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United States Patent (19) [11] 3,772,046 Knapp Et Al

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United States Patent (19) [11] 3,772,046 Knapp Et Al United States Patent (19) [11] 3,772,046 Knapp et al. (45) Nov. 13, 1973 (54) TIO, SLURRIES HAVING A HIGH SOLIDS 3,674,528 7|1972 Bronson.............................. 106.1300 CONTENT 3,510,334 5/1970 Goodspeed.............. ... 106/300 3,506,466 4/1970 Bramekamp et al..... ... 106/300 75 Inventors: Donald Edward Knapp, Savannah, 2,933,408 4/1960 Dempster et al..... ... 106/300 Ga.; Lindo Paul Nageroni, Bound 3,702,773 1 1/1972 Hall et al............................ 1061300 Brook, N.J. (73) Assignee: American Chemical Company, Primary Examiner-Delbert E. Gantz Stamford, Conn. Assistant Examiner-James W. Hellwege 22 Filed: Jan. 17, 1972 Attorney-Roland A. Dexter (21) Appl. No.: 218,453 Related U.S. Application Data 57 ABSTRACT 63 Continuation-in-part of Ser. No. 55,286, July 15, Pigment slurries of 70% by weight solids contents are 1970, abandoned. shown to have long term stability even when exposed to typical paper making chemicals such as calcium (52) U.S. Cl................................................. 106.1300 carbonate. The aqueous slurries are formulated with (51 Int. Cl............................................... C09c 1/62 pigment containing a small but effective admixed 58) Field of Search..................................... 106/300 amount of polyhydric alcohol and an alkanolamine, and with water which contains a small but effective 56) References Cited amount of a second alkanol-amine which provides a UNITED STATES PATENTS slurry pH of at least 9. 3,649,323 3/1972 Roe et al............................ 106/300 5 Claims, No Drawings 3,772,046 2 TIO, SLURRIES HAVING A HIGH SOLIDS bonate which is frequently encountered in the produc CONTENT tion of paper. It is an object of the invention to overcome the fore This is a continuation-in-part of our copending U.S. going and related disadvantages of water dispersed pig Pat. application Ser. No. 55,286, filed July 15, 1970, 5 ment slurries of high solids content. now abandoned. It is a further object of the invention to obtain a high The present invention relates to stable titanium diox solids content pigment slurry which is viscosity stabi ide slurries of high solids content (70% by weight of lized, i.e., has resistance to flocculation and settling in pigment and higher). It particularly relates to pigment water, particularly in the presence of calcium carbon slurries which have stable, low viscosities as the result 10 atte. of the presence of a normal non-volatile polyhydric al It has been discovered that slurries derived from dry cohol in combination with a plurality of alkanolamines. titanium dioxide pigment particles which have been ad Titanium dioxide is at present the premier white pig mixed with a small amount of viscosity stabilizer such ment of commerce. It is generally produced by either as sorbitol and triethanolamine are materially im hydrolyzing an aqueous solution of a titanium salt such 15 proved in their dispersibility and resistance to floccula as a sulfate and calcining the hydrolysate at 750-1000 tion in water, particularly aqueous systems having high C. or oxidizing a titanium halide, e.g., titanium tetra calcium carbonate content when a second alkanola chloride, at elevated temperatures of 800° C. and mine is present. higher, followed by cooling to a temperature below The amount of the viscosity stabilizing agent carried 600 C. The product resulting from the calcination or by pigment of the U.S. Pat. No. 3,649,323 is small. The oxidation contains a substantial amount of oversized, minimum effective amount has not yet been deter gritty TiO, particles which are broken up by either wet mined, but the evidence is that this minimum is about or dry grinding. Drying, following wet grinding, fre 0.2% of the dry weight of the pigment. At the other ex quently causes cementation of agglomerates requiring treme, pigment carrying more than about 3% by weight a further milling treatment before a smooth textured 25 of the agent possesses closely similar properties to pigment product can be obtained. In the dry milling op those possessed by pigment carrying somewhat less eration, suspending agents and dispersing aids are often agent, so that the value of 3% is taken as the upper introduced during the milling to facilitate the reduction practical limit. In practice we find that the optimum of the pigment to fine, uniform-sized particles. An opti amount of agent occurs within the range of about 0.2% mum means for dry grinding is a fluid energy mill in 30 to 1%, and this range is accordingly preferred. The which the pigment particles are conveyed by a gaseous scope of the invention is not restricted by the above in fluid, such as air or steam, into the outer portion of an gredients. The viscosity stabilizing agent is a normal, inwardly spiralling vortex at high velocity and in a man nonvolatile polyhydric alcohol, which