US3464813A - Reduction and purification of reactive metals - Google Patents

Reduction and purification of reactive metals Download PDF

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US3464813A
US3464813A US498500A US3464813DA US3464813A US 3464813 A US3464813 A US 3464813A US 498500 A US498500 A US 498500A US 3464813D A US3464813D A US 3464813DA US 3464813 A US3464813 A US 3464813A
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retort
gas
impurities
pipe
titanium
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US498500A
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Stephen M Shelton
Henry Gordon Poole
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Oregon Metallurgical Corp
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Oregon Metallurgical Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
    • C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/06—Dry methods smelting of sulfides or formation of mattes by carbides or the like
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • This invention relates to the production of reactive metals such as titanium, zirconium, hafnium, etc., and more particularly to a method and means for reducing a reactive metal halide and purifying the resulting product.
  • titanium tetrachloride a liquid, may be added over a period of time to a batch of molten magnesium contained in a closed retort, with a reduction reaction taking place according to the following equation:
  • a porous sponge is formed of titanium, and mixed with this sponge and beneath the sponge the by-product magnesium chloride.
  • the reaction which takes place is not stoichiometric, and only a portion of the magnesium present in the retort is reacted, such as 75-85% of the magnesium.
  • titanium sponge which forms within the reactor be maintained in as shallow a bed as possible, in order that the separation of impurities from the sponge in a subsequent purification step be facilitated.
  • the purification of titanium sponge is further promoted if the sponge is formed as a relatively porous nondense mass, as this results in a larger surface area being produced throughout the sponge, and greater exposure of the impurities sought to be removed from within the sponge.
  • Titanium sponge which forms within a retort clings to the sides of the retort introducing a problem of the removal of the sponge after the process is completed. It is advantageous, therefore, in apparatus used to produce titanium, that a construction be selected for the reaction retort that permits easy loosening of the sponge from the retort walls.
  • One general object of this invention is to provide an improved process for preparing and purifying reactive metals, which is highly reliable, and at the same time relatively economical to carry out.
  • a related object is to provide improved apparatus for preparing and purifying a reactive metal.
  • a more specific object is to provide an improved method for producing a reactive metal, which features the use of the same retort for the reduction of the metal and for its purification, and the same furnace for heating the retort to produce the operating temperatures required within the retort.
  • a further feature of the method is the maintenance of a pressure condition within the retort which is atmospheric or nearly atmospheric pressure, whereby the furnace employed for heating need not be a vacuum furnace, and assurance is had that the retort will not collapse during the manufacturing process.
  • a further object is the provision of a method for producing reactive metals characterized by the use of an inert gas stream passed through a retort at substantially atmospheric pressure, for removing vaporized impurities, and a novel method of removing impurities from this inert gas stream upon such leaving the retort.
  • Another object is to provide an improved method of the type above indicated wherein an inert gas is circulated through a retort with heating of the retort to remove vaporized impurities, the circulated gas is cooled in a region outside of the retort, and a portion of the cooled gas is mixed with hot gas flowing from the return for the purpose of initially cooling the hot gas.
  • solidification of impurities takes place in a novel manner which facilitates the removal of these impurities from the inert gas stream.
  • a still further object is to provide novel apparatus and method for reacting a reactive metal halide and a reducing metal such as magnesium wherein a large area of the reducing metal in molten form is provided during the reaction, and a relatively shallow bed of reactive metal is produced during the process facilitating subsequent purification of the metal by vaporization of impurities.
  • a relatively porous sponge product may be produced, having a relatively large exposed surface area distributed through the sponge exposing impurities contained in the sponge.
