66 results about "Phenyl dichlorophosphate" patented technology

The invention discloses a DOPO-based flame retardant, and a preparation method thereof. According to the preparation method, 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide and paraformaldehyde are taken as raw materials, and a precursor I is synthesized via substitution reaction; active hydroxide radicals of the precursor I, phenyl dichlorophosphate, and hydroxyethyl acrylate are subjected to substitution/esterification reaction so as to prepare a flame retardant which is high in phosphorus content and possesses active double bonds; and the flame retardant is added into an unsaturated polyester resin matrix so as to obtain a flame-retardant unsaturated polyester resin composite material. According to the DOPO-based flame retardant, flame resistance of the unsaturated polyester resin matrix is improved via a gas phase and a condensed phase, problems of conventional additive flame retardants that compatibility with polymer matrix is poor, migration is easily caused, and flame retardant efficiency is low are solved. When the DOPO-based flame retardant is applied to inflaming retarding of unsaturated polyester resin, material vertical flame rating is capable of reaching V-0 grade at a relatively low adding amount, and flame resistance is excellent. The DOPO-based flame retardant is high in purity and yield, and aftertreatment is simple.

Preparation method and application of a phenyl phosphate flame retardant containing DOPO. The method is as below: under the action of methanol, reacting 4-amino phenol, 2-hydroxy benzaldehyde, DOPO and formaldehyde in one pot to synthesize an intermediate I; reacting phenyl dichlorophosphate and resorcinol to synthesize an intermediate II (resorcinol bisphenoxyl phosphoryl chloride); and reacting the intermediate I and intermediate II to obtain a white solid which is the phenyl phosphate flame retardant containing DOPO. The initial decomposition temperature of the flame retardant was about 363, and the rate of residual carbon was 49% at 468, 800, and the flame retardant had good thermal stability, high residual carbon ratio and good flame retardant effect, which can be used for the non halogen flame retardant of polypropylene and ABS.

The invention discloses a phosphorus-containing Schiff base derivative intumescent fire retardant and a preparation method thereof. The method comprises the following steps: reacting hydroxy-aldehyde compounds with diamine compounds or reacting diamine compounds with hydroxy-amine compounds to obtain imine-diphenol, wherein two terminals of the molecule of imine-diphenol have phenolic hydroxyl groups and the skeleton of the imine-diphenol molecule contains a Schiff base structure; and allowing obtained diphenol Schiff base and phenyl dichlorophosphate to undergo interfacial polymerization under the action of a catalyst so as to obtain intumescent fire retardants with different phosphorus and nitrogen content. The synthetic method provided in the invention has the advantages of a simple process, easy reaction operation and suitability for industrial production; and the prepared fire retardant does not contain halogen, belonging to green environment-friendly fire retardants, and has a general structural formula as represented by formula (I).

The invention discloses an ultraviolet light-cured phosphorus-nitrogen-containing halogen-free flame retardant and a preparation method thereof. The preparation method is characterized in that: phenyl dichlorophosphate serving as a reaction matrix is reacted with polyalcohol or polyphenol partially acidified by acrylicacid or methacrylic acid; the product of the reaction is reacted with a nitrogen-containing compound with two reactive amino groups to form a yellow, sticky, transparent, liquid and phosphorus-nitrogen-containing substance which is ultraviolet light-cured monomer of which the molecule has an active double bound and phosphorus-nitrogen flame retardant elements; and the ultraviolet light-cured monomer serving as a reactive flame retardant is added into an ultraviolet light-cured resin substrate to form a transparent coating with high flame retarding efficiency through quick curing in ultraviolet light. The ultraviolet light-cured flame-retardant coating generates 34.0 percent of residue under an air condition at 60 DEG C, and 26.3 percent under a nitrogen condition. The maximum release rate of the ultraviolet light-cured flame-retardant coating is 146.6 W/g. The ultraviolet light-cured halogen-free phosphorus-nitrogen-containing flame retardant can be used for inflaming retarding in wood, textile, plastics, metal or circuit boards.

