38 results about "Diethyl phosphate" patented technology

The invention discloses a cool breathable fiber and a preparation method thereof, and relates to the field of fibers. When the cool-feeling breathable fiber is prepared, shell powder sequentially reacts with 3-chloropropyltrimethoxysilane, 2, 6-dihydroxy naphthol and 3, 3-diphenyl-2-propyne-1-alcohol, and functionalized shell powder is prepared; the preparation method comprises the following steps: reacting (formylmethyl) diethyl phosphate with (4-pyridyl) acetone, firstly polymerizing with dimethyl terephthalate and ethylene glycol, and then reacting with N-[4-(aminomethyl) phenyl] guanidine to prepare modified polyester; and finally, mixing the modified polyester, the functionalized shell powder and zinc acetate, and spinning to obtain the cool breathable fiber. The cool breathable fiber prepared by the invention has flame-retardant, durable and antibacterial capabilities.

The invention discloses a method for detecting phosphate impurities, namely diethyl phosphoacetic acid and diethyl phosphate, in afatinib, and establishes a simple and sensitive ion chromatography detection method based on the hydrolysis property of a phosphate compound under an alkaline condition. Sodium hydroxide or potassium hydroxide solution-water is used as a mobile phase for isocratic or gradient elution, and a conductivity detector is used for detection. According to the present invention, the accurate quantification of the impurities in the afatinib is achieved, the detection speed is fast, the cost is low, the operation is simple, and the good specificity, the sensitivity, the precision and the accuracy are provided, such that the product quality of the afatinib maleate bulk drug synthesized by using the diethyl phosphoacetic acid as the starting material and the related preparation can be further ensured.

The invention discloses a tetrazine probe synthon and a preparation method and application thereof.The preparation method comprises the following steps that under the inert atmosphere, diethyl cyanomethylphosphonate, 3-hydroxypropionitrile, 3-mercaptopropionic acid and hydrazine hydrate are mixed and then react at the room temperature, a sodium nitrite solution is added after the reaction is finished, then acid is continuously added till the reaction system reaches acidity, and a tetrazine probe synthon product is obtained; continuously reacting to obtain an intermediate; and dissolving the intermediate in a solvent in an inert atmosphere, adding triethylamine, slowly adding methanesulfonyl chloride, and reacting at room temperature to obtain the tetrazine probe synthon shown in the formula I. The invention further discloses a preparation method of the tetrazine probe synthon. The tetrazine probe synthon provided by the invention can perform series Heck reaction and HWE reaction, so that controllable combination of functional groups on two sides of a tetrazine coupling probe is realized under mild reaction conditions, and the functional groups on two sides are designed according to actual requirements to regulate and control photophysical properties of the probe. A brand new way is provided for developing a high-performance biological orthogonal fluorescent probe.

The invention discloses a benzoxphosphine ligand and a complex and application thereof. The structure of the benzoxphosphine ligand is shown as a formula (I), in the formula (I), R1 is alkyl or aryl substituted oxazolidinyl or imidazoline, R2 is alkyl and / or aryl, and R3 is at least one of fluorine, carbazolyl and 2, 6-dimethoxyphenyl. According to the benzoxphosphine ligand disclosed by the invention, the metal iridium complex can be used as a catalyst to be applied to an asymmetric hydrogenation reaction of alpha-phenyl vinyl diethyl phosphate, and has excellent activity and relatively high enantioselectivity; moreover, the benzoxphosphine ligand disclosed by the invention can be directly synthesized from simple and easily available chiral aldehyde, and the preparation method is simple and easy to operate.

