Patent GB-370962-A (GB)
Title: Improvements in the manufacture and production of metal carbonyls
IPC: C01G1/04
Filed: 1930-10-08
Abstract: In the production of metal carbonyls for example nickel or iron carbonyl, the reaction heat is led off by conveying a liquid through the reaction vessel and bringing it into direct contact with the reaction materials, the liquid being supplied to and withdrawn from the reaction vessel at one point only or being supplied to and/or withdrawn from the reaction vessel at several places which may be distributed in several zones over the whole space within the reaction vessel.  Alternatively, a gas may be employed provided it is supplied to and/or withdrawn from the reaction vessel at several places.  When the liquid or gas is supplied to and/or withdrawn from the reaction <PICT:0370962/III/1> <PICT:0370962/III/2> <PICT:0370962/III/3> <PICT:0370962/III/4> <PICT:0370962/III/5> vessel at several places they may have the same or a lower temperature on leaving the reaction vessel than when entering, thus supplying heat to one or other place or zone within the reaction vessel.  Inert liquids or melts such as oils, paraffin wax, or hydrocarbons, water or liquid or fused metal carbonyls may be employed and the carbon monoxide may be supplied dissolved in these liquids.  The liquids may vaporize in the reaction vessel and leave as vapour or they may leave in the liquid state. Inert gases such as hydrogen, nitrogen, or carbon dioxide may be employed, but it is preferable to employ the reactant carbon monoxide or a gas containing it.  Additional cooling devices such as pipes, jackets, ribs, &c. may also be used.  The cooling devices may be arranged so that zones of the reaction vessel may be influenced independently of each other and the liquids or gases employed may be supplied to other reaction vessels for the preparation of carbonyls or the liquids and gases employed in different reaction vessels may be brought into heat exchange relation to each other.  If the reaction vessels are operated under the same pressure, the walls of the heat exchangers may be thin.  According to Fig. 1 (Comp.), carbon monoxide is supplied at the inlet 2, the outgoing gases containing carbonyl vapour being passed by a pipe 3 to a cooler 4 wherein a portion of the carbonyl is condensed and returned to the reaction vessel down pipe 3.  The portion uncondensed leaves at the top.  In a modification of this apparatus the reaction vessel is provided with a worm conveyer operating in a cylindrical guide and the whole of carbonyl vapour is condensed in the cooler, a portion being returned to the reaction vessel.  In another modification a high-pressure vessel 1, Fig. 2 (3304/31), is filled with porous nickel in lump form. Carbon monoxide at 200 atmospheres pressure enters by a pipe 2 and leaves by a pipe 4.  The resulting liquid nickel carbonyl enters a cooler 5 through a pipe 10, returns to the reaction vessel through a pipe 6 and control valve 7.  According to Fig. 3 (Comp.), carbon monoxide is supplied to a reaction vessel 1 by a pipe 2 and a paste or suspension of the initial material is introduced by a pipe 11. The materials pass through a pipe 12 to a separator 13.  The gases or vapours pass therefrom via a pipe 3 to a cooler 4.  Liquid carbonyl separates in a vessel 14 and is in part returned to the reaction vessel through a pipe 8.  When a gas is supplied to and/or withdrawn from the reaction vessel at several places, the gas may be supplied by a single pipe passing through the longitudinal axis of the reaction vessel and provided with perforations or nozzles along its length; or a porous tube made by sintering copper or glass powder may be employed.  In a modification several tubes are arranged concentrically one inside another, each tube terminating by nozzles or a ring-burner like device.  If the nozzles are arranged on one side only of supply pipes and the contents of the reaction vessel are liquid, stirring may be effected by the introduction of the gas. According to Fig. 1 (30150/30), pipes c which are closed at their inner ends and are provided with a large number of nozzles serve for the supply of gas, the withdrawal of the gases being effected through openings d, e or a pipe f.  The pipes c can be closed independently by valves.  According to Fig. 1 (3304/31), carbon monoxide is introduced under pressure by pipes 2 provided with control valves 3, gases passing from the reaction vessel by a pipe 4 to a cooler 5.  A portion of the liquid iron carbonyl separated therein is returned to the reaction vessel through pipes 6 provided with valves 7.  The remainder is removed through a pipe 8. Specifications 323,332 and 334,976, [both in Class 1 (ii), Inorganic compounds, other than &c.], are referred to.