41 results about "Potassium heptafluorotantalate" patented technology

The invention relates to a rinsing method and device of a potassium fluotantalate product obtained through sodium reduction. The rinsing method comprises the following steps: using sodium to reduce potassium fluotantalate and obtain coagulum, crushing the coagulum, diafiltrating, rinsing, stirring to rinse, pickling, and drying to obtain raw tantalum powder. The obtained tantalum powder has high purity and good porosity and can be used to prepare condensed tantalum powder which is particularly suitable for the manufacture of the electrolytic capacitor.

The invention relates to a method for reducing usage amount of ammonia gas during the process of tantalum-niobium hydrometallurgical extraction. The method is as follows: 1, concentrated sulfuric acid is added into a niobium-containing acid solution to reduce acidity of the niobium-containing acid solution, and MIBK extraction, back-extraction, ammonia gas neutralization and the like are carried out to prepare a niobium oxide product; 2, as potassium fluotantalate is separated and extracted from a tantalum-containing acid solution by crystallization and filtration processes, a part of fluorotantalic acid is left in a mother liquor. In the prior art, ammonia gas must be utilized for neutralization and recovery. Thus, a lot of ammonia-containing wastewater is caused. According to the invention, part of alkaline matters (such as sodium hydroxide, magnesium hydrate, calcium hydroxide and the like) are used to replace ammonia gas and added into a mother liquor containing a fluorotantalic acid solution, and then ammonia gas is used for neutralization. Through the above two measures, the purpose of reducing consumption of ammonia gas and decreasing discharge of ammonia-containing wastewater is finally achieved.

The invention relates to a stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium. The water-washing method comprises the following steps of: performing stirring water-washing on the tantalum powder obtained by reducing potassium fluotantalate (K2TaF7) via metallic sodium (Na) which removes alkali metal haloids in an electrolyte solution, so as to remove harmful and indissolvable ultrafine-particle impurities in the tantalum powder; and then performing acid-washing and drying to obtain the initial tantalum powder. The method is high in the yield of tantalum powder; and the obtained tantalum powder is high in purity, good in particle size distribution and porosity, and especially suitable for manufacturing a tantalum electrolytic capacitor.

The invention discloses a method for preparing octahedral crystal form Ta2O5 nanoparticles through self-reaction of a single reagent. The method comprises the following steps that 1, potassium fluotantalate powder is selected and dissolved in water, and the potassium fluotantalate solution is placed in a pretreated precious metal pipe and sealed; 2, the sealed precious metal pipe is placed in a hydrothermal reaction kettle and sealed, the temperature inside the hydrothermal reaction kettle is adjusted to be 200-500 DEG C, inert gas or deionized water is adopted for adjusting the pressure inside the hydrothermal reaction kettle to be 50-200 MPa, a hydrolysis reaction is carried out for 12-24 h, and the reaction kettle is cooled to indoor temperature after the reaction is finished; 3, the hydrothermal reaction kettle is opened, the reacted precious metal pipe is taken out and opened, solution residue is recycled, samples are collected, washed and dried, and therefore the octahedral crystal form Ta2O5 nanoparticles are obtained. In the method, the single reagent is adopted as a synthesis raw material, the cost is low, energy consumption is low, pollution is avoided, and the prepared Ta2O5 nanoparticles are intact in crystal form and are in an octahedral shape.

The invention discloses a preparation method for a silicon carbide particle reinforced aluminum-based composite material, and relates to the field of aluminum-based composite materials. The preparation method comprises the operating steps that 1, silicon carbide powder and particles and potassium fluotitanate, or potassium fluozirconate, or potassium fluoborate, or potassium fluosilicate or potassium fluotantalate serve as powder materials, and two kinds or several kinds of the powder materials are uniformly mixed; and 2, aluminum in a furnace is melted, after the aluminum is heated up to 660 DEGC-1500 DEG C, the mixed pulverized raw material is added into the furnace, melt is fully stirred, heat preserving is conducted, and after slagging-off is conducted on the melt, the fully stirred melt is casted into a variety of products. According to the preparation method for the silicon carbide particle reinforced aluminum-based composite material, the performance of the aluminum-based composite material is effectively improved, the process is simple, operating is convenient, the cost is low, and industrial production can be achieved.