The invention relates to a waterborne polyurethane emulsion as well as a preparation method and application thereof. The preparation raw materials of the waterborne polyurethane emulsion comprise the following components: an isocyanate monomer, flame-retardant polyether polyol, polydimethylsiloxane, a hydrophilic chain extender and a small molecular alcohol chain extender. The flame-retardant polyether polyol is a polymer formed by [(bis (2-hydroxyethyl) amino) methyl] diethyl phosphate and an epoxy compound. According to the synthesized waterborne polyurethane coating, the synergistic effect of nitrogen, phosphorus and silicon is utilized, flame propagation can be effectively inhibited, the molten drop phenomenon can be remarkably inhibited, and the limit oxygen index and the vertical combustion grade of the material are greatly improved.

The invention relates to the technical field of organic synthesis, and provides a synthesis method of an important organic synthesis intermediate methyl diethyl phosphonate. Comprising the following steps: firstly, adding paraformaldehyde and alkali into a solvent, heating and stirring, and filtering to obtain an intermediate solution; and adding cation exchange resin and the intermediate solution into a reaction flask, dropwise adding diethyl phosphite, carrying out a heat preservation reaction after dropwise adding is completed, filtering to remove the cation exchange resin (which can be recycled for multiple times) after the reaction is completed, and carrying out reduced pressure distillation to remove the solvent and a trace amount of diethyl phosphite residue, so as to obtain the product. The method has the main advantage that paraformaldehyde is used as a methylation reagent and reacts with diethyl phosphite in one step under the action of a catalyst to obtain a target product.

The present invention relates to methods of treating endometriosis or preventing recurrence of endometriosis. In particular, the present invention relates to a method of treating endometriosis and relapse thereof, comprising administering to a woman suffering from endometriosis a pharmaceutical composition comprising an S-alkyl isothiourea derivative, in particular S-ethyl isothiourea diethyl phosphate. The methods and pharmaceutical compositions of the present invention can retain fertility and can be fertilized.

The invention provides a phosphorus-nitrogen synergistic intumescent flame retardant and a preparation method and application thereof, and belongs to the technical field of flame retardants, the preparation method comprises the following steps: step S1, enabling expandable graphite and isocyanate to react in the presence of a catalyst to obtain activated expandable graphite; s2, under the protection of inert gas, 1, 3-bis (3-aminopropyl)-1, 1, 3, 3-tetramethyldisiloxane and protocatechuic aldehyde are subjected to a Schiff base reaction in a solvent, then diethyl phosphite and zinc chloride are added, a phosphoric acid addition reaction is performed, and a flame-retardant monomer is obtained; s3, adding the activated expandable graphite and a flame-retardant monomer into a solvent, and performing grafting reaction in the presence of a catalyst to obtain the phosphorus-nitrogen synergistic intumescent flame retardant. Through the process design of isocyanate activation of the expandable graphite and flame-retardant monomer grafting, a multi-component synergistic flame-retardant system based on chemical bonding is constructed, so that the flame-retardant property of the composite material is improved, and the flame-retardant durability of the composite material is enhanced.

The application discloses a liquid titanium-based polyester catalyst and a preparation method thereof, and relates to the field of titanium-based catalysts. The catalyst takes titanate as a main raw material and is prepared through modification of an ionic liquid coordination modification; the modified ionic liquid is prepared through quaternary ammonium and ion exchange reactions and is composed of imidazole cations, phosphoric acid groups and bistrifluoromethylsulfonylimide anions. The preparation method comprises the following steps: first, an intermediate chloride is prepared through quaternary ammonium reaction of N-methyl imidazole and 3-chloropropyl phosphoric acid diethyl ester; then, the modified ionic liquid is obtained through ion exchange reaction to replace anions; finally, the modified ionic liquid is subjected to coordination reaction with the titanate to prepare the liquid titanium-based polyester catalyst. The liquid titanium-based polyester catalyst prepared by the application has excellent hydrolysis resistance, catalytic activity and thermal stability performance and is suitable for the industrial production requirements of the polyester.

