US2766033A - Apparatus for production of titanium metal - Google Patents

Apparatus for production of titanium metal Download PDF

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Publication number
US2766033A
US2766033A US251903A US25190351A US2766033A US 2766033 A US2766033 A US 2766033A US 251903 A US251903 A US 251903A US 25190351 A US25190351 A US 25190351A US 2766033 A US2766033 A US 2766033A
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US
United States
Prior art keywords
pot
cover
reaction
reaction pot
titanium metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US251903A
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English (en)
Inventor
John C Priscu
Junior W Whitney
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NL Industries Inc
Original Assignee
Nat Lead Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nat Lead Co filed Critical Nat Lead Co
Priority to US251903A priority Critical patent/US2766033A/en
Priority to GB25255/52A priority patent/GB714993A/en
Priority to FR1064294D priority patent/FR1064294A/fr
Priority to CH317956D priority patent/CH317956A/de
Application granted granted Critical
Publication of US2766033A publication Critical patent/US2766033A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S266/00—Metallurgical apparatus
    • Y10S266/905—Refractory metal-extracting means

Definitions

  • the present invention relates in general to the production of titanium metal and, more particularly, to improved apparatus for reacting titanium tetrachloride with magnesium metal.
  • titanium tetrachloride is reacted with a reducing metal, such as magnesium or calcium, in a retort under normal pressure to form a titanium metal sponge in the presence of the chlorides of the reacting metal.
  • a reducing metal such as magnesium or calcium
  • These lumps of metal are then subjected to prolonged leaching treatments to separate the titanium metal from the occluded metallic chlorides.
  • This process is not only costly and time-consuming but the titanium metal recovered by this process is frequently of inferior quality due to the prolonged exposure of the metal to the atmosphere during the removal of the sponge from the reaction pot and the subsequent leaching operations.
  • An object of the invention is to provide improved apparatus for producing substantially pure titanium metal in an economical and efficient manner.
  • a still further object of the invention is to provide improved reducing and distilling apparatus for forming substantially pure titanium metal wherein the reduction of titanium tetrachloride with magnesium metal and the subsequent removal of the residual reaction products from the titanium metal sponge by distillation is carried out without exposing the titanium metal to the atmosphere and without loss of the reaction products and/or the titanium metal from the reaction pot.
  • FIG. 1 is a front elevation in section of the improved reduction and distillation apparatus of this invention, showing the cover of the reaction pot in its closed position;
  • Fig. 2 is a top plan View of the apparatus of Fig. 1;
  • Fig. 3 is a transfer section of the apparatus on line 33 of Fig. 1;
  • Fig. 4 is a perspective view of the collar of the reaction
  • Fig. 5 is a perspective view of the base plate to the reaction pot
  • Fig. 6 is a perspective view of the inverted cover of the reaction pot.
  • the improved apparatus of this invention comprises a casing, indicated generally at 10, which is a hollow, substantially cylindrical member, as shown on Figs. 1, 2 and 3, having a base-portion 11 at its lower end of reduced cross-section; and a head-portion 12 at its upper end of enlarged cross-section.
  • Both the base-portion 11 and the head-portion 12 are closed by end walls 13 and 14 respectively which are detachably secured, by bolts or equivalent fastening-means 15 and 16, to the corresponding ends of the casing to seal the latter from the atmosphere.
  • the casing and end walls are formed of heavy gauge mild sheet steel but it Will be understood that any other suitable material may be used.
  • Extending substantially laterally from one wall of the enlarged head-portion 12 of the casing is an elbow shaped conduit, indicated generally at 17, the inner end of which intersects the enlarged head-portion of the casing and the outer end of which is flanged so as to be connected into a vacuum line (not shown) for evacuating the air from the casing and maintaining subatrnospheric pressure therein.
  • the enlarged head-portion 12 of the casing constitutes the condensing zone of the apparatus as and for the purpose hereinafter described.
  • the casing is provided on its inner wall with a plurality of annular reinforcing rings 18 in vertically spaced relationship for reinforcing the wall of the casing.
  • the reaction zone of the apparatus is identified by a reaction pot indicated generally at 1?.
