25results about "Antimonates/antimonites" patented technology

The present application relates to the technical field of anode slime treatment, and discloses a method for removing antimony and tellurium from anode slime by multi-stage pressurization and chlorine-free process, which comprises the following steps: S1, anode slime pretreatment, S2, multi-stage pressurization treatment, S3, separation of antimony and tellurium from the anode slime, S4, preparation of sodium antimonate, S5, tail gas treatment, S6, waste liquid treatment, S7, post-treatment. The method is characterized by the following: one-stage pressurized thiourea transformation is used for deep copper removal, and two-stage pressurized sulfuration is used for chlorine-free antimony and tellurium removal. The process flow does not involve chlorine-containing substances, and the pressurized leaching of alkaline medium does not produce substances with strong corrosivity, thereby reducing the damage to the equipment. In the process of removing antimony and tellurium, the harmful substances generated during the reaction can be treated by waste gas and waste liquid treatment, and the by-products, precipitates, incompletely removed heavy metal ions, trace pollutants and the like in the tail liquid can be removed or converted into harmless substances, so that the tail liquid meets the discharge standard and the environmental pollution caused by the tail liquid discharge is reduced.

The invention relates to the technical field of preparation of inorganic chemical materials, and discloses a controlled synthesis process of a high-temperature-resistant sodium antimonate crystal structure, which comprises the following steps: dispersing antimony trioxide in a sodium hydroxide aqueous solution with the initial concentration of 6.5-8.0 mol / L, and adding sodium metaaluminate as a lattice directing agent to prepare a precursor base solution; heating the base solution, maintaining turbulent stirring, executing double-flow-path synchronous compensation, dropwise adding a hydrogen peroxide aqueous solution and synchronously adding sodium hydroxide; the method comprises the following steps: dynamically setting a coupling relationship among an alkali supplementing rate, an oxidation rate and a reaction stoichiometric ratio, counteracting a dilution effect of water generated by reaction and solvent water in real time, and maintaining the concentration of free sodium hydroxide in a mother solution in the whole reaction process at 6.0 mol / L or above until a reaction endpoint is reached. The path of lattice interstitial water or surface hydroxyl is blocked, anhydrous sodium antimonate without crystal water removal steps in the whole temperature range is prepared, and the foaming problem in high-temperature processing is solved.

The present application relates to the field of nonferrous metallurgy, and provides a method for preparing high-quality sodium pyroantimonate by ultrasonic strengthening, comprising the following steps: preparing a mixed solution with the concentration of sodium hydroxide being 200-400 g / L and the concentration of an additive being 10-40 g / L; the additive is potassium hydroxide and / or glycerol; adding antimony oxide into the mixed solution at a proportion of 150-250 kg / m 3 , and heating and performing ultrasonic treatment to obtain a mixed slurry; adding hydrogen peroxide into the mixed slurry, continuing to react for 10-120 min after the hydrogen peroxide is completely added, then performing liquid-solid separation to obtain a solid product; drying the solid product after washing to obtain a sodium pyroantimonate product. The essence of the present application is that the oxidation diffusion process is strengthened by using ultrasonic waves and an additive, and the high-quality sodium pyroantimonate product is prepared by the combined action. The sodium pyroantimonate product prepared by the method has the advantages of good quality, low consumption of oxidizing agent, stable technical indexes, etc.

This invention discloses a composite modified lithium manganese oxide cathode material, its preparation method, and its applications, belonging to the field of cathode material technology. The structural formula of the composite modified lithium manganese oxide cathode material is: LiX a O b @LiYO2 / LiMn2O4, comprising: a core composed of LiYO2 and LiMn2O4, and LiX coating at least a portion of the surface of the core. a O b The coating layer; wherein: LiMn2O4 has a porous structure, and LiYO2 fills the channels of LiMn2O4. The cathode material in this invention uses lithium manganese oxide as a matrix, with LiYO2 filling the channels of the matrix, and LiX coated on the surface of the matrix. a O b Filling the pores with LiYO2 can reduce the Jahn-Teller effect of lithium manganese oxide without affecting the specific capacity of the cathode material. Moreover, LiYO2 can accelerate the lithium-ion diffusion rate, thereby improving the rate performance of the material.

