40 results about "Phosphoric chloride" patented technology

The invention discloses a preparation method of nitrogen-doped hierarchical pore hollow carbon spheres, and relates to the technical field of electrochemical desalination, the preparation method comprises the following steps: carrying out polycondensation on melamine and formaldehyde in the presence of PVP to form a spherical template; resorcinol and HMTA form a phenolic resin coating layer on the surface of the template; calcining at high temperature to realize decomposition and carbonization of the template, and introducing double bonds through a silane coupling agent; introducing a phosphoryl chloride group through free radical polymerization; finally, grafting a sulfonic acid group through nucleophilic substitution to obtain a final product. The nitrogen-doped hollow carbon spheres with a hierarchical pore structure are prepared through a hollowing strategy and surface modification, and N, P and S ternary heteroatom synergy is realized through introduction of a phosphoryl chloride group and a sulfonic acid group, so that the material has high specific surface area, optimized pore structure and strong ion exchange capacity; the composite material shows excellent ion adsorption performance and cycling stability, and has a good application prospect in the field of capacitive deionization.

The invention discloses a flame-retardant fiber and application thereof, the flame-retardant fiber comprises a flame-retardant fiber matrix and an organic-inorganic flame-retardant coating coated on the flame-retardant fiber matrix, and the organic-inorganic flame-retardant coating is formed by adopting an organic-inorganic phosphorus-containing flame retardant; according to the organic and inorganic phosphorus-containing flame retardant, hydroxylated carbon nanospheres are adopted as a core layer, a reaction product of bis (4-chlorphenyl) phosphoryl chloride and derivatives thereof and 4, 4 '-diaminodiphenyl sulfone and derivatives thereof is adopted as a shell layer, and the core layer and the shell layer are connected through acting force including covalent bonds and / or hydrogen bonds to form a core-shell structure; the flame-retardant fiber disclosed by the invention not only has an excellent flame-retardant effect, but also has better effects in other aspects such as antistatic property, spinnability, fiber system stability and the like, and is suitable for preparing flame-retardant textiles.

The invention relates to the technical field of phosphate preparation, and particularly discloses a phosphate preparation method which comprises the following steps: adding phosphoric acid and 1-ethyl-3-methylimidazolium dihydrogen phosphate into a reactor, starting stirring, then adding phosphorus trichloride, starting heating, and starting dropwise adding a mixture of raw materials R-OH and trichloroacetonitrile after the temperature is stable; after the reaction is finished, adding distilled water and 2-methylimidazole zinc salt for heating reaction, and cooling to room temperature after the reaction is finished; in the preparation method of the phosphate ester, trichloroacetonitrile is introduced as a phosphoric acid activating agent, so that the reaction condition required by directly using phosphoric acid as a reaction raw material in the traditional process is improved, the reaction temperature is reduced to 70-75 DEG C, and the efficient synthesis of the phosphate ester is realized; phosphorus trichloride is adopted as a dehydrating agent, water molecules generated in a reaction system are removed, reaction equilibrium is pushed to move towards the product direction, and the kinetic efficiency of phosphoric acid generation through the reaction of phosphorus trichloride and water is remarkably improved.

The present invention relates to a comprehensive treatment method for the process tail gas of lithium hexafluorophosphate, comprising the following steps: 1) absorbing the tail gas containing phosphorus fluoride and phosphorus chloride with water to obtain a mixed acid containing hydrogen chloride, hydrogen fluoride and phosphoric acid; 2) electrolyzing the mixed acid obtained in step 1) until the hydrogen chloride in the mixed acid is completely electrolyzed to obtain a solution; 3) heating the solution obtained in step 2) to cause the water and hydrofluoric acid to escape by heat, and then obtaining hydrofluoric acid after cooling. Through electrolysis and phosphorus removal treatment, fluorine, chlorine and phosphorus in the process tail gas of lithium hexafluorophosphate are fully separated, and hydrofluoric acid and chlorine are respectively prepared. The chlorine can be recycled for the preparation of phosphorus pentachloride in the production of lithium hexafluorophosphate, realizing the recycling of chlorine. At the same time, industrial-grade hydrofluoric acid can be obtained, and the added value of the product is high.

