Patent GB-991318-A (GB)
Title: Finely divided metal oxides
Inventor: ARKLESS KENNETH
IPC: C01B13/28
Filed: 1962-01-30
Abstract: A finely-divided metal oxide is formed by passing into a reaction zone a stream of hot gas containing initial solid particles of smaller average size than the metal oxide particles to be produced; and a metal halide and an oxygenating gas.  At least one of the two latter reactants is introduced through a plurality of inlets spaced along the zone in the direction of the gas flow, one of the reactants may be added to the gas stream as a single addition.  The gas stream temperature is such that the halide and oxygenating gas will react to form metal oxide. The oxygenating gas may be oxygen with or without other gas, as in air.  The initial particles may or may not be of the same metal oxide as that produced; they may be, e.g. SiO2. The gas stream and particles may be formed by vapour-phase oxidation, which may be in a fluidized bed, of a metal halide, with or without the presence of a Group Ia metal and Zn, Cd, Pb, Sb, Mo or Th, or excess oxygen, or in a fast reaction, thus limiting initial particle size; or by hydrolysis of a halide, e.g. in the vapour-phase by water vapour with or without air, or by vaporization of a solid material, e.g. a metal oxide.  The resultant gases containing initial solid particles with or without oxygenating gas and metal halide may be passed as the hot gas stream directly to the reaction zone.  The initial particle size range is 0.001m  to 0.25m  or more.  The pigmentary particle range is 0.15m  to 0.35m ; by particle size is meant average weight particle size.  The hot gas should, for TiCl4, be at at least 600 DEG  C.; the reaction zone temperature should be up to 1400 DEG  C.  The reactant gases may be premixed if sufficiently cool not to react till introduced into the reaction zone; or introduced separately; they may be introduced through the walls of the zone or through a pipe, within the zone, having ports along its length; the reactant introduced at any point into the stream should react before the next reactant entry point, and the stream velocity or rate of introduction of reactant at each point may be adjusted to ensure this.  The whole process of forming the gas and particle stream and oxidation of injected halide, or part thereof, may be conducted autothermally or fuel may be burnt in the reaction zone. The initial solid particles should be introduced into the reaction zone, with or without a deflocculating agent, within 8 seconds of formation. Up to 20 or more introductions of reactant may be made into the reaction zone; when any reactant introduced at a given point has reacted, the weight of metal oxide formed should be 1.01-10.0 times the total weight of oxide present in the gas stream before the introduction.  Minor proportions of modifying substances, e.g. halides of aluminium and silicon, and water vapour, may be added in the preparation of TiO2. Coating-generating substances, e.g. halides of Si, Ti or Al may be made as a final introduction.  Mixed oxides may be formed.  The oxide may be filtered off; halogen produced may be recovered by liquefaction. The examples describe a TiO2 product having tinting strength of about 1700-1800 (Reynold's), rutile content 90-99.5%, particle size 0.17-0.26m .  Specifications 761,770, 913,151, 919,019, 968,832 and 986,660 are referred to.