  • FIG. 1 is a side elevation, somewhat simplified, showing a retort such as may be used in the process of the invention, with the retort mounted within a furnace;
  • FIG. 2 is an end elevation, taken along the line 2-2 in FIG. 1;
  • FIG. 3 is a top plan view, somewhat simplified, showing apparatus for cleansing gas which is circulated in the process of the invention
  • FIG. 4 is a side elevation, with portions broken away along the line 44 in FIG. 3, illustrating in simplified form a cooler unit in the cleansing apparatus;
  • FIG. 5 is a side elevation, with portions broken away along the line 55 in FIG. 3, illustrating in simplified form a filter unit in the cleansing apparatus;
  • FIG. 6 is a cross-sectional view, taken along the line 66 in FIG. 5;
  • FIG. 7 (first sheet of drawings) is a cross-sectional view, somewhat enlarged, taken along the line 77 in FIG. 1.
  • an iron retort is employed for reducing and then purifying the reactive metal halide taking the form of an elongated hollow cylinder, closed at opposite ends, and disposed with the axis thereof horizontal.
  • this retort is indicated at 10, and comprises a cylindrical shell 12 and end walls 14, 16 closing off the ends of the shell.
  • a horizontal, perforated iron plate or reactor grid 18 Slightly above the base of the shell and within the retort is a horizontal, perforated iron plate or reactor grid 18. Titanium sponge forms over this reaction grid upon the reaction of metal halide and reducing metal.
  • Retort is supported on cradle structure 20 mounted on car hearth 22.
  • the car hearth has wheels 24 disposed under it, riding on rails 26.
  • the retort is movable into and out of a furnace indicated generally at 28.
  • Piping of various types is shown communicating with the interior of retort 10.
  • pipe projecting from rear end wall 14 of the retort adjacent its base, and connecting with the inside of the retort at a point located beneath grid 18, is provided for tapping the retort and removing salt by-product produced in the reduction reaction.
  • Connecting with the retort at points 32a, 32b and 34a, 3412 are pipes 32, 34, both of which connect with a common pipe 33, utilized in circulating gas through the inside of the retort.
  • Pipe 35 is a blow off pipe, and at 37 is shown a pipe used in evacuating and back filling the retort.
  • a pipe 38 communicates with the retort adjacent the top of shell 12, and this comprises a feed pipe f r feeding reactive metal halide to the retort.
  • Furnace 28 comprises sides 52 and a top 54 made of refractory furnace lining.
  • the sides are apertured as at 56 to accommodate gas burners which supply the heat for the furnace.
  • Furnace doors 58, 60 (see FIG. 2), slidable laterally of the furnace, and suitably apertured to accommodate the pipes extending out the back end of the retort, are provided adjacent the back end of the furnace to close this end off.
  • Similar furnace doors such as the one shown at 64 (see FIG. 1) close off the front end of the furnace.
  • purification of the reduced reactive metal produced in the retort by the reduction reaction is carried out with atmospheric or close to atmospheric pressure within the retort whereby a vacuum furnace is not required and the same furnace may be used to heat the retort during purification as was used in the reduction process.
  • Purification is preformed by vaporizing impurities, and then sweeping them from the retort by circulating an inert gas such as argon therethrough.
  • the invention also contemplates a novel method of cleansing the argon or other inert gas used in the sweep process, with impurities being condensed and forming as solid particles which are collected.
  • the apparatus producing circulation of gas through the retort while the same is in the furnace, and cleansing of the gas with removal of impurities is shown in plan in FIG. 3, and is designated generally at 70.
  • a platform 72 which is outside the furnace, are three cyclone filter units, given the reference numerals 74, 76 and 78, and a cyclone cooler unit, given the reference numeral 80.
  • Platform 72 has wheels 82 underneath it supporting it on rails 26, enabling movement of the platform along the rails.
  • the filter units and cooler unit may be moved bodily together with the retort on moving of the retort out of the furnace.
  • outlet pipe 36 which gas flows through on leaving the retort is jacketed directly adjacent the retort, at 86, to permit the circulation of cold water around the pipe whereby a water cooled condenser section is formed.
  • a water inlet and water outlet for the condenser section are shown at 86a, 86b.
  • outlet pipe 36 connects with a valve 84 which connects with the top of cyclone cooler unit by way of pipe 85.