The invention discloses a flame-retardant gel polymer electrolyte and a preparation method and application thereof, and belongs to the technical field of supercapacitors. The method comprises the following steps: adding iodine diethyl methyl phosphate and 1, 3-propane sultone into an organic solvent containing 1, 3-dioxolane, and uniformly mixing to obtain a mixed solution; adding lithium salt into the mixed solution to obtain a precursor solution; and dropwise adding the precursor solution on the surface of an electrode to assemble a supercapacitor, and heating to form the flame-retardant gel polymer electrolyte on the surface of the electrode in situ. According to the flame-retardant gel polymer electrolyte prepared by the method, the flame-retardant characteristic of the electrolyte can be remarkably improved, the combustion risk is fundamentally eradicated, a good solid-liquid mixed interface can be formed with an electrode, and high ionic conductivity and low interface impedance are guaranteed.

This invention discloses a method for detecting genotoxic impurities in fosfomycin calcium. The method involves preparing a test solution and a reference solution using hydrochloric acid as a solvent, and then detecting the test solution and reference solution using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) to obtain the content of genotoxic impurities in fosfomycin calcium. The genotoxic impurities are: 1,2-epoxypropyl diethyl phosphate, (2-propenyl)-diethyl phosphate, allyl diethyl phosphate, and propyl diethyl phosphate. This invention develops an analytical method capable of simultaneously detecting four diethyl phosphonate genotoxic impurities in fosfomycin calcium. This method exhibits good specificity, injection precision, linear range, limit of quantitation, limit of detection, accuracy, repeatability, intermediate precision, and robustness. It can be used for the detection and monitoring of diethyl phosphonate impurities in fosfomycin calcium raw materials, ensuring product quality and improving the safety of clinical medication.

This invention discloses an antibacterial air filter material and its preparation method, relating to the field of filter material technology. In preparing the antibacterial air filter material, terephthalaldehyde is reacted sequentially with 2-aminobenzimidazole and diethyl phosphite to obtain a phosphorus-nitrogen composite flame retardant; silica is reacted sequentially with γ-glycidyl etheroxypropyltrimethoxysilane and 1-hydroxymethyl-5,5-dimethylhydantoin to obtain modified silica; the modified silica is chlorinated with sodium hypochlorite to obtain haloaminated silica; 70-80 parts of polyacrylonitrile, 5-6 parts of the phosphorus-nitrogen composite flame retardant, and 3-4 parts of haloaminated silica are formulated into a spinning solution, and electrospinned to obtain a polyacrylonitrile fiber membrane; the polyacrylonitrile fiber membrane is reacted sequentially with ethylenediamine and curcumin to obtain the antibacterial air filter material. The antibacterial air filter material prepared by this invention has the advantages of both antibacterial and flame retardant properties.

The present invention relates to a process for the continuous flow preparation of a mixture of isomers of hexa-1,3-dien-1-yl-diethylphosphate mainly composed of the (E,Z) isomer and essentially free of the (E,E) isomer.

This invention belongs to the field of inorganic nanoparticle technology, and discloses a silicon-phosphorus-containing inorganic nanoparticle, its preparation method, and its application. The silicon-phosphorus-containing inorganic nanoparticle is prepared from inorganic nanoparticles, a phosphorus-containing compound, and a silane coupling agent. The inorganic nanoparticles are selected from at least one of nano-ZrO2, nano-CaCO3, nano-SiO2, and nano-TiO2. The phosphorus-containing compound is selected from at least one of dimethyl phosphite, diethyl phosphite, and diphenyl phosphite. The silane coupling agent is selected from γ-glycidoxypropyltrimethoxysilane and / or γ-glycidoxypropyltriethoxysilane. The silicon-phosphorus-containing inorganic nanoparticles of this invention, due to surface modification, have significant steric hindrance, are not prone to aggregation, and can be well dispersed in a matrix. The inorganic nanoparticles contain silicon and phosphorus, and have a certain flame-retardant effect.