The utility model discloses a sodium antimonate preparation device and a screening mechanism thereof. The sodium antimonate preparation device comprises a reaction kettle, a sodium hydroxide storage tank, a powder conveying mechanism, a hydrogen peroxide storage tank, a soft water storage tank, a centrifugal machine, a filtrate storage tank, a drying machine and a stockpiling warehouse, the powder conveying mechanism, the sodium hydroxide storage tank, the hydrogen peroxide storage tank and the soft water storage tank are used for supplying raw materials into the reaction kettle; the raw materials are conveyed to the centrifugal machine after reaction in the reaction kettle; liquid separated by the centrifugal machine is output to a filtrate storage tank, and formed solid is output to a drying machine and dried by the drying machine; an evaporator is arranged in the filtrate storage tank, and the filtrate is output to the reaction kettle after being heated, evaporated and concentrated by the evaporator. The raw materials in the filtrate are used again for reaction, so that the utilization rate of the raw materials is improved. And by arranging the screening mechanism, unqualified sodium antimonate is removed. And packaging the qualified sodium antimonate for sale.

The invention discloses a method for deeply removing arsenic from sodium antimonate. The method comprises the following steps: retaining a low-arsenic sodium antimonate filter cake obtained by arsenic removal treatment through a leaching-oxidation precipitation method in situ in a filter press; a composite reagent solution is introduced into the closed filter press, soaking and reaction are carried out on the low-arsenic sodium antimonate filter cake, liquid obtained after sulfuration and alkali washing is discharged, a wet sodium antimonate product is obtained, and the composite reagent solution is a mixed solution containing a sulfuration reagent and NaOH; the wet sodium antimonate product is circularly washed with water and dried, and a sodium antimonate product is obtained; in the sodium antimonate product, the content of arsenic is not more than 0.001%. According to the method, the purpose of deeply removing arsenic from the sodium antimonate material with low arsenic content (As2O3lt; 0.05%) is achieved by optimizing the process parameters such as the proportion, the concentration and the temperature of a deep washing reagent.

Disclosed in the present invention is a preparation method for a surface plasmon enhanced Mn4+-doped double perovskite fluorescent powder, which preparation method comprises: S1, selecting specific A, B' and B'' source compounds, mixing same according to a stoichiometric ratio, adding zirconium oxide balls into a ball milling tank, subjecting the mixture to planetary ball milling for 3-8 hours, then placing the mixture into an alumina crucible, sintering same at 900-1300°C for 6-15 hours to obtain a matrix, cooling the matrix, and subjecting same to a particle size treatment and XRD detection; S2, selecting an Mn4+-containing compound, and subjecting same having a concentration of 0.1-5 mol% and the matrix to ball milling for 2-6 hours; and S3, subjecting a metal salt solution and the material obtained in the previous step to an ultrasonic treatment, so as to achieve a metal nano treatment. The luminous efficiency of the fluorescent powder of the present invention is significantly improved; the intensity can be improved by 30-50% compared with that of a traditional fluorescent powder; and color regulation and control are accurate, such that multicolor fluorescence emission can be achieved. The color saturation and luminous efficiency can be improved when the fluorescent powder is applied to a display technology; the color rendering index and luminous efficiency can be improved when the fluorescent powder is used for illumination; and the anti-counterfeiting effect in the anti-counterfeiting field is enhanced. In addition, the fluorescent powder has good chemical stability, and the preparation thereof is easy to control, which are beneficial for industrial production and multi-field application expansion.

This invention relates to the field of inorganic fine chemical material preparation technology, and discloses a method for purifying electronic-grade sodium metaantimonate with low impurity content. The method includes: dissolving antimony trioxide in sodium hydroxide solution and cooling to a first reaction temperature after impurity removal; adding sodium gluconate to construct a coordination metastable system containing a pentavalent antimony precursor; atomizing and dropping hydrogen peroxide to complete the oxidation reaction while maintaining the homogeneous system without precipitation; heating to a second reaction temperature to dissociate the coordination system and induce controlled crystal precipitation; and obtaining the product after separation, washing, and drying. This invention completely decouples the oxidation reaction and crystallization process on the time axis through chemical means, and achieves lattice-level deep self-purification by using a thermally induced dissociation mechanism while suppressing explosive nucleation. The obtained sodium metaantimonate has extremely high purity and a regular cubic crystal morphology.

