23 results about "Phosphoryl chloride" patented technology

The invention belongs to the technical field of epoxy resin flame retardance, and particularly relates to a phosphorus-nitrogen flame-retardant curing agent, preparation thereof and application of the phosphorus-nitrogen flame-retardant curing agent in epoxy resin. In order to prepare the flame-retardant curing agent with both flame retardance and curing, pentaerythritol and phosphorus oxychloride are subjected to a reaction to synthesize an intermediate pentaerythritol diphosphate diphosphoryl chloride; and reacting the intermediate with 4, 4-diaminodiphenylmethane to synthesize the phosphorus-nitrogen flame-retardant curing agent 4, 4-diaminodiphenylmethane pentaerythritol diphosphate. The phosphorus-nitrogen flame-retardant curing agent has good smoke suppression performance, can reduce the combustion rate, is low in cost and environment-friendly, and is mixed with epoxy resin for curing to obtain an epoxy resin composite material with a flame-retardant function, so that the flame-retardant performance of the epoxy resin composite material can be improved, and the fire risk can be reduced.

The invention provides a synthetic method of a novel flame retardant with a phosphaphenanthrene-chloropropyl synergistic structure. The preparation method comprises the following steps: synthesizing bis (1-chloro-2-propyl) phosphoryl chloride from phosphorus oxychloride and epoxypropane in a molar ratio of 1: 2 in a low-temperature condition through a micro-channel reactor, reacting with DOPO-HQ (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-yl-1, 4-benzenediol), adding a specific solvent and a catalyst, reacting to generate a crude product, filtering, washing, carrying out reduced pressure distillation, and recrystallizing to obtain the 2-(1-chloro-2-propyl) phosphoryl chloride, namely the 2-(1-chloro-2-propyl) phosphoryl chloride-DOPO-HQ (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-yl-1, 4-benzenediol). The novel flame retardant with the phosphaphenanthrene-chloropropyl synergistic structure is obtained. A phosphaphenanthrene-chloropropyl synergistic structure is designed, so that the molecular weight and the phosphorus content are improved, and the gas-phase flame-retardant and condensed carbon-forming synergistic flame-retardant effect is improved; the thermal stability and the molecular weight are improved through a molecular bridge chain (hydroquinone), and migration is inhibited. The flame retardant has excellent flame retardant property.

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 present application relates to the technical field of organic synthesis, and particularly relates to a preparation method of beta-nicotinamide mononucleotide. The present application provides a preparation method of beta-nicotinamide mononucleotide, comprising the following steps: mixing a salt corresponding to nicotinamide riboside, phosphorus oxychloride and a polar aprotic organic solvent, performing a phosphorylation reaction, and obtaining beta-nicotinamide mononucleotide. The present application takes nicotinamide riboside as a raw material, takes phosphorus oxychloride as a phosphorylation reagent, and is prepared through a phosphorylation reaction. Compared with a conventional method, the reaction has less by-products and is simple to operate. The subsequent high-purity and high-yield end product can be obtained through simple post-treatment. Meanwhile, the present application is also beneficial to industrial production.

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.

The application discloses a kind of preparation methods of flame-retardant aging-resistant high-transparency polyurethane, the polyurethane is first with 2-amino-1,3-propanediol, 2-chloro-4,6-diphenyl-1,3,5-triazine, diphenyl phosphorochloridate and triphenylchlorosilane composite preparation DADT, then DADT is mixed with polyether polyol, isocyanate to obtain;The preparation method of the application is simple, the process is easy to control, the obtained polyurethane material limit oxygen index reaches 29.6%, meets commercial flame-retardant standard and reaches UL-94 V-0 flame-retardant grade;Material has excellent aging resistance, heat-oxygen tensile strength retention rate is 88.5%, heat-oxygen breaking elongation retention rate is 77.4%, and ultraviolet breaking elongation retention rate is 71.4%, can be applied to automobile ultraviolet protection diaphragm, flame-retardant filled foam, fire guide sign protection film and the like scene.

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.

The invention provides a halogen-free phosphorus flame retardant as well as a preparation method and application thereof, and belongs to the technical field of flame retardants. The preparation method comprises the following steps: mixing a hydroxyl-containing compound, an acid-binding agent and an organic solvent to obtain a mixed solution; dropwise adding pyrophosphoryl chloride into the mixed solution, and reacting to obtain a reaction product; and carrying out post-treatment on the reaction product to obtain the halogen-free phosphorus flame retardant. The hydroxyl-containing compound comprises one or more of epoxy butanol, glycidol, syringaldehyde, vanillin and p-hydroxybenzaldehyde. The halogen-free phosphorus-based flame retardant disclosed by the invention is a flame retardant with a new structure and has an epoxy group capable of participating in a co-curing reaction of epoxy resin; the preparation method of the flame retardant is simple, the flame retardant is prepared from hydroxyl-containing compounds such as glycidol and pyrophosphoryl chloride under the action of an organic solvent and an acid-binding agent through a one-step synthesis method, and a target object can be conveniently and rapidly prepared.

