EP0061411A1 - Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall - Google Patents

Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall Download PDF

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Publication number
EP0061411A1
EP0061411A1 EP82420037A EP82420037A EP0061411A1 EP 0061411 A1 EP0061411 A1 EP 0061411A1 EP 82420037 A EP82420037 A EP 82420037A EP 82420037 A EP82420037 A EP 82420037A EP 0061411 A1 EP0061411 A1 EP 0061411A1
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EP
European Patent Office
Prior art keywords
injection
halogenated
liquid metal
vaporizer
ccl
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.)
Granted
Application number
EP82420037A
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English (en)
French (fr)
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EP0061411B1 (de
Inventor
Gilbert Pollet
Pierre Du Manoir
Pierre Guerit
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Servimetal SA
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Servimetal SA
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Application filed by Servimetal SA filed Critical Servimetal SA
Priority to AT82420037T priority Critical patent/ATE20541T1/de
Publication of EP0061411A1 publication Critical patent/EP0061411A1/de
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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
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • 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
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • C22B21/064—Obtaining aluminium refining using inert or reactive gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • 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
    • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ

Definitions

  • the present invention relates to a method and an apparatus for the precise injection, into a liquid metal, of halogenated derivatives, liquid or in solution.
  • the present invention belongs to this second category. Indeed, the handling and use of chlorine in foundry workshops poses safety, hygiene, pollution and corrosion problems which encourage us to seek other solutions.
  • anhydrous metal chlorides such as TiCl 4 , A1C1 3 , MnCl2, and organic derivatives such as CCl 4 (carbon tetrachloride), C 2 Cl 4 (perchlorethylene) or C 2 Cl 6 were used ( hexachloroethane).
  • This product which is solid at ordinary temperature, sublimes around 187 ° C. For this reason, it is usually introduced into aluminum in the form of pellets arranged in a chamber through which the liquid metal passes, or, by means of '' a perforated bell, made of graphite, which is lowered into the liquid metal.
  • its volatilization and thermal cracking are extremely rapid and require little more than 2 to 3 minutes. But this speed excludes any possibility of precise dosing and, above all, of continuous action on a stream of liquid aluminum.
  • the doses used are much greater than the quantity actually necessary, the excess requires effective capture.
  • the invention is based on the use of a halogenated substance which is liquid at room temperature and has an Cl / C atomic ratio at least equal to 2 and preferably between 2 and 4.
  • the process which is the subject of the invention consists in taking the halogenated substance or the halogenated solution, liquid at room temperature, in introducing it, by means of a metering micropump, into a vaporizer brought to a temperature such as the substance is brought to a temperature higher than its vaporization temperature and to inject the vapor, under the action of a current of inert gas, into the liquid metal to be treated.
  • halogenated substance a defined chemical species, or a mixture of defined chemical species, composed of carbon and at least one halogen chosen from chlorine and fluorine.
  • the apparatus for implementing the process comprises a reservoir of liquid halogenated substance, a micro metering pump, a reactor provided with a heating means, a source of inert pressurized gas, provided with a means for adjusting the pressure and flow, and a means of injection into the liquid metal to be treated.
  • Figure 1 shows schematically the apparatus. It consists of: a tank (1) fitted with a tight cover (2), a closable nozzle (3) for filling, a level gauge (4); a sampling tube (5), fitted with a shut-off valve (6), is connected to a piston metering micropump (7) which can collect and precisely inject the halogenated substance (8), to a rate which can be, for example, between 0.1 and 10 milliliters per minute, without these values constituting a limitation of the invention.
  • the liquid halogenated substance (8) passes through a non-return valve (9) and enters the vaporizer (10) provided with a regulated and thermostatically controlled heating means (11), of any known type, for example with electrical resistance.