The invention relates to the technical field of research, development and manufacturing of functional films, and discloses an eleven-layer co-extruded film, a preparation process and application in aviation cables, and the preparation process specifically comprises the following steps: by taking heptamethyl hydrogen-containing POSS, diallylamine, diethyl phosphite and 10-undecenal as raw materials, carrying out hydrosilylation, Kabachnik-Fields and alkenyl epoxidation reaction to obtain the eleven-layer co-extruded film. The preparation method comprises the following steps: synthesizing a halogen-free reaction type phosphorus-POSS-nitrogen synergistic flame retardant, and carrying out covalent bond interaction on the halogen-free reaction type phosphorus-POSS-nitrogen synergistic flame retardant and amino-terminated functional groups in PA6 resin and PA66 resin through an epoxy-amino ring-opening reaction to prepare flame-retardant PA master batches; the flame-retardant PA master batch is used as a raw material of the eleven-layer co-extrusion film, and an eleven-layer co-extrusion blow molding process is adopted to prepare the eleven-layer co-extrusion film. The flame retardant property of the eleven-layer co-extrusion film is remarkably improved, and meanwhile, the beneficial technical effect of remarkably enhancing the high-temperature resistance of the eleven-layer co-extrusion film is achieved.

The invention provides a preparation method and a preparation device of a phosphine aldehyde intermediate and glufosinate-ammonium. The preparation method comprises the following steps: mixing acrolein with an auxiliary agent, freezing at low temperature, settling and layering to obtain pretreated acrolein, mixing the pretreated acrolein with acetic acid to obtain a first mixed solution, mixing the first mixed solution with diethyl methylphosphite, performing condensation reaction to obtain acetal, and hydrolyzing the acetal to obtain the phosphine aldehyde intermediate. According to the method, acrolein is pretreated in a low-temperature freezing mode, side reactions can be effectively inhibited, and the product yield is increased. Furthermore, a circulation condensation reaction mode is adopted, the reaction heat is effectively diluted through circulation of a large amount of materials, the condensation reaction temperature is stabilized, and the reaction yield is increased. Experimental results show that according to the method provided by the invention, the yield of phosphine aldehyde is increased to 96%, and the yield of glufosinate-ammonium is increased to 88%.

The application discloses a self-repairing magnetic lubricating composition and a preparation method thereof, and relates to the technical field of lubricating oil.The application prepares imidazole ionic liquid containing a double bond in a side chain by subjecting diethyl allylphosphonate and 1-(3-aminopropyl)imidazole to a quaternary amination reaction, and then subjecting the imidazole ionic liquid to reaction with 3-mercapto propionic acid to form ionic liquid containing amino and carboxyl; the ionic liquid can form an amide crosslinking between adjacent molecules in high-temperature friction, the ionic liquid monomer is converted into a polymer network, cracks or pits are filled, and the self-repairing function is realized; then mesoporous ferroferric oxide is selected as a magnetic response component, the ionic liquid containing amino and carboxyl is pre-adsorbed, a magnetic field is applied, the magnetic response component is induced to be directionally enriched to a contact area of a friction pair and a micro-damage site, the ionic liquid is released at a fixed point, and through compounding of the magnetic response component and a polar anchoring monomer, the oil film stability is improved by using the synergistic effect of magnetic induction and polar adsorption.

The invention discloses a rapid cyanogenic glycoside detection kit and a detection method, and belongs to the technical field of agricultural product detection. The kit comprises an enzymolysis reaction reagent and a hydrocyanic acid detection reagent, the enzymatic hydrolysis reaction reagent is prepared from beta-glucosidase, 1-ethyl-3-methylimidazole diethyl phosphate salt and rhamnolipid, and the enzymatic hydrolysis reaction reagent is prepared from beta-glucosidase, 1-ethyl-3-methylimidazole diethyl phosphate salt and rhamnolipid; the hydrocyanic acid detection reagent comprises a picric acid test strip, tartaric acid and a saturated sodium carbonate solution. The detection method comprises the following steps: adding an enzymolysis reaction reagent into a sample to be detected, hydrolyzing cyanogenic glycoside into cyanide, and adding tartaric acid to convert into volatile hydrocyanic acid; a picric acid test strip wetted by a saturated sodium carbonate solution is used for adsorption, and hydrocyanic acid and sodium picrate on the test strip act to generate sodium isocyanurate; and observing the color change of the test strip for qualitative and / or quantitative detection. The detection kit provided by the invention is convenient and rapid, has a short detection period, and is convenient for timely detection in links of agricultural product production, processing, storage, sales and the like.