The invention relates to a method for preparing target-level high-purity tantalum powder. According to the method for preparing the target-level high-purity tantalum powder, a block-shaped mixture of tantalum powder prepared through potassium fluotantalate sodium reduction and one or more of diluted slats including NaCl, KCl and KF is filtered and washed with pure water, when the conductivity of filtering and washing liquid is smaller than 5000 us/cm, the filtered and washed mixture is poured into a horizontal type ball mine for wet-type ball milling, the mixture is taken out, acid pickling, suction filtration and drying are conducted on the mixture, so that raw tantalum powder is obtained, thermal treatment, oxygen reduction, oxygen-reduction acid pickling, secondary drying and detection are conducted on the raw tantalum powder, and then the target-level high-purity tantalum powder is obtained. According to the method for preparing target-level high-purity tantalum powder, the technology is simple, the production cost is low, the tantalum powder prepared according to the method is large in apparent density, high in purity, low in oxygen content and capable of meeting the requirement of a target for the purity and the density of materials, and therefore tantalum target cost and tantalum alloy target cost are greatly reduced.

The invention relates to a preparation method of high-purity potassium fluorotantalate. The preparation method is characterized by comprising the following steps: (1) decomposition: adding tantalum-niobium mineral into hydrofluoric acid and sulfuric acid for decomposition; (2) mineral-pulp extraction: utilizing an MIBK (Methyl Isobutyl Ketone) solvent or sec-octyl alcohol solvent to carry out backflow extraction and extracting fluorine-niobium acid and fluorine-tantalum acid into the solvent; (3) acid pickling: adopting sulfuric-acid solution to be contacted with the solvent obtained after extraction of step (2) in a backflow manner; (4) tantalum extraction by back extraction of niobium: utilizing the sulfuric-acid solution and the obtained solvent to carry out backflow extraction in an extraction groove, extracting the fluorine-niobium acid into an aqueous phase and forming fluorine-niobium acid aqueous solution; (5) back extraction of tantalum: placing the remaining organic solutionin another extraction groove, utilizing pure water to carry out back extraction on fluorine-tantalum acid organic solution into the pure water and forming fluorine-tantalum acid aqueous solution; (6)synthesis; (7) cooling and crystallization. The method for preparing high-purity potassium fluorotantalate by a method of sectional back extraction and sectional crystallization has the beneficial effect that impurities in the potassium fluorotantalate can be effectively removed.

The invention discloses a preparation method for an aluminum matrix composite material, and relates to the field of the aluminum matrix composite material. The operation method includes the steps that two or several kinds of diamond or diamond and silicon carbide mixed powder particles and potassium fluotitanate or potassium fluozirconate or potassium fluoborate or potassium fluosilicate orpotassium fluotantalate are evenly mixed; aluminum in a furnace is melted, the temperature rises to 660 DEG C to 1500 DEG C, and mixed powdery raw materials are added into the furnace to be sufficiently stirred; and after melting liquid is subject to heat preservation, drossing is carried out on the melting liquid, and the sufficiently-mixed melting liquid is cast into various products. According to the preparation method, the performance of the aluminum matrix composite material is effectively improved, the process is simple and convenient, the operation cost is low, and industrial production can be achieved.

The invention discloses a device for preparing tantalum powder by stirring sodium and reducing potassium fluotantalate, which comprises a reaction vessel and a reaction vessel cover, wherein the reaction vessel is hermetically sealed with the reaction vessel cover; the reaction vessel cover is provided with a plurality of through holes; the through holes are respectively provided with a thermocouple, a stirring apparatus and a sodium injection tube; the reaction vessel cover is further provided with a feed inlet, an air inlet and an air outlet; and the reaction vessel is provided with a sodium distributor. The invention further discloses a method for preparing the tantalum powder using the device. In the invention, metal sodium is injected into the reaction vessel in a dispersive manner by the sodium distributor, and the prepared tantalum powder has uniformly-distributed elementary particles.

The invention relates to a preparation method of a phosphorus-containing tantalum powder and a phosphorus-containing tantalum powder prepared by the method, and a preparation method of phosphorus-containing potassium tantalifluoride and phosphorus-containing potassium tantalifluoride prepared by the method. According to the method, a phosphorus-containing compound is added into a potassium tantalifluoride synthesis solution, and an acid leaching process is utilized to synthesize the potassium tantalifluoride from columbite-tantalite ore powder; and the phosphorus-containing potassium tantalifluoride is prepared into the phosphorus-containing tantalum powder. The phosphorus doping process of the phosphorus-containing tantalum powder is performed in the potassium tantalifluoride synthesis process, so the phosphorus is distributed more uniformly on the tantalum powder particles; since the phosphorus is doped in the potassium tantalifluoride synthesis process, the generation of primary particles is directly influenced; and thus, the primary particles are finer and have larger specific area, and the tantalum powder has higher specific capacity, thereby satisfying the requirement of the capacitor product for the specific capacity of the tantalum powder.