The present application relates to fine chemical technology field, especially to a kind of anti-micro pitting additive and its preparation and application.The present application uses starch masking method, uses hydroxylated boron nitride and O, O-dialkyl thiophosphoryl chloride to carry out chemical reaction to prepare this anti-micro pitting additive, and the core skeleton is hexagonal boron nitride nanosheet, one side contains hydroxyl functional group, the other side is covalently connected O, O-dialkyl thiophosphate, and the process condition used is mild;The anti-micro pitting additive prepared by the present application can be used as multifunctional lubricant additive, utilizes the filling and interlayer slip of boron nitride nanosheet, the chemical adsorption of hydroxyl surface and friction pair, the tribological chemical reaction of O, O-dialkyl thiophosphate and friction pair synergistic effect, obtains good extreme pressure, antiwear, anti-micro pitting and anticorrosion etc., suitable for long-acting stable friction and micro pitting lubrication protection under harsh working conditions.

The invention provides a lignin-based reactive flame retardant, a preparation method and application of the lignin-based reactive flame retardant in flame-retardant styrene resin, and belongs to the technical field of flame-retardant polystyrene. The preparation method comprises the following steps: firstly, by taking renewable resources as raw materials, quantitatively converting a lignin phenolic compound into a lignin vinyl phenol monomer through decarboxylation, then carrying out phosphorylation reaction on the lignin vinyl phenol monomer and a phosphoryl chloride monomer to synthesize a lignin-based reactive flame retardant containing a vinyl benzene structure, and applying the lignin-based reactive flame retardant to preparation of lignin-based intrinsic flame-retardant styrene resin. The flame retardant has excellent biocompatibility, stable flame-retardant effect and environmental friendliness, the flame-retardant mechanism of the flame retardant is derived from phosphate groups introduced into molecules, and the dual flame-retardant mechanism is realized in a condensed phase and a gas phase; the flame retardant has modular characteristics, can be used for flexible design and structural regulation of flame-retardant molecules, and has reliable application value in the field of flame-retardant modified styrene materials; the problem of base performance degradation caused by a traditional flame retardant can be effectively avoided under the condition that the basic performance of the material is kept.

The application relates to a high-flame-retardant electronic connecting wire and a preparation method thereof, and belongs to the technical field of high polymer materials. The electronic connecting wire is composed of a wire and a surface flame-retardant protective layer, wherein the components of the flame-retardant protective layer are as follows: modified phosphorus-silicon flame retardant 7.5-10 wt%, plasticizer 14-18 wt%, heat stabilizer 1.7-2.2 wt%, antioxidant 0.12-0.16 wt% and lubricant 0.9-1.3 wt%, and the rest is PVC resin; the modified phosphorus-silicon flame retardant is synthesized by synthesizing a phosphorus oxychloride intermediate 1 with a double spiro ring structure from pentaerythritol and phosphorus oxychloride, carrying out amine-ester exchange between terminal amino polydimethylsiloxane and ketone-based diethyl malonate to prepare an intermediate 2 containing terminal amino groups, and then reacting the intermediate 2 with active phosphorus oxychloride of the intermediate 1 to form a chain-shaped macromolecular phosphorus amide compound, so that in-situ toughening, migration inhibition and carbon net flame retardation are simultaneously realized in the PVC matrix.

The invention discloses a preparation method of flame-retardant anti-aging high-transparency polyurethane, which comprises the following steps: firstly, compounding 2-amino-1, 3-propylene glycol, 2-chloro-4, 6-diphenyl-1, 3, 5-triazine, diphenyl hypophosphorous chloride and triphenylchlorosilane to prepare DADT (diphenyldisiloxane), and then mixing the DADT with polyether polyol and isocyanate to prepare the flame-retardant anti-aging high-transparency polyurethane. The preparation method is simple, the process is easy to control, the limit oxygen index of the obtained polyurethane material reaches 29.6%, the commercial flame retardant standard is met, and the UL-94 V-0 flame retardant grade is reached; the material has excellent aging resistance, the thermo-oxidative tensile strength retention rate is 88.5%, the thermo-oxidative elongation at break retention rate is 77.4%, the anti-ultraviolet elongation at break retention rate is 71.4%, and the material can be applied to scenes such as automobile anti-ultraviolet diaphragms, flame-retardant filling foam and fire-fighting guide sign protective films.

