50results about "Phosphorous acid" patented technology

The present disclosure provides an aluminum phosphite-based complex with dual-peak thermal gravity decomposition characteristics and a preparation method and use thereof. A structural formula of the complex is as follows: ((HPO3)3Al2)·((H2PO3)3Al)x, wherein x is 0.01-0.5 and represents a molar ratio of (H2PO3)3Al to (HPO3)3Al2. The dual-peak thermal gravity decomposition characteristics are as follows: a first gravity peak temperature is 460-490° C., and a second gravity peak temperature is 550-580° C. The preparation method includes: uniformly mixing aluminum phosphite and aluminum hydrogen phosphite according to the ratio in the structural formula, and then performing stepwise heating at a rate of 5° C. / min to raise the temperature of a mixture from the normal temperature to no more than 350° C. within 1-10 hours, so as to obtain the aluminum phosphite-based complex with the dual-peak thermal gravity decomposition characteristics. The complex may serve as or is configured to prepare a flame retardant or a flame-retardant synergist.

The present application relates to the technical field of preparation of disodium hydrogen phosphite, and discloses a method for preparing disodium hydrogen phosphite, comprising the following steps: S1, dissolving phosphorous acid and sodium hydroxide in distilled water under an inert gas atmosphere, wherein the molar ratio of phosphorous acid to sodium hydroxide is 1:(1.9-2.3), and stirring for reaction; S2, evaporating and concentrating the solution obtained in S1 to 1 / 4-1 / 3 of the original volume, cooling the solution to 25-35°C, and filtering to obtain solid disodium hydrogen phosphite; S3, adding disodium hydrogen phosphite seed crystals to the filtrate obtained in S2, cooling the solution to 15-25°C while stirring, and filtering when the crystals no longer increase to obtain disodium hydrogen phosphite; the amount of disodium hydrogen phosphite seed crystals added is 0.5-3% by weight of the phosphorous acid added in S1; the method has the advantages of improving the purity and production efficiency of disodium hydrogen phosphite.

The invention discloses a method for preparing cyclopropanecarboxylic acid by using phosphorus trichloride as a chlorination reagent, and belongs to the technical field of medicines and pesticides, the method comprises the following steps: adding cyclopropanecarboxylic acid into a reactor, starting stirring, heating to the reaction temperature of 40-60 DEG C, introducing nitrogen to carry out nitrogen replacement, carrying out nitrogen sealing in the whole process, starting dropwise adding phosphorus trichloride, controlling the dropwise adding speed, and reacting for 1-2 hours; the temperature of the reaction system is maintained at the reaction temperature, and the fluctuation temperature does not exceed + / -2 DEG C; after the dropwise adding of the phosphorus trichloride is finished, continuously carrying out heat preservation reaction for 0.5-2 hours, and then standing and separating the reaction liquid to obtain an upper layer which is a cyclopropanecarbonyl chloride crude product; and distilling the crude product of cyclopropanecarbonyl chloride to obtain a refined product of cyclopropanecarbonyl chloride. The method provided by the invention solves the problems of low chlorine atom utilization rate, incomplete catalysis of the adopted catalyst, easy generation of impurities, generation of toxic by-products sulfur dioxide and carbon monoxide, great threat to the environment, and three-waste emission in the existing acyl chloride preparation method.

The invention discloses a method for preparing a phosphite positive electrode material, and belongs to the technical field of preparation of phosphite positive electrode materials. The method comprises the following steps: S1, respectively dissolving a phosphorus source, a lithium source or a sodium source and a transition metal source in a solution; s2, an antioxidant is added into the solution, and the solution is mixed after dissolution; s3, transferring the mixed solution into a reaction kettle for hydrothermal reaction; s4, after the hydrothermal reaction is finished, washing and drying the obtained precipitate; and S5, sintering the dried product in the step S4 in an atmosphere, wherein the sintered product is the phosphite positive electrode material. Through the hydrothermal method, the preparation process is simplified, the process steps are reduced, the energy consumption is reduced, various parameters are controllable, the problems of tedious steps and relatively high energy consumption of the current preparation of the battery positive electrode material are solved, and the requirements of high energy density, low cost and high safety are met.

