Treated inorganic particles
Treated inorganic particles with silica, alumina, and organic treatments address dispersion challenges by improving flow characteristics and reducing dispersant demand, resulting in enhanced dispersion efficiency.
Patent Information
- Application Number
- PCT/US2025/043717
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2025-03-25
- Filing Date
- 2025-08-27
- Publication Date
- 2026-03-05
AI Technical Summary
Inorganic particles or pigments, such as titanium dioxide, often re-agglomerate and are difficult to disperse in coating compositions, leading to challenges in achieving uniform dispersion and requiring high dispersant demand.
Treated inorganic particles with a surface treatment comprising silica, alumina, and an organic treatment of polyol and/or siliconate, applied through a process involving aqueous slurry preparation, drying, milling, and organic treatment application, reduce the need for dispersants.
The treated inorganic particles exhibit improved flow characteristics and reduced dispersant demand, enhancing dispersion efficiency and reducing agglomeration issues.
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Figure US2025043717_05032026_PF_FP_ABST
Abstract
Description
TI0009-W001TITLE OF THE INVENTIONTREATED INORGANIC PARTICLESCROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of priority of U.S. Provisional Application No. 63 / 687,968 filed August 28, 2024, and claims the benefit of priority of U.S. Provisional Application No. 63 / 728,409 filed December s, 2024, and claims the benefit of priority of U.S. Provisional Application No. 63 / 777,351 filed March 25, 2025, the disclosures of which are incorporated herein by reference in their entirety.FIELD OF THE INVENTION
[0002] The present disclosure relates to treated inorganic particles having desired dispersion properties while lowering dispersant demand.BACKGROUND OF THE INVENTION
[0003] Coating compositions of interest in the present disclosure are water-borne coating compositions such as latex coating compositions, e.g. acrylic, styrene acrylic, vinyl acetate, ethylene vinyl acetate, polyurethane, alkyd dispersion etc; and solvent based coating compositions such as alkyd coating compositions; urethane coating compositions; and unsaturated polyester coating compositions, acrylic, styrene-acrylic compositions typically a paint, clear coating, or stain. These coatings may be applied to a substrate by spraying, applying with a brush or roller or electrostatically, such as pigment coatings, etc. These coating compositions are described in Outlines of Paint Technology (Halstead Press, New York, NY, Third edition, 1990) and Surface Coatings Vol. I, Raw Materials and Their Usage (Chapman and Hall, New York, NY, Second Edition, 1984).
[0004] Inorganic particles or pigments may be added to the coating compositions. In particular, titanium dioxide pigments have been added to coating compositions for imparting whiteness and / or opacity to the finished article. However, such particles or pigments can re-agglomerate and be difficult to disperse in downstream applications. Therefore, a need exists for an inorganic particle or pigment such as titanium dioxide that has improved flow characteristics.
[0005] Inorganic particles or pigments have a number of other uses, including additives for polymer compositions. When added to polymer compositions, inorganic particles are added to polymers for imparting whiteness and / or opacity to theTI0009-W001 finished polymer article. To deliver other properties to the molded part or film, additional additives are incorporated into the processing step. Therefore, the need exists for an inorganic particle having multiple beneficial properties.SUMMARY OF THE INVENTION
[0006] According to certain aspects of the present invention, a treated inorganic particle may include an inorganic particle having a surface and having a surface treatment on the inorganic particle surface. The surface treatment may include (1 ) silica, (2) alumina, and (3) an organic treatment. The organic treatment may include a polyol and / or siliconate, and the organic treatment may be present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
[0007] In some aspects, the inorganic particle comprises an inorganic oxide pigment. The inorganic particle may comprise, for example, an inorganic oxide selected from TiCh, AI2O3, SiO2, ZnO, SrTiCh, BaSO, PbCOs, BaTiOs, Ce2O3, CaCOs, ZrC>2, or mixtures thereof. In some aspects, the inorganic particle comprises a TiC>2 particle. In some aspects, the inorganic particle comprises a TiC>2 pigment.
[0008] In certain aspects, the polyol comprises H-(O-CH2CH2)n-OH and / or C(H)x(OH)y(R1OH)z , wherein n =1-4, x=0-1 , y=0-1 , z=2-4, such that x+y+z=4, and R1=CI-C3 alkylene. The polyol may be a diol without an alkyl branch, a triol without an alkyl branch, a tetraol without an alkyl branch, or combinations thereof. The polyol may be, for example, glycerol, triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof. In some aspects, the organic treatment consists essentially of glycerol. In some aspects, the polyol is chosen such that z=3- 4.
