50 results about "Phosphorus halide" patented technology

The invention discloses a preparation method of 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. According to the preparation method, triphenyl phosphine is taken as the raw material, triphenyl phosphine reacts with metal sodium and phosphorus halide to generate reaction product (I), the reaction product (I) reacts with acyl chloride to generate reaction product (II), and the reaction product (II) is oxidized to produce 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. The preparation method has the advantages of easily-available raw materials, low cost, easy operation, environment-friendliness, and easiness for industrialization.

The invention relates to an alkyl phosphorus dihalide preparing method and belongs to the technical field of preparation of alkyl phosphorus halide. According to the method, hydrocarbon and phosphorus trihalide are taken as raw materials, alkali metal or alkaline-earth metal is taken as the initiator, and reaction is conducted at -30-170 DEG C. The initiator alkali metal or alkaline-earth metal reacts with the phosphorus trihalide to generate phosphorus dihalide free radicals, and free radical reaction is conducted between the phosphorus dihalide free radicals and the hydrocarbon to generate alkyl phosphorus dihalide, halogen hydride and a small amount of alkali halide or alkaline earth halide. The generated halogen hydride is low in solubility in a reaction system, and therefore the halogen hydride can be separated out in the gas form simply by conducting decompression on products. Compared with existing methods of preparing alkyl phosphorus dihalide with hydrocarbon and phosphorus trihalide as raw materials, the method has the advantage that due to the adoption of the initiator alkali metal or alkaline-earth metal, reaction temperature is reduced remarkably, so that the requirements of reaction for temperature and equipment are reduced, and then cost is reduced greatly.

A process for high temperature hydrolysis of halosilanes and halides with the steps of: providing a bed of fluidized particulate material heated to at least 300° C., injecting steam and an excess of reactants into the reactor, removing solid waste from a bottom outlet, removing the effluent gases through a solids removal device such as a cyclone, condensing and separating some of the unreacted waste from the effluent gas in a distillation column and sending the effluent gases containing hydrogen and hydrogen chloride to a compressor. In a preferred embodiment the reactants contain at least one water reactive halide, selected from the group halosilane, organohalosilane, aluminum halide, titanium halide, boron halide, manganese halide, copper halide, iron halide, chromium halide, nickel halide, indium halide, gallium halide and phosphorus halide and where the halide content is selected from chlorine, bromine and iodine.

The invention provides a new method for preparing a phosphorus-nitrogen-carbon trinity intumescent flame retardant with hexamethylolmelamine, melamine and phosphorus halide as the main raw materials and an inert organic solvent as the reaction medium. The reaction of methylol melamine and phosphorus halide in an inert organic solvent to obtain an esterification product; then adding water to the esterification product for hydrolysis, after the organic phase and the aqueous phase are separated, the organic phase is separated to obtain a hydrolyzate solution; the hydrolyzate Melamine is added to the solution to form a salt, and a white precipitate is produced to obtain hexamethylol melamine phosphate melamine salt. The compound molecule contains three elements of phosphorus, nitrogen and carbon, that is, an intumescent flame retardant of the trinity of phosphorus, nitrogen and carbon. Since an inert organic solvent is used as the reaction medium, the preparation method is convenient to operate and is conducive to realizing industrial production. Excellent combustion performance.

The invention discloses a preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method comprises the following steps: selecting triphenylphosphine as a raw material for reactions with sodium metal and phosphorus halide in the presence of one or more catalysts; carrying out an acyl chloride reaction; carrying out oxidation to prepare phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method has the advantages of being easy in raw material obtaining, low in cost, easy to operate, environmentally friendly, and easy for industrialization.

In a method for making bisphosphonates by reacting a carbonyl compound with a phosphorus halide, the reaction is carried out in a solvent / carrier system which is a mixture of an amine hydrochloride, phosphorous acid and optionally phosphoric acid.

