31 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 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 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 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 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 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.