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All 24.1.1 Alt1-61 June 26, 1945. A. T. McCORD ET AL 2,379,019 PREPARATION OF PIGMENTARY MATERIALS Filed May 29, 1942 2 Sheets-Sheet 1 RUTLE ANATASE Y-TANCACD SPINEL, MgA,0, ZNC TTANATE ZnTO, LMENITE, FeTiO, MAGNESUM TTANATE MgTiO, 9 ZING TANATE NVENTORS Azar (a 2/7 (or a All B24.1.1 (7//ova A'.5ozzzzi Alt1-61 (62/5 ATTORNEYS June 26, 1945. A. T. McCORD ETAL 2,379,019 PREPARATION OF PIGMENTARY MATERIALs Filed May 29, 1942 2 Sheets-Sheet 2 To-Zno w TEORECA RUTLEliot Xzr Toyto, ----- experimeNA ANATASExZnTOy Tot TiO, ZnTorzno 90 80 70 60 SO AO 3O 20 O ZnO O 2. 33 ?: p 60 o 33 90 E. 4. .3 . 67. , 25 . 1000 RuTILE, Tor xZnTidyTo\\\\\\\\\*7ty". Cubic) it.o.ut goo RUTILE, Tot KZnTidy T.O. (HEX) ZnOy TiO, Z ANATASE,-- to ZANATASETO,Z -- xZnTidyTiO,; 10% ZxZntiquid E" ANATASE. Torzno 6 to ido 90 % Znd MoisésMoso Ana,yev ZaacSara COy faroda ASzezzaars 274MeaAt TORNEYS Patented June 26, 1945 2,379,019 UNITED STATES PATENT of FICE 2,379,019 PREPARATION OF PIGMENTARY - MATERIALs Andrew T. McCord and Barold F. Saunders, Ead donfield, N. J., assignors to The Sherwiri-Wi Ohioams Company, Cleveland, Ohio, a company of Application May 29, 1942, serial No. 445,022 23 Claims. (C. 106-300) An object of this invention is to prepare pig found that when a relatively small amount of a Enents of high durability characteristics and ex titanate, especially one of the metatitanate type, cellent pigmentary properties, comprising ti is introduced into the titanium dioxide itself, in tanium dioxide detectable by X-ray analysis as the manner hereinafter described, a consider anatase or rutile, and/or compounds having the 5 able improvement in chalk resistance is obtained general formula acRTiOasyFiOa, where R is a bi at the expense of only a minor reduction in the Valent metal, where gy may be zero or a quantity, hiding power of paints made from this pigment. and where TiO2 is titanium dioxide present in When the quantity of titanate so introduced is solid Solution in the RTiO3, and determinable by very small, there may be an actual improvement chemical analysis as an excess over the theo in the color and brightness. retical proportion for RTiO3. More particularly, Several processes have been devised for the the present invention is concerned with pigments conversion of anatase into rutile, mixtures of in which the R of RTO is zinc, and in the fol rutile and zinc orthotitanate (ZnTiO4) and/or lowing specification we will describe in detail Solid solutions of titanium oxide in zinc ortho Only that embodiment of the broader invention. titanate. The high hiding power or obliterating power of Thus, for example, Goldschmidt U. S. Patent titanium dioxide, particularly when in the pig No. 1348,129 converts precipitated titanium di mentary rutile modification is well known, and oxide to the rutile modification by heating at 900 titanium dioxide is, therefore, a preferred pig C. to 1000 C. in the presence of a volatile halo ment for white paints of all types, where the 20. gen compound, as Zinc chloride. Goldschmidt maximum obliteration of the surface to be paint in U. S. Patent 1,436,164 converts the anatase led is desired. One of the objections to titanium form of titanium dioxide, as precipitated by ther pigments for paint-and other usage is the tend mal hydrolysis of an ilmenite solution, to a ti ency for these pigments to chalk out of the paint tanate by heating it, together with a compound film when exposed to weather. In tinted paints of a bivalent metal compound such as a com using titanium dioxide in combination with a pound of calcium, strontium, barium, magnesium, coloring pigment, the chalking of the titanium lead, zinc, or manganese. Cole in U. S. Patent induces a white, dusty surface on the paint film 2,184,938 obtains mixtures of titanium dioxide which lightens the apparent tint or color of the and solid solutions of titanium dioxide in zinc paint, and the effect is known as “fading." The 30 Orthotitanate by heating titanium dioxide with titanates, such as zinc titanate or lead titanate, varying proportions of a zinc compound in the are far superior to titanium dioxide as respects presence of a phosphate compound. Booge, in chalk resistance and fading resistance when used U. S. Patent 2,253,551 produces titanium oxide with coloring pigments, but lack the superior in the rutile form intimately combined and asso hiding power of the titanium dioxide ciated with minor amounts of zinc orthotitanate The addition of a titanate, such as zinc titanate by heating a mixture of titanium oxide of the or lead titanate, to paints formulated primarily anatase modification and a minor proportion of with titanium dioxide as the principal pigment a zinc compound. has