The invention discloses a method for obtaining a sodium antimonate product based on two-stage circulating leaching, which comprises the following steps: primary sulfuration leaching: adding a sulfurizing agent into an antimony-containing material I under an alkaline condition, and carrying out primary sulfuration leaching to obtain antimony leaching liquid I and antimony leaching slag I; the antimony-containing material II is mixed with the antimony leaching liquid I under the alkaline condition, double-stage leaching is conducted, and double-stage antimony leaching liquid and double-stage antimony leaching slag are obtained; a vulcanizing agent is added into the double-stage antimony leaching slag under the alkaline condition, circulating vulcanization leaching is carried out, antimony leaching slag II and antimony leaching liquid II are obtained, and the antimony leaching liquid II is returned to double-stage leaching for double-stage leaching; oxidation antimony precipitation: mixing the two-stage antimony leaching liquid with an oxidizing agent, and carrying out oxidation reaction to obtain a sodium antimonate product. According to the method, gold leaching can be effectively inhibited without adding a complex inhibitor, meanwhile, gold is enriched in the antimony leaching slag to be recycled, the gold recovery rate can reach 99.6% or above, and the gold content in the sodium antimonate product can be reduced to 0.5 g / t or below.

The invention discloses various low-cost zinc antimonate-based conductive powder and a preparation method thereof, Zn and Sb elements rich in earth crust are used as raw materials, the forbidden band width, the carrier concentration and the mobility of the raw materials are regulated and controlled through doping modification, the high-purity conductive powder is prepared by combining a co-precipitation method and a low-temperature sintering process, and the chemical formula of the high-purity conductive powder is Zn0. 92In0. 08Sb2O6, Zn0. 92Ge0. 08Sb2O6, Zn0. 92Al0. 08Sb2O6 or Zn0. 92Sn0. 08Sb2O6. The method has the advantages of simple equipment, low cost, easiness in control of doping concentration and the like.

The invention provides a method for treating excessive halogen in an ionic photoacid generator, which comprises the following steps: adding a crude product of the ionic photoacid generator to be treated into a reactor, adding a solvent, stirring, then adding a sulfate reagent, reacting, then adding an anion raw material, continuing reacting, and after the reaction is completed, carrying out post-treatment to obtain the excessive halogen in the ionic photoacid generator. The ionic photoacid generator with qualified halogen content is obtained. The halogen content is less than or equal to 10 ppm. And the sulfate reagent is dimethyl sulfate, diethyl sulfate, dipropyl sulfate or dibutyl sulfate. The method for treating the residual halogen in the ionic photoacid generator is mild in reaction condition, simple in technological process, environment-friendly and high in yield, and can be widely applied to preparation of iodonium salt and sulfonium salt photoacid generators.

The invention relates to the technical field of inorganic fine chemical engineering, and discloses a synthesis method of a superfine sodium antimonate flame retardant for engineering plastics, which comprises the following steps: dissolving antimony trioxide, adding sodium gluconate, and stirring at a constant temperature of 43-47 DEG C to prepare a coordination equilibrium precursor solution; pumping the precursor solution and the hydrogen peroxide solution into a three-stage pipeline type high-shear dispersion machine, and controlling the gap between a stator and a rotor to be 0.2-0.3 mm and the rotating speed to be 4000-4500 rpm for reaction; according to the preparation method disclosed by the invention, a chemical coordination potential barrier is constructed by virtue of constant-temperature aging so as to delay a reaction induction period, coordination equilibrium is broken by virtue of mechanical energy dissipation of a high-shear field, nucleation is instantaneously initiated, and the problem that an oxidation reaction rate is mismatched with a micro-mixing rate is solved; the narrowing of the particle size distribution and the regularization of the morphology of the product are realized.

