US3201101A - Apparatus for the purification of metals - Google Patents

Apparatus for the purification of metals Download PDF

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Publication number
US3201101A
US3201101A US214363A US21436362A US3201101A US 3201101 A US3201101 A US 3201101A US 214363 A US214363 A US 214363A US 21436362 A US21436362 A US 21436362A US 3201101 A US3201101 A US 3201101A
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Prior art keywords
antimony
reaction chamber
receptacle
flask
temperature
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Expired - Lifetime
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US214363A
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English (en)
Inventor
Jacques Roland
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LES PRODUITS SEMI CONDUCTEURS
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LES PRODUITS SEMI CONDUCTEURS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
    • C01G30/006—Halides
    • C01G30/007—Halides of binary type SbX3 or SbX5 with X representing a halogen, or mixed of the type SbX3X'2 with X,X' representing different halogens
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/02—Obtaining antimony

Definitions

  • antimony chloride by reducing gases such as hydrogen, but the process, as carried out by the classic method and classic apparatus, does not generally produce antimony of great purity.
  • the highest-purity antimony is generally thought to be electrolytic antimony.
  • antimony having a ratio of resistivity of about 6.2750 when compared at 0 C. and at the temperature of liquid nitrogen; by a method of producing Sb of high purity that comprises refluxing relatively pure SbCl distilling ofi H 0 and its HCl azeotrope, and some heads of SbCl distilling off the main fraction of SbCl and isolating it, vaporizing it in reducing atmosphere, flowing the vapors through a zone of increasing temperature in which the vapors are progressively solidified and melted, and flowing the molten antimony to a zone at solidifying temperature; and by an apparatus for purifying metals such as antimony, or for reducing their salts, which comprises a receptacle adapted to contain metal salts such as antimony chloride, an elongated reaction chamber connected to the receptacle by a measuring connection, means to heat the reaction chamber throughout its length to a temperature at which antimony chloride, or other salts, will vaporize
  • the apparatus which is an object of this invention, produces an extremely high rectification of antimony chloride, which is the preferred raw material, and produces antimony which is very pure and practically free of arsenic, which constitutes the impurity which is most frequently found and most difficult to eliminate.
  • the apparatus includes a rectification column, a reducing chamber and heating means for it which includes a fixed and a movable heat source.
  • the apparatus eliminates any manipulation of intermediate products.
  • the following description is of a preferred apparatus which is diagrammatically described in the accompanying drawing.
  • a condenser tube 21 served by a valve 22 which is encircled by a heating coil 23 and is divided in two parts 24, 25, controlled by valves 26, 27, respectively.
  • a receptacle 28 At the bottom of tube 24 is a receptacle 28 and at the bottom of tube 25 is a receptacle 29.
  • Valve 22 permits the confinement of the materials to the column during the period of reflux, and the valves 27, 28 permit the distillate to be directed to flask 28 or to flask 29 as desired.
  • the reduction chamber is in an elongated tube which is encircled by a heating coil 35 which extends throughout its length and serves to maintain it at a selected temperature, and it is also acted upon by a movable heater 36 which is mounted on rails 37 and can be moved along the chamber to bring any desired portion of it to a temperature higher than that which is provided by the winding 35.
  • the reduction chamber is in communication with a tube 38, which can be supplied on the one hand with an inert gas through tube 39, and on the other hand with a reducing gas through tube 40.
  • the gases are indicated as argon and hydrogen, respectively, in the drawing.
  • the reduction chamber is provided with a tube 41 which permits its content of air to be scavenged by gas flowing through pipe 38.
  • antimony chloride of relative purity is admitted to the flask 11 and is subjected to refluxing in the column 14 for an adequate period, during which water and its azeotrope with HCl are driven ofl through the condenser 19.
  • the valves 22 and 26 are then opened, the valve 27 remains closed, and the head of antimony chloride, for instance 10%, is condensed in the flask 28.
  • the valve 26 is closed, the valve 27 is opened and the SbCl is delivered to the flask 29, in which it is maintained at a temperature near C.
  • the reaction chamber 34 has been prepared by opening the line 39 to argon, or some other inert gas, which sweeps the air out of the reaction chamber.