  • a pipe 88 for feeding cool gas into outlet pipe 36.
  • a temperature is produced in the gas mixture flowing through pipe 36 low enough to produce solidification of impurities in the gas stream with such being carried along as particles entrained in the gas stream.
  • Cyclone cooler unit 80 comprises a hollow cylindrical casing portion 80a forming the top of the unit, and a hollow conically shaped casing portion 80]) forming the bottom of the unit. Flow into the unit through pipe is against the inner surface of cylindrical casing portion 80a. Cooling water may be circulated about the outside of casing portion 80b, with such water flowing through a cooling line 800 extending in helical turns about casing portion 80b. Additional cooling in the unit may be brought about by including a jacket such as that shown at 80d about cylindrical casing portion 80a permitting cooling water to be circulated about the outside of the casing portion.
  • the cyclone cooler unit and cylone filter unit 74 are interconnected by a pipe 90.
  • a cooling water coil 92 intermediate the ends of pipe provides additional cooling of gas flowing to the filter unit. Such cooling is desirable in order that gas entering the filter unit be at a low enough temperature so as not to burn up or otherwise damage filter cloths provided in the filter unit.
  • each includes a casing having a conical base such as the one shown at 74a for unit 74, and also a cylindrical top such as the one shown at 74]) for filter unit 74.
  • a leaf-type filter made of folds of a filter cloth, such as the one shown at 74c, depending from a shield such as the one shown at 74d.
  • Flow of gas out of the unit can take place only through the folds of the leaftype filter and thence out through an outlet such as is provided by pipe 94. Material filtered out by the filter unit collects at the base of the unit in housing portion 74a earlier described.
  • Pipe 94 which provides an outlet for gas from the first filter unit extends from the first unit to the second filter unit 76. Gas flow out from this unit is through outlet pipe 96 which extends to the third filter unit 78. The outlet from the third filter unit is provided by a pipe 98.
  • Pipe 98 Downstream from the third filter unit pipe 98 connects with the inlet side of an impeller pump 100 driven by a motor 102. Gas exhausted from the pump passes through a pipe 104, which pipe branches into two pipes 105, 106. One of these, namely, pipe 105, joins with pipe 88 previously described in connection with the feeding of cool gas to outlet pipe 36 extending from the retort.
  • Pipe 106 connects with pipe 33 provided for circulating gas through the retort. Flow meters for indicating the rate of flow through the pipes are indicated at 108 and 110, and valves controlling flow through the pipes are shown at 112 and 114.
  • the feeding of cool gas into pipe 36 for producing initial cooling of the gas coming from the retort and condensing of impurities contained in such gas is an important feature of this invention.
  • the cool gas as should be apparent from the above description of the apparatus, is obtained by diverting part of the inert gas circulated by the pump after such gas has been cleaned so that while much of the gas after cleaning passes through the retort to sweep it and remove impurities, a good proportion of the gas bypasses the retort to return to the gas flowing from the retort in pipe 36 at a point located in advance of the condenser section provided at 86.
  • the gas is introduced to outlet pipe 36 in a special manner, moreover, whereby a film of moving gas, at a relatively low temperature, is produced which extends about the inside of pipe 36 to envelope hot gas flowing from the retort.
  • pipe 88 which connects with pipe 36 extends in a tangential direction from its point of joinder with pipe 36, and gas flowing into pipe 36 from pipe 88 tends to flow around the inner wall of pipe 36 to produce a spiraling fiow of cool gas within pipe 36 as indicated by the arrow in FIG. 7.
  • the halide is a solid
  • the retort is initially charged with the solid halide as well as with a mass of reducing metal such as magnesium.
  • pipe 38 is not necessary for the addition of the tetrachloride. Reduction of the tetrachloride takes place by sublimation of the halide, with halide vapors traveling in the retort to the region of the reducing metal which is present in the retort on heating as a molten pool.
  • the retort was then mounted within furnace 28, and the furnace doors then closed.
