30 results about "Phosphorous pentachloride" patented technology

The invention discloses a preparation process of high-purity phosphorus pentafluoride, which comprises the following steps of: firstly adding phosphorous pentachloride into a feed hopper of a spiral feeder under the protection of dry gas in a glove box to assemble a gas circulation loop, and simultaneously adding inert gas into the gas circulation loop in advance; starting a spiral stirring reaction furnace, simultaneously injecting mixed gas of hydrogen fluoride and fluorine gas into the spiral stirring reaction furnace, and controlling the reaction process by controlling the rotation frequency of the phosphorous pentachloride in the spiral feeder, the temperature of gas flow at the outlet of the spiral stirring reaction furnace and the pressure of the gas circulation loop; freezing the phosphorus pentafluoride gas and the hydrogen fluoride gas generated in the reaction process and unreacted hydrogen fluoride gas by a condenser-evaporator, and collecting high-purity phosphorus pentafluoride gas after reaction. The method is simple and effective and can be operated easily.

The invention discloses a method for preparing lithium hexafluorophosphate quickly. The method comprises steps as follows: (1) performing distillation to obtain a hydrogen fluoride liquid with the purity higher than 99.99wt%; (2) reacting the hydrogen fluoride liquid with phosphorous pentachloride to obtain a mixed gas of phosphorus pentafluoride and hydrogen chloride; (3) feeding the mixed gas of the phosphorus pentafluoride and the hydrogen chloride into hydrogen fluoride and lithium fluoride to obtain a lithium hexafluorophosphate solution; (4) filtering the lithium hexafluorophosphate solution obtained in Step (3) to remove insoluble impurities, performing stirring crystallization on a filtrate at the stirring speed of 50-100 rpm, and performing rotary drying at the temperature of 120 DEG C-130 DEG C after stirring crystallization to directly obtain the lithium hexafluorophosphate product with the radius ranging from 100 meshes to 400 meshes. According to the method, the operation is convenient, the lithium hexafluorophosphate obtained through stirring crystallization is in uniform granule shape directly, repeated drying and crushing steps are omitted, and the crystallization time is shortened.

The present invention relates to a method for preparing a novel organic field effect transistor material of a pyrrolo[3,2-b]pyrrole fused ring compound. The method includes the main steps of: 1) producing 6,12-dichloro diazocine from a diazocine compound under the action of phosphorus pentachloride; and 2) producing the target pyrrolo[3,2-b]pyrrole fused ring compound through reductive coupling of 6,12-dichloro diazocine under the action of a zinc powder and acid. The invention is characterized in that: 1) compared with the conventional synthetic strategy by a C-N bond to build a key reaction, the synthetic route takes the C-C bond built reduction coupling reaction as a key step, and the mehtod is simple, efficient and wide in universality; 2) reaction raw materials and reagents are cheap and easily available, reaction operation is simple and easy for amplification and for industrial production; 3) the remaining pyrrolo[3,2-b]pyrrole fused ring compounds obtained by the invention are firstly synthesized except for DBPP which has been reported, and the method can provide a variety of novel organic semiconductor materials with potential application values.

The invention discloses an internal circulation reactor and method for continuously preparing phosphorus pentafluoride. The internal circulation reactor comprises a cylinder body with a heat exchange jacket, wherein planar end closures are arranged at the upper and lower ends of the cylinder body, and a concentric inner cylinder body is arranged in the cylinder body; the upper end closure is provided with a mixed gas leading-out pipe; the lower end closure is provided with a three-way gas intake pipe; and a reaction solution eduction pipe and a feed liquid ingress pipe are arranged on the cylinder body. The process of preparing phosphorus pentafluoride comprises the following steps: blowing the reactor with an inert gas; creating a low temperature environment of the reactor with a refrigerant; adding a phosphorous pentachloride solution, anhydrous hydrogen fluoride and the inert gas to the reactor for reaction; and continuously leading out mixed gas containing phosphorus pentafluoride and part of a low-concentration phosphorous pentachloride solution, and at the same time continuously adding a phosphorous pentachloride concentrated solution, anhydrous hydrogen fluoride and the inert gas to realize continuous operation. The internal circulation reactor and method for continuously preparing phosphorus pentafluoride have the advantages that the concentration stability of reactants in the reactor can be maintained, and continuous production and automatic control of phosphorus pentafluoride are realized.

