77 results about "Phosphorous trichloride" patented technology

The invention relates to a process for preparing phosphorous acid by hydrolyzing phosphorus trichloride, and in particular relates to a process for preparing phosphorous acid by hydrolyzing phosphorus trichloride under a mild reaction condition. According to the process, phosphorus trichloride and a hydrogen chloride solution are subjected to hydrolysis reaction in sequence in at least four stages of cascade reaction vessels under the condition that the temperature is 65-85 DEG C and the pressure is not more than 0.1Mpa to generate a phosphorous acid solution and gaseous hydrogen chloride. In the process, the phosphorus trichloride reacts with the water in a hydrochloric acid solution, the phosphorus trichloride is subjected to an exothermic reaction, the temperature of the process can reduce the hydrolysis rate to ensure that the reaction is performed mildly, and at least four stages of cascade bubbling reactions are adopted by the process, so that the utilization ratio of raw materials is improved, the phosphorus trichloride in the reaction vessel of the previous stage can enter the reaction vessel of the next stage, the content of the phosphorus trichloride in the reaction vessel of the previous stage is reduced in other ways, the intensity of the reaction is reduced again, the production safety is improved, and the service life of equipment is prolonged.

The invention belongs to the field of chemical industries, and in particular relates to a preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride. The preparation process comprises the specific steps of: adding hydrochloric acid into a hydrolysis reaction kettle, dripping phosphorous trichloride into the hydrolysis reaction kettle, pumping a phosphorous acid mixture synthesized by hydrolysis reaction into a distillation and deacidification kettle with a stirrer through a pump to perform negative-pressure distillation concentration, cooling and crystallizing a concentration solution to prepare a crystallized phosphorous acid product; and absorbing an HCL gas generated through reaction through a protective trough and a hydrochloric film type absorbing system in sequence to obtain hydrochloric acid. According to the preparation process disclosed by the invention, a bubble absorbing trough (the protective trough) is additionally provided before a hydrolysis reaction film reducing hydrochloric acid absorbing system so that the HCL gas generated through reaction is more rapidly discharged, and thus the effects on the dripping quantity and the speed of the phosphorous trichloride in the hydrolysis reaction are greatly reduced. The mechanical stirrer is used in the distillation and deacidification kettle so as to implement the mechanical transmission stir, carry out the reduced-pressure distillation, enhance the heat transfer, improve the heat transfer efficiency and accelerate the deacidification speed, and thus the deacidification time is shortened and the capacity is increased.

A methylene phosphocarboxylic acid as water quality stabilizer is prepared from carboxy-contained amine, PCl3 (or phosphonous acid and concentrated hydrochloric acid) and water through heating and adding solution of formaldehyde. It has high output rate.

The esterfication of hypophosphorous acid is followed by reaction with another molecule of alcohol under the action of a nickel catalyst to provide a green method for the preparation of H-phosphonate diesters. This method avoids the need for any stoichiometric chlorine unlike those based on phosphorous trichloride.

This invention discloses a method for preparing N-phosphonomethyl iminodiacetic acid (PMIDA) by iminodiacetonitrile hydrolysis. The method comprises: (1) hydrolyzing iminodiacetonitrile (greater than or equal to 95 wt.%) in an alkali solution under stirring at 20-100 deg.C and -(0.01-0.04) MPa to obtain iminodiacetate solution; (2) dropping phosphorous trichloride (1.0-1.5 mol times of iminodiacetonitrile) to the iminodiacetate solution at 20-100 deg.C and -(0.01-0.04) MPa with an acidic catalyst added before or after the phosphorous trichloride addition; (3) adding formaldehyde at a temperature not lower than 80 deg.C; (4) reacting at 100-120 deg.C for 1-7 h to obtain PMIDA suspension; (5) vacuum-distilling to recover formaldehyde; (6) crystallizing, separating, washing and drying to obtain PMIDA with a purity higher than 98%. The method has such advantages as simple process, low cost and high yield.

The invention discloses a method for producing technical-grade fosetyl-aluminum, comprising the steps of continuously mixing phosphorus trichloride and ethanol and esterifying to generate a phosphite ester liquid; continuously saponifying the phosphite ester liquid and inorganic alkali to generate an ammonium phosphite liquid; carrying out continuous double-decomposition on the ammonium phosphate liquid and water-soluble aluminum salt to generate fosetyl-aluminum slurry; precipitating the fosetyl-aluminum slurry, continuously separating and drying to obtain a product with fosetyl-aluminum content of 98% and total yield of 95% (based on phosphorus trichloride). The method has the advantages of simple process, easiness in implementation, high reaction speed, less side reaction, friendly field environment and notable economic benefit.

The present invention relates to fluoric derivative of alpha-aminoalkyl phosphonate compound and its synthesis. Through active group splicing method, fluorine atom is introduced into alpha-aminoalkylphosphonate to synthesize serial fluoric alpha-aminoalkyl phosphate compounds. The synthesis features that substituted aniline, substituted banzaldehyde, anhydrous alcohol and phosphorus trichloride as materials in synthesized through a three-step process into fluoric alpha-aminoalkyl phosphonate compounds in solvent of toluene, benzene, ethanol, methanol, etc. The said derivatives have improved physical and chemical performance, increased liposolubility in organism, membrane permeability, etc.

The invention relates to a preparation method of a phosphonium salt, in particular relates to improvement of a preparation process of a phosphonium salt. The preparation method is characterized by comprising the following steps: carrying out a reaction on an alkane Grignard reagent and phosphorous trichloride so as to generate trialkyl phosphine; directly adding alkyl halide in the reaction in the former step without hydrolysis and separation so as to synthesize the phosphonium salt; and finally, separating and purifying by utilizing a principle that the phosphonium salt can be transferred in an organic phase and a water phase under a certain condition. Compared with the existing technology that the phosphonium salt is synthesized by a Grignard method, the hydrolysis step after trialkyl phosphine is synthesized is omitted in the preparation method provided by the invention, thereby simplifying the synthesis process, saving labor power and material resources and avoiding the side reaction and loss which are possibly brought by a middle operation so that the yield is improved; and the final yield is up to about 80%.

A process for the preparation of biphosphonic acids and pharmaceutical acceptable salts thereof, comprises reacting a carboxylic acid with phosphorous trichloride and phosphorous acid in the presence of an aprotic polar solvent.

The invention discloses an ionic phosphoramidite ligand, a preparation method and application of the ionic phosphoramidite ligand in hydroformylation reaction. A general formula of the ligand is shownin the specification. The preparation method comprises the following steps: dissolving phosphorus trichloride and imidazole in a solvent, conducting stirring for reaction, conducting filtering, dissolving substituted biphenol in a solvent, dropwisely adding the formed solution into the filtrate for reaction, and purifying the obtained product to obtain phosphoramidite; and reacting phosphoramidite with a quaternization reagent in a solvent to obtain a product, and purifying the product to obtain the ionic phosphoramidite. Through the method provided by the invention, a series of neutral phosphoramidite ligands can be conveniently synthesized, and a series of ionic phosphoramidite ligands with different physicochemical properties can be efficiently synthesized through a quaternization method.