Magnesium-reduced method of production of sponge zirconium and device for realization of this method
FIELD: metallurgy of zirconium.
SUBSTANCE: 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.
EFFECT: reduced specific consumption of magnesium per ton of sponge zirconium; reduced labor consumption at servicing the device.
4 cl, 1 dwg, 2 ex
The invention relates to magnesium obtaining sponge zirconium.
Known for magnesium is a method of obtaining sponge zirconium and device for its implementation (Angelican, Gasperson. "Metallurgy of rare metals". M.: metallurgy, 1973, s-397).
The method consists in the fact that the entire recovery process in the apparatus is loaded magnesium, and then on the mirror of molten magnesium serves a couple of zirconium tetrachloride. The wall temperature in the reduction zone is maintained within 780-920°S. Of apparatus periodically drained magnesium chloride. Then from the reaction mass of sponge zirconium, magnesium chloride, filling the pores of sponge zirconium, distilled magnesium and chloride under vacuum of 10-4-10-6mm Hg at 920-930°C.
The device for implementing the method is a recovery apparatus, in which the recovery of zirconium tetrachloride with magnesium to form a reaction mass (Zr, MgCl2, Mg) with periodic draining of the magnesium chloride from the device recovery. After recovery of the reaction mass in the crucible is loaded into the retort up-side down. This retort is connected from the bottom of the condenser. The retort from the reaction mass heated Kolpakova oven. In the condenser precipitated magnesium and chloride.
The disadvantages of this method of idevices include increased labor costs for maintenance of the described devices and increased loss of condensate magnesium when dismantling a very complex device due to oxidation and combustion.
The closest analogue in essential characteristics and purpose of this method is the patent US 2787539 (CL 22 In 34/14, publ. 02.04.1957). It opened for magnesium is a method of obtaining sponge zirconium, including the preparation of magnesium to the process, the recovery of zirconium from his tetrachloride in the presence of condensation of the magnesium chloride from the previous processes, obtaining the reaction mixture, the purification of the reaction mass from magnesium chloride separation in vacuum deposition in the condenser condensate magnesium chloride.
The disadvantage of this method is the dissection apparatus vacuum separation, resulting in prolonged contact condensation of magnesium chloride with air, resulting in flooding of magnesium chloride, combustion and oxidation of the magnesium. Consequently, there was a significant loss of magnesium.
The closest analogue of the device is the Japan patent No. 3047929 (From 22 In 34/14, publication 91.02.28). The patent describes a device for obtaining magnesium zirconium way. The device consists of a combined system (installed in the furnace), which carried out the process of recovery of metal chloride magnesium and vacuum separation of the data points from the reaction mass, condenser installed in the refrigerator, and connecting these devices pipeline.
Not what atcom this device is when it comes to installation and dismantling requires increased labor costs due to the complexity of the cover apparatus with the reaction mass for additional loading of magnesium on the recovery process. Due to the fact that before the recovery process removed the cover of the device with condensation magnesium and installed the cover apparatus of recovery, after which the precipitated condensate is loaded liquid magnesium or magnesium ingots (solid), the oxidation and combustion of magnesium, increased its loss. In connection with the deposition of condensate magnesium on the wall of the retort-condenser also its inevitable loss when doing the recovery process and education of the lower chlorides of zirconium (Lower chlorides of zirconium - deadweight losses.), which are formed at low temperature and with a lack of magnesium in the mounting clearances.
The task, which directed the claimed invention, is to reduce the specific consumption of magnesium per 1 ton of sponge zirconium and reduce labor costs when servicing the device.
The technical result is achieved by the fact that in the inventive magnesium production method of sponge zirconium, including the preparation of magnesium to the process of recovery of zirconium from his tetrachloride in the presence of condensation of the magnesium chloride from the previous processes, obtaining the reaction is mass, purification of the reaction mass from magnesium chloride separation in vacuum deposition in the condenser condensate magnesium chloride, what is new is that for magnesium recovery of zirconium from his tetrachloride and receiving the reaction mass used is filled with condensate magnesium chloride capacitor with the separation process with the addition of refined magnesium.
