US1944849A - Production of metal carbonyls - Google Patents

Production of metal carbonyls Download PDF

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Publication number
US1944849A
US1944849A US597752A US59775232A US1944849A US 1944849 A US1944849 A US 1944849A US 597752 A US597752 A US 597752A US 59775232 A US59775232 A US 59775232A US 1944849 A US1944849 A US 1944849A
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US
United States
Prior art keywords
reaction chamber
reaction
production
continuously
carbonyl
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Expired - Lifetime
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US597752A
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English (en)
Inventor
Schlccht Leo
Naumann Max
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.)
IG Farbenindustrie AG
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IG Farbenindustrie AG
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Filing date
Publication date
Application filed by IG Farbenindustrie AG filed Critical IG Farbenindustrie AG
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Publication of US1944849A publication Critical patent/US1944849A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/04—Carbonyls

Definitions

  • the present invention relates to improvements in the production of metal carbonyls.
  • fresh material is introduced in a similar manner at the top of thereaction chamber h by means of a sluice 1', valves r and y and pipe m.
  • the height to which the reaction chamber h is filled is supervised by means of a level indicator (not shown).
  • the material may also be introduced at the bottom for example by an arrangement similar to a pump, the residue then being withdrawn at the top.
  • the period of time occupied when working as hereinbefore described by releasing the pressure on the sluices and emptying or filling the same, during which time no supply or withdrawal of material takes place, may be avoided by providing two sets of sluices which are operated alternately or by providing between the reaction chamber and the sluices a buffer vessel which is always under the same pressure as-the reaction vessel and into which the exhausted residue may be withdrawn continuously for example by means of a conveyor worm, or from which fresh material may be continuously supplied to the reaction chamber. Then, especially when the buffer vessels are not too small, more time is available for emptying and filling the sluices without the yield per unit of time and space being injuriously affected.
  • injection apparatus working similarly to pumps many types of which are known, may be used for example.
  • the reaction material In order to facilitate the convenient sliding of the material through the reaction vessel, and to establish a uniform passage of the gas through the material, it is advantageous to employ the reaction material at least partly in a coarse form or in theform of granules the size of which at the top is substantially limited by the dimensions of the filling apparatus employed.
  • Mav terials which are not too large in size and having for example an average size between 0.3 and 20 millimetres and which before the treatment with carbon monoxide have passed through a rotary tubular furnace, as for example for the purpose of reduction by means of carbonaceous materials, are especially suitable because the grains are then rounded and the material is capable of trickling or sliding readily.
  • Material which is present entirely in the form of a powder may be mixed with coarse, if desired briquetted, material or supplied to the reaction chamber alternately therewith. If desired, additional materials which have a loosening effect and which facilitate the passage of gas, as for example rings or tubes which may consist for instance of clay, aluminium or copper may be mixed with the powder or supplied to the reaction chamber in alternate sequence with the powder.
  • the shape of the reaction chamber may be varied within wide limits. When working under comparatively low pressures, even wide containers with a comparatively slight height of column, as for example those of 1 metre height and lmetre in diameter, are suitable. Conical reaction vessels which become narrower in the direction of movement of the reaction material may be employed, but more advantageously containers which become wider in the direction of movement are used in order to facilitate the flow of the reaction materials.
  • the cross section of the containers may be circular or of other shapes favorable for the radiation of heat, as for example rectangular; the inner surface of the walls should be so constructed, however, that the forward movement of the reaction materials is not hindered.
  • an undesirably great mechanical pressure of the material on the bottom may be avoided for instance by a certain arrangement of the reaction vessel, as for example by inclining the same.
  • a certain arrangement of the reaction vessel as for example by inclining the same.
  • care must be taken that the material is continuously rendered compact, so that it completely fills the reaction chamber for example by introducing the fresh material under an excess of pressure by means of a suitable pump or an eflicient conveyor worm.
  • the movement of the material in nearly horizontal, or horizontal reaction containers may be effected or assisted by causing the reaction container to rotate.
  • the container itself is caused to rotate, but one or more insertions, as for example tubes having not too strong walls and therefore being easily revolvable.
  • the inserted tubes, rotating if desired, at different speeds are kept filled with solid reaction material, while the container bears the pressure and is not moved.
  • the withdrawal of the heat of reaction may be effected for example in the usual manner by internal cooling with cooling tubes or cooling coils or by external cooling with cooling ribs, or cooling jackets or by means of gases led through the reaction chamber, preferably by the reaction gas itself.
  • the introduction and/ or withdrawal of the care bon monoxide or gases containing carbon mom oxide which may be led in the same direction as, or in counter current to, the material, is preferably effected at several places in the reaction container.
  • the gas is advantageously led in a cycle.
  • the process according to the present invention is particularly suitable for the production of the carbonyls of nickel and cobalt from initial mate rials containing these metals, though of course it may be used as well for the production of other metal carbonyls, as for example iron carbonyl.
  • the process of producing a metal carbonyl by the action of carbon monoxide on a material capable of forming a metal carbonyl in a closed reaction chamber which comprises the steps of continuously withdrawing from the reaction chamber spent material and continuously introducing fresh material into the reaction chamber at a rate corresponding to the amount of material used up and the amount of spent material withdrawn, thereby keeping the reaction chamber at all times substantially completely filled with the material.
  • the process of producing nickel carbonyl by the action of carbon monoxide on a material capable of forming nickel carbonyl in a closed reaction chamber which comprises the steps of continuously withdrawing from the reaction chamber spent material and continuously introducing fresh material into the reaction chamber at a rate corresponding to the amount of material used up and the amount of spent material withdrawn, thereby keeping the reaction chamber at all times substantially completely filled with the material.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
US597752A 1931-03-13 1932-03-09 Production of metal carbonyls Expired - Lifetime US1944849A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1944849X 1931-03-13

Publications (1)

Publication Number Publication Date
US1944849A true US1944849A (en) 1934-01-23

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ID=7750688

Family Applications (1)

Application Number Title Priority Date Filing Date
US597752A Expired - Lifetime US1944849A (en) 1931-03-13 1932-03-09 Production of metal carbonyls

Country Status (3)

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US (1) US1944849A (en, 2012)
BE (1) BE387015A (en, 2012)
FR (1) FR732907A (en, 2012)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2548727A (en) * 1948-01-22 1951-04-10 Rohm & Haas Preparation of nickel carbonyl
US2554194A (en) * 1950-06-06 1951-05-22 Gen Electric Synthesis of molybdenum and tungsten carbonyls

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2548727A (en) * 1948-01-22 1951-04-10 Rohm & Haas Preparation of nickel carbonyl
US2554194A (en) * 1950-06-06 1951-05-22 Gen Electric Synthesis of molybdenum and tungsten carbonyls

Also Published As

Publication number Publication date
BE387015A (en, 2012)
FR732907A (fr) 1932-09-28

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