The invention discloses an axial-flow fan of an automobile air conditioner and a preparation method thereof. The preparation method comprises the following steps: 1) blending and mixing PC (polycarbonate), ASA (acrylonitrile styrene acrylate copolymer), CPE (chlorinated polyethylene), p-tert-butylphenol-formaldehyde resin, nano titanium dioxide, tungsten disulfide, calcium naphthenate, aspartic acid, tributyl citrate, triethylene tetramine, diazolidinyl urea, diatomite, carbon fibers, ethyl cellulose, boron nitride, potassium fluotantalate, diborane and silane coupling agents to form a mixture; and 2) curing the mixture, thus preparing the axial-flow fan of the automobile air conditioner. The automobile air conditioner prepared by the method has excellent mechanical properties. Meanwhile, the method is simple in steps and raw materials are easy to obtain.

The invention relates to a preparation method of potassium fluotantalate. In the method, potassium fluotantalate is prepared by a mother liquid internal-circulation process instead of the crystallized mother liquid in recycling treatment of a liquid ammonia neutralizing process; the mother liquid instead of water is sufficiently decomposed with hydrofluoric acid and sulfuric acid; then fluorosilicic acid, sulfuric acid and mother liquid are added for low-acid blending and low-acid extraction; potassium fluotantalate is obtained through transformation and cooling crystallization. According to the method provided by the invention, the use of liquid ammonia is abandoned, and the pollution of ammonia nitrogen is reduced from the source; compared with the traditional process, the discharge of wastewater and the dosage of hydrofluoric acid are greatly reduced, the recycling of industrial potassium fluorosilicate from the mother liquid is realized, and the recycling rate of potassium fluotantalate is as high as 98%.

The invention relates to a thermal decomposition preparation method of potassium fluotantalate. The method is simple and convenient in operation, low in cost and high in direct yield, all volatile components volatilize, and the problem of carbon impurities is solved. Hydrogen tantalum oxide or tantalum pentoxide, potassium fluoride and ammonium bifluoride serve as raw materials, small amount of carbinol, ethanol or water serves as solvent, and a precursor is obtained through full grinding and drying. The prepared precursor is roasted at the temperatures of 150 DEG C, 200 DEG C and 250 DEG C for 3 hours, wherein the precursor is roasted at the temperature of 200 DEG C for respectively 15 minutes, 30 minutes, 60 minutes, 90 minutes and 120 minutes. Influences of the roasting temperature and the roasting time on synthesis of the potassium fluotantalate are investigated. The research shows that K2TaF7 crystals can be obtained by roasting the precursor at the temperature of 200 DEG C for 15 minutes, and the K2TaF7 crystals have high relative crystallinity and small particle sizes.

The invention discloses a fluorine-doped nano-tantalum carbide/graphitized carbon composite material and a preparation method thereof. The preparation method comprises the steps of carrying out ion exchange resin pretreatment and transition metal salt ion exchange, adding potassium fluotantalate into water, stirring, carrying out thermal treatment in the presence of inert gas, and carrying out grinding and acid treatment on obtained materials, so as to obtain the composite material. The preparation method has the advantages that the raw materials are rich in sources and low in costs, and the doped nano-tantalum carbide/graphitized carbon composite material is synthesized at a relatively low temperature, so that the preparation cost is low, the process is simple and convenient, the preparation is rapid, safe and environmental friendly, and the large-scale production is easy to implement; furthermore, the composite material has a utilization potentiality in an anode catalyst of a fuel cell as well as certain active effects for relieving energy crisis, improving air pollution and generalize new energy electric vehicles.