  • the argon may be turned off and the hydrogen admitted or they may be admitted in admixture, and the reaction chamber is heated at the zone nearest the flask 29 to a temperature at which antimony chloride is vaporized, for instance 250 C.
  • the heater 36 is moved some distance away from the inlet 33 and is heated to about 700800 C., bringing the zone of the reaction chamber which is within it to comparable temperature. There is thus established a minimum temperature of 250 C. at the inlet and a maximum of possibly 750 C. inside the heater 36.
  • the heater may be placed, for example, 25 cm. away from the inlet.
  • the joints in the apparatus may be of some inert plastic such as polytetrafluoroethylene.
  • the argon is turned off and pure hydrogen is admitted to the inlet, which is maintained at 250 C. throughout the operation, the hydrogen being reduced to about that temperature during its passage through tube 38.
  • the valve 33 is opened slightly to allow the antimony chloride to drop into the reaction chamber.
  • the reduction is carried out at a temperature of 700800 C.
  • reaction chamber 34 between the heater 36 and the inlet, a deposit of antimony needles which filter the later formed particles of anti- 7 mony.
  • the input of antimony chloride may be increased to accelerate the process.
  • the antimony deposit moves nearer and nearer to the hot zone of the furnace.
  • the heater 36 was heated to 750 C. and placed 25 cm. from the inlet.
  • the reaction chamber was swept clear by argon and the hot hydrogen was turned on to fill the chamber.
  • the chloride was admitted in one drop in two seconds while the hydrogen was admitted at 20' liters per hour.
  • black antimony needles formed on the walls between the heater and the inlet.
  • the chloride was then addedat a rate of 1 drop per second, and the deposit of metallic antimony was increased and progressed little by little toward the heater. When it reached the zone of the tube which was at 630 C., it melted and ran down the tube through the heater at the other end.
  • the operational efliciency is about the antimony ingots obtained are 5 mm. thick and 15 mm. wide. Its content of impurities was not over:
  • the antimony thus obtained is considered as ultra pure, which is attested by the results of electrical resistivity test. If one compares the ratio of resistivity at 0 with that of the temperature of liquid nitrogen one obtains a ratio of 5.9728 for electrolytic antimony, the purest heretofore known, which corresponds to 99.999% purity.
  • the antimony-prepared according to the present invention has a ratio of resistivity of 6.2750, which is superior to that of electrolytic antimony and is accordingly a purer and superior product.
  • Apparatus for the purification of metals, especially antimony comprising a reflux still, a condenser, and a receptacle capable of holding antimony chloride, means to heat the receptacle, a tubular reaction chamber at tached to the receptacle by a valve, means to supply the reaction chamber with inert and reducing gases, means whereby the chambermay be scavenged by the inert gases, means to heat the reaction chamber more or less uniformly throughout its length, and a second heating means movable along the reaction chamber adapted to heat a localized part thereof to higher temperature than that provided by the first heating means;
  • Apparatus adapted to the production of pure antimony substantially consisting of a distillation vessel adapted to receive antimony chloride, a rectification column provided with a sequence of individually controllable heaters along its length, discharge means connected to the column adapted to the release of gases, condenser means connected to the columns provided with heating means, a first discharge for the condenser, a second discharge for the condenser including a heated conduit and a receptacle, an elongated reaction chamber connected to the receptacle and to sources of inert gas and of reducing gas, fixed heating means embracing the reaction chamber throughout a substantial length thereof, movable heating means embracing the reaction chamber through a lesser length thereof, and means to extract a product from the reaction chamber.
  • Apparatus adapted to the production of pure Sb comprising in interconnected sequence distillation means, rectification means having stages of controllable temperature, heated condenser means, flow control means for the condensate from the condenser, a reaction chamber having fixed heating means and movable heating means, means to supply the reaction chamber With gases, and means to discharge the reaction chamber.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US214363A 1961-08-03 1962-08-02 Apparatus for the purification of metals Expired - Lifetime US3201101A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR869937A FR1305488A (fr) 1961-08-03 1961-08-03 Perfectionnement à la fabrication d'antimoine pur

