RussianPatents.com

Apparatus for iodide refining of zirconium. RU patent 2261287.

FIELD: production of pure zirconium by iodide refining method.

SUBSTANCE: proposed apparatus has retort and cover making it hermetic, current leads, cooling system and mechanism for delivery of iodine to retort. Peripheral screen chambers located inside retort are used for pouring initial material. Trapezium-shaped multi-loop zirconium wire tightened in space between chambers is used for deposition of pure metal on it. Upper and lower horizontal sections of wire loop are secured to metal disks by means of hooks on which electric insulating rings are fitted; length of horizontal sections does not exceed double diameter of finished bar. Wire is stretched by lower metal disk whose mass ratio to initial mass of wire ranges from 2.0 to 3.0.

EFFECT: increased productivity of apparatus; reduced amount of substandard metal.

3 dwg, 1 tbl

IPC classes for russian patent Apparatus for iodide refining of zirconium. RU patent 2261287. (RU 2261287):

C22B9/10 - with refining or fluxing agents; Use of materials therefor (C22B0009180000 takes precedence);;

C22B34/14 - Obtaining zirconium or hafnium

Another patents in same IPC classes:

Method for producing aluminum-lithium alloys / 2255997
Method comprises steps of loading and melting components of charge in furnace; treating melt with flux of halide containing salts, adding lithium, refining melt by means of gaseous chlorine, further vacuum treatment of melt in mixer and casting ingots. Eutectic mixture of lithium ad potassium chlorides is used as halide containing salts. Silver is added to melt after refining. Melt is subjected to vacuum treatment in mixer at 730 - 765°C. Ingots are cast in mold at applying on surface of melt flux containing eutectic mixture of lithium and potassium chlorides and in addition 5 - 20% of calcium chloride and(or) fluoride.

Method for production of exothermal mixture for steel treatment in liquid state / 2244754
Claimed method includes crushing of burning components and blending with reflux agent (e.g. synthetic calcium fluoride). Oxides of doping elements used as oxidizing components are premixed with melted reflux agent preliminary with lower melting point than the same of steel, at volume ratio preferably 1:1-1:5, respectively, cooled, crushed in form of failing, and introduced to mixture of burning components and reflux agent.

Method for reprocessing of junks of magnesium containing based-based alloys / 2244027
Claimed method includes junk charge into premelted flux at ratio of 1:(5-10); heating up to melt temperature; smelting under flux layer, and separation of metal from flux. Equimolar mixture of sodium chloride and potassium chloride with addition of 2.9-52.6 % (in respect to total flux weight) magnesium fluoride is used as flux, and in melting process flux layer with thickness of 4.5-20 cm is maintained. Method affords the ability to conserve original composition and eliminate additional burdening with magnesium.

Magnesium-reduced method of production of sponge zirconium and device for realization of this method / 2261286
Magnesium-reduced method of production of sponge zirconium includes preparation of magnesium for process, reduction of zirconium from its tetrachloride in presence of magnesium concentrate and its chloride of previous processes, obtaining reaction mass, cleaning this mass by separation in vacuum at precipitation of magnesium condensate and its chloride in condenser. For reduction, use is made of condenser filled with magnesium condensate and its chloride after separation process at addition of refined magnesium in form of ingots before precipitation of magnesium condensate and its chloride. Addition of refined magnesium may be performed by pouring its melt on magnesium condensate and its chloride before reduction of zirconium. Device proposed for realization of this method includes apparatus placed in vacuum separation furnace and filled with reaction mass and condenser interconnected by means of heated vapor line fitted with valve. Condenser is made in form of retort closed with cover with reaction sleeve placed inside it. Reaction sleeve is closed with shield of bottom part of cover sunken in it.

Zirconium production process / 2257426
Process comprises steps of electrolysis of melt of fluoride-chloride electrolyte containing, mass %: zirconium, 3 - 5, chlorine, 8 - 13; sodium, 2 - 4; cyclically charging to melt potassium fluozirconate, potassium chloride and sodium chloride for sustaining predetermined content of electrolyte; further separation of zirconium powder by hydraulic metallurgy; performing electrolysis at adding to melt magnesium chloride additive in quantity providing mass content of magnesium in electrolyte 0.05 - 0.5%.

Method for acid decomposition of calcium silicate and recovery of zirconium / 2244035
Invention aims at recovering uncommon metals from silicate ores and concentrates in processing of zirconium concentrates. Method according to invention envisages treating cake obtained by caking zircon concentrate with calcium oxide in presence of nitric or sulfuric acid. Concentrated acid is added to water-slurried cake at constant speed during 30-60 min in two steps so that 18-25% of acid is added during first 30 min, whereupon zirconium is leached at 80-90^оС.

Apparatus for iodide refining of zirconium / 2261287
Proposed apparatus has retort and cover making it hermetic, current leads, cooling system and mechanism for delivery of iodine to retort. Peripheral screen chambers located inside retort are used for pouring initial material. Trapezium-shaped multi-loop zirconium wire tightened in space between chambers is used for deposition of pure metal on it. Upper and lower horizontal sections of wire loop are secured to metal disks by means of hooks on which electric insulating rings are fitted; length of horizontal sections does not exceed double diameter of finished bar. Wire is stretched by lower metal disk whose mass ratio to initial mass of wire ranges from 2.0 to 3.0.