  • An inert gas such as nitrogen, argon or helium, taken from the pressurized storage means (12) using a pressure reducer (13) and a flow meter (14), also enters the reactor where it mixes with the vapors. of the halogenated substance and drives them, via the injection pipe (15) to the injection means (16) which can be, for example, a graphite rod, immersed in the liquid metal (17) passing through the treatment (18).
  • a variant of the device, for higher treatment gas flow rates consists in adding to the system described above, an additional flow of gas: nitrogen, argon or helium, introduced downstream of the vaporizer (10) by a nozzle. (24) on the pipe (15); this allows, in the operating range of the micro-pump, to ensure the desired amount of halogen with a predetermined dilution level without passing the entire gas flow through the vaporizer.
  • This solution has the advantage of a higher chlorine content by weight than that of pure C 2 C1 4 , while retaining the advantage of the liquid state, which allows its precise injection by a metering pump. If you want to keep the mixture its liquid state at temperatures close to ambient, you can introduce up to about 500 grams / liter of C 2 Cl 6 .
  • the halogenated substance may also consist, partially or wholly, of chlorofluorinated derivatives, and in particular CC1 3 F, CCl 3 -CF 3 , CCl 2 F-CClF 2 , CCl 3 -CClF 2 , CC1 2 F-CC1 2 F , CCl 3 -CCl 2 F, whose boiling points range from 24 to 138 ° C.
  • the injection pump is a positive displacement piston pump designed to deliver precisely small volumes of predetermined liquid and with a reliability of ⁇ 1% by volume.
  • a diaphragm pump could also be used.
  • the vaporizer preferably comprises a spiral tube or a bundle of parallel tubes, so that the halogenated substance and the carrier gas can exit therefrom at a temperature which can reach 200 ° C. and even beyond, if this is necessary, but sufficient to avoid any condensation and which must be adapted to the halogenated derivative chosen and to the pressure under which the injection is carried out.
  • the heating is ensured by an electric resistance regulated from a temperature sensor arranged on the path of the gases leaving the. spray.
  • the injection into the liquid metal can be carried out by various known means, for example, by a graphite rod (16) disposed in the upstream compartment (19) of the treatment bag (18) into which the metal to be purified arrives or by a porous plug (20) placed at the bottom of the pocket according to a well-known technique (French patent FR No. 1,031,504).
  • the downstream compartment (21) is separated from the upstream compartment by a partition (22) and it may include any known filtration means such as alumina beads or granules (23).
  • the injection can also be carried out in rotary devices such as the "Spinning Nozzle Inert flotation System” (SNIF) of UNION CARBIDE (US patent 3,870,511) as a replacement for the injection of chlorine, or in devices similar to propeller or turbine, in which the arrival of the halogenated vapors and the carrier gas is done by the axis.
  • rotary devices such as the "Spinning Nozzle Inert flotation System” (SNIF) of UNION CARBIDE (US patent 3,870,511) as a replacement for the injection of chlorine, or in devices similar to propeller or turbine, in which the arrival of the halogenated vapors and the carrier gas is done by the axis.
  • the metal is continuously treated in passing, by injection of the halogenated substance. But he is not contrary to the invention to treat, in the same way, successive metal charges in a crucible or in a basin furnace.
  • An injection device was constructed, according to the diagram in FIG. 1, comprising a 10-liter reservoir, of a mixture at 80% by weight of perchlorethylene and 20% by weight of hexachloroethane.
  • the dosing micropump has an adjustable flow rate between 1 and 10 milliliters / minute.
  • the vaporizer is preheated to (280 ⁇ 5 ° C).
  • the carrier gas is nitrogen, injected at a pressure of 2.5 bars and a flow rate of 2 m3 / hour.
  • the amount of perchlorethylene-hexachlorethane mixture was adjusted to 250 milliliters / hour corresponding to 100 grams of chlorine for a flow rate of aluminum, in the treatment bag, of 2 tonnes / hour.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Seal Device For Vehicle (AREA)
  • Catching Or Destruction (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Lubricants (AREA)
EP82420037A 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall Expired EP0061411B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82420037T ATE20541T1 (de) 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen einblasen einer gasfoermigen halogenverbindung in fluessiges metall.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8106134 1981-03-23
FR8106134A FR2502181B1 (fr) 1981-03-23 1981-03-23 Procede et appareillage pour l'injection precise et continue d'un derive halogene a l'etat gazeux dans un metal liquide

