-(3-hydroxypropyl)-6-methylphenol into a reaction kettle, keeping the reaction temperature at 45-50 DEG C during dropwise adding, reacting for 3-6 hours after dropwise adding, then dropwise adding a toluene solution containing 2-(tert-butyl)-4-(3-hydroxypropyl)-6-methylphenol at 45-50 DEG C, heating to 95-100 DEG C after dropwise adding, reacting for 2-3 hours, cooling, washing, carrying out reduced pressure distillation, crystallizing and filtering to obtain the antioxidant GP, the effect of shortening the production time of the antioxidant GP is achieved.

The invention provides a preparation process of 2-(p-chlorphenyl)-5-trifluoromethyl-pyrrole-3-nitrile, which comprises the following steps: taking p-chlorphenylglycine and trifluoroacetic acid as raw materials, carrying out acylation reaction under the action of a catalyst to generate 4-(4-chlorphenyl)-2-trifluoromethyl-3-oxazole-5-ketone, then adding 2-chloroacrylonitrile, and carrying out reaction under the action of a catalyst to generate 4-(4-chlorphenyl)-2-trifluoromethyl-3-oxazole-5-ketone. And carrying out cyclization reaction to generate the 2-(p-chlorphenyl)-5-trifluoromethyl-pyrrole-3-nitrile product. According to the method, acylation reagents such as phosphorus trichloride and phosphorus oxychloride are not used, so that the generation of phosphorus-containing and high-ammonia-nitrogen wastewater is reduced, the wastewater treatment difficulty and cost are reduced, and meanwhile, the production risk and the environmental harm are also reduced; the final product is directly prepared by a one-pot method, and the operation of separating and purifying the intermediate product by using another solvent is avoided, so that the steps are greatly simplified, the production efficiency is improved, the use of the solvent can be reduced, and the hidden danger in the solvent recovery process is reduced.

The invention provides a synthesis process of isophthaloyl dichloride, which comprises the following steps: firstly, adding quantitative isophthalic acid into a reaction kettle, then adding quantitative phosphorus trichloride, mixing and stirring, adding quantitative phosphorus pentachloride, then introducing chlorine, and reacting to obtain isophthaloyl dichloride. The melting point of the isophthaloyl dichloride prepared by the process is 43.2-42.8 DEG C, the purity reaches 99.95% or above, and the yield is greater than 98%. The process has the advantages of no solvent mixing, no catalyst, easily available raw materials, low cost, short reaction period, low energy consumption, high yield, convenient reactant separation and purification, simple process control, safety, reliability, high byproduct value, easy tail gas treatment and the like, and is suitable for industrial production.

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 relates to the technical field of synthesis of hexafluorophosphate, in particular to a synthesis method and a synthesis system of liquid hexafluorophosphate. The synthesis method of the liquid hexafluorophosphate is a new process route, phosphorus trichloride is used as an initial raw material, and a reaction is carried out with a reaction kettle; phosphorus pentafluoride sequentially subjected to oxidation, fluorination, deep fluorination and solvent in-situ capture reacts with alkali metal fluoride to obtain liquid hexafluorophosphate; the whole technical route process has the advantages of controllability, low cost, greenness, high safety and few impurities.

The invention relates to the technical field of synthesis of chlorine-containing pyridine intermediates, and discloses a method for synthesizing 2, 3, 4, 5-tetrachloropyridine by using 2, 5-dichloropyridine, which comprises the following steps: step 1, preparation of 2, 5-dichloropyridine nitrogen oxide: taking 2, 5-dichloropyridine as a raw material, reacting in the presence of a catalyst and acetic acid, and then filtering to remove the catalyst to obtain 2, 5-dichloropyridine nitrogen oxide; adding an acetic acid solution of 2, 5-dichloropyridine nitrogen oxide; step 2, nitration reaction: adding sulfuric acid and nitric acid, and reacting to obtain 2, 5-dichloro-4-nitropyridine nitrogen oxide; step 3, nitrogen and oxygen removal reaction: adding acetyl chloride to replace 4-position nitro to obtain 2, 4, 5-trichloropyridine nitrogen oxide, and then adding phosphorus trichloride to remove nitrogen and oxygen to obtain 2, 4, 5-trichloropyridine; and 4, chlorination and refining: adding Lewis acid into the 2, 4, 5-trichloropyridine, reacting to obtain a 2, 3, 4, 5-tetrachloropyridine crude product, and refining the crude product to obtain the finished product 2, 3, 4, 5-tetrachloropyridine. The invention solves the problems of more byproducts and unsatisfactory product purity and yield in the prior art.

The utility model discloses an automatic reduction device for vaporizing phosphorus trichloride and premixing the vaporized phosphorus trichloride with hydrogen in proportion, relates to the technical field of compound reduction reaction devices, and aims to solve the problem of low yellow phosphorus yield caused by insufficient reduction reaction of phosphorus trichloride and hydrogen. According to the device, an automatic parameter control cabinet is electrically connected to an automatic reduction device, the bottom end of a first reaction kettle is communicated with a hydrogen inlet pipeline through a pipeline, a hydrogen premixing and dispersing device is arranged at the bottom in a cavity of the first reaction kettle, and a plurality of premixing and heating devices are arranged on the outer wall of the first reaction kettle; the top end of the first reaction kettle is connected with a premixing gas-liquid separator through a pipeline, the premixing gas-liquid separator is mounted in a cavity of the second reaction kettle, and one side of the bottom of the first reaction kettle is connected with the second reaction kettle through a pipeline provided with a stop valve; the bottom end of the second reaction kettle is communicated with a phosphorus trichloride liquid inlet pipeline through a pipeline, and the top end of the second reaction kettle is connected with a premixed gas reduction pipeline.