The invention discloses a synthesis method of hexafluorophosphate, which belongs to the technical field of chemical synthesis, and is characterized by comprising the following steps: dissolving phosphorus pentahalide in an inert solvent to obtain a phosphorus pentahalide inert solvent solution, dissolving alkali metal halide salt in anhydrous hydrogen fluoride to obtain an alkali metal villiaumite hydrogen fluoride solution, the method comprises the following steps: inputting hexafluorophosphate, hydrogen fluoride, an inert solvent and hydrogen halide into a reactor in proportion for reaction to obtain a mixture consisting of the hexafluorophosphate, the hydrogen fluoride, the inert solvent and the hydrogen halide, firstly removing hydrogen halide gas through gas-liquid separation, then recovering the hydrogen fluoride through heating evaporation, finally recovering the inert solvent through solid-liquid separation, and drying a solid to obtain the hexafluorophosphate, the synthesis method disclosed by the invention has the advantages of simplicity in operation, good safety, high reaction yield, excellent product quality, capability of realizing continuous production and the like.

The invention discloses a preparation method of tris(trimethylsilyl)phosphate. The preparation method comprises the steps that an alkane or ether solvent is selected, two reactants including alkali metal silicon alkoxide and phosphorus halide are added into the solvent according to the mole ratio of 1:1, and stirring is intensely conducted in the adding process; inorganic salt is removed through filtration, and reduced pressure distillation is conducted on the solution under the condition of 90 DEG C / 20 mmHg to obtain the target product, wherein the purity of the product can reach 99.6% or above. Accordingly, industrialized production is achieved, and great market prospects and economic values are achieved.

The invention discloses a preparation method of tris(trimethylsilyl)phosphate; through selection of an alkane or ether solvent, two reactants of an alkali metal silicon alkoxide and phosphorus halide are added to the above solvent in accordance with the molar ratio of 1:1, and vigorous stirring is carried out in the process of adding; and finally an inorganic salt is filtered to remove, and the solution is subjected to reduced pressure distillation under the condition of 90 DEG C / 20 mmHg to obtain the target product, wherein the purity of the product can reach more than 99.6%. Industrialized production is achieved, and the preparation method has huge market prospects and economic values.

Disclosed is a process for the preparation of phosphine-aminophosphines that are useful in the formation of catalysts useful in carrying out a wide variety of reactions such as asymmetric hydrogenations, asymmetric reductions, asymmetric hydroborations, asymmetric olefin isomerizations, asymmetric hydrosilations, asymmetric allylations, asymmetric conjugate additions, and asymmetric organometallic additions. The process comprises the steps of (1) contacting a compound of formula 2R2P—L—NHR3  2with phosphorus trihalide PX3 in the presence of an inert, organic solvent and an acid acceptor to produce intermediate compound having formula 3 (2) contacting intermediate compound 3 with a reactant having the formula R1—M1, R2—M1 or a mixture thereof.

The invention provides a preparation method and an application of phosphorus-halide-cooperation inflaming retarding polyether polyol. The preparation method of the polyol mainly comprises the following steps of: performing hydrolysis on epoxy chloropropane to generate 3-chloro-1,2-propanediol; reacting a halide aromatic diphenol compound with alkalis hydroxide with phosphorus flame retardant serving as a dissolvent, and then reacting the halide aromatic diphenol compound with the 3-chloro-1,2-propanediol under the action of a catalyst; and performing reduced pressure distillation and filtration on a reaction liquid to obtain a light yellow liquid, wherein the contained halide component is halide aromatic diphenol diglycerol ether, the contained phosphorus component is the phosphorus flame retardant, and the total recovery of products is more than 90%. A polyurethane material prepared with the novel phosphorus-halide-cooperation inflaming retarding polyether polyol being inflaming retarding polyol has excellent thermal stability and flame retardance and good mechanical properties.

