EP0261042B1 - Procédé et dispositif de fabrication de zirconium métal par réduction de tétrachlorure de zirconium - Google Patents

Procédé et dispositif de fabrication de zirconium métal par réduction de tétrachlorure de zirconium Download PDF

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Publication number
EP0261042B1
EP0261042B1 EP87420240A EP87420240A EP0261042B1 EP 0261042 B1 EP0261042 B1 EP 0261042B1 EP 87420240 A EP87420240 A EP 87420240A EP 87420240 A EP87420240 A EP 87420240A EP 0261042 B1 EP0261042 B1 EP 0261042B1
Authority
EP
European Patent Office
Prior art keywords
chimney
hearth plate
sponge cake
reactor
cap
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
EP87420240A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0261042A1 (fr
Inventor
Jean Boutin
Pierre Brun
Airy-Pierre Lamaze
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.)
Compagnie Europeenne du Zirconium Cezus SA
Original Assignee
Compagnie Europeenne du Zirconium Cezus SA
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 Compagnie Europeenne du Zirconium Cezus SA filed Critical Compagnie Europeenne du Zirconium Cezus SA
Publication of EP0261042A1 publication Critical patent/EP0261042A1/fr
Application granted granted Critical
Publication of EP0261042B1 publication Critical patent/EP0261042B1/fr
Anticipated expiration legal-status Critical
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Classifications