[0009] In some aspects, the siliconate may be an alkali metal salt of alkyl and / or aryl siliconate. The siliconate may comprise R2-Si(OM)3, wherein M is independently alkali metal or H, R2is linear or branched C1-C18 alkyl or aryl, and at least one M comprises alkali metal. The siliconate may be a sodium and / or potassium salt of alkyl and / or aryl siliconates. For example, the siliconate may be sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof. In some aspects, the siliconate comprises:TI0009-W001or combinations thereof, wherein R = alkyl (Ci-Cis); aryl.
[0010] The treated inorganic particle may have a mean particle size of about 100 nm to about 500 nm.
[0011] In some aspects, the organic treatment is present in an amount of about 0.3 wt% to about 0.4 wt% of the treated inorganic particle. Silica may be present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle, or about 1 wt% to about 5 wt% of the treated inorganic particle. Alumina may be present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle, or about 1 wt% to about 5 wt% of the treated inorganic particle. Polyol may be present in an amount of about 0.01 to about 1 wt% of the treated inorganic particle, about 0.1 wt% to about 1 wt% of the treated inorganic particle, about 0.1 wt% to less than 0.5 wt%, or about 0.3 wt% to about 0.5 wt% of the treated inorganic particle. Siliconate may be present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle, about 0.1 wt% to about 1 wt% of the treated inorganic particle, or about 0.3 wt% to about 0.5 wt% of the treated inorganic particle. In some aspects, the organic treatment comprises a polyol and a siliconate. In some aspects, the organic treatment does not comprise trimethylolpropane (TMP). In some aspects, the organic treatment does not include trimethylolethane (TME).
[0012] In some aspects, the present invention relates to a process of producing a treated inorganic particle comprising:TI0009-W001 a. producing an aqueous inorganic particle slurry having an inorganic particle with silica and alumina surface treatments; b. drying the aqueous inorganic particle slurry to form dried inorganic particles; c. milling the dried inorganic particles to form milled inorganic particles; and d. contacting the aqueous inorganic particle slurry, dried inorganic particles, or milled inorganic particles with an organic treatment, where the treated inorganic particle comprises an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1 ) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
[0013] In some aspects, the present invention relates to a process of producing a treated inorganic particle comprising: a. producing an aqueous inorganic particle slurry having an inorganic particle with silica and alumina surface treatments; b. drying the aqueous inorganic particle slurry by flash drying or spray drying to form dried inorganic particles; c. steam milling the dried inorganic particles to form milled inorganic particles; and d. contacting the aqueous inorganic particle slurry, dried inorganic particles, or milled inorganic particles with an organic treatment, where the treated inorganic particle comprises an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1 ) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
[0014] In some aspects, the treated inorganic particle does not comprise an amine-based dispersant. In some aspects, the treated inorganic particle does not comprise a polymeric dispersant.
[0015] In other aspects, the invention relates to a slurry composition comprising a treated inorganic particle, water, and dispersant. Treated inorganic particles as described herein may be included in a coating composition such as a solvent-borne coating composition or a water-borne coating composition. In other aspects, theTI0009-W001 invention relates to a polymer composition comprising a polymer and a treated inorganic particle.BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 shows dispersant demand curves for various samples of treated inorganic particles.
[0017] Figure 2 shows dispersant demand curves for various samples of treated inorganic particles at an apparent viscosity below 1500 cPs.
[0018] Figure 3 shows dispersant demand curves of Tamol™ 1124 for Sample F and Comparative Sample 3.
[0019] Figure 4 shows dispersant demand curves of Tamol™ 165A for Sample F and Comparative Sample 3.
[0020] Figure 5 shows dispersant demand curves of Tamol™ 963 for Sample F and Comparative Sample 3.
[0021] Figure 6 shows dispersant demand curves of Tamol™ 731 A for Sample F and Comparative Sample 3.
[0022] Figure 7 shows dispersant demand curves of Disperbyk-199 for Sample F and Comparative Sample 3.DETAILED DESCRIPTION OF THE INVENTION
[0023] Compositions of the present invention relate to treated inorganic particles having desired properties such as those associated with dispersion. The treated inorganic particle may include an inorganic particle with a surface, where the surface has a surface treatment. In some aspects, the surface treatment includes (1) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate. Such organic treatment may be present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
[0024] The present invention also relates to a process of producing a treated inorganic particle comprising: a. producing an aqueous inorganic particle slurry having an inorganic particle with silica and alumina surface treatments; b. drying the aqueous inorganic particle slurry by flash drying or spray drying to form dried inorganic particles; c. steam milling the dried inorganic particles to form milled inorganic particles; andTI0009-W001 d. contacting the aqueous inorganic particle slurry, dried inorganic particles, or milled inorganic particles with an organic treatment, where the treated inorganic particle comprises an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1 ) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.Particles
[0025] It is contemplated that any inorganic particle may benefit from the surface treatment of this disclosure. By inorganic particle, it is meant an inorganic particulate material that becomes uniformly dispersed throughout a polymer melt, a paper slurry, or coating resin and imparts color and opacity to the polymer melt, paper slurry, or coating resin.