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 utility model discloses a hydrolysis reaction system for preparing chloromethyl ether, which comprises a hydrolysis reaction kettle, the top of the hydrolysis reaction kettle is provided with a first port and a second port which are arranged side by side, a dripping kettle is arranged above the first port, an etherification kettle is arranged above the second port, and the first port and the second port are communicated with each other. The dripping kettle and the etherification kettle are respectively connected with the first port and the second port through supporting cylinders; a dripping pipe is arranged in the supporting cylinder above the first port in a penetrating manner, and an air outlet pipe is arranged in the supporting cylinder above the second port in a penetrating manner; the hydrolysis reaction kettle is located in the shell, and a closed clamping cavity is formed between the outer wall of the hydrolysis reaction kettle and the inner wall of the shell. The hydrolysis reaction system provided by the utility model not only can solve the problem that hydrochloric acid mist is generated in the process of conveying phosphorus trichloride to the reaction kettle and dropwise adding the phosphorus trichloride, but also can solve the problems that hydrogen chloride gas is difficult to discharge immediately and the phosphorus trichloride is not completely hydrolyzed.

The method for manufacturing an intermediate compound for shikonin synthesis of the present invention comprises the steps of: reacting 1,5-dihydroxynaphthalene with dimethyl sulfate to prepare 1,5-dimethoxynaphthalene; reacting 1,5-dimethoxynaphthalene with N-bromosuccinimide (NBS) to prepare 1,5-dibromo -4,8-dimethoxynaphthalene; introducing a methoxy group into 1,5-dibromo-4,8-dimethoxynaphthalene using copper iodide (CuI) and 1,10-phenanthroline as a catalyst to prepare 1,4,5,8-tetramethoxynaphthalene; performing formylation of 1,4,5,8-tetramethoxynaphthalene using phosphoryl chloride (POCl3) to prepare 2-formyl-1,4,5,8-tetramethoxynaphthalene; and forming a boron complex using pinacolborane (HBpin) and 3,3-dimethylallyl bromide and reacting the boron complex with 2-formyl -1,4,5,8-tetramethoxynaphthalene to prepare a prenylated shikonin intermediate. Compared to conventional synthetic methods, the method of the present invention offers milder reaction conditions, shorter reaction time, and improved yield, thereby greatly enhancing the economic feasibility of shikonin synthesis.

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.

The invention discloses a flame-retardant high-temperature-resistant vehicle body film and a preparation method thereof, and relates to the technical field of high polymer materials. When the flame-retardant and high-temperature-resistant automobile body film is prepared, after 8 (aminophenyl trioxosilane) is diazotized, the diazotized 8 (aminophenyl trioxosilane) reacts with dimethyl phenyl silane to prepare azobenzene POSS; the preparation method comprises the following steps: reacting cellulose acetate with N2, N4, N6-tris (2-aminoethyl)-1, 3, 5-triazine-2, 4, 6-triamine and divinyl phosphoryl chloride in sequence to prepare modified cellulose acetate; the preparation method comprises the following steps: carrying out reaction on polyurethane, pyridine-2, 6-dicarboxylic acid and europium chloride hexahydrate to prepare modified polyurethane; and uniformly mixing the modified polyurethane, the modified cellulose acetate and azobenzene POSS, and carrying out mold pressing to form a film, so as to prepare the flame-retardant high-temperature-resistant vehicle body film. The flame-retardant and high-temperature-resistant vehicle body film prepared by the invention has excellent ultraviolet resistance, flame retardance and high-temperature resistance.