    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/14—Obtaining zirconium or hafnium
    • 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 invention relates to a process and a device for manufacturing zirconium metal by reduction of Zr tetrachloride by molten magnesium in a reactor comprising a sole, and more particularly the process for the separation of magnesium chloride formed in the Zr reduction reaction. metal formed and residual magnesium, as well as the device allowing this separation.
  • Patent JP 78-035888 describes an apparatus for manufacturing Zr metal by reduction of ZrC1 4 by molten Mg, which comprises on the one hand an internal reaction cylinder containing at the end of the reaction the reduced sponge of Zr metal, the chloride of Mg molten and the magnesium metal not consumed by the reduction reaction, on the other hand an external cylinder placed in an oven with a reducing atmosphere.
  • This apparatus further comprises a siphon tube, the inner end of which is placed in a pot of the inner cylinder, a pot provided for the molten magnesium chloride to be kept there so as to prevent an overflow of molten Mg through the siphon tube, and the outer end of which is open in the space between the inner cylinder and the outer cylinder, so that the molten Mg chloride, produced continuously in the inner cylinder by the reaction of ZrC1 4 with the molten Mg which there is also introduced continuously, can be extracted from the inner cylinder by means of the siphon tube when the level of Mg chloride reaches a determined level at the other end of this siphon tube. The molten Mg chloride is then extracted from the outer cylinder by a pumping system.
  • the aim of the process of the invention is a simplification in which the use of such an external envelope is avoided, and in which the separation of the molten magnesium chloride from the Zr metal formed and the Mg residual metal is facilitated.
  • the subject of the invention is a process for the manufacture of metal zirconium by molten magnesium in a reactor or crucible comprising a hearth, this process typically comprising the following steps: the magnesium chloride formed in the reduction reaction is reduced from the Zr metal formed and magnesium, then the metal mass of Zr and Mg is subjected to vacuum evaporation, then the mass of metal Zr or "sponge bread" is cooled as well as the interior of the reactor (typically below 150 ° C), then extract the sponge Zr metal obtained.
  • the magnesium chloride formed is separated by drawing off towards the bottom of the reactor by means of a preferably substantially vertical chimney, the lower end portion of which is fixed to an orifice in the hearth and the opening of which
  • the high or usually transverse withdrawal opening is slightly above the portion of the metallic mass bordering the chimney at the end of the reduction reaction, and at the level of the layer of magnesium chloride which floats.
  • This upper opening of the chimney advantageously horizontal, is preferably surmounted by a covering cap which avoids the fall of Zr into the chimney, this cap being separated from this high opening and connected to the chimney by spaced supports, leaving between them passages to the withdrawal opening sufficient for the flow of magnesium chloride.
  • the metallic mass surrounding the chimney is then a pseudo-alloy (Zr, Mg) consisting essentially of globules of Zr distributed in the magnesium metal, and it is pasty at the temperature of the reduction reaction, that is to say between 750 and 850 ° C approximately.
  • Zr, Mg pseudo-alloy
  • This mass of pseudo-alloy itself corresponds to the maximum weight and volume of sponge Zr that we want to obtain at the end of treatment.
  • the difference in level of the chimney withdrawal opening, with respect to the maximum level of the pseudo-alloy in this location is typically at least 10 mm, and preferably between 10 and 50 mm, and more preferably between 25 and 40 mm, and the internal diameter of the chimney and in particular of its withdrawal opening is preferably between 50 and 250 mm in the case of a reactor with maximum internal diameter between 1000 and 2000 mm.
  • the magnesium chloride withdrawn from the chimney flows to the bottom of the crucible, where it is taken up by suction.
  • the racking chimney according to the invention can be provided with lifting means, which makes it possible to extract the sponge bread from the top of the crucible and thus avoid its overturning.
  • These lifting means comprise at least, above the high end of the chimney bordering its withdrawal opening, a gripping or lifting part of the same general shape and the same role as the usual cover cap and its supports spaced apart, but of mechanical strength and structure specially adapted for lifting the whole (chimney + Zr sponge bread) or possibly the whole (chimney + Zr sponge bread + sole).
  • This lifting part thus typically consists of a horizontal part or cap with a thickness greater than or equal to 10 mm and typically between 10 and 25 mm, connected to the upper end of the chimney by an openwork connecting portion so as to be able to introduce through the openings in this connecting portion, a lifting means, for example a key, this connecting portion itself comprising at least 2 tabs, these tabs each having at any level a horizontal cross section greater than 400 mm2.
  • the lifting means may further comprise one or more reliefs for supporting the sponge bread, relief (s) preferably based on this on the hearth so as to consolidate the base of the chimney during the reduction operation.
  • the chimney must also have sufficient mechanical strength for the mass to be lifted.
  • the invention also relates to the device used in this process, device comprising a reactor comprising a hearth, as well as means for sublimation of Zr tetrachloride and means for bringing this gaseous tetrachloride into the reactor enclosure, means for separating the magnesium chloride formed from the metal Zr formed and magnesium, heating means and vacuum means, device according to the invention, the means for separating the magnesium chloride comprise a chimney the lower end portion is fixed to an orifice in the hearth and the upper end of which is slightly above the upper level of the portion of the metallic mass (Zr, Mg) bordering the chimney at the end of the reduction reaction .