The invention relates to a flame-retardant polystyrene/layered inorganic nanocomposite and a preparation method thereof, which is characterized in that phenyl dichlorophosphate is taken as a reaction matrix for being reacted with polyol or polyphenol which is partially acrylated or partially methacrylated, and then the reaction with a nitrogen-containing compound with a reactive amino group is carried out, thereby obtaining the flame-retardant comonomer which simultaneously has an active double bond and a phosphorus-nitrogen flame-retardant element; the phosphorus-nitrogen monomer and styreneare used for preparing the flame-retardant polystyrene/layered inorganic nanocomposite through the free radical in-situ intercalation polymerization method in the presence of a layered inorganic; a phosphorus-nitrogen-containing flame retardant which is connected with a polymer molecular chain by the chemical bond way has better compatibility with a resin substrate and is more environment-friendly, and the flame retardant has no migration and no loss; the layered inorganic can further improve the thermal stability and the flame-retardant performance of a polymer substrate; and the flame-retardant polystyrene/layered inorganic nanocomposite can be directly prepared into a flame-retardant polystyrene material and can also be prepared into a flame-retardant masterbatch to be added in other plastics.

The invention discloses a preparation method of a Niraparib intermediate 4-(3S-piperidine-3-yl)aniline. The preparation method is characterized by comprising the following steps: 1) carrying out a contact reaction on a compound shown as a formula I and hydroxylamine hydrochloride to obtain a compound shown as a formula II; 2) carrying out a catalytic reaction on the compound shown as the formula II in the presence of phenyl dichlorophosphate to obtain a compound shown as a formula III; 3) carrying out a reduction reaction on the compound shown as the formula III to obtain the Niraparib intermediate 4-(3S-piperidine-3-yl)aniline shown as a formula X. A specific reaction process is shown in the description. By adopting the method provided by the invention, the utilization of a metal catalyst and transaminase with a high price is avoided, so that the production cost is lower, and a target product has high yield and stereoselectivity.

The invention discloses reaction-type flame-retardant glycol containing a phenyl phosphate-based symmetrical structure and a preparation method thereof. The preparation method is characterized by comprising the following steps: reacting phenyl dichlorophosphate with dihydric alcohol in a tetrahydrofuran or ethyl acetate solution in the presence of triethylamine, placing the tetrahydrofuran or ethyl acetate solution of dihydric alcohol and triethylamine into an ice-water bath, stirring and dropwise adding the tetrahydrofuran or ethyl acetate solution of phenyl dichlorophosphate; and filtering a precipitate and then removing the solvent in the filtrate to obtain the product with a structural general formula specified in the description, wherein n is an integer ranging from 2 to 6. According to the preparation method disclosed by the invention, micromolecular dihydric alcohol is introduced in the phenyl dichlorophosphate group in a manner of chemical bonding, so that the obtained dihydric alcohol molecular structure contains both the phenyl dichlorophosphate group and two hydroxyl groups with symmetrical structures and same reaction activity, and can partially or completely replace the micromolecular dihydric alcohol without a flame-retardant characteristic, so that the prepared polymer material has a flame-retardant characteristic; the raw materials in the preparation method disclosed by the invention are easily available, synthesis and post-treatment processes are simple, the cost is low, and the yield can achieve more than 90%.

The invention discloses a polymeric flame retardant containing silicon, phosphorus and nitrogen elements and a flame retardant polylactic acid material therefrom. The polymeric flame retardant is synthesized by the reaction between phenyl dichlorophosphate and 1,3-bis(3-aminopropyl)tetramethyldisiloxane, and the flame retardant polylactic acid material made from the polymeric flame retardant is prepared by steps of dissolving polylactic acid and the polymeric flame retardant containing silicon, phosphorus and nitrogen elements in chloroform in certain proportion and blending. The polymeric flame retardant contains high-content flame retardant elements such as phosphorus, nitrogen, and silicon simultaneously, and is high in relative molecular mass, not easy to migrate, and degradable. The flame retardant polylactic acid material of the polymeric flame retardant is simple in formula and good in flame retardant effect, does not contain halogen, and is low in degree of harm and pollution to the human body and the environment.