The invention relates to the technical field of preparation of disodium hydrogen phosphate, and discloses a preparation method of disodium hydrogen phosphate, which comprises the following steps: S1, dissolving phosphorous acid and sodium hydroxide in distilled water in an inert gas atmosphere according to a molar ratio of phosphorous acid to sodium hydroxide of 1: (1.9-2.3), and stirring for reaction; s2, evaporating and concentrating the solution obtained in S1 to 1 / 4-1 / 3 of the original volume, cooling to 25-35 DEG C, and filtering to obtain a disodium hydrogen phosphate solid; s3, adding a disodium hydrogen phosphate seed crystal into the filtrate obtained in the step S2, cooling to 15-25 DEG C while stirring, and filtering when crystals are not increased any more to obtain disodium hydrogen phosphate; the adding amount of the disodium hydrogen phosphate seed crystal is 0.5-3% of the weight part of the phosphorous acid added in the S1; the method has the advantage of improving the purity and production efficiency of disodium hydrogen phosphate.

A method of producing lithium difluorophosphate, the method including: a step of obtaining a first raw material mixture by mixing lithium hexafluorophosphate, at least one selected from the group consisting of an oxide of phosphorus (A) and a lithium salt of a phosphoric acid (B), and a hydrocarbon solvent having from 6 to 12 carbon atoms; a step of obtaining a second raw material mixture by removing at least a part of the hydrocarbon solvent contained in the obtained first raw material mixture; and a step of producing a crude product containing lithium difluorophosphate by reacting the second raw material mixture.

This invention belongs to the field of flame retardant materials technology, and specifically relates to a crystalline aluminum phosphite, its preparation method, and its applications. The XRD pattern of the crystalline aluminum phosphite of this invention shows diffraction peaks at 2θ of 12.0, 14.0, 15.0, 15.5, 16.0, 17.5, 20.0, 22.5, 23.5, 29.0, 30.0, 30.5, 31.0, 32.0, 33.0, 36.5, 38.5, and 45.0 ± 0.2°. The crystallization-directing agent of this invention is in a cross-linked state and has high activity. As a crystallization-directing agent, it promotes product growth along the crystallization-directing agent structure, improves the crystal structure of the product, reduces crystal defects, and results in a crystalline aluminum phosphite with high purity and high temperature resistance. Its use in the preparation of plastics gives the plastics good mechanical and flame-retardant properties, meeting the processing requirements of polymer materials with high heat resistance.

This application relates to an organic compound, a perovskite precursor solution, a perovskite film, a perovskite cell, and an electric apparatus. The organic compound includes: a cation M; and an anion Q bonded to the cation M; where M includes one or more of CH3NH3+, CH5N2+, Cs+, and C2H5NH3+; and Q includes one or more of H2POx− and H2NOy−, where x and y are each independently an integer from 2 to 4.

This invention belongs to the field of oxyacid synthesis technology of phosphorus, specifically relating to a method for producing phosphorous acid. The production method includes: (1) adding a metal precursor, organic ligand, reaction promoter, structure directing agent and swelling resistant agent to a pore-forming agent and heating to react, to obtain a mixture; then mixing the mixture with a polymer monomer, crosslinking agent and initiator to obtain an oil phase for later use; mixing a dispersant with water and removing oxygen to obtain an aqueous phase for later use; (2) mixing the oil phase and the aqueous phase to carry out a crosslinking reaction to obtain a crude product; (3) washing, acidifying and vacuum drying the crude product to obtain a porous polymer carrier; (4) after the porous polymer carrier swells in water, adding phosphorus trichloride to it, carrying out a heat preservation reaction, and post-treatment to obtain phosphorous acid. This invention improves the production efficiency of phosphorous acid while ensuring a high yield of phosphorous acid by preparing a porous polymer carrier and using it as a medium for the hydrolysis of phosphorus trichloride to prepare phosphorous acid.