Additive refined magnesium can be done or in the form of ingots in the capacitor before the deposition of condensate magnesium chloride, or fill it melt condensation of magnesium chloride before recovery of zirconium.
The achievement of the technical result is strengthened by the fact that in the inventive device for magnesium obtain sponge zirconium, comprising the apparatus with a reaction mass mounted in a vacuum oven separation, the capacitor connected to the apparatus is heated by a steam pipe fitted with a valve, it is new that the capacitor has a closed lid of the retort, within which is mounted a glass covered are embedded in the screen bottom of the cover.
Distinctive features of the method and device allow to exclude replacement cover condenser cover apparatus of recovery, which prevents oxidation and combustion of magnesium in the apparatus of recovery,flooding, magnesium chloride, reduces its losses. The simplicity of the device, and the use of a capacitor as a device restore from the full sample of magnesium to reduce the labor in his service.
Condenser design, to be used later to restore operations as recovery apparatus, allows to prevent the condensation of magnesium chloride on the wall of the retort-condenser due to the penetration of the screen fixed to the bottom cover, in a glass that reduces loss of magnesium deficiency of which in the course of the recovery process contributes to the formation of the lower chlorides of zirconium, and also reduces the labor for disassembly of the device recovery. In the presence of lower chlorides of zirconium in the retort, it may be fire and increasing labor costs when they are fighting, as well as increased loss of magnesium due to burning.
The use of condensate magnesium chloride immediately after vacuum separation in the recovery process significantly reduces the loss of magnesium and work for its disposal.
The deposition of condensate magnesium chloride on ingots of refined magnesium allows to obtain a complete sample of magnesium, prepared for the recovery process, bypassing the purification of magnesium in the apparatus of the recovery, i.e. by decreasing the loss of magnesium and trudos the rata on its preparation, as the elongation process leads to additional loss of magnesium due to in-leakage of air and moisture in the device.
Known from the practice of pouring molten refined magnesium condensate magnesium chloride also reduces additional operations on the preparation of the magnesium before the recovery process and its loss with additional operations.
Consequently, the novel features of the claimed invention provide reduced losses of magnesium (reduction of specific consumption of magnesium per 1 ton of sponge zirconium) and reduced labor costs for maintenance of the device.
Apparatus for producing sponge zirconium is shown in the drawing.
It consists of:
Capacitor 1 has mounted on it a false bottom 2 of the Cup 3, intended for loading a magnesium ingots 4. The capacitor 1 is closed by a cover 5 attached to it by the screen 6, which is embedded in the glass 3. In the drawing, the condenser 1 is placed in the refrigerator 7.
Apparatus 8 with a false bottom 2 to put on it is depicted in the drawing, the reaction mass 9. The apparatus 8 is closed by the cover 10 and is installed inside the furnace vacuum separation 11. To the nozzle 12 of the cover 10 through the flange 13 is attached to the valve 14.
- Working volume of the Cup 3 and the apparatus 8 are connected through the flange 13 of the steam pipe 15 with heating 16. coumarouna apparatus and the flow of argon is produced through the nozzles 17.
The operation of the device and the example of the method.
Once loaded into the apparatus 8 of the reaction mass 9 (sponge zirconium, magnesium and magnesium chloride) in the Cup 3 magnesium ingots 4 hold the Assembly device according to the scheme shown in the drawing, check it for leaks, and make the way for magnesium obtain sponge zirconium.
When you open the valve 14 condensate magnesium chloride from the reaction mass in the number of ˜ 600 kg precipitated on refined magnesium ingots 4 and on the inner walls of the Cup 3. Vapors do not get on the wall of the retort through the cavities in the glass of the screen 6, is fixed on the bottom cover 5.