The invention discloses a biphenol polyphosphate fire retardant which is characterized in that n is an integer ranged from 300 to 1000. The preparation method comprises the following steps: weighing p-methyl phenyl dichlorophosphate or p-methylphenyl dibromo phosphate and biphenol based on mol ratio of 1:(0.9-1.2), and catalyst and biphenol based on mol ratio of 0.001 to 0.01; adding the weighed biphenol and catalyst to a reacting device; agitating and heating to 60-70 DEG C; adding p-methyl phenyl dichlorophosphate or p-methylphenyl dibromo phosphate within half an hour; keeping the temperature for 1 to 4 hours; and then heating to 200 DEG C to react for 3 to 4 hours to obtain white solid fire retardant; adding solvent to the prepared white fire retardant to completely dissolve; and then precipitating through the precipitating agent which is 5 to 10 times the amount of the solvent; and filtering; and finally drying in vacuum to obtain the white solid product. The biphenol polyphosphate fire retardant disclosed by the invention can be well compatible with a polymer base, is hard to shift, and has an excellent durable performance.

The invention discloses a preparation method of sofosbuvir. The preparation method includes following steps: in the absence of water and oxygen, enabling (2'R)-2'-deoxidized-2'-fluorine-2'-methyluridine, N-[(S)-(2, 3, 4, 5, 6-pentafluorophenoxy) phenoxy phosphoryl]-L-alanine isopropyl ester and Grignard reagent to react in the presence of a reaction solvent; dissolving mother liquid of sofosbuvir in a solvent, adding an adsorbent, depressurizing for concentration to be dry, adding solvent, pulping at room temperature, suction filtering, collecting filtrate, depressurizing for evaporation to dryness to obtain a oily product, adding solvent into the oily product, heating for dissolving to clearness, and cooling to 0-5 DEG C for crystallization to obtain recycled pentafluorophenyl; enabling D-alanine isopropyl ester and phenyl dichlorophosphate to be in reaction at minus 70-minus 80 DEG C, and adding a solvent solution of pentafluorophenyl and alkali for reaction to obtain a compound shown in a formula II. In the synthesis process of sofosbuvir, molecular pentafluorophenyl is removed, and pentafluorophenyl is recycled and used for preparation of an intermediate of sofosbuvir synthesis materials, so that pentafluorophenyl is recycled and influence on environment is reduced.

The invention discloses a topiroxostat preparation method. According to the method, 2-chloroisonicotinic acid which is cheap and easy to obtain serves as an initial material, potassium ferrocyanide serves as a green cyanogens source, AgI-KI-PEG generates 2-cyanoisonicotinate through cyanation of a mixed catalysis system and then directly acts with hydrazine hydrate to obtain 2-cyanoisonicotinate hydrazide under the action of an amide condensing agent phenyl dichlorophosphate (PDCP), and the product and 4-cyanopyridine are condensed to obtain topiroxostat. Through technological improvement of the reaction, reaction steps are shortened, the reaction yield is obviously increased by 90% or above, and the technological cost is obviously reduced. Meanwhile, a 2-chloroisonicotinic acid raw material which is cheaper and easy to obtain is used, use of corrosive thionyl chloride and other chlorinating agents is avoided, and the technology is suitable for industrial production. The method is short in synthesis step, easy to operate, mild in reaction condition, economical, environmentally friendly and suitable for industrial production, and the yield is obviously increased.

The invention relates to an artistic design packaging film material, which is composed of the following components: barium petroleum sulfonate, zinc ethyl phenyl dithiocarbamate, vermiculite powder, phenyl dichlorophosphate, zeolite powder, ethoxyquin Phenoline, Sodium Metabisulfite, Disodium Octaborate Tetrahydrate, Diacylglycerol, Magnesium Oxide, Polyvinyl Chloride Resin, Polydimethylsiloxane, Tricresyl Phosphate, Diatomaceous Earth, Carbendazim, Phosphite, Polyurethane Rubber powder, Phytectin, Polycarbonate, Sodium Ricinoleate, Ethylene Glycol Salicylate, Styrene Acrylic Emulsion, Imperata. The art design packaging film material has a simple preparation process, and the prepared product has relatively superior flame retardancy, acid and alkali resistance, anti-mildew and antibacterial properties, and improves product performance.

