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Chila..., ATTORNEYS 3,434,799 United States Patent Office Patented Mar March 25, 1969 W. L. Wilson 3,434,799 FROCESS FOR PREPARING PIGMENTARY TITANIUM DIoxIDE Filed April 14, 1965 INVENTOR WILLIAM L. WIL5ON FG, 2. BY Chila..., ATTORNEYS 3,434,799 United States Patent Office Patented Mar. 25, 1969 1. 2 of at least 1500, usually at least 1700, and a blue under 3,434,799 m tone (tint tone) for a particle size distribution range be PROCESS FOR PREPARNG PGMENTARY TTANIUM DOXDE low 1.0 micron, preferably, 0.2 to 0.5 micron. William L. Wilson, Barberton, Ohio, assignor to PPG In the practice of this invention, it has been discovered Industries, Inc., a corporation of Pennsylvania that the pigmentary and optical properties, particularly Continuation-in-part of application Ser. No. 190,140, undertone (tint tone), of rutile titanium dioxide pigment Apr. 25, 1962. This application Apr. 14, 1965, Ser. can be substantially increased by reacting the titanium No. 448,121 tetrahalide with an oxygenating gas in the vapor phase Int, C. C01g 23/04 in the presence of a silicon source or additive selected U.S. C. 23-202 11. Claims O from the group consisting of metallic silicon and a silicon compound and a further source which will provide at least one ion selected from the group consisting of potassium, ABSTRACT OF THE DISCLOSURE zinc, rubidium, and cesium. The preparation of pigmentary titanium dioxide by va To more specifically describe the process of this inven por phase oxidation of titanium tetrahalide is described. 5 tion, reference is made to the drawing, and FIGURES 1 A process for improving the pigmentary properties of the to 3, inclusive which depict apparatus for practicing the pigment by conducting the oxidation reaction in the pres process invention. ence of additives, particularly silicon and potassium is FIGURE 1 describes a diagrammatic cross-section view discussed. of a concentric orifice-annulus burner fitted in a furnace. 20 FIGURE 2 further illustrates the construction of the burner of FIGURE 1, representing a view along line I-I CROSS-REFERENCE TO RELATED APPLICATIONS of FIGURE 1. This application is a continuation-in-part of U.S. ap FIGURE 3 illustrates a diagrammatic cross-section view plication Ser. No. 190,140, filed Apr. 25, 1962, now U.S. of a burner which may be fitted in the furnace of FIGURE Letters Patent 3,214,284. 25 1 to produce pigmentary titanium dioxide according to the This invention relates to a process for producing pig process of this invention. mentary titanium dioxide having superior optical proper Referring to FIGURES 1 and 2, reaction zone chamber ties by the vapor phase oxidation of a titanium tetrahalide of furnace A comprises a concentric steel shell 1 and an selected from the group consisting of titanium tetrachlo internal lining of firebrick 5 (or other heat resistant insu ride, titanium tetraiodide, and titanium tetrabromide. 30 lation). At the lower part of furnace A is a conical bot Titanium dioxide is currently produced commercially by tom terminating at outlet 7. At the upper part of furnace at least two different basic processes, the so-called Sulfate A' is a burner A. process and the chloride process. The latter involves the Burner A is composed of three concentric tubes, 2, 3, vapor phase reaction of titanium tetrahalide and an oxy and 4. Tube 3 is arranged so as to circumscribe tube 4 genating gas at a temperature of at least 800° C., usually 35 (forming annulus 6) and tube 2 is arranged so as to cir 1000 to 1400° C., in the absence or presence of a fluidized cumscribe tubes 3 and 4 (forming annulus 9). Each of bed, e.g., as disclosed in U.S. Letters Patent 2,964,386, the tubes 2 and 3 are evenly spaced from the wall of the U.S. Letters Patent 2,240,343, issued to Muskat, U.S. tube it circumscribes. This is more clearly shown in FIG Letters Patent 2,394,633, issued to Pechukas et al., or U.S. lure 2, which shows the tube arrangement taken along line Letters Patents 2,968,529 and 3,069,281, issued to William 40 I-I of FIGURE 1. L. Wilson. The oxygenating gas may comprise any oxidiz In the operation of the reactor of FIGURES 1 and 2, ing or oxygenating agent, such as oxygen, air, oxides of an oxygenating gas typically preheated 900° C. to 1750 nitrogen, H2O, oxides of phosphorus, or mixtures of C. is fed to the upper opening in tube 4, while an inert Sale. gas at room temperature up to the temperature of the Pigmentary titanium dioxide has unique optical proper 45 oxygenating gas is fed to the opening at the top of tube ties which make it useful, particularly in the paint indus 3. The inert gas may comprise chlorine, nitrogen, bro try. Such optical properties, for example, tinting strength