24results about "Hypophosphorous acid" patented technology

The invention provides a treatment process of a byproduct sodium hypophosphite in a phosphorane preparation process, and aims to efficiently remove impurities and prepare a high-purity hypophosphorous acid product. The process comprises the following steps: carrying out small-volume sampling on reaction mother liquor, introducing carbon dioxide gas, and drawing an acidification curve of pH and conductivity; according to the plateau phase of an acidification curve, the CO2 flow rate and the pH value are controlled, step-by-step selective precipitation of impurities such as PO4 < 3->, HPO4 < 2->, Fe < 3 + >, AsO4 < 3-> and S < 2-> is achieved, and loss of a target component H2PO4 < 2-> is avoided; calcium hydroxide turbid liquid is introduced at a proper time to supplement Ca < 2 + > and promote efficient removal of phosphorus, arsenic and sulfur impurities; and subsequently removing excessive Na < + > and Ca < 2 + > through cation exchange, and concentrating to obtain a hypophosphorous acid product with the purity of more than or equal to 99.5%. The method is accurate in process control, thorough in impurity removal and good in repeatability and industrial adaptability, and the resource utilization efficiency of by-products and the added value of products are remarkably improved.

The application discloses a kind of synthesis methods of high-purity electronic grade sodium hypophosphite, dilute phosphine gas is passed into to the mixed solution of sodium hypochlorite and sodium hydroxide that has been pre-cooled with sufficient stirring, and sodium hydroxide is added to carry out reaction;After reaction is completed, filtration, concentration, crystallization, separation are carried out, and the obtained product is purified by resin to obtain high-purity electronic grade sodium hypophosphite product.Compared with the traditional "yellow phosphorus-lime-soda" oxidation-reduction method for preparing industrial grade product and then preparing high-purity electronic grade sodium hypophosphite, the product purification difficulty of the application is low, by using 7N grade ultra-high purity phosphine without any metal impurities, the problem that arsenic, silicon, germanium, nickel, chromium and other metal impurities cannot be completely removed by traditional process can be effectively solved.In addition, the application also has the advantages of effectively solving the problem of three wastes, high recycling rate of by-products, high economy and the like.

The invention provides a method for preparing calcium-based nano particles by a reversed-phase microemulsion method, an organic calcium salt nano material and application of the organic calcium salt nano material as a nano drug, and belongs to the field of biomedical nano materials. The calcium-based nanoparticles can be formed by reacting calcium dodecyl benzene sulfonate with ammonium salt of corresponding ions or a hydroxyl-containing organic matter aqueous solution; the preparation method of the calcium-based nanoparticles has certain universality, and nano-material drugs including calcium succinate, calcium hypophosphite, calcium gluconate, calcium formate, calcium citrate and the like are successfully synthesized. The synthesis method is simple, mild in reaction condition, environment-friendly, high in repeatability, capable of realizing batch preparation and low in raw material cost. When the calcium salt nano-drug such as calcium succinate enters tumor cells through endocytosis, a large number of ions are brought into the cells, and suddenly excessive ions can cause osmotic pressure and homeostasis imbalance in the cells, activate a pyroptosis pathway of the cells and induce death of immunogenic cells.

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.

The present invention relates to a hypophosphite flame retardant and a method for producing the same, and more particularly to a method for producing a particle-size-adjusted hypophosphite flame retardant by supplying a divalent to tetravalent metal salt through a nozzle. The particle-size-adjusted hypophosphite flame retardant of the present invention can impart excellent flame retardancy to adhesive compositions that require a thin thickness and flame-retardant compositions that require heat resistance, without impairing the physical properties of the product.

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 present application relates to a kind of methods for preparing nanoscale uniform spherical aluminum hypophosphite based on hydrothermal method, the present application uses aluminum chloride six-water and sodium hypophosphite monohydrate as raw material, by adding ethylene glycol, the product morphology is adjusted under lower temperature hydrothermal route, the spherical structure with regular morphology and relatively smooth surface is obtained, preparation operation is simple, synthesis step is simple, raw material cost is low, process can be completed under lower temperature, is suitable for large-scale industrialization.By introducing ethylene glycol, the supersaturation of the system is controlled to affect the generation of crystal nucleus, the solvent viscosity is increased, which is beneficial to the growth of crystal nucleus diffusion control, further uniformizes the size of product, and forms uniform spherical particles.The preparation process of the present application is simple, the aluminum hypophosphite product synthesized has excellent morphology and good dispersibility, and is helpful for subsequent modification of aluminum hypophosphite.