The invention relates to a method for preparing an emamectin benzoate intermediate by a microreactor. In particular, the method comprises the following steps: dissolving abamectin and tetramethylethylenediamine into dichloromethane to form a homogeneous solution, pumping the homogeneous solution and allyl chloroformate into a microchannel modular reaction device respectively to generate a compoundI; after mixing the reaction liquid of the compound I and dimethyl sulfoxide, pumping the mixture and phenyl dichlorophosphate into the next modular microreactor respectively to obtain a compound II;adjusting the pH of the reaction to 6 to 8 by alkaline water, standing and separating out an organic phase; distilling the organic phase and removing the dichloromethane to obtain the emamectin benzoate intermediate 4''-surface-4''-carbonyl-5-allyl formate-abamectin B1. According to the technical scheme of the invention and by adoption of the microchannel reaction device, mass transfer efficiencyand heat transfer efficiency are high, the raw materials are mixed instantaneously and completely, the reaction rate is accelerated, the selectivity is improved, the reaction time is greatly shortened and the production efficiency is improved; continuous production operation can be conducted, product quality stability is improved, the equipment integration level is high and occupied space can bereduced; and the product has high yield and high purity.

The invention belongs to the field of flame retardants for epoxy resin, and particularly relates to preparation of phosphorus-containing bismaleimide and application thereof in flame-retardant epoxy resin. The preparation method comprises the following steps: dissolving reactant N-(4-hydroxyphenyl) maleimide in tetrahydrofuran in a container with a nitrogen protecting device under ice bath, aftertotally dissolving, adding triethylamine and dispersing uniformly, and slowly dropwise adding a mixed solution of phenyl dichlorophosphate and tetrahydrofuran; after dropwise adding is finished, stirring at the room temperature, reacting for 8-12 h, carrying out suction filtering and rotary evaporation, successively washing obtained faint yellow sticky solid with ethyl acetate, ethanol and deionized water and then purifying and drying, further refining with an ethyl acetate and petroleum ether mixed solvent to obtain the phosphorus-containing bismaleimide as a target product. The prepared phosphorus-containing bismaleimide and epoxy resin can form an interpenetration polymer network structure under the effect of an amines curing agent, a flame-retardant effect is remarkable, and purposes of low addition and efficient flame retardancy can be achieved.

The invention relates to a flame-retardant waterborne polyurethane material. The flame-retardant waterborne polyurethane material comprises a composite flame retardant and polyurethane, the composite flame retardant is an attapulgite composite material and comprises anion modified attapulgite, cation modified attapulgite and modified nano montmorillonite; the anion modified attapulgite is prepared by the following steps: firstly, grafting KH-570 to acidified attapulgite, and then polymerizing an unsaturated alkenyl sulfonic acid compound; the cationic modified attapulgite is prepared by introducing unsaturated double bonds to acidified attapulgite through a chlorine substitution reaction of phenyl dichlorophosphate and then polymerizing with an unsaturated alkenyl ammonium chloride compound. According to the invention, attapulgite is modified step by step, so that the attapulgite has good flame retardance and self dispersibility, and can be stably dispersed in a coating system through electrical attraction and steric hindrance effect; the modified nano montmorillonite powder has a synergistic effect, so that the compatibility stability with a polyurethane emulsion system is further improved, and the toughness of the coating is improved.

The invention relates to a preparation method of flame-retardant and anti-corrosive metallic paint with high adhesion and belongs to the technical field of paint preparation. According to the method,phenyl dichlorophosphate, tetrahydrofuran and triethylamine are stirred and mixed firstly; then boric diglyceride is added dropwise, and a viscous polymer is obtained through a reaction; the viscous polymer is mixed with epoxy resin, and phosphorus-boron hybridized epoxy resin is obtained; attapulgite is modified; resin, the phosphorus-boron hybridized epoxy resin, modified attapulgite powder andother substances are stirred and mixed, and the flame-retardant and anti-corrosive metallic paint with high adhesion is obtained. Phosphate can be subjected to a reaction with base metal to form an insoluble phosphate film, surface area of the attapulgite is increased by acidification, so that adsorption capacity of the attapulgite is improved greatly, attapulgite surface is changed from hydrophilicity to hydrophobicity, and corrosion resistance is improved; a phosphorus-containing flame retardant is decomposed to generate metaphosphoric acid and the like to catalyze charring of a base material, a boron-containing flame retardant is decomposed to generate vitreous boron oxide, oxygen is isolated, heat transfer is stopped, and the method has broad application prospect.