Publications (2)

Publication Number Publication Date
EP0061411A1 true EP0061411A1 (de) 1982-09-29
EP0061411B1 EP0061411B1 (de) 1986-06-25

Family

ID=9256686

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82420037A Expired EP0061411B1 (de) 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall

Country Status (16)

Country Link
US (1) US4402741A (de)
EP (1) EP0061411B1 (de)
JP (1) JPS57164945A (de)
KR (1) KR830008767A (de)
AT (1) ATE20541T1 (de)
AU (1) AU541804B2 (de)
BR (1) BR8201584A (de)
CA (1) CA1180164A (de)
DE (1) DE3271823D1 (de)
DK (1) DK127382A (de)
ES (1) ES510623A0 (de)
FR (1) FR2502181B1 (de)
GR (1) GR76038B (de)
HU (1) HU186486B (de)
NO (1) NO820940L (de)
YU (1) YU59782A (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4552667A (en) * 1984-06-25 1985-11-12 Shultz Clifford G Destruction of organic hazardous wastes
US4666696A (en) * 1985-03-29 1987-05-19 Detox International Corporation Destruction of nerve gases and other cholinesterase inhibitors by molten metal reduction
EP0436465A1 (de) * 1989-12-20 1991-07-10 Alusuisse-Lonza Services Ag Reinigung von Metallschmelzen
FR2669041A1 (fr) * 1990-11-09 1992-05-15 Sfrm Procede pour le traitement d'un metal en fusion et son transfert dans un espace recepteur et systeme pour la mise en óoeuvre de ce procede.

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6274030A (ja) * 1985-09-27 1987-04-04 Showa Alum Corp アルミニウム溶湯の処理方法
US4770697A (en) * 1986-10-30 1988-09-13 Air Products And Chemicals, Inc. Blanketing atmosphere for molten aluminum-lithium alloys or pure lithium
US4959101A (en) * 1987-06-29 1990-09-25 Aga Ab Process for degassing aluminum melts with sulfur hexafluoride
US5935295A (en) * 1997-10-16 1999-08-10 Megy; Joseph A. Molten aluminum treatment
RU2213794C2 (ru) * 2001-10-01 2003-10-10 ОАО "Каменск-Уральский металлургический завод" Способ рафинирования алюминия и его сплавов
WO2004033736A1 (en) 2002-10-07 2004-04-22 International Titanium Powder, Llc. System and method of producing metals and alloys
US7501089B2 (en) * 2002-09-07 2009-03-10 Cristal Us, Inc. Method and apparatus for controlling the size of powder produced by the Armstrong Process
EA006616B1 (ru) 2002-09-07 2006-02-24 Интернэшнл Тайтейнием Паудер, Ллк Способ отделения титана от содержащей титан суспензии
US20070017319A1 (en) 2005-07-21 2007-01-25 International Titanium Powder, Llc. Titanium alloy
EP1945394A2 (de) 2005-10-06 2008-07-23 International Titanium Powder, LLC. Titanborid
US7753989B2 (en) 2006-12-22 2010-07-13 Cristal Us, Inc. Direct passivation of metal powder
US9127333B2 (en) 2007-04-25 2015-09-08 Lance Jacobsen Liquid injection of VCL4 into superheated TiCL4 for the production of Ti-V alloy powder

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1998467A (en) * 1934-06-30 1935-04-23 Aluminum Co Of America Method of treating aluminum-base alloys
US2085697A (en) * 1933-08-05 1937-06-29 Nat Smelting Co Method for treating aluminum and aluminum alloys
US2447672A (en) * 1944-11-20 1948-08-24 American Smelting Refining Apparatus for chloridizing aluminum-base alloys
FR1463079A (fr) * 1965-10-21 1966-06-03 Air Liquide Procédé de traitement des métaux liquides, applicable notamment à l'élaboration de fonte nodulaire
FR2002510A1 (de) * 1968-02-23 1969-10-17 Alusuisse
FR2233406A1 (de) * 1973-06-18 1975-01-10 Olin Corp
US3972709A (en) * 1973-06-04 1976-08-03 Southwire Company Method for dispersing gas into a molten metal