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 method for producing hypophosphorous acid, comprising the following steps: 1) adding an ether-based organic solvent and distilled water into a reaction kettle, adding yellow phosphorus under a nitrogen flow, heating at normal pressure to melt the yellow phosphorus, and stirring at high speed to emulsify the yellow phosphorus; 2) dropwise adding a reactant into the reaction kettle to react with the yellow phosphorus until the solution is stirred into a transparent solution, and distilling the transparent solution product under reduced pressure to remove the solvent and the reactant to produce a crude product salt; 3) acidifying the crude product salt with hydrochloric acid to a pH of 2-3, and then extracting with n-butanol and water, and distilling off the organic phase to obtain hypophosphorous acid. The method uses an excess of water-soluble amine to change the disproportionation reaction of yellow phosphorus under alkaline conditions. Compared with traditional alkaline methods and ion exchange resin methods, the method can achieve recycling of raw materials, reduce costs, and is environmentally friendly.

The present invention relates to a method for producing a compound comprising at least one of hydrogen or oxygen. The method comprises providing water and a first substance, producing a mixture comprising water and gas bubbles comprising the first substance, reducing the diameter of the gas bubbles comprising the first substance, decomposing a portion of the water, and synthesizing a compound comprising at least one of hydrogen or oxygen from at least the decomposed water and the first substance. The invention also relates to an apparatus for producing a compound comprising at least one of hydrogen or oxygen.

The invention relates to a method for producing a compound comprising at least one of hydrogen or oxygen. The method comprises providing water and a first substance, producing a mixture comprising the water and bubbles comprising the first substance, decreasing diameter of bubbles comprising the first substance, decomposing a part of the water, and composing a compound at least from the decomposed water and the first substance, and the compound comprising at least one of hydrogen or oxygen. The invention further relates to apparatus for producing a compound comprising at least one of hydrogen or oxygen.

The invention relates to the technical field of hypophosphite synthesis, and provides a hypophosphite synthesis device and method.The hypophosphite synthesis device comprises a reaction tower body and further comprises a three-stage reaction mechanism, a liquid separation mechanism, a reaction prolonging mechanism, an anti-scaling mechanism and a bottom discharging mechanism; the liquid separation mechanism is mounted in the reaction tower body, the liquid separation mechanism is matched with the three-stage reaction mechanism and is used for uniformly distributing product liquid at a reaction position, the reaction extension mechanism is mounted in the reaction tower body and is used for delaying the time of a reaction product entering a next-stage reaction, and the anti-scaling mechanism is mounted in the reaction extension mechanism and is used for washing blocked yellow phosphorus particles. By means of the technical scheme, the problems that in the prior art, the maintenance process of a reaction tower is tedious, the tower needs to be disassembled for cleaning internal components, and the production efficiency is greatly influenced by frequent shutdown inspection and maintenance are solved.

The invention discloses a continuous solid-liquid separation and recovery method and system for sodium hypophosphite. The method comprises the following steps: conveying sodium hypophosphite mixed slurry into a hydrocyclone group for pre-concentration; wherein concentrated slurry with high solid content is discharged from an underflow port of the first-stage cyclone, overflow liquid of the concentrated slurry enters the second-stage cyclone for secondary separation, slurry with low solid content is discharged from an underflow port of the second-stage cyclone, and clear liquid is discharged from an overflow port of the second-stage cyclone to serve as finished product mother liquor; respectively, simultaneously and continuously conveying the underflow concentrated slurry and the underflow slurry to different feeding points in a horizontal spiral discharge sedimentation centrifuge; in a centrifugal machine, one or more strands of washing liquid are adopted to carry out continuous countercurrent washing on a solid-phase filter cake which is being conveyed, so that a diluted sodium hypophosphite solution generated by washing and separated mother liquid are converged in a rotary drum in a partitioned manner. The full-closed and continuous technological process is adopted, and the defects that traditional intermittent operation is low in efficiency, high in labor intensity and prone to product loss are effectively overcome.