been recommended for the purpose of in In all of these processes the titanium oxide proving resistance to chalking. In general, it has 40 used in the starting mixture has been the anatase been found, however, that the proportion of ti modification either as precipitated by thermal tanate required to effect a satisfactory improve hydrolysis from ilmenite solutions or titanium . ment in the resistance to chalking has been so Sulphate solutions, or from the calcination of great that the consequent drop in hiding power these precipitates. The titanate obtained has and color of the paint is excessive. We have 45 been the 2inc orthotitanate of cubic symmetry, 2 2,379,019 formula aczngTiO4.gTiO2, in which ac and 2) are and of the spinel structural type. (Cole and Nel whole numbers and ac is greater than 2), and we son, J. Phys. Chem. vol. 42, Feb. 1938, pp. define the term "zinc-titanium-oxygen Con 245-251.) pound of the ilmenite structure type' as mean We have found that when mixtures in varying ing either the pure zinc metatitanate of hexag proportions of ?y-titanic acid and a metal oxide, onal symmetry and the ilmenite structure type, such as zinc oxide, are heated, entirely differ or a solid solution of titanium dioxide therein, ent results are obtained as compared to similar and of the general formula, acznTiO3.gTiO2. treatment of similar mixtures but in which the We are aware that Lederle in U. S. Patent titanium is supplied as anatase. As will be later 0 2,140,235 states that zinc titanate pigments are pointed out, titanium dioxide in the y-titanic obtained by heating zinc oxide with titanium acid modification does not conform to the teach dioxide in the proportion of at least 0.9 moi of ings of prior art dealing with reaction between zinc oxide to 1 mol of titanium dioxide at tem a titanium compound and a metal compound to peratures between 500° C. and 1100° C. He also form titanates. The tendency for combination of the y-titanic states that between the limits of 1 to 1.5 mois of acid and an oxide, as zinc oxide, for example, is zinc oxide to 1 mol of titanium dioxide, with tem so noticeable even at 100 that, although the X peratures of 900 to 1100° C., mixtures of zinc ray does not reveal conversion to titanate, the titanate crystals of the spinel crystalline form metal oxide is so tightly bound to the titanium with those of the corundum crystalline form are oy adsorption or otherwise that it cannot be ex obtained, while at lower temperatures, for in tracted therefrom by leaching with the usual sol stance 500 to 900° C., mixed crystals of spinel vents for zinc oxide, such as ammoniacal am-- form only are produced; that with proportions of monium chloride. (See Table I.) The titan more than 1.5 mols of zinc oxide to 1 mol of ates prepared from y-titanic acid and a metal titanium dioxide, exclusively mixed crystals of oxide in the manner described herein are highly 25 zinc titanate having the structure of Spinel are suitable for use as pigments, possessing excellent obtained. Lederle in U. S. Patent 2,140,236 states texture, whiteness, brightness, hiding power, and that the undesirable texture characteristics resistance to Weathering. usually found in titanates obtained by heating to It is well known that the compound ZingTiO4, gether titanium dioxide and a metal oxide may zinc orthotitanate, Crystallizes in the cubic sys 30 be avoided by a combination of steps comprising tem and possesses crystalline structure of. the mutual precipitation of the compounds, a two spinel type (Wyckoff's MgAl2O4(k). (Wyckoff, The stage calcination, and pressure treatment of the structure of crystals, 2nd edition (1931), p. 292.) in-process materials. (It will be understood that The terms "symmetry" and 'structure types' are the corundum crystalline form as referred to by used in this specification and the claims attached 5 Lederle is the same as the ilmenite structural thereto in the same sense that they are employed type, the latter being the more recent nomen in Wyckoff. On p. 287 of the reference, Wyckoff clature as employed by Wyckoff and Hanawalt describes compounds, R2MXA, type (k) with the for compounds of this type.) space group Oh. The pattern of ZnTiO3 has not The probable phase diagram covering the sys hitherto been published, and this compound has 40 tem. TiO2/ZnO obtained by heating proportions been found by us to be of hexagonal symmetry of titanium dioxide in the form of anatase, such and of the FeTiO3 or ilmenite structure type. for instance as is derived from thermal hydroly Wyckoff's ilmenite, FeTiO3 (aac). (Wyckoff, The sis of sulphate solutions of titanium in the usual structure of crystals, Supplement, 2nd ed.
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