The application discloses a method for removing copper from sodium antimonate at low temperature and at high speed, and the method comprises the following steps: under the conditions of negative pressure, microwave heating and stirring, removing copper from sodium antimonate, a water solvent and a composite copper removal reagent; after the reaction is completed, solid-liquid separation is performed; the obtained liquid part is a reaction mother liquor, and the obtained solid part is copper-removed sodium antimonate; and the copper removal substance in the composite copper removal reagent is an ammonium source substance. The method has the advantages of low reaction temperature, short reaction time, fast reaction speed, energy saving and environmental protection, good copper removal effect, high product yield, and the like. The obtained sodium antimonate product can meet the requirements of various glass fining agents and decoloring agents; the method reduces the requirement for copper in raw materials in the preparation of sodium antimonate, expands the source of the sodium antimonate raw material, reduces the cost of the raw material, and thus reduces the production cost of the sodium antimonate product.

The utility model discloses efficient sodium antimonate production equipment. The efficient sodium antimonate production equipment comprises a supporting seat, a rotary switching disc and a function partitioning seat, a drainage cavity, a drying cavity and a recovery cavity are formed in the supporting seat in a penetrating manner; the rotary switching disc is mounted between the supporting seat and the function partition seat through a slewing bearing, a material groove is formed in the rotary switching disc, a filter screen is arranged at the bottom end of the material groove, and a rotary driving part is connected to the exterior of the rotary switching disc; a material injection cavity, a cleaning cavity, a drying cavity and a material collecting cavity are formed in the function partition base in the length direction of the function partition base in a penetrating mode, and the cleaning cavity, the drying cavity and the material collecting cavity are coaxially arranged with the drainage cavity, the drying cavity and the recycling cavity correspondingly. According to the sodium antimonate continuous production device, the supporting base and the function partition base are in butt joint through rotation of the rotary switching disc, then feeding, cleaning, drying and recycling of sodium antimonate are sequentially achieved, continuous production of the sodium antimonate is achieved, the production efficiency of the sodium antimonate is greatly improved, and the sodium antimonate continuous production device has the advantages of being simple in structure, efficient and convenient to use.

The utility model relates to the technical field of sodium pyroantimonate production, and discloses a reaction kettle for sodium pyroantimonate production, which comprises a kettle body, a stirring assembly is arranged in an inner cavity of the kettle body, the stirring assembly comprises a motor, an output shaft of the motor is fixedly connected with a transmission rod, and two sides of the transmission rod are fixedly connected with stirring rods. According to the sodium pyroantimonate production device, mixing and stirring can be performed during sodium pyroantimonate production by arranging the stirring assembly, sodium pyroantimonate particles can be ground and processed before stirring, so that the sodium pyroantimonate particles can be ground into powder and can better react with a solution, and external air can be blown to the aeration plate by arranging the pneumatic assembly, so that the sodium pyroantimonate production device can be used for producing sodium pyroantimonate. According to the sodium pyroantimonate reaction kettle, the solution is turned under the operation of the bubbles, so that the reaction time of the sodium pyroantimonate and the solution can be shortened, air entering the kettle body can be filtered through the arrangement of the filtering assembly, and pollution caused by external impurities to the sodium pyroantimonate during production is avoided.

The disclosure relates to a method of recycling a battery comprising flour-containing electrolyte salts. These salts may therefore undergo thermal hydrolysis to form HF, which is problematic as heating is needed for efficient removal of liquids. This disclosure aims to solve the problem by adding a treatment step prior to drying that serves to convert the fluorine-containing electrolyte salts into derivatives, which are not prone to thermal degradation. The present disclosure therefore offers a safe approach to recycle batteries comprising flour-containing electrolyte salts.