Publications (1)

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US3201101A true US3201101A (en) 1965-08-17

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FR (1) FR1305488A (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3294575A (en) * 1962-12-03 1966-12-27 Charles R Barnes Vapor plating copper
US3316121A (en) * 1963-10-02 1967-04-25 Northern Electric Co Epitaxial deposition process
US4010937A (en) * 1974-04-13 1977-03-08 Preussag Aktiengesellschaft Metall Method and apparatus of refining crude cadmium
FR2572384A1 (fr) * 1984-10-31 1986-05-02 Sumitomo Metal Mining Co Procede de fabrication de trioxyde d'antimoine a faible niveau de rayonnement alpha
US4629501A (en) * 1984-10-31 1986-12-16 Sumitomo Metal Mining Company Limited Method for manufacture of antimony of high purity

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1799102A (en) * 1929-08-13 1931-03-31 Gen Electric Furnace
US2366881A (en) * 1943-03-31 1945-01-09 Research Corp Thermoelectric alloys
US2596100A (en) * 1946-10-30 1952-05-13 Penarroya Miniere Metall Obtention of metallic antimony
US2615706A (en) * 1949-08-05 1952-10-28 Broken Hill Ass Smelter Distillation of metals
US2710253A (en) * 1953-10-19 1955-06-07 Battelle Development Corp Semiconducting alloy
US2944885A (en) * 1959-06-02 1960-07-12 Guenter A Wolff Method of purifying arsenic and antimony
US3006734A (en) * 1957-11-14 1961-10-31 Plessey Co Ltd Process for preparing pure silicon
US3039755A (en) * 1960-12-06 1962-06-19 Texas Instruments Inc Apparatus for reduction of arsenic trichloride to elemental arsenic

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1799102A (en) * 1929-08-13 1931-03-31 Gen Electric Furnace
US2366881A (en) * 1943-03-31 1945-01-09 Research Corp Thermoelectric alloys
US2596100A (en) * 1946-10-30 1952-05-13 Penarroya Miniere Metall Obtention of metallic antimony
US2615706A (en) * 1949-08-05 1952-10-28 Broken Hill Ass Smelter Distillation of metals
US2710253A (en) * 1953-10-19 1955-06-07 Battelle Development Corp Semiconducting alloy
US3006734A (en) * 1957-11-14 1961-10-31 Plessey Co Ltd Process for preparing pure silicon
US2944885A (en) * 1959-06-02 1960-07-12 Guenter A Wolff Method of purifying arsenic and antimony
US3039755A (en) * 1960-12-06 1962-06-19 Texas Instruments Inc Apparatus for reduction of arsenic trichloride to elemental arsenic

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3294575A (en) * 1962-12-03 1966-12-27 Charles R Barnes Vapor plating copper
US3316121A (en) * 1963-10-02 1967-04-25 Northern Electric Co Epitaxial deposition process
US4010937A (en) * 1974-04-13 1977-03-08 Preussag Aktiengesellschaft Metall Method and apparatus of refining crude cadmium
FR2572384A1 (fr) * 1984-10-31 1986-05-02 Sumitomo Metal Mining Co Procede de fabrication de trioxyde d'antimoine a faible niveau de rayonnement alpha
US4629501A (en) * 1984-10-31 1986-12-16 Sumitomo Metal Mining Company Limited Method for manufacture of antimony of high purity

Also Published As

Publication number Publication date
FR1305488A (fr) 1962-10-05

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