The invention discloses phosphate matrix composite fluorescent powder and a preparation method thereof, belongs to the technical field of solid luminescent materials, and aims to solve the problems that a single phosphate fluorescent material in the prior art is low in luminous efficiency and short in excitation spectrum; the thermal stability of the added organic light-emitting material is poor, and the like. The invention relates to a preparation method of phosphate matrix composite fluorescent powder. The preparation method comprises the following steps: coating a composite inorganic fluorescent material containing divalent europium and ammonium phosphite with modified polylactic acid; benzidine and (3-bromophenyl)-9H-carbazole react and then are matched with iridium trichloride hydrate, and the high-molecular organic fluorescent material is obtained. And self-assembling the high-molecular organic fluorescent material and calixarene to obtain the composite high-molecular fluorescent material. The phosphate matrix composite fluorescent powder prepared by the invention has the advantages of long spectral range and high thermal stability.

To provide: a novel organic ammonium salt which has excellent freezing point lowering function; and a composition which is capable of forming the salt.SOLUTION: An organic ammonium salt according to the present invention contains a cation and an anion; the cation is an ammonium cation that is represented by a formula (I) (wherein each R1 independently represents an organic group having 1 to 22 carbon atoms; each R2 independently represents a hydroxy hydrocarbon group that has one or more hydroxyl groups and a hydrocarbon moiety having 1 to 22 carbon atoms and optionally having an oxygen atom, or the like; and each of l, m and n represents an integer of 0 to 4, with the total of l, m and n being 4); and the anion is a phosphonate ion or a phosphinate ion.SELECTED DRAWING: None

The utility model relates to the technical field of production deacidification, in particular to a phosphorous acid crude product deacidification device with a gas collecting mechanism, which comprises a deacidification reaction kettle, a supporting outer frame is assembled outside the deacidification reaction kettle in a supporting manner, and a gas collecting seat is assembled on the right side of the top of the deacidification reaction kettle. A collecting butt joint seat is integrally arranged at the upper end of the gas collecting seat, a collecting connecting pipe is connected to the upper end of the collecting butt joint seat, a collecting pump is connected to the lower end of the collecting connecting pipe, a gas pumping pipe is connected to the lower end of the collecting pump, a gas collecting tank is assembled below the collecting pump, and the gas pumping pipe is assembled in the gas collecting tank in an inserted mode through a sealing flange. The gas collecting tank is assembled on the outer wall of the right side of the supporting outer frame. According to the reaction kettle, gas generated during operation reaction can be conveniently collected and stored, and the situation that gas spills to affect safety production is not easily caused.

The invention relates to the technical field of chemical intermediates, and relates to C07F, in particular to a preparation method for co-production of acetyl chloride and phosphorous acid as well as a product and application thereof. The preparation method at least comprises the following steps: S1, stirring and cooling acetic acid and a catalyst, dropwise adding phosphorus trichloride, heating to 20-45 DEG C, and reacting for 0.5-6 hours; s2, after the reaction is finished, carrying out negative pressure desolvation to obtain a crude product acetyl chloride, and continuously heating to remove excessive phosphorus trichloride, so as to obtain a crude product phosphorous acid; s3, rectifying the crude product acetyl chloride to obtain an acetyl chloride product; recrystallizing the crude phosphorous acid to obtain a phosphorous acid product; the catalyst comprises at least one of aluminum trichloride, ferric trichloride, titanium tetrachloride, ytterbium trifluoromethanesulfonate and iodine; the mass ratio of the acetic acid to the catalyst is 1: (0-0.003). The method provided by the invention has the characteristics of high conversion rate, high yield, high content, small amount of three wastes, no solvent pollution, simple process, easy industrial preparation of acetyl chloride and the like.

Methods and systems for capturing carbon dioxide and utilizing calcium sulfate to produce useful products are disclosed.

Disclosed are methods and systems for capturing carbon dioxide and utilizing calcium sulfate to generate useful products.