  • the features and variants of this device are those already described with regard to the method of the invention.
  • FIG. 1 we can see a reactor (1) of cylindrical inner side surface (2) provided with a hearth (3) having a central orifice (4) in which is embedded the lower end portion (5) d '' a chimney (6) according to the invention, chimney (6) whose open transverse high end (7) is at a level corresponding to the level of the layer of magnesium chloride which floats above the metallic mass comprising Zr and Mg at the end of the reduction reaction, necessarily above the top of the internal edge of said metallic mass so that the flow of magnesium chloride does not entail this metallic mass or "pseudo-alloy" (Zr, Mg) .
  • the chimney (6) Above its lower end portion (5) thus embedded in the orifice (4) of the hearth (3), the chimney (6) has a flange (8) resting on the hearth (3) and wide enough to allow the lifting of the sponge by the chimney (6), then a cylindrical part (9) ending with the open end high trans versal (7) located above the metallic mass of Zr and Mg bordering this chimney (6) at the end of the reaction.
  • This open end (7) being surmounted by a perforated connection portion (11), itself surmounted by a cap (12), in the days or lateral openings (13) of the perforated connection (11), it is possible to make pass a lifting means (14) for example a key ( Figure 2).
  • FIG. 1 a pipe or means for injecting ZrC1 4 in the form of vapor from a sublimation device has also been shown diagrammatically, and the levels (16, 17) between which, reduction reaction of ZrC1 4 by Mg, giving rise to small clusters of reduced Zr (18) typically from 5 to 20 ⁇ m.
  • the magnesium chloride which has formed and condensed floats above the metallic mass (Zr, Mg) s, that is to say above the upper surface (20), and it flows from the open end (17) of the chimney (6), passing through the side openings (13) located between this open end (7) and the cap (12).
  • the magnesium chloride is sucked into the bottom of the reactor (1) by a pipe or conduit (21) which discharges it during the reactor (1) by means of suitable vacuum means.
  • the means for closing the top of the reactor (1) during the reduction reaction and then during vacuum evaporation, as well as the pumping means from the top and the heating means, are not shown.
  • Figures 3 and 4 show in a simplified way the sole (3) provided with the chimney (6) and on the one hand ( Figure 3) the metallic mass (Zr, Mg) (22) after reduction and before evaporation, on the other share (FIG. 4) in a comparative manner the mass or cake of Zr (23) or "zirconium sponge” after evaporation under vacuum.
  • the presence of the chimney (6) creates an internal lateral evaporation surface (24) in addition to the external lateral surface (25) and the upper surface (20). This results in the evaporation-sublimation of magnesium a decrease in the central annular volume (240), the inner lateral surface (24) which borders it having at the end of evaporation a shape (241) in inverted truncated cone .
  • the decrease in volume is in fact, by the game of evaporation and release of vapors, all the more important as one approaches the top of the metallic mass during evaporation then at the end of evaporation ( 23).
  • the additional surface of evaporation thus due to the chimney (6), surface evolving from the initial geometry (24) to the final geometry (241), typically represents an increase in the surface of evaporation from 12 to 25%.
  • the reactor (1) is made of AISI 302 type steel with a thickness of 25 mm and it has an internal diameter of 1.6 m in its cylindrical central part, an internal height of 3 m, and it has at 350 mm from its bottom a sole (3) made of stainless steel with a total thickness of 30 mm having a central hole (4) with a diameter of 200 to 200.5 mm.
  • the stainless steel chimney (6), the lower end portion (5) of which is embedded in the orifice (4) has a total height of 750 mm and a cylindrical central inner surface with a diameter of 150 mm.
  • the lower end portion (5) is 40 mm high and has a diameter of 199.8 to 200 mm, it is immobilized relative to the sole (3) by its embedding.
  • This lower portion (5) is surmounted by a collar (8) with an external diameter of 240 mm and a thickness of 10 mm resting on its bottom on its base (3), then with the slightly frustoconical part (9) with external diameter.
  • connection portion (11) consisting of 4 openings (13), and also in 4 connection tabs (110) spaced 10 mm thick, 40 mm wide and 40 mm high, lugs (110) themselves surmounted by a cap (12) 20 mm thick.
  • the magnesium chloride which has flowed through the chimney (6) was removed in 5 to 8 times by pumping from the bottom of the reactor (1), by means of a conduit (21).
  • the residual Mg and MgCl 2 are evaporated under vacuum, heating as usual by the side surface of the reactor and maintaining the temperature between 1000 and 1100 ° C.
  • zirconium sponge At the end of this vacuum operation phase, a mass of 3990 kg of metallic zirconium is obtained, known as "zirconium sponge" because of its vacuolar structure, having the following geometry: height near the chimney (6) 400 mm, height near the inner side surface (2) of the reactor (1) 600 mm, distance from the chimney (6) increasing from 10 mm at the flange (8) to 25 mm at the junction of the inner side surface (24) and its upper surface (201).
  • the evaporation time can also be shortened by 5 to 10% by using the chimney (6) of the invention.
  • the interior of the reactor and the sponge cake (23) are cooled, optionally using one or more fillings of neutral gas to accelerate the cooling, and preferably brought to atmospheric pressure. below 150 ° C.
  • the upper reactor cover (1) being removed, the ingot is then lifted from the top of the chimney (6), by means of a key (14) passing through the lateral openings (13 ) between the open end (7) and the cap (12) of the chimney (6) and known lifting means.