  • the gas burners of the furnace were ignited, and the retort was heated with the temperature of the walls of the retort rising to about 800 C. (1472 F.).
  • Titanium tetrachloride was then fed to the retort through pipe 38, at a rate of about 600-800 pounds per hour, until 3000 pounds of the tetrachloride had been added over a period of about 4- /2 hours.
  • the temperature of the walls of the retort was maintained within the range of about 850-900 C. (1562-1742 F.).
  • Argon was bled from the retort through pipe 35 so as to maintain the pressure within the retort constant.
  • by-product magnesium chloride formed in the reduction reaction was drained from the retort through pipe 30.
  • the reduction reaction was about 75% efiicient, and resulted in the production of about 600 pounds of titanium sponge. Estimated to be contained in the sponge was about pounds of unreacted magnesium and pounds of magnesium chloride and subchlorides.
  • Cleansing and circulating apparatus 70 which previously had been evacuated and back filled with argon, was placed in operation by adjusting of the valves controlling the fiow of gas through pipe 33 and by-pass pipe 88, to produce a sweep of argon gas through the retort with such then being recirculated through the filter units. Gas flowed through the retort at the rate of approximately 50 cubic feet per minute, and the same rate of gas flow was maintained through the bypass pipe. A pressure on the downstream side of the pump of about 5 p.s.i.g. was sufficient to produce proper circulation of gas through the equipment.
  • the sponge was relatively easily removed by forcing the web of sponge upwardly toward the middle of the retort (not that the sides of the retort diverge from each other progressing upwardly toward the middle of the retort promoting loosening of the web).
  • a relatively porous pure titanium sponge product resulted, containing not more than 0.1% chlorine.
  • Titanium has also been prepared employing a process similar to the one just set forth save that the inert gas helium was substituted for argon.
  • the use of helium as the inert gas has some particular advantages. For one thin-g, having a lower density than argon, less power is required in pumping the gas whereby it circulates through the system. Furthermore, helium being less dense than argon there is more mobility of the molecules within the system which results in such advantages as the minimizing of hot spots in the retort during the reduction reaction.
  • the method of the invention features a number of advantages contributing to the relatively efiicient production of large quantities of titanium sponge, of requisite purity, which method is reliable, and economical to perform.
  • the retort used in the reduction reaction and in the purification step is the same retort, and this retort is heated to operating temperatures while residing in the same furnace. Removal of impurities during the purification step is produced by vaporizing of these impurities, and relies upon sweeping of the retort with an inert gas at approximately atmospheric pressure (which may be defined herein as within the range of from atmospheric pressure to about 10 p.s.i. above atmospheric pressure) for bringing of the impurities out of the retort. Because of the pressure condition in the retort, heating during the reduction and purification steps need not be done in a vacuum furnace, but a conventional furnace may be used.
  • the shallow bed promotes better vaporization of impurities from the sponge during the purification step.
  • Another advantage of the type of retort disclosed is that the reactor grid covers a relatively large area, and presents a large filtration surface through which the magnesium chloride formed in the reaction may pass.
  • the sponge product is below a horizontal plane passing through the middle of the retort, it is easily removed by being forced upwardly into a region of wider dimension than the region the product originally occupied.
  • the magnesium chloride is not drained from the retort until at least about 60% of the titanium tetrachloride has been added. This tends to produce a more porous sponge product. If the magnesium chloride is drained earlier, the level of liquid magnesium in the reactor (which floats on magnesium chloride) tends to remain low, and new sponge tends to be produced on the addition of titanium tetrachloride in the interstices of already formed sponge to produce a dense product. With a more porous product, vaporization of impurities during the purification step is facilitated.
  • the invention further contemplates, in combination with the sweep system of withdrawing vaporized impurities from the retort, a unique method of removing impurities as particles from the gas utilized to sweep the retort.
  • cyclone units have been described where the impurities separate as particles and collect at the bases of the units.