The application belongs to the field of organic synthesis, and particularly relates to a synthesis method of TMS protected alkyne. An alkyl amide derivative shown in formula 1 and N,N-dimethylformamide shown in formula 2 are mixed with an organic solvent (tetrahydrofuran) in the presence of a strong base (lithium bis(trimethylsilyl)amide) and an activating agent (diethyl chlorophosphate), and a reaction is performed to synthesize TMS protected alkyne shown in formula 3. The raw materials used in the application are common chemicals on the market. The application has a wide range of applications, and not only can common TMS protected alkyne compounds be synthesized, but also a series of TMS protected alkyne derivatives can be synthesized according to the need of adjusting the reaction substrate. This provides certain support for the research in the fields of medicine, material science and the like.

The invention discloses a preparation method of a low-VOC (volatile organic compound) polyurethane structural adhesive, and relates to the technical field of adhesives. The low-VOC polyurethane structural adhesive prepared by the invention comprises a component A and a component B, wherein the component A is prepared from castor oil, polyester glycol, a dimethyl alcohol composite flame retardant, modified aluminum oxide and a catalyst; the component B is prepared from an isocyanate terminated prepolymer, polymethylene polyphenyl polyisocyanate and a water removal agent; the dimethyl alcohol composite flame retardant is prepared by carrying out a reaction on 5-(aminomethyl)-2-furfuryl alcohol, 5-hydroxymethylfurfural and diethyl phosphite; the modified aluminum oxide is prepared by sequentially reacting aluminum oxide with aminopropyltriethoxysilane, triglycidyl isocyanurate and 4-(2H-benzo [D] [1, 2, 3] triazole-2-yl) benzene-1, 3-diol, and the modified aluminum oxide is prepared by sequentially reacting aluminum oxide with aminopropyltriethoxysilane, triglycidyl isocyanurate and 4-(2H-benzo [D] [1, 2, 3] triazole-2-yl) benzene-1, 3-diol. The low-VOC polyurethane structural adhesive prepared by the invention has the advantages of flame retardance, heat conduction and ultraviolet aging resistance.

The invention discloses a biochar material for recycling rare and precious metals from waste solar cells and a preparation method of the biochar material, and relates to the technical field of biochar materials. When the biochar material for recycling the rare and precious metals from the waste solar cells is prepared, firstly, biomass raw materials are dried, smashed, carbonized and carboxylated, and then biochar is prepared; growing a metal organic framework on the surface of the biochar in situ to prepare metal organic framework modified biochar; enabling the metal organic framework modified biochar to react with paraformaldehyde and diethyl phosphite to prepare phosphating modified biochar; reacting the phosphatized modified biochar with 3-bromopropylene to obtain modified biochar; and coating the surface of the modified biochar with an ion imprinting layer to prepare the biochar material for recycling rare and noble metals from waste solar cells. The biochar material for recycling rare and precious metals from waste solar cells prepared by the invention has the advantages of selective ion adsorption, high adsorption capacity and recyclability.