Disclosed is a method that is for producing 1-bromo-1-[3,5-bis(trifluoromethyl)phenyl] ethane having high optical purity, and that is a method containing a step for brominating optically active 1-[3,5-bis(trifluoromethyl)phenyl] ethanol using, as a brominating agent, either a) the combination of a phosphorus halide and hydrogen bromide, b) the combination of 1,2-dibromo-1,1,2,2-tetrachloroethane and the organophosphorus compound represented by general formula I, which is P(R1)(R2)(R3) (in the formula: R1, R2 and R3 each independently indicate a C6-10 aryl group, a C6-10 aryloxy group, a C1-10 alkyl group, a C1-10 alkoxyl group, a C3-6 cycloalkyl group, or a C3-6 cycloalkoxyl group), or c) the combination of N-bromosuccinimide and a dialkyl sulphide.

The invention relates to a synthesis method of etretinate ether. The synthesis method adopts (1-(5, 6, 7, 8-tetrahydrophthalic-5, 5, 8, 8-tetramethyl-2-naphthyl)-ethyl)-terphenyl phosphorus halide (II) and p-eormylbenzoic acid ester (III) as raw materials, carries out two-phase reaction under the condition of adding aqueous alkali into an organic solvent, and then obtains the etretinate ether. The method has mild reaction condition, short reaction time, simple and convenient operation, low cost and high yield.

The invention relates to an MOP flame retardant, a flame-retardant UV / moisture dually-cured conformal coating, and a preparation method and application of the flame-retardant UV / moisture dually-curedconformal coating. The MOP flame retardant is obtained through the end-capping reaction of non-halogenated phosphorus polyol and isocyanate acrylate. The MOP flame retardant provided by the inventionis excellent in flame retardant effect and can be used in a UV / moisture cured system; the flame-retardant UV / moisture dually-cured conformal coating provided by the invention has excellent flame retardancy, can be cured by UV and moisture, and has no influence on other properties. Besides, the monomer with a special function is added into the flame-retardant UV / moisture dually-cured conformal coating, so that the viscosity of the conformal coating can be stabilized during long-time placement, the stability of the conformal coating is improved, and the conformal coating does not foam when beingcured.

The invention relates to a preparation method of tris(2-furyl) phosphine, which comprises the following steps of: in the atmosphere of inert gas, at the room temperature, dripping a butyl lithium solution in a normal hexane solution containing furan and tetramethylethylenediamine, raising the temperature to 40-60 DEG C, and keeping for 0.5-3 hours to produce a furyl lithium reagent; dripping phosphorus halide in the normal hexane solution at the temperature of minus 10 to 0 DEG C, carrying out heat insulation for 0.5-2 hours, naturally raising the temperature to the room temperature, and stirring for 1-8 hours; and pouring a reaction solution into a saturated strong acidic-weak basic inorganic salt solution, concentrating an organic phase to obtain a crude product, and then recrystallizing with of petroleum ether to obtain tris(2-furyl) phosphine. With the adoption of the preparation method, the preparation cost is greatly lowered, the yield is greatly increased, and the product purity is high. In the embodiment of the invention, anhydrous cerium trichloride is added into produced furyl lithium to obtain an organic cerium reagent, and the organic cerium reagent is further reacted with phosphorus trihalide, so the yield can be further increased, and the by-products can be reduced.

A process for preparing a 3-cephem compound represented by the formula (3), the process comprising the steps of reacting a beta -lactam compound represented by the formula (1) with a phosphorus halide compound in the presence of an organic base to give an imino- beta -lactam compound represented by the formula (2), adding a phenol to the same reaction system to cause decomposition due to reaction with an alcohol and simultaneously to remove the protection of carboxylic acid ester, giving a 3-cephem compound represented by the formula (3) or a salt thereof <CHEM> <CHEM> wherein R1, R2 R3 and X are as defined above.

The catalytic reforming method for hydrocarbons includes reformation of hydrocarbon material in the presence of reforming catalyst, and adding phosphorus halide in 0.1-50 ppm of hydrocarbon material into the hydrocarbon material during reformation. The method can reduce carbon deposition on reforming catalyst effectively and prolong the service life of catalyst.