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3958980A (en) * 1974-11-08 1976-05-25 Union Carbide Corporation Process for removing alkali-metal impurities from molten aluminum
JPS5223514A (en) * 1975-08-19 1977-02-22 Showa Denko Kk Treatment method for metal melt
JPS5819589B2 (ja) * 1976-03-29 1983-04-19 三菱電機株式会社 エレベ−タのドアレ−ル
JPS5652457Y2 (de) * 1977-08-27 1981-12-07
US4149615A (en) * 1977-09-15 1979-04-17 Westinghouse Electric Corp. Apparatus for mounting an elevator door operator
JPS5917719B2 (ja) * 1978-02-02 1984-04-23 三菱電機株式会社 自動ドア−の安全装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2085697A (en) * 1933-08-05 1937-06-29 Nat Smelting Co Method for treating aluminum and aluminum alloys
US1998467A (en) * 1934-06-30 1935-04-23 Aluminum Co Of America Method of treating aluminum-base alloys
US2447672A (en) * 1944-11-20 1948-08-24 American Smelting Refining Apparatus for chloridizing aluminum-base alloys
FR1463079A (fr) * 1965-10-21 1966-06-03 Air Liquide Procédé de traitement des métaux liquides, applicable notamment à l'élaboration de fonte nodulaire
FR2002510A1 (de) * 1968-02-23 1969-10-17 Alusuisse
US3972709A (en) * 1973-06-04 1976-08-03 Southwire Company Method for dispersing gas into a molten metal
FR2233406A1 (de) * 1973-06-18 1975-01-10 Olin Corp

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
REVUE DE METALLURGIE, volume 64, septembre 1967, PARIS (FR) P. KARINTHI et al.: "Procédé d'insufflation de chlore naissant dans les bains métalliques à partir de tétrachlorure de carbone liquide insufflé à l'aide de réfractaires poreux. Application à l'affinage sélectif du manganèse des fontes" pages 721 à 738 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4552667A (en) * 1984-06-25 1985-11-12 Shultz Clifford G Destruction of organic hazardous wastes
US4666696A (en) * 1985-03-29 1987-05-19 Detox International Corporation Destruction of nerve gases and other cholinesterase inhibitors by molten metal reduction
EP0436465A1 (de) * 1989-12-20 1991-07-10 Alusuisse-Lonza Services Ag Reinigung von Metallschmelzen
US5090998A (en) * 1989-12-20 1992-02-25 Alusuisse-Lonza Services Ltd. Purification of metal melts with halogen gas generated in an electrolysis cell
FR2669041A1 (fr) * 1990-11-09 1992-05-15 Sfrm Procede pour le traitement d'un metal en fusion et son transfert dans un espace recepteur et systeme pour la mise en óoeuvre de ce procede.

Also Published As

Publication number Publication date
ES8306803A1 (es) 1983-06-01
NO820940L (no) 1982-09-24
BR8201584A (pt) 1983-02-08
YU59782A (en) 1985-03-20
ES510623A0 (es) 1983-06-01
DE3271823D1 (en) 1986-07-31
FR2502181A1 (fr) 1982-09-24
CA1180164A (fr) 1985-01-02
EP0061411B1 (de) 1986-06-25
HU186486B (en) 1985-08-28
GR76038B (de) 1984-08-03
DK127382A (da) 1982-09-24
AU541804B2 (en) 1985-01-17
KR830008767A (ko) 1983-12-14
US4402741A (en) 1983-09-06
AU8176882A (en) 1982-09-30
ATE20541T1 (de) 1986-07-15
FR2502181B1 (fr) 1985-09-27
JPS57164945A (en) 1982-10-09

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