The process of vacuum separation of the reaction mass 9 is carried out at 1000°C, under vacuum of 10-3mm Hg, created through pipe 17. Pair magnesium chloride pass through the steam pipe 15, is heated to 800°using heating 16. The vapor deposition of magnesium chloride in the glass 3 is at 300°C. the Number of condensate magnesium 450 kg, a MgCl2- 150 kg At the end of the process vacuum separation in the retort 8, the Cup 3 of the capacitor 1 and the steam line 15 ask argon through the nozzles 17, turn off the furnace 11 and the heat of the 16 steam line 15, close the valve 14. Then disassemble the steam pipe 15, under the flow of argon choke tube 12 of the capacitor 1. Then condense the tor 1 in Assembly with the cover 5, provided in the bottom part of the screen 6, the crane is transported and installed in is not shown on the drawing furnace repair, where the full sample of magnesium in the recovery process is downloadable through pipe 12 of zirconium tetrachloride get the reaction mass used in the future to put on a false bottom 2 of the apparatus 8. Thus, the capacitor 1 is re-used in the process as a vehicle for recovery.
The separation apparatus 8 is removed from the furnace separation 11 and mounted on the extracted position of the condenser 1, where it is cooled in the refrigerator for 7 to 50°, then remove from the refrigerator and disassemble, getting a sponge zirconium, in the example shown in the 1500 kg
Once loaded into the apparatus 8 of the reaction mass 9 (sponge zirconium, magnesium and magnesium chloride) is produced by an Assembly device according to the scheme shown in the drawing, check it for leaks, and make the way for magnesium obtain sponge zirconium.
When you open the valve 14 condensate magnesium chloride from the reaction mass in the number of ˜ 600 kg precipitated on the inner wall of the Cup 3. Vapors do not get on the wall of the retort through the cavities in the glass 3 screen 6, is fixed on the bottom cover 5.
The process of vacuum separation of the reaction mass 9 conduct ol the 1000° C, under vacuum of 10-3mm Hg, created through pipe 17. Pair magnesium chloride pass through the steam pipe 15, is heated to 800°using heating 16. The vapor deposition of magnesium chloride in the glass 3 is at 300°C. the Number of condensate magnesium 450 kg, and its chloride - 150 kg At the end of the process vacuum separation in the retort 8, the condenser 1 and the steam line 15 ask argon through the nozzles 17, turn off the furnace 11 and the heat of the 16 steam line 15, close the valve 14. Then disassemble the steam pipe 15, under the flow of argon choke tube 12 of the capacitor 1. Then the capacitor 1 in Assembly with the cover 5, is provided in the bottom part of the screen 6, embedded in the glass 3, with condensation magnesium chloride crane is transported into the furnace of the recovery (in the drawing furnace repair not shown). Furnace repair condensate magnesium chloride is melted and add the additive refined magnesium through the pipe 12 in an amount to provide a complete sample of magnesium on the recovery process of zirconium tetrachloride, and get the reaction mass used in the future to put her on the false bottom 2 of the device 8 device.
The separation apparatus is removed from the furnace separation 11 and set in the refrigerator for 7 to place the extracted condensate 1, where it is cooled to 50°C, after which the extract is from the refrigerator 7 and disassemble. The result sponge zirconium in the example shown in the 1500 kg
The result of using the proposed method and device for its implementation was able to reduce the loss of magnesium by 20% for 1 ton of sponge zirconium and approximately 30% reduction in work in process and operation of the device compared to the prototype.
1. Magnesium is a method of obtaining sponge zirconium, including the preparation of magnesium to the process, the recovery of zirconium from his tetrachloride in the presence of condensation of the magnesium chloride from the previous processes, obtaining the reaction mixture, the purification of the reaction mass from magnesium chloride separation in vacuum deposition in the condenser condensate magnesium chloride, characterized in that for magnesium reduction of zirconium and its tetrachloride and receiving the reaction mass used is filled with condensate magnesium chloride capacitor with the separation process with the addition of refined magnesium.
2. The method according to claim 1, characterized in that the additive refined magnesium in the capacitor is carried out in the form of ingots before deposition of condensate magnesium chloride.