The application discloses a preparation method of modified superfine sodium hypophosphite and belongs to the technical field of sodium hypophosphite preparation. The preparation method of the modified superfine sodium hypophosphite comprises the following steps: step (1), mixing quicklime and water to prepare lime milk, then adding a sodium hydroxide solution into a reaction kettle containing the lime milk, uniformly mixing and obtaining a mixed solution; step (2), heating the mixed solution while introducing nitrogen, adding yellow phosphorus into the reaction kettle, heating and reacting to obtain a reaction solution, collecting generated gas through a pipeline during the reaction process, and treating the gas; and step (3), adding a modified surfactant into the reaction solution, stirring and mixing, filtering, removing calcium, adjusting pH, concentrating, crystallizing, centrifuging, drying and obtaining the modified superfine sodium hypophosphite. The prepared sodium hypophosphite has small and uniform particle size, and the content of phosphine gas in the preparation process is low.

The utility model discloses a sodium hypophosphite acid regulation automatic control system which comprises a plurality of acid regulation kettles (12) connected in parallel, a feed port of each acid regulation kettle (12) is connected with a feed pipeline (3) through an acid regulation kettle feed valve (5), and an air inlet of each acid regulation kettle (12) is connected with a compressed air pipeline (10) through a compressed air feed valve (11). An acid inlet of each acid adjusting kettle (12) is connected with a hypophosphorous acid feeding pipeline (7) through a hypophosphorous acid feeding valve (9), a discharging port of each acid adjusting kettle (12) is connected with an acid adjusting kettle discharging pump (16) in parallel through an acid adjusting kettle discharging valve (15), and all operations can be automatically controlled by a DCS computer, so that interference of manual control is reduced, control is accurate, and the automation degree of the device is greatly improved.

The invention discloses a low-consumption and environment-friendly hypophosphite purification process, and belongs to the technical field of hypophosphite purification. Comprising the following steps: S1, heating and dissolving hypophosphite raw material powder and ultrapure water according to a certain proportion, mixing, and filtering by adopting a microfiltration membrane to remove particulate matters; s2, adding a proper amount of chelating agent into the filtrate of the hypophosphite, conveying the filtrate into a dynamic crystallization kettle, and slowly cooling and crystallizing; s3, separating hypophosphite mother liquor from crystals, and drying the hypophosphite crystals; and S4, purifying the hypophosphite mother liquor by using macroporous adsorption resin so that the hypophosphite mother liquor is used for the crystallization process of a new batch of materials again.

The application discloses a device for preparing electronic-grade sodium hypophosphite dearsenicated salt sodium salt, and belongs to the technical field of electronic chemical preparation. The device realizes the efficient dispersion of phosphine gas into micron-sized bubbles through a membrane dispersion reaction system, realizes the full and stable reaction of the phosphine gas with sodium hypochlorite solution, guarantees the high efficiency and uniformity of the main synthesis reaction from the source, and provides a composition-stable crude product liquid for subsequent continuous purification. Through a bypass arsenic removal unit integrated in a buffer adjustment system, the on-line circulation oxidation-precipitation-separation of arsenic impurities is realized without interrupting the main synthesis process, and the problem of the interruption of the synthesis route caused by the intermittent arsenic removal in the traditional process is solved. By arranging yellow phosphorus storage tanks in parallel and alternately working, the continuous and stable supply of the raw material yellow phosphorus to the phosphine reaction kettle is realized. The device ensures the long-term continuous and stable operation of the synthesis route and the high consistency of product batches, and is particularly suitable for the large-scale continuous production of electronic-grade sodium hypophosphite.

The invention discloses a preparation method and flame-retardant application of hypophosphorous acid, and relates to the technical field of flame retardants. The preparation method comprises the following steps: adding a hypophosphorous acid aqueous solution into a kneading machine, adding water for dilution under a stirring condition, then adding guanidine carbonate, closing a cover under a heating condition, stirring and reacting for 0.8-1.2 hours, condensing, refluxing and evaporating water, continuing to react for 1.5-2.5 hours, leading out generated excessive water, and finally drying in vacuum to finish the preparation. The invention also discloses application of guanidine hypophosphite as a flame retardant. According to the invention, high-yield preparation of guanidine hypophosphite is realized by regulating and controlling reaction conditions, the prepared guanidine hypophosphite is relatively high in water solubility, and meanwhile, the flame retardant efficiency is remarkably superior to that of flame retardant products of the same type, so that the preparation method has relatively high application value.