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 invention relates to the technical field of bisphenol A bis (diphenyl phosphate) synthesis, in particular to a synthesis method of BDP with low TPP content, which at least comprises the following steps: taking a phosphoryl chloride reaction solution as a raw material, controlling the dropwise adding temperature and the dropwise adding time, dropwise adding phenol into a container containing the phosphoryl chloride reaction solution, and extracting negative pressure in the dropwise adding process; the method comprises the following steps: dropwise adding TPP, heating after dropwise adding, controlling the degassing pressure and preserving heat to obtain a BDP crude product, and refining the BDP crude product to obtain a BDP product, thereby effectively reducing the TPP content, improving the BDP product quality and better meeting the actual production requirements by optimizing the reaction conditions.

The application belongs to the technical field of fluorine chemical synthesis, and particularly relates to a preparation method of tetra (fluorophosphoryl) imide alkali metal salt, at least comprising the following steps: mixing phosphoryl chloride, alkyl primary amine and acid binding agent in an organic solvent, stirring and reacting, and filtering to remove byproducts; adding a fluorination reagent, stirring and reacting, and filtering to remove byproducts; adding alkyl secondary amine, stirring and reacting, washing with deionized water, and removing the organic solvent under reduced pressure; adding a polar solvent and an alkali metal compound, stirring and reacting, filtering, concentrating, adding a weakly polar organic solvent to perform recrystallization, and drying under reduced pressure to obtain a finished product. Compared with the prior art, the raw materials used in the application are easy to obtain and low in cost, the production process is simple, no dangerous unit operation of high temperature and high pressure is involved, the product is easy to separate and purify, three-waste emissions are small, the application is friendly to the environment, the operation steps are simple, the product is easy to separate and purify, the purity and yield are high, the application is suitable for industrial mass production, and the like.

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 discloses a compound and a preparation method thereof, a perovskite solar cell, a power utilization device and a power generation device, the compound is used for an electron transport layer of the perovskite solar cell, the compound comprises a fullerene pyrrolidine group and an R group connected with the fullerene pyrrolidine group, the R group comprises an alkane group and a halogen group, and the halogen group is a halogen group. The alkyl group is at least one of an ether group, a sulfonyl group, a phosphoryl chloride group, a halogen ether group, a ketene group, an amide group and an amino ester group. The invention provides a new material capable of being used for an electron transport layer, and the perovskite solar cell containing the electron transport layer of the compound provided by the invention has the photoelectric conversion efficiency basically equal to or better than that of a perovskite solar cell with an electron transport layer formed by an electron transport material in related technologies. The compound has a relatively high oil-water distribution coefficient, and is beneficial to preparation of large-size perovskite solar cells.

The invention provides an aryl phosphate diester compound as well as a synthesis method and application thereof. The synthesis method comprises the following steps: under an inert atmosphere condition, carrying out a first reaction on a first mixed reaction system containing a phosphodiesters compound, thionyl chloride and a catalyst to obtain a phosphoryl chloride compound; under the inert atmosphere condition, a halogenated benzene compound and organic lithium are subjected to a lithium halogen exchange reaction, a second mixed reaction system containing the phosphoryl chloride compound and a product of the lithium halogen exchange reaction is subjected to a nucleophilic reaction, and the aryl phosphate diester compound is obtained. The synthesis method is relatively mild in reaction condition, high in raw material preparation yield and rich in applicable substrate variety. The invention also provides a mixed extraction system taking the o-hydroxybenzoic acid n-octyl ester as the extraction agent and the prepared aryl phosphate diester compound as the synergistic extraction agent, the extraction system is suitable for extracting lithium from an alkaline lithium-containing solution, the configuration of the extraction agent is subjected to enol transformation during extraction, and the lithium extraction rate is relatively high.