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  • 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)
EP87420240A 1986-09-19 1987-09-16 Procédé et dispositif de fabrication de zirconium métal par réduction de tétrachlorure de zirconium Expired - Lifetime EP0261042B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8613306A FR2604184B1 (fr) 1986-09-19 1986-09-19 Procede et dispositif de fabrication de zirconium metal par reduction de tetrachlorure de zirconium
FR8613306 1986-09-19

Publications (2)

Publication Number Publication Date
EP0261042A1 EP0261042A1 (fr) 1988-03-23
EP0261042B1 true EP0261042B1 (fr) 1990-09-12

Family

ID=9339211

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EP87420240A Expired - Lifetime EP0261042B1 (fr) 1986-09-19 1987-09-16 Procédé et dispositif de fabrication de zirconium métal par réduction de tétrachlorure de zirconium

Country Status (9)

Country Link
US (2) US4752331A (xx)
EP (1) EP0261042B1 (xx)
JP (1) JPS6386828A (xx)
KR (1) KR910001609B1 (xx)
AU (1) AU592892B2 (xx)
CA (1) CA1323199C (xx)
DE (1) DE3764916D1 (xx)
FR (1) FR2604184B1 (xx)
ZA (1) ZA876996B (xx)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060188436A1 (en) * 2005-02-18 2006-08-24 Linnard Griffin Apparatus and method for the production of hydrogen
US20050042150A1 (en) * 2003-08-19 2005-02-24 Linnard Griffin Apparatus and method for the production of hydrogen
US20050109162A1 (en) * 2003-11-24 2005-05-26 Linnard Griffin Apparatus and method for the reduction of metals
KR100976825B1 (ko) * 2009-11-18 2010-08-20 한국기계연구원 스폰지 형태의 고순도 금속 지르코늄의 제조방법, 및 이에 의한 고순도 금속 지르코늄의 제조장치
CN110550911A (zh) * 2019-09-30 2019-12-10 周学东 一种海绵砖的制备方法

Family Cites Families (16)

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US1049181A (en) * 1912-03-11 1912-12-31 Gustav Wallin Motor.
US1187875A (en) * 1915-03-27 1916-06-20 Elbert E C Welty Folding chicken-coop.
FR1049181A (fr) * 1952-01-16 1953-12-28 Electro Metallurg Du Planet So Méthode et appareil pour l'élaboration du titane
US2825642A (en) * 1954-03-09 1958-03-04 Du Pont Method of producing group iv-a metals
US3158671A (en) * 1954-08-12 1964-11-24 Montedison Spa Apparatus for producing titanium sponge
DE1124247B (de) * 1956-10-23 1962-02-22 Femipari Ki Vorrichtung und Verfahren zur Herstellung von Titan
US3692294A (en) * 1971-02-16 1972-09-19 Nippon Mining Co Apparatus for production of zirconium metal
FR2126061A1 (en) * 1971-02-22 1972-10-06 Nippon Mining Co Zirconium appts - permitting discharge of magnesium chloride
US3966460A (en) * 1974-09-06 1976-06-29 Amax Specialty Metal Corporation Reduction of metal halides
JPS585252B2 (ja) * 1975-02-13 1983-01-29 ニホンコウギヨウ カブシキガイシヤ ジルコニウムスポンジルイノ セイゾウホウホウ オヨビ ソノソウチ
US4242136A (en) * 1979-04-10 1980-12-30 Hiroshi Ishizuka Process for producing metallic zirconium
CA1179144A (en) * 1981-04-04 1984-12-11 Hiroshi Ishizuka Method and an apparatus for producing titanium metal from titanium tetrachloride
JPS58189340A (ja) * 1982-04-28 1983-11-05 Hiroshi Ishizuka 金属塩化物から金属を得る方法
US4447045A (en) * 1982-07-21 1984-05-08 Mitsubishi Kinzoku Kabushiki Kaisha Apparatus for preparing high-melting-point high-toughness metals
JPS59226127A (ja) * 1983-04-27 1984-12-19 Mitsubishi Metal Corp 高融点高靭性金属の製造装置
US4668287A (en) * 1985-09-26 1987-05-26 Westinghouse Electric Corp. Process for producing high purity zirconium and hafnium

Also Published As

Publication number Publication date
US4752331A (en) 1988-06-21
EP0261042A1 (fr) 1988-03-23
KR910001609B1 (ko) 1991-03-16
ZA876996B (en) 1988-03-21
AU7837587A (en) 1988-03-24
US4893790A (en) 1990-01-16
AU592892B2 (en) 1990-01-25
JPS6386828A (ja) 1988-04-18
CA1323199C (fr) 1993-10-19
KR880004116A (ko) 1988-06-01
FR2604184A1 (fr) 1988-03-25
FR2604184B1 (fr) 1988-11-10
DE3764916D1 (de) 1990-10-18
JPH0261530B2 (xx) 1990-12-20

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