  • the latter is a container in which the reaction of the titanium tetrachloride with the magnesium metal takes place and preferably comprises a relatively heavy gauge stainless steel cylindrical shell 29 closed at its bottom by a separable base-plate and at its top by a removable cover as hereinafter described.
  • the overall diameter of the shell of the pot is less than the inside diameter of the casing so that when the reaction pot is mounted therein there will be an annular clearance space 21 between the outer wall of the reaction pot shell and the reinforcing rings 13 of the casing as shown in Fig. l.
  • the overall length of the reaction pot is shown as being substantially one-third the overall length of the casing such that the reaction pot is adapted to be mounted therein intermediate its lower reduced end and its upper enlarged head-portion.
  • the upper end of the cylindrical wall of the reaction pot shell is preferably formed as a separable collar 2% the lower end of which is adapted to slip into the open upper end of the cylindrical shell of the reaction pot 19 and to be supported therein by an annular external head 24)! arranged to seat on the upper edge of the pot.
  • the upper end of the separable pot collar Ztla is open and provided with an annular inwardly turned flange 22 which is substantially inverted V shaped in cross-section and provides an annular outwardly and downwardly sloping cover-seat 23, and an annular inwardly and downwardly sloping flow-control lip 24.
  • a separable pot collar is lid/766,033
  • the pot collar may be formed as an integral part thereof.
  • the lower end of the cylindrical reaction pot shell is also open and is adapted to rest upon a substantially flat circular base-plate 25 which serves as an end-wall for closing the lower end of the reaction pot shell whenever the latter is mounted thereon, the base-plate 25 being, in turn, mounted on suitable supporting means indicated generally at 26.
  • the supporting means 26 comprises a pair of I-beams secured in spaced, substantially parallel relationship in the lower part of the casing; and an apertured supporting-plate resting on the I-oearns and serving as a support for the aforesaid base-plate 25.
  • the base-plate is essentially dish-shaped and comprises a disk having an annular upstanding peripheral flange 27 the upper edge of which constitutes a substantially flat annular seat which serves to support the lower end of the reaction pot shell.
  • the annular flange 27 may constitute a separate ring-shaped member fastened to the base-plate disk by a welded joint or the like.
  • the joint formed between the lower end of the reaction pot shell and the annular seat of the base-plate is elevated above the plane of the base-plate.
  • This construction insures against the molten magnesium metal and magnesium chloride leaking out from beneath the lower end of the reaction pot shell during the initial stages of the reaction and accumulating between the walls of the pot and the casing. Thereafter, as the titanium metal sponge begins to form over the bottom of the base-plate and to extend up the side walls of the reaction pot, it automatically seals off the joint between the reaction pot shell and the base-plate, thereby preventing the egress of molten magnesium products therefrom during the remainder of the reaction.
  • the practical convenience of a reaction pot having a separable base-plate is retained while avoiding the severe losses of molten magnesium products and titanium metal sponge which have been experienced with earlier types of reaction pots.
  • the baseplate 25 is provided with a vertical aperture 28 which is adapted normally to be closed by valve-means, such as, for example, a tapered plug 29 adapted to be actuated externally of the apparatus by operating-means, such as, for example, a rod 30 which is attached at its lower end to the plug and extends upwardly through a fluid tight seal 39 in the casing in the manner shown.
  • valve-means such as, for example, a tapered plug 29 adapted to be actuated externally of the apparatus by operating-means, such as, for example, a rod 30 which is attached at its lower end to the plug and extends upwardly through a fluid tight seal 39 in the casing in the manner shown.
  • the upper open end of the reaction pot is adapted to be selectively closed and opened by means of a cover 31 so that during initial stages of the operation the reacting products in the reaction pot may be confined therein by closing the cover on the pot.
  • the cover is adapted to be raised to permit the reaction products to be distilled therefrom in the manner hereinafter described.
  • the cover 31 of the pot comprises a relatively thick disk-shaped member formed of cast iron or equivalent material and provided with a substantially central aperture 32 extending substantially vertically therethrough.
