13 results about "Phosphoric chloride" patented technology

Provided is a method for producing an anhydrous cyclic phosphonic acid by reacting phosphonic acid (A) with a basic compound (B) and at least one type of halogenating agent (C) selected from thionyl chloride, phosphoryl chloride, and oxalyl chloride. Also provided is a method for producing a phosphonic acid monoester by reacting the anhydrous cyclic phosphonic acid obtained by said production method with an alcohol.

The invention discloses a synthesis process of chiral UNA phosphoramidite, phosphoryl chloride and phosphoramidite and application of the chiral UNA phosphoramidite, phosphoryl chloride and phosphoramidite in oligonucleotides, and particularly designs preparation and synthesis of (2S)-UNA monomer phosphoramidite, phosphoryl chloride and phosphoramidite. And the method can also be used for solid-phase synthesized oligonucleotides in the conventional 3-to-5 direction, and the influence of introduction of monomers with different chirality to design sites on the structure, the biological activity and the like is researched.

The invention provides a rigid photocurable flame-retardant compound as well as a preparation method and application thereof. The rigid photocurable flame-retardant compound is synthesized by taking pentaerythritol, phosphorus oxychloride and hydroxyethyl acrylate as raw materials through two steps of nucleophilic substitution reaction: firstly, enabling the pentaerythritol to react with the phosphorus oxychloride, and then enabling a phosphoryl chloride intermediate to further react with the hydroxyethyl acrylate. The method is simple in process and environment-friendly. The obtained light-cured resin monomer has a rigid spiro structure, a phosphate group and a polymerizable double bond, and has a rapid light-curing characteristic and an excellent flame retardant property. The cured material is high in hardness, excellent in flame retardant property, high in thermal stability, excellent in mechanical property and wide in application prospect. The monomer not only can be independently used as flame-retardant light-cured resin, but also can be applied to various flame-retardant light-cured formulas as a reactive flame retardant.

This invention relates to the field of flame retardant preparation technology, and more particularly to a method for preparing an environmentally friendly and highly efficient flame-retardant polyolefin cable sheath material. The invention uses compounds containing primary amino and amide bonds and compounds containing phenyl and phosphoryl chloride groups as raw materials. The reaction is carried out at room temperature for 0.5-1 h, then heated to 45 °C for 3-4 h, and then to 65 °C for 5-6 h. Through a condensation reaction, a phosphoramide macromolecular flame retardant containing phenyl and amide bonds is obtained, with a yield as high as 80.5-95.6%. This flame retardant is added to polyolefin cable sheath material at a mass ratio of 25%, then compounded and extruded to obtain a halogen-free flame-retardant polyolefin cable sheath material. The flame retardant molecule prepared by this invention simultaneously contains phosphorus and nitrogen flame-retardant elements and amide bonds forming a char skeleton. During combustion, it can exert a phosphorus-nitrogen synergistic flame-retardant effect and promote the catalytic char formation of the matrix, which can significantly reduce the heat and toxic gas release of polyolefin cable sheath material during combustion, thereby providing protection for the lives of people in fire scenes.

The invention provides a phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand which is prepared by the following steps: in an inert gas atmosphere, mixing a compound benzoxazole with anhydrous tetrahydrofuran, cooling to-95 to-65 DEG C, adding an n-butyllithium solution dissolved in an organic solvent, stirring at-95 to-65 DEG C for 0.5-4 hours, adding diphenylphosphoryl chloride, stirring at room temperature for 8-10 hours, filtering, washing, and drying to obtain the phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand. Carrying out post-treatment on the obtained reaction liquid to obtain a phenyl phosphonic acid bis (o-isocyano phenol) ester ligand; compared with the most common organic dye photosensitizer, the copper-based photosensitizer prepared from the phenyl phosphonic acid bis (o-isocyano-phenol) ester ligand overcomes the defect that the catalytic activity of the organic dye photosensitizer is rapidly reduced under long-term illumination, and in addition, the organic dye photosensitizer is easy to generate an aggregation-induced quenching effect; the photosensitizer disclosed by the invention does not generate an aggregation-induced quenching effect; compared with an iridium complex photosensitizer which is commonly used at present, the cuprous photosensitizer provided by the invention is more environment-friendly.

This invention provides a method for producing 2-chloro-5,6-diphenylpyrazine in high yield. [Solution] In one aspect, a method for producing 2-chloro-5,6-diphenylpyrazine is provided. This method includes contacting 2-hydroxy-5,6-diphenylpyrazine and phosphoryl chloride at a temperature of 70°C or higher and less than 120°C to obtain a first mixture. The first mixture contains 2-chloro-5,6-diphenylpyrazine. The contact temperature is preferably 80°C or higher and 100°C or lower.

A method for preparing and using an organic matter extractant in wastewater, comprising: 1) reacting hypoxanthine I with phosphorus oxychloride to obtain a chloro product II, then condensing the chloro product II with 5-(2-acetyloxyethyl)tetrahydrofuran-2,3,4-triyl triacetate to obtain compound III, and then subjecting the compound III to ammonolysis to obtain compound IV; 2) adding glycerol distearate and phosphorus oxychloride to a mixed solution of tetrahydrofuran and triethylamine to react to generate a phosphoryl chloride intermediate V; 3) hydrolyzing and acidifying the compound IV and the intermediate V in a mixed solution of tetrahydrofuran and triethylamine to obtain an extractant adenosine phosphate glycerol distearate VI; and 4) mechanically mixing the extractant adenosine phosphate glycerol distearate VI and aviation kerosene to obtain an organic matter extractant product in wastewater. The organic matter extractant in wastewater of the present application mainly uses adenosine phosphate ester compounds and related derivatives as a main extractant, extracts and separates various organic matters in wastewater, has a high removal rate of organic matters, and has a high recovery rate of the extractant.