The invention discloses a method for preparing a sofosbuvir intermediate by using a microfluid reaction device. The method comprises the following steps: pumping phenyl dichlorophosphate and pentafluorophenol into a first micro-channel reactor, carrying out a first-step acylation reaction, pumping the product obtained in the first step and L-alanine isopropyl hydrochloride into a second micro-channel reactor, carrying out a second-step substitution reaction to prepare a racemic sofosbuvir intermediate mixture, enabling the product to directly enter a micro-flow extraction device, and finally re-crystallizing to obtain a single-configuration target compound. Compared with the method in the prior art, the method disclosed by the invention has the advantages that the integration of efficientreaction and separation can be realized, the operation is simple, the problems caused by intermittent operation of extraction after product collecting are avoided, the reaction steps are few, the yield of the final product is high, the energy consumption is low, and the continuous large-scale production operation can be realized.

The invention discloses a silicon-containing flame retardant polyether surface treating agent. The silicon-containing flame retardant polyether surface treating agent contains three flame retardant elements including phosphorus, nitrogen and silicon, has the average molecular weight of 1,020-4,720, has the functionality of 6 and is a deep yellow transparent liquid. According to the preparation method, polyether polyol or polyether polyamine reacts with phenyl dichlorophosphate to generate flame retardant polyether, gamma-aminopropyltriethoxysilane is added, and the silicon-containing flame retardant polyether surface treating agent is prepared, wherein the gamma-aminopropyltriethoxysilane chain segment can be combined with a solid inorganic flame retardant through chemical bonds, and the polyether polyol chain segment and a polyether component for preparation of polyurethane resin have good compatibility. The surface treating agent has a flame retardant function, thus, solid inorganic flame retardant particles treated through the silicon-containing flame retardant polyether surface treating agent can be taken as flame retardant master batch and added to a formula material of polyurethane, and polyurethane foam with the solid inorganic flame retardant uniformly dispersed is obtained.

The invention discloses modified polyurethane elastomer based on in-situ polymerization of titanium dioxide and a preparation method of the modified polyurethane elastomer. The modified polyurethane elastomer is prepared from the following components, according to a weight part ratio, 18-34 parts of polyurethane, 12-28 parts of phenyl dichlorophosphate, 13-32 parts of isocyanate, 8-24 parts of dihydroxy diphenyl sulfone, 7-19 parts of polyester glycol, 11-19 parts of titanium dioxide, 7-18 parts of silicon carbide, 6-14 parts of magnesium oxide, 7-18 parts of montmorillonite and 5-12 parts of talcum powder. (1) The modified polyurethane elastomer based on in-situ polymerization of titanium dioxide is modified polyurethane with flame-retardant nature. (2) The polymerization components of the polyurethane elastomer are good in compatibility and dispersion. (3) The original mechanical properties of the polyurethane elastomer are ensured.

The invention discloses an environmental-friendly phosphorus-rich hybrid polystyrene composite material. The composite material is prepared from the following raw materials in parts by weight: 10 to 14 parts of graphite phase carbon nitride, 3 to 4 parts of hypophosphorous monohydrate, 1 to 2 parts of paraformaldehyde, 0.8 to 1 part of triethylamine, 3 to 5 parts of phenyl dichlorophosphate, 1 to 2 parts of aluminum sulfate octadecahydrate, 2 to 3 parts of 0.1 to 0.2 mol/l hydrochloric acid, 100 to 110 parts of polystyrene, a proper amount of acetonitrile, a proper amount of deionized water, a proper amount of absolute ethyl alcohol, 3 to 4 parts of allyl polyethylene glycol, 4.6 to 5 parts of sodium myrastate, 1 to 2 parts of nickel aminosulfonate, 3 to 5 parts of triethyl acetyl citrate, 0.4 to 1 part of calcium lactobionate, 2 to 3 parts of magnesium stearate, 0.3 to 1 part of hexamethyl phosphoric triamide, 0.3 to 1 part of trimethylol propane, 2 to 3 parts of hydrolytic polymaleic anhydride, and a proper amount of absolute ethyl alcohol and acetonitrile. The composite material does not contain toxic and harmful volatile substance, and is high in surface strength, good in safety and environmental protection property and excellent in comprehensive performances.