  • the under side of the cover is adapted to be suitably shaped to control the egress of volatile chlorides from the reaction pot when the cover is lifted, and in one form of the invention the under side or bottom of the cover is provided with an inverted substantially conical-shaped center-protuberance 33, the periphery of which comprises an annular flange 34, the slope of which is opposite to that of the conical protuberance and corresponds substantially to the slope of the cover-seat 23 on the upper end of the reactive pot collar.
  • the annular reverse flange 34 of the cover makes a relatively close fit with the cover-seat of the reaction pot collar to prevent the escape of the volatile products of the reaction.
  • the surface of the cone-shaped center protuberance 33 of the cover in conjunction with its reverse flange 34, will direct the volatile chlorides upwardly and outwardly away from the central aperture 32 in the cover thus inducing the volatile chlorides to flow up into the condensing portion of the casing thereby minimizing the escape of the volatile chlorides from the reaction pot by way of the central feed pipe hereinafter described.
  • a substantially cylindrical guide-sleeve 35 Extending upwardly from the top surface of the cover and circumscribing the central aperture 32 thereof, is a substantially cylindrical guide-sleeve 35 which is adapted to slidingly engage the exterior walls of a cylindrical feed pipe 36 which is secured at its upper end in the end wall 14 of the casing and extends downwardly therefrom with its lower end terminating adjacent the upper end of the reaction pot.
  • the diameter of the feed pipe 36 is slightly less than the diameter of the guide-sleeve 35 and the central aperture 32 of the cover so that the latter may slide up and down on the feed pipe.
  • the feed pipe 36 constitutes guide-means for the cover. As shown especially well in Figs.
  • the upper end of the feed pipe 36 is provided with a lateral branch 37 which intersects the end wall 14 of the casing and which is used to feed volatile titanium tetrachloride into the reaction pot; the main portion of the feed pipe constituting feed-means for delivering solid pieces of magnesium or sodium metal into the reaction pot.
  • the portion of the feed pipe which extends above the top end wall 14 of the casing is provided with an air lock chamber, indicated schematically at 38, whereby the magnesium metal may be introduced into the feed pipe without permitting the admission of air into the reaction pot.
  • a pair of lifting rods 4 )40 are provided, the lower ends of which are secured in the cover at substantially diametrically opposite points thereof.
  • the upper ends of the lifting rods 4040 project upwardly through suitable apertures in the end wall 14 of the casing and are provided at their upper extremities with lifting rings 41 by means of which the lifting rods may be engaged for lifting and lowering the cover of the reaction pot.
  • each lift-rod aperture in the end wall 14 of the casing is sealed by a sealing gland 42.
  • one or both of the lift rods may be provided with an adjustable clamp, such as indicated at 43, which may be tightened on one of the lift rods at any predetermined position thereon and by engagement with the corresponding sealing gland of the casing thus serve to hold the cover of the pot in open position.
  • an adjustable clamp such as indicated at 43
  • the cover 31 is lowered into engagement with the cover-seat on the upper end of the reaction pot collar to close the latter whereupon magnesium metal billets are introduced into the pot through the feed pipe 36 by way of the air lock 38.
  • Titanium tetrachloride vapors are then fed into the pot by way of the branch pipe 37 of the feed pipe and are reacted with the magnesium metal in the reaction pot.
  • ture in the reaction pot may be controlled by adjusting the temperature of the furnace, indicated generally at 44, in which the assembled casing and reaction pot are mounted. Titanium metal, molten magnesium and magnesium chloride are formed in the reaction pot as reac tion products.
  • the dish-shaped The temperasynapse base-plate constitutes, in efiect, a reservoir which retains the molten magnesium products against leaking out of the joint formed between the upper edge of the base-plate .and the lower end of the pot shell during the initial stages of the reaction.
  • the titanium sponge formed on the bottom and side walls of the pot automatically seals the joint between the upper edge of the base-plate and thelower end of the reaction pot shell.
  • the'plug 29in the base-plate may be withdrawn periodically to allow the magnesium chloride being formed to drain out of the pot, the molten magnesium chloride being collected in the lower reduced end of the casing in which it solidifies.
  • the volume of the magnesium chloride in the pot may be controlled and preferably kept at an optimum minimum value to insure maximum production of titanium metal, maximum efliciency of reaction and most efiicacious sponge density.
  • the provision of a cover one the reaction pot efiectively prevents the reacting products from escaping thereby etfecting an increased economy in production.