The invention discloses a preparation method of chlorine/phosphorus-codoped carbon quantum dots. The method comprises the following steps: mixing liquid alcohol or carboxylic acid with phosphorous pentachloride, repeatedly heating and cooling, and carrying out chromatography to obtain the purified chlorine/phosphorus-codoped carbon quantum dots. The preparation method has the advantages of mild reactions, high controllability, high carbon quantum dot yield and the like, and is suitable for mass production.

The invention relates to a synthesis method of dimethylheptyl methylphosphonate, and aims to solve the difficulty in raw material measurement and the safety problem caused by the use of the high-pressure reaction kettle in the existing technique, thereby lowering the production cost. The invention has the advantages of simple operating procedure, high output and high yield, and is suitable for industrial production. The method comprises the following steps: adding an acyl-chlorination reagent into a reaction vessel, wherein the acyl-chlorination reagent is thionyl chloride, phosphorous pentachloride or triphosgene; dropwisely adding dimethyl methyl phosphonate (DMMP) into the acyl-chlorination reagent at room temperature and adding catalytic amount of catalyst, wherein the consumption of the acyl-chlorination reagent is 2-5 times of the DMMP (0.6-1.5 times for triphosgene) on mol basis, and the catalyst is N,N-di-substituted-formamide or N-containing aromatic heterocyclic ring or N-substituted N-containing aromatic heterocyclic ring or tertiary amine; and uniformly stirring at room temperature.

The invention provides a post-transition metal complex having a structure shown in a formula (I). The invention also provides a preparation method of the post-transition metal complex, which comprises the following steps: performing first reaction on di(substituted phenylamine)-2,6-pyridine dicarboxamide and phosphorous pentachloride in a first organic solvent to obtain a ligand having a structure shown in a formula (II); and performing second reaction on the ligand and post-transition metal halide in a second organic solvent to obtain the post-transition metal complex having the structure shown in the formula (I). The invention also provides a polyethylene preparation method which comprises the following specific step: under the effects of a cocatalyst and the post-transition metal complex having the structure shown in the formula (I), performing polymerization reaction on ethylene in an organic solvent to obtain polyethylene. The post-transition metal complex provided by the invention has high catalytic activity in catalytic ethylene polymerization.

The invention discloses a preparation method of trandolapril midbody (2S, 3aR, 7aS)-octahydro-1H-indole-2-carboxylic acid, and the preparation method comprises the following steps of: preparing 3-chlorine-2-amino-propionic acid methyl ester hydrochloride by using phosphorous pentachloride and dichloromethane; preparing 3-chlorine-2-acetyl amino-propionic acid methyl ester hydrochloride by using the 3-chlorine-2-amino-propionic acid methyl ester hydrochloride, methylbenzene and acetyl chloride; preparing 2,3,4,5,6,7-hexahydro-1H-indole-2-carboxylic acid by using the 3-chlorine-2-acetyl amino-propionic acid methyl ester hydrochloride, DMF (Dimethyl Formamide) and 1-pyrrole cyclohexene; preparing (2S)-octahydro-1H-indole-2-methyl carboxylat by using the 2,3,4,5,6,7-hexahydro-1H-indole-2-carboxylic acid, methanol and palladium on carbon; preparing the (2S, 3aR, 7aS)-octahydro-1H-indole-2-carboxylic acid by using the (2S)-octahydro-1H-indole-2-methyl carboxylat and the methanol. Compared with the prior art, the preparation method of the trandolapril midbody (2S, 3aR, 7aS)-octahydro-1H-indole-2-carboxylic acid, which is disclosed by the invention, has the advantages of easiness and convenience for process, easiness for control, safety, reliability and low cost.