The invention discloses a phosphorus-containing hybrid metal salt compound and a preparation method and application thereof, the phosphorus-containing hybrid metal salt compound and dialkyl phosphinate have good flame-retardant synergy, the flame-retardant efficiency can be improved, and meanwhile, the corrosivity of a dialkyl phosphinate flame retardant can be reduced.

The utility model relates to the field of phosphoric acid extraction equipment, and discloses a sulfuric acid dispersing device for extracting semi-hydrated phosphoric acid, which comprises a reaction tank, a top plate is arranged on the upper end face of the reaction tank, a support is arranged at the center of the upper end face of the top plate, and a motor is fixedly connected to the center of the upper end face of the support. The output end of the motor sequentially penetrates through the support and the upper end face of the top plate and extends into the reaction tank, a stirring rod is fixedly connected to the end, a dispersing structure is arranged on the upper portion of the outer side wall of the stirring rod, and stirring blades are vertically arranged on the lower portions of the centers of the two side walls of the stirring rod. According to the device, the connecting sleeve is limited through the two fixing structures, the height of the connecting sleeve is conveniently adjusted, then the input end of the three-way pipe is clamped through the limiting structure, the height of the connecting sleeve is conveniently adjusted in a matched mode, sulfuric acid is injected through the three-way pipe, and the sulfuric acid drops into the dispersing disc; sulfuric acid is uniformly sprayed into the reaction tank through centrifugal force when the stirring rod rotates, so that the mixing effect is remarkably improved.

The invention relates to the technical field of inorganic phosphorus chemical industry, in particular to a method for preparing phosphorous acid crystals from yellow phosphorus through a one-step method and phosphorous acid crystals. Dispersing agents are dissolved in water and heated, yellow phosphorus is added, stirring and ultrasonic treatment are started after the yellow phosphorus is melted, the stirring rate, the ultrasonic frequency and the temperature are maintained, then catalysts are added into the solution, oxidizing agents are dropwise added, and stirring and ultrasonic treatment are conducted; continuously reacting to obtain a yellow transparent aqueous solution, namely a phosphorous acid aqueous solution; cooling the phosphorous acid aqueous solution to room temperature, filtering, and concentrating at normal pressure to obtain a phosphorous acid concentrated solution; carrying out ultrasonic treatment on the phosphorous acid concentrated solution, cooling to room temperature, scattering phosphorous acid seed crystals, sealing, crystallizing at a set temperature, taking out, and filtering to obtain crystals; and washing the obtained crystal with vaporous water, and drying in a vacuum drying oven to obtain the phosphorous acid crystal. The method solves the problem that phosphorous acid crystals are difficult to obtain in a conventional crystallization mode in the existing method for preparing phosphorous acid by a one-step method of yellow phosphorus.

Provided is a non-aqueous electrolyte solution for a lithium secondary battery containing a lithium salt, an organic solvent and a phosphoric acid-based additive of specific structure. By adding the phosphoric acid-based additive according to an embodiment of the present invention to the electrolyte solution, the lithium secondary battery can significantly improve the high temperature stability.

This application relates to an organic compound, a perovskite precursor solution, a perovskite film, a perovskite cell, and an electric apparatus. The organic compound includes: a cation M; and an anion Q bonded to the cation M; where M includes one or more of CH3NH3+, CH3N2+, Cs+, and C2H5NH3+; and Q includes one or more of H2POx- and H2NOy-, where x and y are each independently an integer from 2 to 4.

The invention discloses a clean production method for co-producing phosphorous acid with ethyl chloride, wherein phosphorus trichloride is mixed with a hydrochloric acid solution for hydrolysis reaction to generate a phosphorous acid solution and gaseous hydrogen chloride; the phosphorous acid solution is vacuum concentrated, crystallized and centrifuged to obtain phosphorous acid; a catalyst is filled in a reaction tower, and the gaseous hydrogen chloride is mixed with gasified ethanol and then introduced into the reaction tower for reaction to obtain ethyl chloride. The invention has a simple process, realizes the co-production of phosphorous acid with ethyl chloride, has low requirements for reaction temperature and reaction time, and has good prospects for promotion and application.