  • the flowcontrol lip of the reaction pot likewise aids in preventing the reacting materials from spilling over the rim of the reaction pot and being lost against recovery.
  • the magnesium chloride which does not drain through the aperture in the bottom of the base-plate and the unreacted magnesium metal occluded in the titanium metal sponge may then be removed from the titanium metal sponge by distillation.
  • This is readily effected without exposing the titanium metal to the atmosphere by lifting the cover 31 upwardly away from the open upper end of the reaction pot whereupon the subatmospheric pressure in the casing causes the unreacted magnesium metal and the residual magnesium chloride to vaporize and rise upwardly from the titanium sponge and to condense on the walls of the head-portion of the casing and/or be carried ofi by way of the evacuating-means thereof.
  • the titanium metal in the reaction pot is thus left in a substantially purified state.
  • the latter is removed from the casing, whereupon its separable collar 20a and base-plate 25 are removed leaving a substantially straight cylindrical shell from which the metal sponge may be readily removed.
  • the production of substantially pure titanium metal sponge by reaction of titanium tetrachloride with magnesium metal may be carried out under controlled conditions, in the absence of contact with the atmosphere and with substantially no leakage of the reacting products from the reaction pot.
  • the improved apparatus of this invention thus provides for the production of substantially pure titanium metal efliciently and economically and actual test runs on the the apparatus have shown an efiiciency as high as 97% based on the recovery of titanium.
  • an apparatus for producing titanium metal by reacting titanium tetrachloride with a reducing metal including: a substantially air-tight unitary enclosure having a head portion at its upper end defining a condensing zone; evacuating means connected to said head portion to evacuate the condensing zone; a base portion at the lower end of said enclosure; a reaction pot supported in said enclosure between said head portion and said base portioma cover for said reaction pot, said cover having a central aperture extending therethrough; a reactant feed pipe fixedly supported in said head portion and arranged to extend through the aperture of said cover both to feed the reactants into said reaction pot and to constitute guide means for movement of said cover vertically relative to said pot; pot cover operating means arranged externally of said air-tight enclosure to move said pot cover relative to said pot; and means to heat the reactants in said reaction pot to form volatile reactants and titanium metal therein, said evacuating means being arranged to evacuate said condensing zone when said pot cover is raised relative to said reaction pot,
  • an apparatus for producing titanium metal by reacting titanium tetrachloride with a reducing metal including: a substantially air-tight unitary enclosure having a head portion at its upper end defining a condensing zone; evacuating means connected to said head portion to evacuate the condensing zone; a base portion at the lower end of said enclosure; a reaction pot supported in said enclosure between said head portion and said base portion; a collar on the upper end of said reaction pot, said collar having an inwardly extending lip; a cover for said reaction pot, said cover having a central aperture extending therethrough and a downwardly projecting protuberance arranged to seat on the inwardly projecting lip of said reaction pot collar; a reactant feed pipe secured in the head portion of said enclosure, said feed pipe being arranged to extend through the aperture of said cover both to feed the reactants into said reaction pot and to constitute guide means for movement of said cover vertically relative to said pot; pot cover operating means arranged externally of said air-tight enclosure to move the protuberance of
  • an apparatus for producing titanium metal by reacting titanium tetrachloride with a reducing metal including: a substantially air-tight unitary enclosure having a head portion at its upper end definmg a condensing zone; evacuating means connected to said head portion to evacuate the condensing zone; a base portion at the lower end of said enclosure; a reaction pot supported in said enclosure between said head portion and said base portion, said reaction pot com prising a substantially cylindrical shell open at its upper and lower ends, a base plate arranged to be removably supported against the bottom open end of said shell, and a collar arranged to be removably supported on the upper open end of said shell, said collar having an inwardly and downwardly inclined lip; a cover for said reactor pot, said cover having a central aperture extending therethrough, and a downwardly projecting protuberance arranged to seat on the inwardly projecting lip of said reaction pot cellar; a reactant feed pipe secured in the head portion of said enclosure, said feed pipe being