The invention discloses a method for synthesizing 2-chloropyridine. The steps of the method are to add pyridine and solvent into a 500mL container, control the pressure at normal pressure, stir for 10-20min, then add fluorine acetate dropwise, and control the temperature not to exceed 30°C; move the reaction mixture to a 500mL container, The temperature is raised to 50°C-70°C, vacuum distillation is carried out under the conditions of vacuum degree 0.07-0.09MPa, and after no liquid is evaporated, the remaining material is 2-chloropyridine. The chlorination of the inventive method does not need highly toxic substances such as chlorine gas, phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride and phosgene as the chlorination reagent, but uses dichloromethane as the chlorination reagent. It is safe and reliable; the reaction is carried out under normal temperature and pressure, and the yield of 2-chloropyridine reaches 80%.

The invention discloses a novel method for synthesizing and purifying phosphonitrilic chloride trimer by taking Lewis acid as the catalyst and adopting the sublimation method. The method disclosed by the invention is characterized by comprising the following steps of: synthesizing phosphonitrilic chloride trimer in chlorobenzene as the solvent by selecting Lewis acid as the catalyst and taking ammonium chloride and phosphorus pentachloride as the raw materials, after removing chlorobenzene, dissolving phosphonitrilic chloride trimer by using normal hexane to eliminate linear polymer, and finally, purifying by adopting the sublimation method to obtain phosphonitrilic chloride trimer with the purity of above 99%, wherein the total yield is about 60%. Compared with the prior art, the catalytic system is optimized; the purity of the prepared phosphonitrilic chloride trimer is high; and the novel method disclosed by the invention is applied to industrialized mass production.

The invention discloses a method for synthesizing phosphorus pentachloride. Phosphorus trichloride is injected into a reactor, chlorine gas is passed into the bottom of the reactor through a pipeline, and stirred at a stirring speed of 500 rpm and a pressure of 0.6kpa. Control the reaction temperature to 75-83°C, stop the reaction until no solid matter is generated, and obtain solid phosphorus pentachloride; then put the solid phosphorus pentachloride into a sublimation tank for decompression sublimation; collect the sublimation gas, and carry out Cool and recrystallize to obtain high-purity solid phosphorus pentachloride. Beneficial technical effects of the present invention: the present invention has the advantages of simple preparation, low cost and easy popularization.

The invention relates to the field of lithium batteries, and discloses phosphate as well as a preparation method and application thereof. In the phosphate, R1 is alkyl with the carbon atom number of 1-8, or fluorine-substituted alkyl with the carbon atom number of 1-8, or fluorine-substituted aryl or fluorine-free aryl; R2 is a hydrocarbon group having 1-8 carbon atoms and containing an alkenyl group or an alkynyl group; and R3 is a group containing a cyano group. The preparation method comprises the following steps: S1, reacting alcohol R1OH with phosphorus pentachloride in a solvent to obtain an intermediate; S2, reacting another alcohol R2OH with the intermediate to obtain a product or another intermediate; S3, reacting a third alcohol R3OH with the intermediate in the second step to obtain a product. The electrolyte prepared from the phosphonate can improve the cycling stability, safety performance and storage stability of the secondary battery.

The invention discloses a synthesis method of N-cyclohexyl-5-(4-chlorobutyl)-1H-tetrazole. The synthesis method comprises the following steps: firstly, synthesizing N, N-dimethylformamide; the synthesis method comprises the following synthesis steps: taking 5-chlorovaleronitrile and cyclohexanol as raw materials, controlling the molar ratio of the 5-chlorovaleronitrile to the cyclohexanol to be (1: 1)-(1: 1.5) and the reaction temperature to be 5-55 DEG C, and carrying out a catalytic reaction for 1-6 hours by virtue of concentrated sulfuric acid, so as to obtain 5-chloro-N-cyclohexylvaleramide; wherein the molar ratio of the 5-chlorovaleronitrile to the concentrated sulfuric acid for catalysis is (1: 3)-(1: 10); the preparation method comprises the following steps: treating 1, 5-chloro-N-cyclohexylvaleric amide with phosphorus pentachloride; wherein the molar ratio of the 3, 5-chloro-N-cyclohexylvaleric amide to the phosphorus pentachloride is (1: 1)-(1: 1.5) and the molar ratio of the 2, 5-chloro-N-cyclohexylvaleric amide to the phosphorus pentachloride is (1: 1)-(1: 1.5); according to the invention, trimethyl silicon azide is used as a cyclization reagent instead of azoic acid or sodium azide, so that the synthesis method has the advantages of higher stability, no explosion and higher safety, the cost can be effectively reduced, the synthesis method is environment-friendly,and the purity of the obtained product is high.