The present invention discloses a phosphoric acid-modified aluminum-lithium adsorbent and a method for preparing the same, as well as preparing battery-grade lithium carbonate and co-producing potassium chloride from carbonate-type salt lake brine. In the present invention, a polymer containing a styrene chain segment is dissolved in an organic solvent, a phosphating catalyst and phosphorus trichloride are added to carry out a phosphating reaction to obtain a phosphoric acid-modified polymer, which is then blended and granulated with an aluminum-lithium adsorbent to obtain a phosphoric acid-modified aluminum-lithium adsorbent. The phosphoric acid-modified aluminum-lithium adsorbent of the present invention solves the problem that traditional aluminum-lithium adsorbents are easily poisoned and deactivated in carbonate-type salt lakes, and can be directly applied to the lithium extraction process of carbonate-type salt lakes, and has the characteristics of long service life and long-term stable performance. The lithium extraction process of the present invention can directly produce battery-grade lithium carbonate and co-produce industrial-grade potassium chloride by coupling the aluminum-lithium adsorbent, a separation membrane and an ion exchange resin, and has the advantages of high automation and low construction and production costs. It is particularly suitable for extracting lithium from carbonate-type salt lake brine in areas such as Tibet.

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 field of analytical chemistry, and particularly discloses a method for detecting chiral purity of carnitine. The detection method provided by the invention comprises the following steps: respectively reacting a carnitine sample and a DL carnitine standard substance with a novel chiral derivatization reagent (S)-(-)-1, 2, 4-triazole; the method comprises the following steps: carrying out a derivatization reaction on (R)-(-)-1, 1 '-binaphthalene-2, 2'-dibasic phosphoryl chloride or (R)-(-)-1, 1 '-binaphthalene-2, 2'-dibasic phosphoryl chloride in an organic solvent to generate a diastereomer, separating and detecting derivatization products through reversed-phase high performance liquid chromatography, determining the retention time of the carnitine derivative according to the retention time of the DL carnitine derivative, and determining the content of the DL carnitine derivative according to the retention time of the DL carnitine derivative. And calculating the chiral purity through an area normalization method. Compared with the traditional method, the method provided by the invention has the advantages that the cost is reduced by more than 50%, the analysis accuracy is equivalent, the sensitivity is high, the chiral purity of carnitine can be accurately measured, and the market demand on an efficient and economic detection method is met.

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 novel alkaline hydrogen bond-assisted chiral bicyclic guanidine ion pair catalyst and its preparation and application, the present invention carries out certain structural transformation to traditional PN ion pair catalyst, without destroying the original structural basis, adds the structure of hydrogen bond, makes this novel H PN in various asymmetric catalytic reactions can play the dual role of hydrogen bond and ion pair catalysis, successfully constructs chiral phosphoramide compounds with higher yield (70% 80%) and enantioselectivity (80% 90%), solves the problem that traditional ion pair catalyst is difficult to construct chiral phosphoramide compounds. With phosphoryl chloride or secondary phosphorus oxide as substrate, various primary amine secondary amines as nucleophilic reagent, using 4% 10% catalyst of the present invention, successfully obtains phosphoramide with high yield (60% 80%) and high enantioselectivity (70% 90%).

The invention discloses a preparation method of a phosphite antioxidant P-EPQ, and relates to the technical field of antioxidants. The preparation method comprises the following steps: sequentially weighing biphenyl and phosphorus trichloride, adding into a reaction flask, stirring and dissolving at room temperature, adding a catalyst A, stirring and heating, controlling the internal temperature to be 70-76 DEG C, condensing and refluxing phosphorus trichloride, reacting for a certain time, stopping the reaction, and distilling to obtain a product which is an intermediate 4, 4 '-biphenyl bis-phosphine dichloride; the method comprises the following steps: transferring an intermediate 4, 4 '-biphenyl bis-dichlorophosphine into a three-neck flask, filling a mixed solution of 2, 4-di-tert-butylphenol and a catalyst B into a constant-pressure dropping funnel, dropwise adding the mixed solution into a reaction flask, keeping the temperature for reaction after the dropwise addition is completed, adding a solvent into a reaction solution after the reaction is stopped, raising the internal temperature, stirring and dissolving, carrying out suction filtration on the solution in the reaction flask, and drying to obtain the 2, 4'-biphenyl bis-dichlorophosphine. And carrying out negative pressure rotary evaporation on the filtrate to remove the solvent, wherein the distilled product is the target product P-EPQ. The preparation method of the antioxidant P-EPQ provided by the invention has relatively high yield.