The invention provides a compound antimony phosphite, an antimony phosphite nonlinear optical crystal and a preparation method and application thereof, the chemical formula of the compound is SbH3P2O6, the molecular weight is 282.7, and the compound is prepared by adopting a vacuum packaging method or a room temperature solution method; the chemical formula of the compound of the crystal is SbH3P2O6, the molecular weight is 282.7, the compound belongs to a monoclinic system, the space group is Pc, the cell parameters are as follows: a = 7.6318 (12), b = 5.3723 (9), c = 7.5537 (12), alpha = 90 degrees, beta = 108.154 (6) degrees, gamma = 90 degrees, the unit cell volume is 294.29 (8) 3, the frequency-doubled effect of the crystal is about two times that of KH2PO4 (KDP), the ultraviolet cut-off edge is lower than 204 nm, the crystal is grown by adopting a hydrothermal method, a vacuum packaging method or a room temperature solution method, the chemical stability of the crystal is good, and the crystal is suitable for large-scale production. The short-wavelength nonlinear optical crystal can be applied to an all-solid-state laser as a short-wavelength nonlinear optical crystal.

The present invention belongs to the technical field of chemical production, and specifically relates to a method for preparing phosphorous acid from fatty acyl chloride byproducts. The present invention injects the fatty acyl chloride byproduct into water, the initial temperature of the water is ≤20°C, the temperature of the injection process is <60°C, and a reaction liquid is obtained after the injection is completed; the reaction liquid is subjected to a heat preservation reaction to obtain a heat preservation reaction liquid; the heat preservation reaction liquid is allowed to stand for stratification to obtain a lower layer of clear liquid; the lower layer of clear liquid is subjected to a decolorization treatment to obtain a phosphorous acid solution. In summary, on the one hand, the present invention recovers phosphorous acid from the fatty acyl chloride byproduct, reduces the production cost of fatty acyl chloride, improves the competitiveness of the product, and generates huge economic benefits; on the other hand, it solves the problem that the fatty acyl chloride byproduct cannot be utilized, greatly reduces liquid waste, and recycles phosphorous acid in the acyl chloride byproduct. Finally, the method provided by the present invention has mild reaction conditions, a simple process, and is suitable for wide industrial application.

The present invention relates to a method for producing a composition containing a phosphonate salt by mixing the reaction partners in solid form. The invention also relates to solid compositions A obtainable by said method and to the use of these compositions for combating harmful fungi.The invention moreover relates to compositions B comprising (a) a phosphonate salt of an alkali or earth alkaline metal or of two or more alkali and / or earth alkaline metals, and (b) sulfur and / or urea. In one embodiment, this composition B is solid. In another embodiment, this composition B comprises calcium phosphonate, magnesium phosphonate and sulfur.The invention also relates the use of these compositions A or B for combating harmful fungi.

The invention belongs to the technical field of oxygen-containing acid synthesis of phosphorus, and particularly relates to a phosphorous acid evaporation and concentration process. According to the phosphorous acid evaporation and concentration process, a phosphorous acid crude product is treated by an evaporation and concentration system to obtain a phosphorous acid finished product; wherein the evaporation and concentration system comprises a first-stage falling film evaporator, a second-stage falling film evaporator and a third-stage falling film evaporator which are connected in sequence, auxiliaries are added from the third-stage falling film evaporator, and the auxiliaries comprise polyethylene glycol diamine, N, N-diethyl hydroxylamine and sodium octyl sulfosuccinate. According to the invention, the evaporation and concentration system is designed and the auxiliary agent is supplemented, so that the residual quantity of hydrogen chloride in the phosphorous acid crude product is further reduced, the high-purity phosphorous acid finished product is prepared, and the phosphorous acid finished product can be used in the fields with high purity requirements, such as semiconductor wafer cleaning agents.