The invention relates to the technical field of pesticides and herbicides, in particular to a method for efficiently preparing L-refined glufosinate ammonium, which comprises the following steps of: adopting a one-pot method to prepare reaction liquid A by taking a compound as shown in a formula I and diethyl methylphosphite as synthesis starting points, treating the reaction liquid A at high temperature to rearrange byproducts in the reaction liquid A to generate a target object, so as to obtain reaction liquid B; and finally, hydrolyzing the reaction liquid B with hydrochloric acid, and then removing the hydrochloric acid to obtain the L-refined glufosinate-ammonium. According to the method for efficiently preparing the L-refined glufosinate-ammonium, the process steps are simpler and more convenient, and the yield and ee value of the L-refined glufosinate-ammonium are synchronously improved while the preparation cost is reduced.

The invention discloses a dyeable flame-retardant polyester yarn and a preparation method thereof, and relates to the field of polyester spinning. The easy-to-dye flame-retardant polyester yarn is prepared from a polyester melt through a melting direct spinning process, the polyester melt is obtained by esterification and polycondensation of terephthalic acid, ethylene glycol and a phosphate monomer as raw materials according to a molar ratio of 1: (1.2-1.8): (0.07-0.12), and the phosphate monomer is prepared by aldehyde amine condensation of an alcohol amine compound and (formyl methyl) diethyl phosphate according to a molar ratio of 1: (1.1-1.3). The polyester yarn prepared by the preparation method disclosed by the invention has excellent flame retardant property and mechanical property, and has relatively low broken filament breakage rate in a spinning process.

The invention provides a fluorescent single-particle membrane device for detecting nerve agent simulant diethyl chlorophosphate and a preparation method of the fluorescent single-particle membrane device. According to the single-particle film device, a lattice structure is formed on a glass substrate by utilizing photoresist or an ultraviolet curing adhesive material through mask exposure, and a tetraphenylethylene covalent organic framework material is loaded by means of a rubber substrate; and then the two are attached, positive pressure is applied, heating is conducted, the photo-curing material in the molten state is made to adhere to the frame material, and finally the single-particle film is formed. After the device is in contact with a diethyl chlorophosphate atmosphere and a methanol solution thereof, the fluorescence of the device at 543 nm is specifically quenched, so that high-sensitivity, high-selectivity, on-site rapid and visual detection of diethyl chlorophosphate is realized.

The invention relates to a lubricant composition for use in fluid dynamic bearing systems containing brass alloys, comprising at least one base fluid comprising an ester oil and an anti-wear additive, wherein the additive comprises at least one phosphonium-based ionic liquid of the general formula [A+] [B-], wherein a cation [A + ] selected from tributylethylphosphonium [P (C4H9) (C2H5) 3] + and / or trihexyl (tetradecyl)phosphonium [P (C6H 13 ) (C 14 H 29 ) 3] + , and an anion [B - ] selected from bis(2-ethylhexyl)phosphate [O=P(OC2H5)2] - , Decanoate [O2C9H 19 ] -and / or diethyl phosphate [O=P (OC2H5) 2] the use of such a lubricant composition in a brass alloy-containing fluid dynamic bearing system; the use of such a brass alloy-containing fluid dynamic bearing system in a motor; as well as the use of such a motor in a hard disk drive, a fan or a laser scanner.

The invention discloses a method for detecting the content of diethyl phosphite in an FRC-6 flame retardant. The detection method comprises the following steps: adding carbon tetrachloride, 4-dodecylaniline and triethylamine into an FRC-6 flame retardant sample, uniformly shaking, heating in a constant-temperature water bath kettle at 70 DEG C for 15 minutes, derivatizing diethyl phosphite to obtain a diethyl phosphite derivatization reaction product, and detecting by adopting a liquid chromatography external standard method and a quantitative method. According to the method, diethyl phosphite in the FRC-6 flame retardant sample is derivatized through carbon tetrachloride and 4-dodecylaniline, then the content of the FRC-6 flame retardant sample is measured through a liquid chromatography external standard method, the relative standard deviation RSD of the measurement result is smaller than 3.3%, the precision is high, the analysis and test method is simple, consumed time is short, multiple groups of parallel test results of the method are close, and the method is suitable for industrial production. The method has the advantages of simple operation, good repeatability and high accuracy, the adding standard recovery rate is 95-105%, the recovery rate is stable, the method is suitable for popularization and application, and tests show that the detection method is also suitable for determining the content of diethyl phosphite in other phosphate esters.