The invention discloses a solvent-participation-free synthesis process of p-ethyl propiophenone, which comprises the following steps: by taking ethylbenzene and propionyl chloride as raw materials and phosphorus trichloride and lewis acid as catalysts, carrying out Friedel-Crafts acylation reaction without adding other reaction solvents to obtain the p-ethyl propiophenone. Compared with the prior art, the method has the advantages that the generation of disubstituted impurity 1-(2, 4-diethyl phenyl) propan-1-ketone is unexpectedly and effectively avoided, the impurity generation amount is less than 5%, the yield and the purity of p-ethyl propiophenone are greatly improved, and the synthesis process is green, environment-friendly, low in cost and convenient for realizing industrial production, and can be used for industrial production of eperisone.

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 of tris (2-cyanoethyl) phosphate, which comprises the following steps of: 1, adding 3-hydroxypropionitrile, an organic alkali acid-binding agent and a reaction organic solvent which is one of dichloromethane and dichloroethane into a reaction container, and reacting at the temperature of between 20 and 30 DEG C for 1 to 3 hours; controlling the temperature not to exceed 20 DEG C, dropwise adding a mixture formed by phosphorus trichloride and a reaction organic solvent, after dropwise adding is completed, performing heating reflux reaction, and after the reaction is completed, performing suction filtration to remove generated organic alkali hydrochloride so as to obtain filtrate; and 2, controlling the temperature of the filtrate obtained in the step 1 at 30-40 DEG C, introducing oxygen for reaction until the reaction is finished, and removing the reaction organic solvent to obtain the final product tris (2-cyanoethyl) phosphate. The method has the advantages of simplicity in operation, mild and controllable reaction, high product purity and suitability for industrial popularization.

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.

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.

The invention discloses a method for continuously preparing trimethylolpropane phosphite, which comprises the following steps of: metering and conveying a trimethylolpropane solution containing a catalyst and phosphorus trichloride serving as raw materials into a single-stage or multi-stage series falling film reactor respectively through a pump for continuous reaction, and arranging a jacket outside the reactor for temperature control, solvent steam and generated hydrogen chloride gas in the reaction process are discharged from the upper part of the reactor, and after a certain retention time, reaction completion liquid flows out from the bottom of the reactor to obtain the product trimethylolpropane phosphite. The continuous preparation of the trimethylolpropane phosphite ester is realized through the falling film reactor, the synchronous removal of the solvent and the byproduct hydrogen chloride is realized while the reaction is completed, the reaction efficiency is high, the system is simple, the cost is low, the yield is high, the intrinsic safety is high, and industrial production is easy to realize.

The application provides a reaction device and method for continuously synthesizing trimethyl phosphite, and belongs to the technical field of trimethyl phosphite synthesis. The reaction device comprises a raw material tank group, a composite reaction kettle, a solvent tank, a pre-cooler, a water washing kettle, an alkali liquid buffer tank, a layered system and a rectification system. The raw material tank group comprises a methanol tank and a phosphorus trichloride tank. The raw material tank group and the solvent tank are connected with the composite reaction kettle through pipelines via the pre-cooler, and the composite reaction kettle is connected with the water washing kettle through a pipeline. The phosphorus trichloride drop-like feed is efficiently converted into a uniform liquid film by a centrifugal disc, and then the liquid film is converted into a fine jet flow by a spraying ring. The fine jet flow is instantaneously and highly intensively sheared with a strong vortex-shaped methanol / solvent flow formed through a tangential feeding pipe. The secondary intensified mixing mode replaces the macroscopic mixing limitation of a traditional stirred tank, realizes instant and uniform mixing of materials at a micro level, thereby inhibiting a side reaction and effectively improving a reaction rate.

This invention discloses a chiral monophosphine ligand, its preparation method, and its application in asymmetric synthesis. The ligand preparation method involves mixing an N,N',1,2-tetrasubstituted ethane-1,2-diamine compound, phosphorus trichloride, triethylamine, and solvent under a nitrogen or argon atmosphere at -80 to -70°C, and reacting at 60 to 80°C for 6 to 8 hours. The resulting reaction mixture is then cooled to room temperature, and an alcohol, phenol, or Grignard reagent is added dropwise, reacting at 60 to 80°C for 8 to 12 hours. The resulting mixture is then post-treated to obtain the chiral monophosphine ligand. The application involves stirring a nickel catalyst, a chiral monophosphine ligand, a solvent, a diene, and an aldehyde under an argon or nitrogen atmosphere at a specified temperature for 12 to 15 hours. The mixture is then post-treated to obtain the target product. This method utilizes widely available and inexpensive raw materials, and the operation is simple, achieving high stereoselectivity and enantioselectivity in the synthesis of alcohol compounds containing chiral conjugated dienes through a one-step reaction.