The invention belongs to the technical field of flame retardants, and particularly relates to a preparation method of a high-strength water-resistant halogen-free flame retardant, the prepared halogen-free flame retardant and application of the high-strength water-resistant halogen-free flame retardant. Phosphorus oxychloride and hydroquinone react to introduce phosphorus into reactants to obtain hydroquinone phosphoryl chloride; the preparation method comprises the following steps: reacting 2, 6, 7-trioxa-1-phosphoric acid bicyclo [2.2. 2] octane-4-yl methanol with a hydroxyl group of pentaerythritol, and introducing a bicyclic cage into a reactant by reacting halogen of phosphorus oxychloride with the hydroxyl group of pentaerythritol to obtain 2, 6, 7-trioxa-1-phosphoric acid bicyclo [2.2. 2] octane-4-yl methanol; finally, the halogen group of hydroquinone phosphoryl chloride and the hydroxyl group of 2, 6, 7-trioxa-1-phosphoric acid bicyclo [2.2. 2] octane-4-yl methanol are subjected to nucleophilic substitution, and redundant halogen and the amino group of 4, 4 '-diaminodiphenylmethane and 1, 6-hexamethylenediamine are subjected to an amination reaction to generate the high-strength water-resistant halogen-free flame retardant with a cross-linked structure, so that the stability and consistency of the material are improved, and the flame retardant property is improved. The flame retardant shows excellent mechanical strength, so that the flame retardant has longer service life in a severe environment.

The present invention provides a mepivacaine preparation method, which comprises that in an organic solvent, 1-methylpiperidine-2-formic acid and 2, 6-dimethylaniline are subjected to a condensation reaction in the presence of a condensing agent to obtain mepivacaine, and the condensing agent is selected from one or more of phosphorus oxychloride, phosphorus trichloride and phosphorus pentachloride. The condensing agent used for preparing mepivacaine is one or more of phosphorus oxychloride, phosphorus trichloride and phosphorus pentachloride, toxic substances such as phosgene and the like are not generated, the safety is high, the cost is low, and the preparation method is suitable for industrial popularization.

The invention discloses a triazinyl phosphorus and silicon-containing reactive intumescent flame retardant as well as a preparation method and application thereof, and the flame retardant is prepared by taking melamine, a phosphoryl chloride-containing reagent, a chlorosilane-containing reagent, phosphorus oxychloride and organic polyamine as raw materials through multi-step substitution reaction. A triazine ring, multi-oxidation-state phosphorus and an active silicon group are creatively integrated into a single molecule. The design breaks through the bottlenecks that a traditional blended flame retardant is easy to migrate, poor in synergism and capable of damaging the mechanical property of a matrix, and synergistic improvement of flame retardance and performance is achieved. Meanwhile, through a flexible molecular mechanism of the flame retardant, the material is endowed with excellent flame retardance (such as high LOI and UL-94 V-0), and meanwhile, good mechanical strength and toughness are kept. The flame retardant is simple in synthesis process, easy in product purification, high in yield and easy for industrial production.

A method of making a flame retardant, and phosphorylated bio-based flame retardants, are provided. The method includes reacting a bio-based-derived starting compound with a phosphate-containing compound or o-phosphoric acid to obtain a phosphorylated bio-based material. The phosphate-containing compound may be diphenyl phosphoryl chloride. The obtained phosphorylated bio-based material may be phosphorylated cardanol, vanillin diphenyl phosphate, vanillyl alcohol diphenyl phosphate, methyl gallate triphenyl phosphate, bis(dihydrogenphosphate) of vanillyl alcohol diglicidyl ether, or bis(dihydrogenphosphate) of bisphenol A diglicidyl ether. An article including the phosphorylated bio-based flame retardant is also provided. The article may be a building material, a textile, a plastic, a foam, an adhesive, packaging, and an electrical housing.

The invention discloses a waterproof flame-retardant polylactic acid material and a preparation method thereof, and relates to the technical field of material preparation, anhydrous toluene, alkali lignin, tributyl borate, diphenoxy phosphoryl chloride, aminopropyltriethoxysilane and triethylamine are mixed, and a waterproof flame-retardant modifier is prepared through an in-situ grafting reaction; polylactic acid is dissolved in a spinning solvent, then a waterproof flame-retardant modifier is added, and an outer-layer spinning solution, a middle-layer spinning solution and an inner-layer spinning solution are prepared; the concentration of the polylactic acid is gradually reduced, and the concentration of the waterproof flame-retardant modifier is gradually reduced; respectively injecting the outer-layer spinning solution, the middle-layer spinning solution and the inner-layer spinning solution into an outer-layer channel, a middle-layer channel and an inner-layer channel of a coaxial nested three-channel spinning nozzle, and carrying out electrostatic spinning to obtain the film-shaped waterproof flame-retardant polylactic acid material. Through in-situ grafting synthesis of the waterproof flame-retardant modifier, gradient spinning solution design and coaxial three-channel electrostatic spinning forming, the technical problems that a pure polylactic acid material is high in water absorption rate, poor in flame retardance and insufficient in mechanical toughness are effectively solved.

The present invention relates to one pot process for preparation of salts of bis[2- (perfluorohexyl)ethyl]phosphate or its solution comprising, reacting perfluorohexyl ethyl alcohol with phosphoryl chloride in the presence of organic base in first solvent to obtain bis[2-(perfluorohexyl)ethyl]phosphorochloridate, which is hydrolyzed with water to give bis[2-(perfluorohexyl)ethyl] hydrogenphosphate, further the reaction mass is treated with base in second solvent to obtain desired product with high yield, which is not only cost-effective but also industrially scalable.