The invention relates to a preparation method and application of hypophosphorous acid double salt, and the preparation method comprises the following steps: I, adding water and various metal salts into an ultrasonic grinding reactor, and starting the ultrasonic grinding reactor to obtain metal salt slurry; iI, adding sodium hypophosphite and water into a reaction kettle for dissolving and clarifying, heating to 70-90 DEG C, adding the first batch of metal salt slurry, uniformly stirring, adding the sol, and continuously stirring and reacting for 1-2 hours; and III, after the reaction is completed, heating to 90-110 DEG C, adding a second batch of metal salt slurry, regulating the pH value of the system by using a pH buffer reagent, controlling the pH value to be 4.0-8.0, and stirring to react for 1-3 hours. According to the invention, the problems in the prior art that particles formed by agglomeration of hypophosphite crystals produced by an inorganic double decomposition synthesis method are irregular and large in particle size, so that the product is large in particle size and wide in distribution, and the flame retardance, the mechanical property and the like of the product are unfavorably influenced are solved.

The invention provides a method for preparing phosphorane by pyrolyzing sodium hypophosphite based on raw material pretreatment, the pretreatment method comprises the following steps: carrying out mechanical activation and dry granulation on sodium hypophosphite, and firstly, carrying out intermittent ball milling treatment on sodium hypophosphite powder in an inert atmosphere to form primary activated sodium hypophosphite; and then granulating by the steps of tabletting, crushing, screening and the like to obtain the granular sodium hypophosphite with the particle size of 0.8-1.2 mm, the porosity of 20-35% and the bulk density of 0.75-0.95 g / cm < 3 >. According to the pyrolysis method, on the basis of pretreatment, staged heating is carried out, a pyrolysis reaction is carried out under inert gas protection, the product phosphine is subjected to multi-stage condensation and low-temperature rectification purification, and then high-purity phosphine gas is obtained, the pyrolysis starting temperature can be remarkably reduced, the phosphine release rate and yield are increased, side reactions and impurity entrainment are reduced, and the method is suitable for industrial production. The method has the advantages of high raw material utilization rate, centralized and controllable pyrolysis reaction, high product purity and the like, and is suitable for efficient and safe preparation of phosphorane.

The application discloses a kind of green treatment methods of nickel-phosphorus chemical plating aging liquid.The method is first reacted with aluminium sulfate and phosphite and hypophosphorous acid in nickel-phosphorus chemical plating aging liquid, respectively generate insoluble in water aluminium phosphite and aluminium hypophosphite, solid-liquid separation and washing solid while hot, recycle solid as the mixture of aluminium phosphite and aluminium hypophosphorous acid, then liquid is frozen so that sodium sulfate is solid, solid-liquid separation while cold, recycle solid sodium sulfate decahydrate, i.e., mirabilite, recycle liquid is used as plating bath evaporation makeup liquid, to make up the evaporation loss of plating solution in plating process.The treatment method of nickel-phosphorus chemical plating aging liquid of the application has little influence on the composition and content of various additives in plating solution, resources are recycled and utilized, simple operation, low cost, environment-friendly.

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 utility model discloses a sodium hypophosphite causticizing device. The sodium hypophosphite causticizing device comprises a stock bin, a glove box, a conveyor, a feeding assembly and a causticizing kettle, the stock bin is located at one end of a feeding port of the conveyor. One end of the glove box is connected with a discharging port of the stock bin, and the other end of the glove box is connected with a feeding port of the conveyor. The feeding assembly is arranged above the causticizing kettle, the top end of the feeding assembly is connected with a discharge port of the powder conveyor, and the bottom end of the feeding assembly is connected with a feed port of the causticizing kettle. Through the design of the stock bin, the glove box, the conveyor, the feeding assembly and the causticizing kettle and the formation of the closed feeding space, lime dust can be effectively prevented from entering the atmosphere in the feeding process, environmental pollution is effectively prevented, and the causticizing device is high in practicability.

The present application relates to organic compounds, perovskite precursor solutions, perovskite films, perovskite batteries and power consumption devices, the organic compounds comprising a cation M and an anion Q associated with the cation M, wherein M is CH3NH3 + , CH5N2 + , Cs + and C2H5NH3 + and Q is HPO x - and H2NO y - wherein x and y are each independently an integer of 2 to 4.