The present invention belongs to the field of asphalt flame retardants, and provides an asphalt flame retardant, which comprises the following components in parts by weight: 10-30 parts of metal organic phosphate, 20-60 parts of magnesium hydroxide, 2-5 parts of titanate coupling agent, and 10-30 parts of expandable graphite; its preparation method comprises the following steps: dissolving phenol in an organic solvent, adding phosphorus oxychloride and triethylamine, reacting for a period of time to generate organic phosphoryl chloride, and then carrying out a hydrolysis reaction to obtain an organic phosphate ester; sequentially adding the above-mentioned organic phosphate ester and an alkaline substance containing metal ions into the organic solvent to obtain a metal organic phosphate; mixing the titanate coupling agent and the organic solvent to prepare an organic solution, sequentially adding the above-mentioned metal organic phosphate, expandable graphite and magnesium hydroxide into the organic solution, soaking for a period of time, filtering the organic solution, and drying and cooling the obtained filter body to obtain the asphalt flame retardant; the present invention can improve the flame retardancy and smoke suppression performance of asphalt, reduce the fire hazard of asphalt pavement, and at the same time improve the high-temperature performance of asphalt.

The invention discloses a phosphite antioxidant and a preparation process thereof, and belongs to the field of chemical assistants. The phosphite antioxidant is prepared from the following raw materials: cardanol, phosphorus trichloride and modified branched chain alcohol, the molar ratio of the cardanol to the phosphorus trichloride to the modified branched chain alcohol is (2.4-2.6): (1-1.1): (0.7-0.9); the modified branched-chain alcohol is prepared by reacting epoxybutane with medium-chain amine according to a molar ratio of 1: 1 and then reacting the obtained intermediate product with chloropropane according to a molar ratio of 1: (1.05-1.1). The antioxidant has the effect of improving the processing stability while improving the thermal stability of the antioxidant to the material.

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.

Process for the preparation of N-(2-nitrophenyl)phosphoric triamide (2-NPT) by reaction of 2-nitroaniline and phosphorus pentachloride to an iminophosphoric trichloride (I), subsequent hydrolysis of the iminophosphoric trichloride (I) without its prior isolation or purification with a hydrolyzing agent to the phosphoric amide dichloride (II), and subsequent ammonolysis of the phosphoric acid amide dichloride (II) without its prior isolation or purification to 2-NPT, characterized by that the 2-nitroaniline is dosed into a suspension of phosphorus pentachloride in an inert solvent via a dip tube within 0.5 to 5 h at a temperature between 40 and 60 °C and then heated to boiling. and the addition of the hydrolyzing agent to the iminophosphoric acid trichloride (I) a) at a temperature of 70 to 100 °C for a period of less than one hour or b) at a temperature of 45 to 60 °C over a period of up to 5 h or simultaneously, within a period of up to 5 h, approximately equimolar amounts of the solution of iminophosphoric acid trichloride (I) and the hydrolyzing agent are dosed into a separate reactor, wherein the temperature of the iminophosphoric acid trichloride solution and the reactor temperature are 50-100 °C.

The invention discloses a preparation method of a phosphorus-nitrogen synergistic flame retardant. The method comprises the following steps: by taking neopentyl glycol and phosphoryl chloride as initial raw materials, reacting to obtain corresponding cyclic phosphoryl chloride, and further reacting with methanol to obtain corresponding methyl phosphate; and reacting with different diamines under the action of a strongly alkaline catalyst to obtain the phosphoramidate. The target phosphoramidate is obtained through amine-ester exchange and by selecting the specific strong basic catalyst, the problems that in the traditional acyl chloride and amine reaction process, by-products are many, and the separation cost is high can be effectively solved, and the preparation method is high in product yield and easy to separate. The phosphoramidate can be used as a phosphorus-nitrogen synergistic flame retardant.