The invention provides steam purification equipment for preparing phosphorous acid and a control system thereof, and relates to the technical field of purification equipment, the steam purification equipment comprises a shell, an auxiliary part, a control part and a heating part; two supporting legs are symmetrically welded to the bottom end face of the shell and make contact with the ground, a containing barrel is installed in the shell, and a mounting plate is welded to the right end face of the shell. A mounting seat is mounted on the top end face of the rotating shaft, and nozzles are mounted on the top end face of the mounting seat in a linear array shape and located below the containing barrel; the rotating shaft is of a hollow structure and communicates with the mounting base and the spray head; the rotating shaft is rotationally connected with an air inlet pipe, the air inlet pipe communicates with the rotating shaft, and in the using process, when the rotating shaft rotates, uniform heating of the containing barrel can be achieved through a spray head. The problems that according to an existing device, after a worker touches purification equipment, the worker is prone to being scalded, and the condensation effect is reduced due to the fact that the airflow flowing speed is high during condensation are solved.

The invention discloses a green synthesis process of anhydrous sodium phosphite capable of being used as an antioxidant, and relates to the technical field of chemical engineering, and the green synthesis process comprises the following steps: firstly, adding anhydrous phosphorous acid and methanol into a reactor to obtain an anhydrous phosphorous acid-methanol solution; then slowly dropwise adding a sodium methoxide solution into the anhydrous phosphorous acid-methanol solution, stopping dropwise adding the sodium methoxide solution when the pH value of the solution in the reactor is 6-9, and cooling the solution in the reactor to 20 DEG C to obtain a reaction product; separating the reaction product through a solid-liquid separation device to obtain a filtrate and a filter cake; distilling and recovering the filtrate to obtain recovered methanol; carrying out vacuum drying on the filter cake to obtain anhydrous sodium phosphite; according to the green synthesis process of the anhydrous sodium phosphite capable of being used as the antioxidant, by strictly controlling reaction conditions, generation of by-products is effectively reduced, the output of wastes is reduced, and environmental pollution is relieved; meanwhile, methanol is recycled, the green chemistry concept is met, and sustainable development of the chemical industry is facilitated.

The invention discloses a preparation method and application of surface-modified aluminum phosphite, belongs to the field of flame-retardant synergists, and aims to solve the problem of high probability of moisture absorption and caking in the storage process. After the reaction for synthesizing aluminum phosphite is completed, the pH value is adjusted to be neutral, a cationic surfactant is added, and the surface-modified aluminum phosphite is prepared. And carrying out suction filtration, washing and drying on the suspension to obtain powder, adding an anti-caking agent into the powder for dispersion, and finally screening to obtain the surface-modified aluminum phosphite flame-retardant material. The method has the advantages of simple operation, low production cost and easy batch production, solves the problem of low screening passing rate caused by easy moisture absorption and caking of the product after drying or in the storage process, increases the product yield, prolongs the storage and use period of the product, and obviously improves the flame retardant property of the flame retardant prepared from the product.

The application discloses a kind of nitrogen-doped sodium ion battery polyanion positive electrode materials and preparation method thereof, by chromium doping or replacement nitrogen triphosphoric polymeric vanadium trisodium polyanion positive electrode material, citric acid is dissolved with transition metal in deionized water, V source, Cr source, ascorbic acid and transition metal, Na source and P source are added respectively, while the deionized water solution of 12wt% polyvinylpyrrolidone dissolved, urea is added to mixed solution and is magnetically stirred, evaporates by water, drying, grinding, is formed into tablet by mould pressing;With urea grinding and tabletting by mould are together to the test tube and are vacuum sealed, and are placed in muffle furnace and are kept at high temperature, then are taken out and are naturally cooled to room temperature, obtain the positive electrode material.The application does not need to continuously pass in ammonia in preparation process, and reduces the V source consumption, significantly reduces the manufacturing cost is low and manufacturing equipment is simple, improves safety, and is convenient to implement;The cycle of the material prepared is good, and the specific capacity is high.