The invention relates to the technical field of battery production, and particularly discloses a preparation method of lithium hexafluorophosphate. The preparation method of the lithium hexafluorophosphate comprises the following steps: (1) uniformly mixing phosphorus pentachloride, triethylamine and a fluorinating agent to obtain a raw material solution; (2) mixing and uniformly stirring lithium hydroxide, ammonium fluoride, a pore-forming agent, a combustion improver and the binder dispersion liquid, and drying to obtain a lithium fluoride mixture; (3) calcining the lithium fluoride mixture to constant weight at 700-750 DEG C to obtain porous lithium fluoride; and (4) uniformly mixing the porous lithium fluoride with the raw material solution under the protection of nitrogen, keeping the temperature at 5-15 DEG C for 60-80 minutes, filtering and concentrating under reduced pressure to obtain a crude product lithium hexafluorophosphate, and purifying the crude product lithium hexafluorophosphate to obtain the lithium hexafluorophosphate. According to the porous lithium fluoride, the generation rate of lithium hexafluorophosphate can be increased, and the time required for producing the lithium hexafluorophosphate can be shortened.

The invention discloses a production method of diacetyl monoxime, and relates to a method for producing diacetyl monoxime by reacting butanone with alkyl nitrite in a microtube reactor under the catalysis of a mixed catalyst system. . The method comprises the following steps: respectively adding premixed liquid of the catalyst and the butanone and the alkyl nitrite into the microtube reactor through a metering pump, wherein the mass ratio of the catalyst to the butanone is (0.1-0.2): 1, the molar ratio of the alkyl nitrite to the butanone is (1.01-1.1): 1, and the reaction pressure in the microtube reactor is 0.1-0.5 MPa, the reaction temperature is set to be 30-50 DEG C, the reaction time is 30-60 seconds and the catalyst is a mixture of concentrated hydrochloric acid, phosphorus pentachloride and concentrated phosphoric acid. The method has the beneficial effects that the moisture in the reaction system is reduced, the excessive use of raw materials is avoided, the production cost issaved, the production efficiency is improved and the pollution of excessive reactants to the environment is reduced and the reaction safety is improved; and the equipment investment is low, the occupied area is small and mass production is facilitated.

A process for manufacturing phosphorous trichloride, phosphorous pentachloride and cement comprising of heating at elevated temperature of 1100° C. to 1500° C. pulverised mixture of phosphate ores, carbonaceous substances, silica and/or alumina and treating the resultant gaseous products with chlorine in the ratio of 1 to 5 moles of chlorine per mole of phosphorous oxide contained in the phosphate ores while maintaining the temperature between 400° C. to 1000° C. by cooling and thereafter firstly separating gaseous mixture of primarily phosphorous trichloride and phosphorous pentachloride, from cement and later separating phosphorous trichloride and phosphorous pentachloride, both separations by known methods.

The invention relates to a preparation method of a diphosphorus ligand, which comprises the following steps: carrying out Grignard reaction on a compound (1) and magnesium metal to prepare a compound (2); carrying out first substitution reaction on the compound (3) and phosphorus pentachloride to prepare a compound (4); then carrying out second substitution reaction on the compound (2) and a compound (4) to prepare a compound (5); finally, the compound (5) is subjected to a reduction reaction, and the diphosphine ligand shown in the formula (6) is obtained. The process is simple, raw materials are simple and easy to obtain, the process conditions in the preparation process are easy to control, phosphorus-hydrogen intermediates do not need to be prepared, the diphosphine ligand can be prepared under the mild process conditions, and large-scale production of the diphosphine ligand is facilitated.