The invention relates to the technical field of inorganic chemical synthesis, and discloses a preparation method of particle-size-controllable high-end flame-retardant sodium pyroantimonate, which comprises the following steps: completely dissolving antimony trioxide in a sodium hydroxide solution, and carrying out hot filtration to construct a homogeneous metastable state precursor without solid phase residue; excessive oxidant and seed crystal are preset in the base solution, and an oxidant-rich bearing phase is established; reverse continuous feeding of a precursor into an undertaking phase is strictly controlled, the injection rate of antimonite ions and the surface area of a seed crystal are dynamically matched in real time under the condition that excessive strong oxidation potential energy of a peroxidant is maintained in the whole process, and the reaction is carried out in a dynamic metastable region for inhibiting secondary nucleation until feeding is finished; according to the preparation method disclosed by the invention, a homogeneous precursor is constructed and reverse lean solute dynamic locking is implemented, so that solid-liquid interface hot spots and explosive nucleation caused by forward charging are eliminated, and monodispersity of particle size distribution of sodium pyroantimonate and high regularity of crystal morphology are realized.

The invention relates to the technical field of luminescent materials, in particular to a rare earth halide perovskite scintillator and a preparation method and application thereof. The preparation method comprises the following steps: mixing the raw materials according to the chemical formula of the rare earth halide perovskite to obtain mixed powder, mixing and dissolving the mixed powder and concentrated hydrochloric acid to obtain a clear solution, cooling the clear solution to 20-30 DEG C at a cooling speed of 2-5 DEG C at 130-180 DEG C, and collecting precipitate; washing and drying the precipitate to obtain rare earth halide perovskite powder; and mixing the rare earth halide perovskite powder with polystyrene, and performing hot pressing to obtain the rare earth halide perovskite scintillator. The preparation method of the rare earth halide perovskite scintillator has the advantages of simple operation and low preparation temperature; the rare earth halide perovskite scintillator provided by the invention has the advantages of high luminescence brightness (the light yield is 20000-60000ph. / MeV) and good high-temperature luminescence stability (the brightness decay at 180 DEG C is less than 10%).

This invention discloses a method for separating and recovering antimony and bismuth from copper-, arsenic-, antimony-, and bismuth-containing materials. The method involves adding sulfuric acid during the processing of the copper-, arsenic-, antimony-, and bismuth-containing materials, allowing copper to enter the liquid and enriching antimony and bismuth elements into the slag. Liquid alkali is then added to the slag, allowing arsenic to enter the liquid and further enriching antimony and bismuth elements into the slag. Liquid alkali and sodium hydrosulfide are then added to the slag, allowing antimony to enter the liquid for recovery, while bismuth remains in the slag, achieving antimony-bismuth separation. The slag composition meets the requirements for bismuth concentrate. A composite silicate is added to the sulfidation liquid to remove impurities such as bismuth, copper, and lead into the slag. The liquid then enters a pressurized reactor, where a catalyst is added and forced-air oxidation is applied, oxidizing antimony and allowing it to enter the slag. After drying, sodium antimonate is obtained. This is the first time a process has been achieved that does not use a chloride salt system to separately produce bismuth concentrate and sodium antimonate. This process shortens the wet separation and recovery process of antimony and bismuth, eliminates the high-chlorine wastewater generated by the chloride salt system, is environmentally friendly, and achieves antimony and bismuth recovery rates of over 98%.

The invention discloses a composite modified lithium manganate positive electrode material as well as a preparation method and application thereof, and belongs to the technical field of positive electrode materials. The structural formula of the composite modified lithium manganate positive electrode material is LiXaOb-coated LiYO2 / LiMn2O4, and the composite modified lithium manganate positive electrode material comprises an inner core consisting of LiYO2 and LiMn2O4, and an LiXaOb coating layer coating at least part of the surface of the inner core, wherein the LiMn2O4 has a porous structure, and pores of the LiMn2O4 are filled with the LiYO2. According to the positive electrode material disclosed by the invention, the lithium manganate is used as the matrix, the pore channels of the matrix are filled with the LiYO2, the surface of the matrix is coated with the LiXaOb, the specific capacity of the positive electrode material is not influenced on the basis of reducing the Jahn-Teller effect of the lithium manganate by filling the pore channels with the LiYO2, and the lithium ion diffusion rate can be accelerated by the LiYO2, so that the rate capability of the material is improved.