3. The method according to claim 1, characterized in that the additive refined magnesium exercise fill it melt condensation of magnesium chloride before restore what oulanem Zirconia.
4. Device for magnesium obtain sponge zirconium, consisting of a set in a vacuum oven separation apparatus with a reaction mass and a capacitor connected equipped with a valve heated by steam, characterized in that the capacitor has a closed lid of the retort, within which is mounted a glass covered are embedded in the screen bottom of the cover.
FIELD: nonferrous metallurgy; devices for purification of a spongy titanium.
SUBSTANCE: the invention is pertaining to the field of nonferrous metallurgy, in particular, to devices for purification of a spongy titanium. The technical result is an increase of productivity of the apparatus due to decrease of labor input for its servicing and acceleration of the process of a vacuum separation due to stabilization of a temperature mode in a retort-condenser. The apparatus contains a retort-reactor with a bottom branch-pipe and a false bottom closed by a cover with a central branch-pipe closed by a fusible stopper plug, a retort-condenser with a bottom branch-pipe with a stopper plug, a caisson with a distributor of water, a heated screen and with a fusible stopper plug. The apparatus in addition is supplied with a metallic nozzle mounted rigidly in the central branch-pipe of the cover under the fusible stopper plug and made in the form of a truncated cone with its smaller base facing a fusible stopper plug and with an inlet and outlet holes, a metallic shell mounted in the bottom branch-pipe of the retort-condenser and rigidly connected with the stopper plug, and with a sealed cover mounted rigidly in the upper part of the caisson. Under the sealed cover there are a bottom branch pipe of the retort-condenser and a water distributor.
EFFECT: the invention ensures increased productivity of the apparatus, decreased labor input for its servicing, acceleration of the vacuum separation process, stabilization of a temperature mode in the retort-condenser.
7 cl, 1 dwg
FIELD: non-iron metallurgy, in particular gallium refining.
SUBSTANCE: crude gallium is converted to highly volatile gallium(I) oxide Ga2O by metal heating in presence of gallium(III) oxide Ga2O3 at 500-7000C in vacuum to provide a slop. Highly volatile gallium(I) oxide Ga2O is fed into disproportionation zone under the same conditions followed by disproportionation to form metal gallium and gallium(III) oxide Ga2O3 at 700-9000C Obtained slop is recycled to reuse by addition to starting crude gallium.
EFFECT: purified gallium with decreased content of Sn, Fe, Al, Si, Ni impurities; reduced waste; and low cost process.
4 tbl, 1 ex
SUBSTANCE: method comprises steps of melting charge and discharging melt products. Charge contains chrome oxide, aluminum, lime, oxidizing agent such as sodium nitrate according to variant 1 and sodium (potassium) anhydride and dichromate according to variants 2,3; in addition according to variants 2, 3 - calcium hydroxide and sodium chloride and according to variant 2 - fluorspar concentrate. In variant 2 chrome containing nitrogen up to 0.05 mass % is produced. In variant 3 chrome containing nitrogen up to 0.01 mass % is produced. Variants have different features, namely: preset relation of lime (and calcium hydroxide in variants 2,3) to aluminum; limited content of carbon in lime; addition of large part of lime with minimum content of carbon directly to charge and remaining part of lime with more content of carbon - to charging bed; predetermined relations of charge components; loading and melting charge by one stage at high speed 310 - 450kg/m2 min; feeding fluorspar concentrate onto liquid slag remained after draining to lining slag (variant 2).
EFFECT: optimization of thermodynamic and kinetic conditions of reducing process, increased content of chrome, lowered content of impurities such as aluminum, carbon, nitrogen, improved yield of higher kinds of aluminothermic chrome.
3 cl, 1 tbl, 7 ex
FIELD: metallurgy; method of alumino-thermal production of ferro-niobium.