  • a novel bypass of cool gas into the gas emanating from the retort is contemplated, producing initial cooling of the gas mixture and condensation of the impurities in such a manner that clogging of the outlet pipe for the retort is inhibited.
  • cooling of the inert gas is done in such a manner as to produce particles of impurities carried in a gas stream, and such particles are separated from the gas stream by gravity means.
  • cooling of the inert gas is performed by mixing gas leaving the retort with cooler inert gas from another source, with such mixing producing condensation of impurities while such are being carried along by the gas stream leaving the retort.
  • cool inert gas comprises circulated gas which bypasses the retort.
  • the steps comprising introducing into the retort mag nesium and titanium tetrachloride and heating the retort to an elevated temperature whereby the titanium tetrachloride reacts with the magnesium to produce titanium,

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US498500A 1965-10-20 1965-10-20 Reduction and purification of reactive metals Expired - Lifetime US3464813A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3880652A (en) * 1970-11-09 1975-04-29 Crucible Inc Method for purification of titanium sponge
FR2670802A1 (fr) * 1990-12-24 1992-06-26 Westinghouse Electric Corp Procede pour purifier une eponge de zirconium.

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
US2663634A (en) * 1950-05-27 1953-12-22 Nat Lead Co Production of titanium metal
US2745735A (en) * 1953-04-28 1956-05-15 Kaiser Aluminium Chem Corp Method of producing titanium
US2766113A (en) * 1953-02-11 1956-10-09 Dow Chemical Co Method of making titanium alloys
US2772875A (en) * 1953-02-18 1956-12-04 Levy Joseph Peppo Production of pure titanium and zirconium
US2778726A (en) * 1952-04-29 1957-01-22 Du Pont Purification of refractory metals
US2817585A (en) * 1953-10-23 1957-12-24 Du Pont Process of refining metals
US2982645A (en) * 1952-11-18 1961-05-02 Du Pont Titanium production
US2992098A (en) * 1957-11-22 1961-07-11 Titanium Metals Corp Purification of crude titanium metal
US3158671A (en) * 1954-08-12 1964-11-24 Montedison Spa Apparatus for producing titanium sponge
US3252823A (en) * 1961-10-17 1966-05-24 Du Pont Process for aluminum reduction of metal halides in preparing alloys and coatings

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
US2663634A (en) * 1950-05-27 1953-12-22 Nat Lead Co Production of titanium metal
US2778726A (en) * 1952-04-29 1957-01-22 Du Pont Purification of refractory metals
US2982645A (en) * 1952-11-18 1961-05-02 Du Pont Titanium production
US2766113A (en) * 1953-02-11 1956-10-09 Dow Chemical Co Method of making titanium alloys
US2772875A (en) * 1953-02-18 1956-12-04 Levy Joseph Peppo Production of pure titanium and zirconium
US2745735A (en) * 1953-04-28 1956-05-15 Kaiser Aluminium Chem Corp Method of producing titanium
US2817585A (en) * 1953-10-23 1957-12-24 Du Pont Process of refining metals
US3158671A (en) * 1954-08-12 1964-11-24 Montedison Spa Apparatus for producing titanium sponge
US2992098A (en) * 1957-11-22 1961-07-11 Titanium Metals Corp Purification of crude titanium metal
US3252823A (en) * 1961-10-17 1966-05-24 Du Pont Process for aluminum reduction of metal halides in preparing alloys and coatings

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3880652A (en) * 1970-11-09 1975-04-29 Crucible Inc Method for purification of titanium sponge
FR2670802A1 (fr) * 1990-12-24 1992-06-26 Westinghouse Electric Corp Procede pour purifier une eponge de zirconium.

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DE1533115A1 (de) 1969-11-20
DE1533115B2 (de) 1975-02-27
SE314209B (xx) 1969-09-01
DE1533115C3 (de) 1975-10-09
GB1127034A (en) 1968-09-11
FR1502781A (fr) 1967-11-24

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