The invention discloses a photo-erasable double-capture center photosynaptic material CaSb2O6: Ti as well as a preparation method and application of the photo-erasable double-capture center photosynaptic material CaSb2O6: Ti. The material is charged under excitation of 275 nm light, carriers are stored in a capture center, the stored carriers are erased under excitation of 365 nm light, and thermoluminescence returns to zero after erasing; the capture center comprises a shallow energy level capture center and a deep energy level capture center; the shallow energy level capture center is used for realizing a common short-term photosynaptic function, and the deep energy level capture center is used for realizing a long-term memory function; the dipulse facilitation index in the synaptic behavior is greater than or equal to 172%, and the facilitation curve is S-shaped and can be used for an activation function in a neural network. The photosynapse response signal is regulated and coded by various parameters such as pulse intensity, pulse number, pulse time, pulse frequency, duty ratio, pulse light wavelength and the like of the excitation light pulse. The thick film technology of the material is compatible with polydimethylsiloxane, the material can be used for duty ratio coding handwritten anti-counterfeiting and reconfigurable reservoir calculation, vegetable-fruit double-task end side identification is achieved, and the accuracy rate is gt; 90%. The material is simple in composition, convenient to prepare, flexible and suitable for artificial intelligence edge equipment.

The application provides a modified sodium iron pyrophosphate phosphate positive electrode material and a preparation method and application thereof, and comprises a sodium iron pyrophosphate phosphate positive electrode material, carbon and a sodium ion conductor. x MO y The composite phase material formed by the carbon and the sodium ion conductor is used for coating primary particles and secondary particles of the positive electrode material, a three-dimensional conductive / ionic network is formed on the material crystal boundary and the surface, the charge and ion transmission rate of the material is high; and the three-dimensional coating layer can protect the material from the erosion of electrolyte, has good structural stability, and has excellent cycle performance and rate performance.

A lithium garnet material has the formula Li7+δLa3Zr2-x-y-zM1xM2yM3zO12, where M1 is one or a combination of (Y, In, Mg, Ca, Ba, Sc, Sr, Ru) with oxidation number (valence) lower than 4+, M2 is one or a combination of (Bi, Ta, Nb, Mo, Sb, Te) with oxidation number (valence) higher than 4+, and M3 is one or a combination of (Hf, Ti, Sn, Si) with oxidation number (valence) equal to 4+, subject to 0<x≤1, 0<y≤1, 0≤z≤2, 0<x+y+z≤2, and -0.2<δ<0.2. Also provided is a lithium garnet material which is the same as the aforementioned lithium garnet material except that M1 is one or a combination of (Y, In, Mg, Ca, Ba, Sr, Ru) and M2 is one or a combination of (Bi, Ta, Nb, Mo, Sb, Te, W). Lithium oxide solid-state electrolyte materials have the same formula as the aforementioned lithium garnet materials but also include Ge for M3.

The application relates to the technical field of inorganic chemical materials, and discloses a control synthesis process of a high-temperature-resistant sodium meta-antimonate crystal structure, which comprises the following steps: dispersing diantimony trioxide in a sodium hydroxide aqueous solution with an initial concentration of 6.5-8.0 mol / L, adding sodium meta-aluminate as a crystal lattice directing agent to prepare a precursor bottom solution; heating the bottom solution and maintaining turbulent stirring, performing double-flow path synchronous compensation, adding hydrogen peroxide aqueous solution drop by drop and synchronously adding sodium hydroxide; dynamically setting the coupling relationship of the alkali supplementing rate, the oxidation rate and the reaction stoichiometric ratio, and real-timely offsetting the dilution effect of reaction generated water and solvent water, so that the free sodium hydroxide concentration of the mother liquor in the whole reaction process is maintained to be above 6.0 mol / L until the reaction endpoint is reached; the application dynamically clamps the reaction boundary, blocks the path of the lattice gap water or the surface hydroxyl group, and prepares anhydrous sodium meta-antimonate without a crystallization water removal step in the whole temperature range, so that the foaming problem in high-temperature processing is solved.