mine, iodine, argon, helium, krypton, Xenon, carbon di and undertone, are a function of particle size, dispersion oxide, or mixtures thereof. Concurrently therewith, tita and color. Pigmentary titanium dioxide of a given particle nium tetrahalide is fed to the opening at the upper part size distribution range, e.g., mean diameter of 0.2 to 0.5 50 of tube 2. The titanium tetrahalide has a temperature of micron, may be prepared by the vapor phase oxidation 140 C. to about 1200° C. processes of Muskat, Pechukas, or Wilson, noted herein Referring to FIGURE 3, burner B, which may be fitted before, as well as by other processes, e.g., Canadian Pat in furnace A of FIGURE 1 in replacement of burner ent 517,816, issued to Krchma et al., or British patent A, is composed of three concentric tubes annularly ar specifications 876,672 and 922,671. 55 ranged. Central oxygenating gas tube 12 is circumscribed However, it has been discovered that the Surface ac by tube 11, which in turn is circumscribed by tube 10 tivity of the titanium dioxide particles produced by the such that there is formed annuli 17 and 16. Tube 11 is, aforementioned processes may be such that electrostatic provided with an annular lip 13, at its lower end and charges or forces are set up between individual particles tube 10 is provided with annular lip 14, such that the whereby the particles come together and combine in groups 60 titanium tetrahalide and inert gas streams are emitted of two or more. Such grouping is termed chaining or ag from the annuli 17 and 16 in a direction substantially gregation. The result of such grouping, chaining, or aggre perpendicular to the direction of flow of the oxygenating gation is a deficient pigment having less than optimum gas from tube 12. In operation, burner B is fed in the dispersibility and decreased optical properties, particular same manner as burner A of FIGURE 1. ly undertone. 65 It has been discovered that if titanium dioxide is pre The silicon source or additive and the selected ion of pared in accordance with the present invention, there is potassium, zinc, rubidium, and cesium can be added to produced a pigmentary titanium dioxide particle having gether or separately to the inert stream or added together optimum dispersion and undertone for a given particle or separately in one of the reactants, e.g., titanium size distribution range. More particularly, there is pro 70 tetrahalide or oxygenating gas. duced a raw, uncoated pigmentary titanium dioxide par When the process is operated in accordance with U.S. ticle having high, superior dispersion, a tinting strength Letters Patents 3,069,282 and 3,105,742 and a combusti 3,434,799 3 4. ble carbon-containing or sulfur-containing fuel is fed into (C4H9)SiH, the reaction zone 30, the silicon source and selected ion (CHg) Si (silicon tetrabutyl), can also be introduced separately or together directly to CHSiH, the reaction zone 30 independently of the inert stream, (C5H11)2SiH2, reactants, and combustible fuel. (C5H11)SiH, Thus, in the practice of this invention, the silicon source 5 (C5H11) Si (silicon tetraisoamyl), can be added directly to the reaction Zone 30 or incor C6H13SiH, porated with one or more streams of inert gas, reactants, (C6H13)2SiH2, or fuels being fed to the zone. Likewise, the selected ion (CH3)3SiH, of potassium, zinc, rubidium, and cesium can be added (C6H13) Si, directly to the Zone 30 or incorporated with one or more O CH-15SiH, streams being fed to the zone. The selected ion may be (CH15)2SiH2, added separately or in conjunction with the silicon source. (CH15)SiH, The silicon source and the selected ion additives can (CH15) Si, be added directly to the reaction Zone as an atomized (C6H5) Si (silicon tetraphenyl), spray in a solid, liquid, or gaseous state. (CHT) Si (silicon tetra-m-tolyl or tetra-p-tolyl), Furthermore, such additives may be added to the Zone (C6H5CH2) Si (silicon tetrabenzyl), by employing an inner furnace wall 5 constructed of a (C12H9)4Si (silicon tetraxenyl), ceramic or firebrick material which contains either one (CH3)3CH5Si (trimethylphenylsilane), or both of the silicon and ion additives. Such material is 20 (CH3)2(C6H5)2Si (dimethyldiphenylsilane), gradually eroded into the reaction zone due to the high CH3(CH) Si (methyltriphenylsilane), temperature oxidation environment in Zone 30, as noted (C2H5)3CH5Si (triethylphenylsilane), for example in British patent specification 672,753. (C2H5)2(C6H5)2Si (diethyldiphenylsilane), One or both of the additives may also be introduced C2H5 (CH5)3Si (ethyltriphenylsilane), into the reaction Zone by employing a ceramic dedusting (CH3) (C2H5) (n-CH) (C6H5)Si (methylethyl edge, as disclosed in copending U.S. application Ser.
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