The invention discloses a Ta metallurgical by-product composite salt recycling method. The method comprises the following steps: (1) after separating by-product composite salt produced during the Ta metallurgical process from Ta powder, the composite salt is rinsed with deionized water to remove the residue Na, and then the rinsed composite salt is crushed by a crusher and dried to obtain the treated composite salt; and (2) the treated composite salt is used as diluent, and is mixed with potassium fluotantalate based on certain proportion according to the process requirements and the mixture is taken to a furnace, and the Na is inlet for metallurgy process restoration to obtain the Ta powder. The by-product composite salt produced during the Ta metallurgical production process is used to produce the metallurgical-level Ta powder as the diluent, so that the recycling of the by-product composite salt is realized, the environmental problem caused by the by-product composite salt is avoided, and at the same time, cost is greatly saved. The method also has the advantages that the reuse of waste resources is realized, environmental pollution is reduced, direct yield of the Ta powder is effectively improved, and the Ta powder prepared according the recycling method meets the industry standard of metallurgical Ta powder.

The production of tantalum powder having a low impurity level is provided by a method in which potassium heptafluotantalate is added to a mixture of alkali metal halides in reactor vessel in which the internal surface and auxiliary input accessories of the reactor are covered with a tantalum coating. In one embodiment, the production of tantalum powder with low impurity level includes depositing a protective tantalum coating onto an internal surface of the reactor vessel and auxiliary accessories of a reactor by electrolysis of a mixture of alkali metals halides and potassium heptafluotantalate.

The invention belongs to the technical field of chemical reaction vessels, and relates to dynamic crystallization equipment for potassium fluotantalate. Cold water enters the circuitous hole through the cold medium inlet pipe, the cooling capacity of the cold water is transmitted to the stirring blades and the surrounding potassium fluotantalate solution, and the cold water is discharged from an outlet of the circuitous hole, then enters the connecting vertical pipe, flows upwards, enters the water return ring through the water return elbow and the water passing hole of the sealing ring, and flows into the water receiving ring through the water drainage hole of the water return ring. And the water is buffered and temporarily stored in the space between the water return ring and the water receiving ring, and then flows out of the tank body through the water receiving ring drain hole and the drain pipe. The laser particle analyzer detects the size of particles in the potassium fluotantalate solution in real time and sends information to the PLC, and the PLC controls the rotating speed of the stirring blade assembly through the motor according to the received information. The invention has the advantages of high heat exchange efficiency, uniform size of crystal grains separated by crystallization, good product quality, no serious crystal adhesion, automatic detection of granularity size, automatic adjustment of stirring speed, and small cleaning workload.

The invention provides a preparation method of coralline high-purity tantalum powder, and the mehtod comprises the following steps of (1) activating needle-shaped potassium fluotantalate into powder;(2) making NaCl free of water; (3) filtering and purifying the metal sodium to obtain purified sodium; (4) filling powdery potassium fluotantalate and NaCl into a reduction tank, hoisting the reduction tank into a well chamber reduction furnace, vacuumizing, filling argon for replacement, heating to 100 DEG C, inputting purified sodium, and continuously heating; (5) when the temperature increasesto 750 DEG C, carrying out sodium reduction; (6) after the sodium injection is finished, keeping constant temperature, lifting out the reduction tank, naturally cooling, taking out and crushing into amixture; (7) washing with water and acid to obtain washing powder; and (8) carrying out heat treatment on the washing powder, taking out of the furnace, sieving, and analyzing the qualified undersizeto obtain the coralline high-purity tantalum powder. By controlling the reaction process of preparing the tantalum powder by reducing potassium fluotantalate with the sodium metal, the preparation method of coralline high-purity tantalum powder can absorb metal impurities as little as possible and prevent the reaction product metal tantalum from being oxidized, and can directly prepare the coralliform high-purity tantalum powder with low metal impurity content and low oxygen content.

The invention relates to the technical field of potassium fluotantalate preparation methods, in particular to a method for preparing large-grain potassium fluotantalate by a hydrothermal crystallization method. The problems that potassium fluotantalate prepared through an existing method is low in purity, small in crystal grain, long in crystallization time and the like are solved. The method comprises the steps of adding hydrofluoric acid into a tantalum-containing solution to adjust the acidity, adding potassium chloride, and fully stirring to obtain a mixed solution; adding the mixed solution into a closed reaction kettle, heating to the temperature of 150-220 DEG C, keeping the constant temperature for 4-24 hours, and carrying out a synthetic reaction to obtain a potassium fluotantalate solution; and cooling the potassium fluotantalate solution to 25-30 DEG C in a gradient cooling manner, separating a sample from a mother solution, and washing and drying the sample to obtain the large-grain potassium fluotantalate.