[0026] Inorganic particles include natural or synthetic materials or minerals. They typically have a high melting point, for example, above 200°C. Types of inorganic particles include, but are not limited to, inorganic oxide; inorganic carbide, such as silicon carbide; inorganic nitride, such as silicon nitride, aluminum nitride, or boron nitride; inorganic boride, such as titanium boride; inorganic silicide, such as molybdenum silicide; inorganic sulfate, such as aluminum sulfate or barium sulfate; inorganic carbonate, such as calcium carbonate or magnesium carbonate; inorganic silicates, such as aluminum silicate or magnesium silicate; or mixtures thereof. Inorganic oxides include but are not limited to metallic oxides, such as oxides of Ti, Al, Si, Zn, Sr, Ba, Pb, Ce, Zr, Sn, or mixtures thereof. In some aspects, an inorganic particle comprises an inorganic oxide selected from TiOs, AI2O3, SiOs, ZnO, SrTiOs, BaSC , PbCCh, BaTiOs, Ce2C>3, CaCOs, ZrC>2, or mixtures thereof. Mixtures of inorganic compounds listed above may be present in the formation of the particle; for example, they may be part of the same particle core. Mixtures of inorganic particles of different inorganic compounds may also be physically blended and used. In one aspect, the inorganic particle comprises at least two inorganic compounds.
[0027] In some aspects, the inorganic particle comprises an inorganic pigment. The term "pigment" is understood to mean a particle having an average size of less than 1 micron. Typically, the pigments have an average size of from about 0.020 toTI0009-W001 about 0.95 microns, more typically, about 0.050 to about 0.75 microns and most typically about 0.075 to about 0.60 microns, as measured by Horiba LA300 Particle Size Analyzer.
[0028] In some aspects, the inorganic particle is a titanium dioxide particle. In some aspects, the inorganic particle is a titanium dioxide pigment. The TiO? particle may be in rutile or anatase crystalline form, and it may be made by either a chloride process or sulfate process. In the chloride process, TiCl4 is oxidized to TiC particles. In the sulfate process, sulfuric acid and ore containing titanium are dissolved, and the resulting solution goes through a series of steps to yield TiC>2. Both the sulfate and chloride processes are described in greater detail in "The Pigment Handbook", Vol. 1 , 2nd Ed., John Wiley & Sons, NY (1988), the teachings of which are incorporated herein by reference.
[0029] The titanium dioxide particle may be substantially pure titanium dioxide or may contain other components, such as silica, alumina, aluminosilicates, phosphates, and zirconia. These components may become incorporated into the particles and / or may be coated on the surfaces of the particles, for example, by an oxidation process and / or a precipitation process. These components may be present in an amount of about 0.1 to about 20 wt%, about 0.1 to about 12 wt%, or about 0.5 to about 10 wt%, based on the total particle weight.Surface Treatment
[0030] Treated inorganic particles of the present invention may include a surface treatment which may include one or more components.
[0031] In some aspects, the inorganic particles may include a surface treatment including one or more inorganic components. The one or more inorganic components may be selected from inorganic oxide; inorganic carbide, such as silicon carbide; inorganic nitride, such as silicon nitride, aluminum nitride, or boron nitride; inorganic boride, such as titanium boride; inorganic silicide, such as molybdenum silicide; inorganic sulfate, such as aluminum sulfate or barium sulfate; inorganic carbonate, such as calcium carbonate or magnesium carbonate; inorganic silicates, such as aluminum silicate or magnesium silicate; or mixtures thereof. Inorganic oxides include but are not limited to metallic oxides, such as oxides of Ti, Al, Si, Zn, Sr, Ba, Pb, Ge, Zr, Sn, or mixtures thereof. Specific examples of inorganic oxides include TiC , AI2O3, SiC>2, ZnO, SrTiOs, BaTiOs, Ce2O3, ZrO2, or mixturesTI0009-W001 thereof, selected from the inorganic materials noted above. In some aspects, the one or more inorganic components may be selected from AI2O3, SiC>2, ZrC>2, or mixtures thereof. In some aspects, the one or more inorganic components may be selected from AI2O3, SiCh, or mixtures thereof. In some aspects, the one or more inorganic components comprise AI2O3 and SiC>2. In some aspects, the one or more inorganic components comprise AI2O3, SiC>2, and at least one additional inorganic component.