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  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US251903A 1951-10-18 1951-10-18 Apparatus for production of titanium metal Expired - Lifetime US2766033A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US251903A US2766033A (en) 1951-10-18 1951-10-18 Apparatus for production of titanium metal
GB25255/52A GB714993A (en) 1951-10-18 1952-10-08 A new or improved apparatus and method for the production of titanium metal
FR1064294D FR1064294A (fr) 1951-10-18 1952-10-10 Appareil pour la préparation du titane métallique
CH317956D CH317956A (de) 1951-10-18 1952-10-17 Einrichtung zur Herstellung von metallischem Titan

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US251903A US2766033A (en) 1951-10-18 1951-10-18 Apparatus for production of titanium metal

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CH (1) CH317956A (fr)
FR (1) FR1064294A (fr)
GB (1) GB714993A (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3245673A (en) * 1962-06-18 1966-04-12 Wyandotte Chemicals Corp Reduction apparatus

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1202183A (fr) * 1982-05-31 1986-03-25 Hiroshi Ishizuka Dispositif et methode de production d'un metal refractaire affine a partir de son chlorure

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US243850A (en) * 1881-07-05 claek
US503556A (en) * 1893-08-15 Apparatus for treating pulverulent materials with gases
US1731223A (en) * 1928-07-21 1929-10-08 United Gas Improvement Co Apparatus for effecting contact between gases and divided solids
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
US2243406A (en) * 1938-09-14 1941-05-27 Wolf Harry Comer Apparatus for unlocking ore bodies to extract sulphur and iron therefrom
CH220334A (fr) * 1938-01-16 1942-03-31 Louis Gentil Henri Four métallurgique.
US2493823A (en) * 1947-04-02 1950-01-10 Nat Zinc Company Inc Process for zinc smelting
US2556763A (en) * 1948-06-30 1951-06-12 Battelle Development Corp Production of refractory metals
US2564337A (en) * 1948-11-02 1951-08-14 Battelle Development Corp Production of refractory metals

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US243850A (en) * 1881-07-05 claek
US503556A (en) * 1893-08-15 Apparatus for treating pulverulent materials with gases
US1731223A (en) * 1928-07-21 1929-10-08 United Gas Improvement Co Apparatus for effecting contact between gases and divided solids
US2205854A (en) * 1937-07-10 1940-06-25 Kroll Wilhelm Method for manufacturing titanium and alloys thereof
CH220334A (fr) * 1938-01-16 1942-03-31 Louis Gentil Henri Four métallurgique.
US2243406A (en) * 1938-09-14 1941-05-27 Wolf Harry Comer Apparatus for unlocking ore bodies to extract sulphur and iron therefrom
US2493823A (en) * 1947-04-02 1950-01-10 Nat Zinc Company Inc Process for zinc smelting
US2556763A (en) * 1948-06-30 1951-06-12 Battelle Development Corp Production of refractory metals
US2564337A (en) * 1948-11-02 1951-08-14 Battelle Development Corp Production of refractory metals

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3245673A (en) * 1962-06-18 1966-04-12 Wyandotte Chemicals Corp Reduction apparatus

Also Published As

Publication number Publication date
FR1064294A (fr) 1954-05-12
GB714993A (en) 1954-09-08
CH317956A (de) 1956-12-15

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