SUBSTANCE: proposed method includes stage-by-stage loading and melting of charge containing niobium concentrate, sodium nitrate, lime, iron ore, aluminum and drainage products of melt; used as niobium concentrate is commercial niobium concentrate. At first stage, charge is loaded at rate of 300-380 kg/m2/min; this charge contains total mass of commercial niobium concentrate and sodium nitrate, 30-70% of iron ore of mass of melt, 20-80% of lime of mass of melt and aluminum in the amount of 0.85-0.99 of amount stoichiometrically required for reduction of elements of ferro-niobium alloy; at second stage, charge is loaded in the amount of 35-55% of mass of niobium pentoxide in commercial niobium concentrate of first stage at rate of 210-270 kg/m2/min, 30-70% of iron ore of mass of melt, 20-80% of lime of mass of melt and aluminum in the amount of 1.6-2.0 of amount stiochiometrically required for reduction of elements of ferro-niobium alloy; before draining, melt is held during period equal to 0.1-0.6 of charge melting time.
EFFECT: increased extraction; improved quality of ferro-niobium alloy.
3 cl, 1 tbl, 9 ex
FIELD: metallurgy, namely production of refractory metal alloys by out-of-furnace aluminothermic reduction.
SUBSTANCE: process comprises steps of preparing charge of compound of refractory metal, aluminum and oxides of alkali-earth metals; placing charge in metallic crucible on surface of ignition mixture of alkali-earth metal peroxide and aluminum; reducing it and melting; adding to charge in addition waste material of previous melting and chlorate while providing relation of aluminum powder to peroxide of alkali-earth metal in ignition mixture 4 : 1.
EFFECT: enhanced degree of metal transition to alloy, lowered impurity content such as carbon, reduced explosion hazard of process.
FIELD: metallurgy; methods of preparation of charges for production of niobium-bearing material.
SUBSTANCE: the invention is dealt with production of niobium-bearing materials used for production of special steels. The technical result is an increased degree of transition of niobium into an alloy, decreased share of impurities in the alloy, decreased production costs. For this purpose the charge for production of a niobium-bearing material contains the raw material containing niobium pentaoxide, a nickel-bearing material, aluminum, calcium oxide, calcium fluoride and an exothermic oxidative additive. At that in the capacity of the exothermic oxidative additive it contains potassium chlorate with moisture of 2-12% at the following ratio in shares in respect to the total weight of the charge: niobium pentaoxide - 0.470-0.520, nickel - 0.190-0.270, aluminum - 0.180-0.200, calcium oxide - 0.030-0.040, calcium fluoride - 0.003-0.004, potassium chlorate with moisture of 2-12% - 0.043-0.049. At preparation of the charge after mixing of components it is exposed to compaction in the crucible up to the value of the plastic strength of 0.4-10.0 MPa.
EFFECT: the invention ensures an increased degree of niobium transition into an alloy, decreased share of impurities in the alloy, decreased production costs.
2 cl, 1 tbl, 3ex
FIELD: production of pure niobium.
SUBSTANCE: method includes reducing fusion of niobium pentoxide with aluminum and calcium to provide crude ingots followed by heat treatment and multiple electron beam refining. As an additional raw material in step of reducing fusion sublimates (preferably in non-oxidized form) from second and subsequent electron beam refining are used. Such sublimates are obtained by subsequent cooling of furnace smelting chamber under residual pressure of 10-2-10-4 mmHg for 1.0-3.0 h, letting-to-helium under 1-3 mmHg for 1.0-3.0 h, and letting-to-air for 20-40 min. Sublimates are added in amount of 4.5 % based to feeding niobium pentoxide. Claimed method affords the ability to increase niobium pentoxide consumption by 73 kg in respect to 1000 kg of pure niobium in crude ingots.
EFFECT: production of pure niobium with increased effectiveness without deterioration of refined niobium quality.
2 cl, 1 tbl
FIELD: production of refractory metals, namely zirconium by electrolysis of melt salts.
SUBSTANCE: 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%.
EFFECT: improved current yield of zirconium powder at electrolysis, extraction of zirconium from initial salt to powder, lowered specific consumption of DC power.
1 tbl, 1 ex