The present invention relates to a novel additive, and to a non-aqueous liquid electrolyte and a gel-type or solid polymer electrolyte containing same. More specifically, the present invention relates to a novel additive and a non-aqueous liquid electrolyte and a gel-type or solid polymer electrolyte containing same, the novel additive comprising a siloxane compound that includes an amine group substituted with an electron-withdrawing functional group, or an isocyanate group, a boronate pinacol ester group, a butylate group, a hexanoate group, a heptanoate group, a cyclohexanopropionate group, and a diethyl phosphate group, and improving electrochemical stability, thermal stability, flame retardancy, and cycle life of an alkali metal battery to which the additive is added.

The present application relates to the technical fields of functional film research and manufacturing, and discloses a kind of eleven-layer co-extrusion film, preparation process and application in aviation cable, specifically: with seven methyl hydrogen-containing POSS, diallylamine, diethyl phosphite and 10-undecenal as raw material, through silicium hydrogen addition, Kabachnik-Fields and alkenyl epoxidation reaction, synthesis of halogen-free reactive phosphorus-POSS-nitrogen synergistic flame retardant, it is with the end amino functional group in PA6 resin, PA66 resin through epoxy-amino ring-opening reaction Covalent bond effect, prepare flame-retardant PA masterbatch;Flame-retardant PA masterbatch is used as the raw material of eleven-layer co-extrusion film, adopts eleven-layer co-extrusion blow molding process, and eleven-layer co-extrusion film is prepared.The present application significantly improves the flame-retardant performance of eleven-layer co-extrusion film, and also achieves the beneficial technical effect of significantly enhancing the high-temperature resistance of eleven-layer co-extrusion film.

The application discloses a preparation method and equipment of diethyl methyl phosphite, and belongs to the technical field of chemistry and chemical industry. The preparation method of diethyl methyl phosphite comprises the following steps: (1) reacting aluminum powder and chloromethane to obtain a sesqui-reaction solution; (2) mixing phosphorus trichloride, a solid acid catalyst and the sesqui-reaction solution and reacting; (3) removing the phosphorus trichloride, adding sodium chloride and performing a dissociation reaction to obtain methyl phosphorus dichloride and sodium tetrachloroaluminate; and (4) putting the methyl phosphorus dichloride, ethanol, liquid nitrogen and isohexane into an esterification reaction kettle, performing an esterification reaction, purifying and obtaining pure diethyl methyl phosphite. The application further discloses an esterification reaction kettle which comprises a barrel, a feeding pipe, a stirring main shaft and a special-shaped umbrella body, and the surface of the special-shaped umbrella body is provided with grooves. The preparation method has high product purity and high yield, and the equipment is uniformly stirred, so that the reaction can be completely performed.

This invention discloses a phosphorus-modified Pd-Fe bimetallic catalyst, its preparation method, and its application. SBA-15 mesoporous silica is used as a support, and diethyl phosphite is used as a phosphorus modifier to support the Pd-Fe bimetallic catalyst. The preparation process involves pretreatment with SBA-15 to activate the silanol groups, followed by transesterification of diethyl phosphite to form -Si-O-P(O)(OEt)- bonds for anchoring, and then calcination and reduction to generate P-O-Si bonds that coordinate with Pd-Fe. This catalyst utilizes the ordered mesopores of SBA-15 to promote TNT diffusion, and diethyl phosphite to regulate the electronic states and dispersion of Pd-Fe, achieving a waste TNT conversion rate ≥99.5%, a TAT selectivity ≥96%, and a conversion rate ≥98% after 15 cycles. This solves the problems of poor stability, low selectivity, and easy clogging of mesopores in existing catalysts, making it suitable for the harmless treatment of waste TNT.