Method of separating metals such as zirconium and haffnium / 2288892
Invention relates to a method allowing separation of some metals, in particular zirconium and haffnium. Method comprises separating metal 1 from metal 2 in aqueous solution of these metals. Being in solution, metals form polymers and/or copolymers, which prevents their passage through nanofiltration membrane. Method involves following stages: treating aqueous medium with ligand such as amino acid or poly(amino acid) to form complex with metal 1 or metal 2 followed by passing treated aqueous medium through filtration membrane. Membrane permeates through ligand-metal complexes but retains non-liganded metals.

Method of iodide refining of hafnium / 2291214
Interaction of iodine with black metal is carried out at temperature of 250-350°C. Sedimentation of refined hafnium is carried out at temperature of 1200-1600°C on heater (filament) made from molybdenum or zirconium wire in form of one or several loops connected to electrode end-pieces. Heater is formed in iodide refining apparatus in such way that lower part of each wire loop is suspended above insulator surface at clearance equal to 1/3-1/2 of final thickness of bar. Proposed method may be used for production of iodide hafnium bars more than 17 mm in diameter at height of heater loop more than 0.8 m.

Method for separating hafnium from zirconium / 2296172
Invention relates to a method for separation of hafnium and zirconium. Method involves extraction step of the parent aqueous mixture containing zirconium oxychloride, hafnium oxychloride and thiocyanate salt with a thiocyanate-containing organic solvent for preparing zirconium-containing aqueous raffinate flow and hafnium-containing organic raffinate flow, separation of organic raffinate flow from aqueous raffinate flow. In the aqueous parent mixture the ratio value of total acidity to the total sum of zirconium and hafnium oxides (TA/MO₂) in maintained in the range from about above 2.55 to about less 3.5. Method provides optimization process for separating zirconium from hafnium by extraction procedure.

Baddeleyite processing method / 2297464
Method comprises steps of adding potassium ion in the form of potassium fluoride after complete dissolving of baddeleyite in acid and returning filtrate containing hydrofluoric acid to step of baddeleyite dissolving. Zirconium hydroxide is obtained by processing recrystallized crystals with solution of potassium hydroxide and prepared pulp is filtered. 1/3 of filtrate volume is returned to step of producing potassium fluorozirconate and 2/3 of filtrate volume is directed to step of recovering potassium fluoride. The last is recovered from filtrate due to processing filtrate with calcium hydroxide for producing potassium hydroxide. Generated calcium fluoride is directed to step of recovery where it is subjected to processing with sulfuric acid for producing hydrofluoric acid to be returned to step of dissolving baddeleyite. Potassium sulfate is used for different purposes in national economy.

Zirconium powder manufacturing process / 2304488
Invention relates to manufacturing zirconium powder for making pyrotechnic articles, in particular explosive and inflammable mixtures. By-layers prepared powered mixture of potassium fluorocirconate and alkali metal chloride, preferably sodium chloride, at ratio 1:(0.15-0.6) and sodium metal in amount exceeding its stoichiometrically required amount by 10-20%. Preparation involves grinding of potassium fluorocirconate and alkali metal chloride to fineness below 50 μm as well as preliminary recrystallization of potassium fluorocirconate. Charge is heated to temperature 450-600°C, at which reduction reaction starts and during this reaction reaction mixture heats to 700-800°C and reduction of potassium fluorocirconate takes place. Reaction products are cooled to 400-650°C and freed of sodium through vacuum distillation at residual pressure 1.3-13.3 Pa for 0.5-2.0 h, after which they are discharged from reaction vessel and ground. Zirconium powder is washed with water to remove fluoride and chloride salts and then dried. Zirconium powder contains 95-98% of fine fractions, including fraction below 10 μm in amount 45-55%.

Zirconium and hafnium separation process / 2307182
Zirconium and hafnium separation process comprises steps of preparing aqueous solution of initial mixture containing salts of zirconium and hafnium; further multiple separation by crystallization of zirconium salts from saturated solution of hafnium; before crystallization providing generation of gaseous hydrates in order to remove excess solvent from solution due to saturating solution with hydrate-generating gas at lowered temperature.

Method of production of powdered fluxes / 2261927
The invention is pertaining to the field of nonferrous metallurgy, in particular, to the methods of production of fluxes for melting and casting of magnesium and its alloys. The method of production of powdered fluxes includes dehydration of the solid carnallite and flux-forming additives containing a water of crystallization. At that the dehydration is conducted in several stages in a multichamber furnace of a boiling layer. On the first stage the carnallite is treated with chimney gases, on the second stage the carnallite is treated with the chimney gases containing hydrogen chloride, and on third stage it is mixed with the flux-forming additives containing the water of crystallization and conduct the air separation. The chimney gases are produced due to feeding of chlorine-containing gases in the flare of the natural gas burning. Specific consumption of chlorine per 1 ton of a dehydrated carnallite makes 50-200 kg ensuring a raise of productivity of the flux production process and improvement of its quality.