The invention discloses a preparation method of vitamin K1 with different cis-trans isomer proportions and an intermediate halogenated phytol thereof. The method comprises the following steps: carrying out a halogenation reaction on a raw material phytol and phosphorus trihalide under the catalysis of phosphoric acid to obtain halogenated phytol, reacting the halogenated phytol with cyclopentadienyl menadione, and carrying out high-temperature depolymerization to obtain the vitamin K1. The addition amount of phosphoric acid in the halogenation reaction can be controlled, so that the proportionof the obtained vitamin K1 cis-isomer can be regulated between 1% and 21%.

In a method for making bisphosphonates by reacting a carbonyl compound with a phosphorus halide, the reaction is carried out in a solvent / carrier system which is a mixture of an amine hydrochloride, phosphorous acid and optionally phosphoric acid.

The invention discloses a method for compounding organphosphorus by using black phosphorus. The method takes the black phosphorus as a reaction raw material, safely and efficiently compounds organic phosphate, sulpho-phosphite ester, amino phosphite ester, alkylphosphine, alkylphosphine oxide and other organphosphorus with wide usages, a conventional synthsis route by using phosphorus halide and phosphate to compound the organphosphorus is avoided, the synthesis steps are simple and short, the production technology is operated simply and easily, the reproducibility is good, the reaction is simple and green, the use of a phosphorus halide reagent is avoided, the range of the synthetic organphosphorus is wider, the method satisfies the requirements of green chemical development, and the large-scale production can be achieved.

The invention belongs to a method for preparing a ceftibuten mother nucleus 7-ANCE. The method for preparing the ceftibuten mother nucleus 7-ANCE comprises the following steps: S1, reacting a compound A as shown in a formula I with halogenated phosphorus and an acid-binding agent; S2, adding an acid solution to react to generate ammonium salt; and S3, adjusting the pH value of the ammonium salt generated in the step S2 to be neutral or alkaline to obtain a crude product, and purifying to obtain the ceftibuten mother nucleus 7-ANCE, wherein the molar ratio of the compound A to the halogenated phosphorus is 1: (2.5-3.5). Compared with the prior art, the method has the beneficial effects that the reaction is carried out in the rearrangement direction by controlling the molar ratio of the compound A to the phosphorus halide, so that the hydroxyl protection step in the prior art can be omitted, the use of a methylsulfonyl chloride irritant raw material is avoided, and a product with higher purity and yield is obtained.

A process for producing a halogen-containing phosphate ester includes the steps of: (i) reacting a phosphorus halide selected from the group consisting of phosphorus oxyhalides and phosphorus pentahalides with a halogen-containing hydroxy compound to obtain a reaction mixture including a halogen-containing phosphate ester, (ii) purifying the halogen-containing phosphate ester by adding an aqueous medium selected from the group consisting of water, neutral aqueous solutions, acidic aqueous solutions and basic aqueous solutions to the reaction mixture to crystallize the halogen-containing phosphate ester, and (iii) distilling waste water from the purification step.

The invention relates to a preparation method of phospholene oxide, substituted phospholene oxide and a preparation method of the substituted phospholene oxide and belongs to the technical field of organic synthesis. The preparation method of the phospholene oxide comprises the following steps: 1) enabling phosphorus trihalide and chloroethanol to react at -10 to 40 DEG C for 0.5 to 3h so as to obtain a compound shown as a formula I; 2) enabling the compound shown as the formula I, a catalyst, a polymerization inhibitor and 1,3-butadiene to react at room temperature for 4 to 10h; then raisingthe temperature to 40 to 80 DEG C and reacting for 12 to 24h; then raising the temperature to 80 to 100 DEG C and reacting for 8 to 14h to obtain the phospholene oxide. The e preparation method of thephospholene oxide, provided by the invention, takes the phosphorus halide and the chloroethanol as raw materials, and the raw materials are easy to obtain and the price is low; reaction conditions are moderate and the method is simple and feasible and is low-cost.