[0032] In some aspects, such inorganic components are between the inorganic particle and the organic treatment and may be composed of the same or different inorganic compounds compared with the inorganic particle composition. For example, the inorganic particle may have a titanium dioxide core and a surface treatment including one or more additional inorganic oxide components. Such components may be adsorbed onto the surface of the inorganic particle, or they may be chemically bonded to the surface of the inorganic particle by chemical reaction. In one aspect, the inorganic components are applied by wet treatment process, from an aqueous basic or acidic metal salt compound. This method is described in US 5,993,533. Another method of adding an inorganic component is by deposition of pyrogenic inorganic compounds onto a pyrogenic titanium dioxide particle as described in US 5,922,120.
[0033] The inorganic components may be continuous or discontinuous layers on the surface of the inorganic particle. Mixtures of inorganic compounds listed above may be present in each of the inorganic layers. In some aspects, inorganic components may be present in separate inorganic layers, may be mixed together in an inorganic layer, and / or may be mixed together with the organic treatment.
[0034] In some aspects, the inorganic particle comprises a surface treatment including at least one inorganic layer between the inorganic particle and the organic treatment; in some aspects, the inorganic particle comprises a surface treatment including at least two inorganic layers between the inorganic particle and the organic treatment. Such inorganic layers may be, for example, inorganic oxides, inorganic hydroxides, inorganic carbonates, or mixtures thereof. In one aspect, the inorganic layer or layers are metal oxides, metal hydroxides, or metal carbonates. In one aspect, the inorganic particle comprises at least two inorganic compounds and the treated inorganic particle further comprises at least one inorganic layer, where the at least one inorganic layer is between the inorganic particle and the organicTI0009-W001 treatment layer. Inorganic oxides may include but are not limited to metallic oxides, such as oxides of Ti, Al, Si, Zn, Sr, Ba, Pb, Ce, Zr, Sn, or mixtures thereof. Specific examples of inorganic oxides include TiC>2, AI2O3, SiO2, ZnO, SrTiOs, BaTiOs, Ce2O3, ZrC>2, or mixtures thereof. Oxides of P, such as P2Os or P2O5; oxides of B such as B2O5; oxides of Ca such as CaO; or oxides of Mg such as MgO may also be incorporated. Other specific inorganic layers, including but not limited to Mg(OH)2, Ca(OH)2, CaCOs, or MgCOs, may also be used.
[0035] In some aspects, a treated inorganic particle can include a layer of silica and a layer of alumina located between the inorganic particle and the organic treatment; such treated inorganic particle could also contain additional layers between the inorganic particle and the organic treatment such as oxides as described herein. In some aspects, a treated inorganic particle can include a layer having a blend of silica and alumina located between the inorganic particle and the organic treatment; such treated inorganic particle could also contain additional layers between the inorganic particle and the organic treatment such as oxides as described herein, require one layer of silica and one layer of alumina, or a blend.
[0036] In one aspect, the inorganic particle is a TiC>2 particle, and the treated inorganic particle comprises at least one additional metal oxide selected from TiO2, AI2O3, SiC>2, ZnO, SrTiOs, BaTiOs, Ce2O3, ZrO2, or mixtures thereof. In one aspect, the at least one additional metal oxide is present in an amount of about 0.1 -20% by weight; in another aspect, the at least one additional metal oxide is present in an amount of about 0.1-7% by weight; and in another aspect, the at least one additional metal oxide is present in an amount of about 0.5-7% by weight; based on the total weight of the treated inorganic particle. The at least one additional metal oxide may be part of the inorganic particle, or it may present in one or more inorganic layers. The inorganic particle may be made by co-oxygenation of inorganic tetrachloride with titanium tetrachloride, as described in US 5,562,764, and US 7,029,648. Examples of suitable commercially available titanium dioxide particles having at least one additional metal oxide include alumina-coated titanium dioxide particles such as Ti-Pure™ R700 and Ti-Pure™ R706, alumina / phosphate coated titanium-dioxide particles such as Ti-Pure™ R796+; and alumina / phosphate / ceria coated titanium-dioxide particles such as Ti-Pure™ R794; all available from The Chemours Company, Wilmington DE.TI0009-W001
[0037] The inorganic particles having inorganic treatments may be in the form of an aqueous inorganic particle slurry. Optionally, the aqueous inorganic particle slurry is milled by a wet milling technique to reduce the particle size. Wet milling techniques may include, but are not limited to, media milling, sand milling, immersion milling, or basket milling.