incluses sorbitol ner which will maintain the vortex at a high rotative and mannitol, and it is combined with an alkanolamine. speed and a relatively low inward speed whereby the 35 Representative of the alkanolamines are: mixed iso pigment aggregates may be fractured. propanolamines; diisopropanolamine; diisopropyle Triethanolamine alone and with aerogel has been thanol-amine; 2-amino-2-methyl-1,3-propanediol; suggested as a dispersion aid during grinding to en 2-amino-2-methyl-1-propanol; 2-amino-2-ethyl-1,3- hance the fineness and gloss of titanium dioxide pig propanediol; 2-dimethylamino-2-methyl-1-propanol; ments. It has also been suggested that water dispersible 40 aminoethanolamine; diethylethanolamine; N titanium dioxide pigments can be produced from cal methylethanolamine; methyldiethanolamine; cined pigment material which has been wet milled and N-aminopropyl-morpholine; digylcolamine; and trieth preferably hydro-separated by utilizing certain amines anolamine. as organic dispersants, which amines includes mono Of these alkanolamines, triethanolamine is preferred ethanolamine, morpholine and triethanolamine. Unfor 45 because of its unique slurry stabilization property when tunately, aqueous slurries of high solids content (70% used in combination with sorbitol and 2-amino-2- by weight and higher) of such pigments tend to settle methyl-1-propanol. All of these alkanolamines are and form, upon standing, a hard sediment which is diffi characterized by the unique property of providing sta cult to redisperse. bility to high solids content pigment slurries when ad It is also known that generally water-dispersible TiO, SO mixed with a normal, nonvolatile polydydric alcohol pigments form a deflocculated slurry in hard water and such as sorbitol. They can all be considered water solu consequently settle within 2-3 hours into a very coher ble in the contect of this invention. ent sediment which is extremely difficult to reincorpo As noted above in the present invention a second al rate to a uniform slurry. kanolamine is present in the slurry, however, not all al The sedementation characteristics of such aqueous 55 kanolamines are suitable. The suitable second alkanol dispersions of titanium dioxide particles have been im amines, characterized by exhibiting a pH at or above 9 proved by the presence of normal water soluble poly in aqueous slurry systems, include: monoethanolamine; ols, including sorbitol and mannitol. Unfortunately, aminoethylethanolamine; N-methylethanolamine; di such polyols frequently degrade when exposed to high ethanolamine; dimethylethanolamine; diisopropyle temperatures and cause noticeable discoloration. 60 thanolamine; methyldiethanolamine; monoisopropa A copending U.S. Pat. application, Ser. No. 857,583, nolamine; diisopropanolamine; morpholine; N-amino filed Sept. 12, 1969 now U.S. Pat. No. 3,649,323, propylmorpholine; 2-amino-2-methyl-1-propanol; 2 teaches that high solids content pigment slurries can be amino-1-butanol; 2-amino-2-methyl-1,3-propane diol; stabilized to useful viscosities by the presence of nor and tris-(hydroxymethyl) aminomethane. mal, non-volatile polyhydric alcohol in combination 65 The amount of the second alkanolamine present in with an alkanolamine. Unfortunately such slurries are the slurry may vary within the wide limits but an unstable in the presence of dry or slurried calcium car amount of at least 0.05% to 5.0% (based on the amount 3,772,046 3. 4. CaCOs Compatibility of the titanium dioxide present) is preferred. Below %AMP** initial 16 hr. 0.5% no useful enhancement of stabilization is discern Sample % TiO, Added Consistency Viscosity*** ible. Amounts in excess of 5% do not appear to give 730 0.0 Thick > 0 2 74.O. 0.25 Fluid 1790 sufficiently improved results to warrant the use of the 3 73.5 0.50 Fluid 1000 additional alkanolamine is such concentrations. 4 73.0 0.75 Fluid 1080 The titanium dioxide pigment, both anatase and ru 5 740 1.00 Fluid 970 References *, **, and *** are the same as in Table . tile, benefited by the present invention includes those h. This test procedure specifies that equal volumes of slurries of about grades which contain small amounts of alkali metal, al 70% by weight each of TiO, and “Snowflake Whiting" CaCO, are kaline earth metal salts and other cations as condition thoroughly hand mixed and the viscosity of the resultant mixture is ing agents. In addition the salts of other metals such as 10 then measured as a function of time. antimony and zinc as brighteners and rutile converters EXAMPLE 3 may be present. The amount of these salts and agents is usually less than 5% of the weight of the pigment; The second alkanolamine as noted is characterized but, is not restricted to that level. by providing a pH of at least 9 in aqueous high-solids Dry pigment described in copending application Ser. 15 content pigment siurry systems and will retain such a No. 857,853 can be prepared according to a number of pH over long periods of time, 4 weeks or longer.
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