The invention discloses a preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane, belonging to the field of organic synthesis. The preparation method comprises the following steps: carrying out a heating reaction on pentaerythritol and phosphorus trihalide in the presence of a catalyst, and carrying out distilling to obtain an intermediate 3,9-dihalogeno-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane; reacting the intermediate with a fluorination reagent, and carrying out cooling and filtering after the reaction; and carrying out reduced-pressure distillation to obtain the 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane. The raw materials used in the method are low in price, and the method is simple and convenient to operate and suitable forindustrial production.

A method for preparing optically active 1-bromo-1-[3,5-bis(trifluoromethyl)-phenyl]ethane having a high optical purity, which comprises the step of brominating optically active 1-[3,5-bis(trifluoromethyl)phenyl]ethanol by using, as a brominating agent, (a) a combination of a phosphorus halide and hydrogen bromide, (b) a combination of 1,2-dibromo-1,1,2,2-tetrachloroethane and an organic phosphorous compound represented by the general formula (I): P(R1)(R2)(R3) (in the formula, R1, R2, and R3 independently represent a C6-10 aryl group, a C6-10 aryloxy group, a C1-10 alkyl group, a C1-10 alkoxyl group, a C3-6 cycloalkyl group, or a C3-6 cycloalkoxy group), or (c) a combination of N-bromosuccinimide and a dialkyl sulfide.

The catalytic reforming method for hydrocarbons includes reformation of hydrocarbon material in the presence of reforming catalyst, and adding phosphorus halide in 0.1-50 ppm of hydrocarbon material into the hydrocarbon material during reformation. The method can reduce carbon deposition on reforming catalyst effectively and prolong the service life of catalyst.

The invention relates to a preparation method of tris(2-furyl) phosphine, which comprises the following steps of: in the atmosphere of inert gas, at the room temperature, dripping a butyl lithium solution in a normal hexane solution containing furan and tetramethylethylenediamine, raising the temperature to 40-60 DEG C, and keeping for 0.5-3 hours to produce a furyl lithium reagent; dripping phosphorus halide in the normal hexane solution at the temperature of minus 10 to 0 DEG C, carrying out heat insulation for 0.5-2 hours, naturally raising the temperature to the room temperature, and stirring for 1-8 hours; and pouring a reaction solution into a saturated strong acidic-weak basic inorganic salt solution, concentrating an organic phase to obtain a crude product, and then recrystallizing with of petroleum ether to obtain tris(2-furyl) phosphine. With the adoption of the preparation method, the preparation cost is greatly lowered, the yield is greatly increased, and the product purity is high. In the embodiment of the invention, anhydrous cerium trichloride is added into produced furyl lithium to obtain an organic cerium reagent, and the organic cerium reagent is further reacted with phosphorus trihalide, so the yield can be further increased, and the by-products can be reduced.

The invention relates to a synthesis method of etretinate ether. The synthesis method adopts (1-(5, 6, 7, 8-tetrahydrophthalic-5, 5, 8, 8-tetramethyl-2-naphthyl)-ethyl)-terphenyl phosphorus halide (II) and p-eormylbenzoic acid ester (III) as raw materials, carries out two-phase reaction under the condition of adding aqueous alkali into an organic solvent, and then obtains the etretinate ether. The method has mild reaction condition, short reaction time, simple and convenient operation, low cost and high yield.

The invention discloses a preparation method of 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. According to the preparation method, triphenyl phosphine is taken as the raw material, triphenyl phosphine reacts with metal sodium and phosphorus halide to generate reaction product (I), the reaction product (I) reacts with acyl chloride to generate reaction product (II), and the reaction product (II) is oxidized to produce 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. The preparation method has the advantages of easily-available raw materials, low cost, easy operation, environment-friendliness, and easiness for industrialization.