This invention provides a method for preparing melamine pyrophosphate and its application, belonging to the field of flame retardant technology. The invention uses pyrophosphoryl chloride and melamine as raw materials, reacting them in an alcohol-water mixed solvent. After the reaction, the mixture is neutralized with alkali, and post-processed to obtain melamine pyrophosphate. This invention uses pyrophosphoryl chloride as the phosphorus source, solving the problems of insufficient reaction due to the high viscosity of raw materials in the traditional pyrophosphate method and the hygroscopic and difficult-to-store raw materials in the phosphorus pentoxide method. The reaction process does not require strong acid catalysis; the byproduct hydrogen chloride is converted to ammonium chloride after neutralization with ammonia water, avoiding the generation of high-salt wastewater, making the process environmentally friendly. The method of this invention features mild reaction conditions, simple operation, high product purity, and good thermal stability. The obtained melamine pyrophosphate has a purity ≥95% and a 5% thermal decomposition temperature ≥300℃, making it suitable as a halogen-free flame retardant for widespread application in epoxy resins, polyolefins, nylon, coatings, rubber, and other fields.

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 high-weather-resistance wide-temperature-range bottom filling adhesive for semiconductor packaging and a preparation method thereof, and relates to the technical field of filling adhesives for semiconductor packaging, and the preparation method comprises the following steps: synthesizing glycidyl sulfonate by taking bio-based glycidyl and sulfonyl chloride as raw materials, and synthesizing halogen-free DGEBA resin by taking bisphenol and glycidyl sulfonate as raw materials; the preparation method comprises the following steps: synthesizing phosphorylated modified resin by taking halogen-free DGEBA resin and phosphoryl chloride as raw materials; the preparation method comprises the following steps: uniformly stirring and melting halogen-free DGEBA resin and phosphorylated modified resin, adding a cross-linking agent, and uniformly stirring to obtain a resin matrix; the preparation method comprises the following steps: sequentially adding the siloxane latent accelerator and the composite filler into the resin matrix, stirring in vacuum, defoaming, adding the initiator, uniformly stirring, injecting into a mold, heating, curing, and cooling to room temperature to obtain the filling adhesive for semiconductor packaging, the composite filler is prepared from KH550 modified FeNi alloy particles.

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.

The invention relates to a method for producing phosphorus-chlorine compounds, characterized in that i. A material containing phosphorus oxides is reacted in the presence of tetrachloroethylene at a temperature of 500 DEG C to 1000 DEG C, and ii. The formed phosphorus-chlorine compounds, in particular phosphoryl chloride, are withdrawn and separated from an exhaust gas stream.

The application provides a chiral morpholino phosphorus oxychloride monomer and a preparation method and application thereof, and the structure of the monomer is shown in formula I or II: wherein X represents an oxygen atom or a sulfur atom; B represents a base; R 1 is selected from an optionally substituted secondary substituted amine group, an optionally substituted alkoxy group, an optionally substituted phenoxy group, a guanidino group, and a linked nitrogen forming an optionally substituted heterocyclic ring; R 2 is selected from an optionally substituted or unsubstituted tertiary alkyl group, an optionally substituted or unsubstituted benzyl group, an optionally substituted sulfonyl group, and an optionally substituted acyl group. The application can obtain the chiral morpholino phosphorus oxychloride monomer in a stereochemically pure or substantially pure form by using an efficient catalytic asymmetric desymmetrization strategy. And the corresponding morpholino oligonucleotide chain can be synthesized based on the monomer, thereby providing a powerful synthesis platform for developing a new generation of morpholino oligonucleotide drugs with precise stereostructure and optimized performance.

The application discloses a spirocyclic phosphate ester and a preparation method and application thereof. The structural formula of the spirocyclic phosphate ester is shown in the application. The preparation method of the spirocyclic phosphate ester comprises the following steps: 1) reacting furfurylamine and vanillin to obtain a Schiff base intermediate; 2) reacting the Schiff base intermediate and pentaerythritol bisphosphate dichloride to obtain a flame retardant precursor; and 3) reacting the flame retardant precursor and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to obtain the spirocyclic phosphate ester. The spirocyclic phosphate ester is used as an epoxy resin flame retardant and has the advantages of excellent flame retardant performance, good smoke suppression effect, good thermal stability, good compatibility with the epoxy resin, green environmental protection and the like. Moreover, the preparation method is simple, raw materials are widely sourced, production cost is low, and the spirocyclic phosphate ester is suitable for large-scale industrial production and application.