[0038] The aqueous inorganic particle slurry may be dried by any drying process capable of forming dried inorganic particles. In one aspect, the aqueous inorganic particle slurry is dried by flash drying or spray drying to form dried inorganic particles. Without wishing to be bound by theory, it is believed that such quick drying methods allow for any treatments, including inorganic and organic, to distribute uniformly on the inorganic particles rather than migrating to one area of the particle bulk. The dried particles may then be milled by steam milling or other milling techniques to reduce the particle size of the dried particles. Steam milling is a dry grinding technique that uses steam as a milling gas to achieve fine particles. Steam milling techniques employ elevated temperatures, such as those necessary to maintain steam without condensation of water. In one aspect, the steam is superheated during milling to achieve high velocity. Steam milling techniques include, but are not limited to, jet milling and micronizing.Organic Treatment
[0039] A surface treatment may further include an organic treatment. An organic treatment may include a polyol and / or silconate. In some aspects, an organic treatment includes a polyol and a siliconate.
[0040] In some aspects, a polyol may be selected from H-(O-CH2CH2)n-OH and / or C(H)x(OH)y(R1OH)z , wherein n =1-4 x=0-1 y=0-1 z=2-4 such that x+y+z=4 R1=CI-C3 alkylene.
[0041] In some aspects, a polyol may be selected from a diol without an alkyl branch, a triol without an alkyl branch, a tetraol without an alkyl branch, or combinations thereof. In some aspects, a polyol may be selected from glycerol,TI0009-W001 triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof. In some specific aspects, the organic treatment consists essentially of glycerol. In some aspects, the organic treatment comprises a polyol, siliconate, mixture of siliconate and glycerol, or mixture of siliconate and polyol, where the polyol is selected from H-(O-CH2CH2)n-OH and / or C(H)x(OH)y(R1OH)zas defined above, and where z=3-4.
[0042] In some aspects, a polyol may have one or more of the following formulae: HOCH2(CH2OCH2)nCH2OH n = 1 , 2, 3, or 4,or combinations thereof.
[0043] A polyol may be present in an amount of about 0.01 to about 1 wt%, about 0.1 to about 1 wt%, or about 0.3 to about 0.5 wt% of the treated inorganic particle. In some aspects, the polyol is present in an amount of at least about 0.01 wt%; at least about 0.05 wt%; at least about 0.1 wt%; at least about 0.15 wt%; at least about 0.2 wt%; at least about 0.25 wt%; at least about 0.3 wt%; at least about 0.31 wt%; at least about 0.32 wt%; at least about 0.33 wt%; at least about 0.34 wt%; at least about 0.35 wt%; at least about 0.36 wt%; at least about 0.37 wt%; at least about 0.38 wt%; at least about 0.39 wt%; at least about 0.40 wt%; at least about 0.41 wt%; at least about 0.42 wt%; at least about 0.43 wt%; at least about 0.44 wt%; at least about 0.45 wt%; at least about 0.46 wt%; at least about 0.47 wt%; at least about 0.48 wt%; or at least about 0.49 wt%, all based on the weight of the treated inorganic particle. In some aspects, the polyol is present in an amount of at most about 1 wt%; at most about 0.9 wt%; at most about 0.8 wt%; at most about 0.7 wt%; at most about 0.6 wt%; at most about 0.55 wt%; at most about 0.54 wt%; at most about 0.53 wt%; at most about 0.52 wt%; at most about 0.51 wt%; at most about 0.5 wt%; at most about 0.49 wt%; at most about 0.48 wt%; at most about 0.47 wt%; at most about 0.46 wt%; at most about 0.45 wt%; at most about 0.44 wt%; at most about 0.43 wt%; at most about 0.42 wt%; at most about 0.41 wt%; at most about 0.4 wt%; at most about 0.39 wt%; at most about 0.38 wt%; at most about 0.37 wt%; atTI0009-W001 most about 0.36 wt%; at most about 0.35 wt%; or at most about 0.3 wt%, all based on the weight of the treated inorganic particle.
[0044] In one specific aspect, the organic treatment consists essentially of glycerol, and the organic treatment is present in an amount of at least about 0.1 wt%; at least about 0.15 wt%; at least about 0.2 wt%; at least about 0.25 wt%; at least about 0.3 wt%; at least about 0.31 wt%; at least about 0.32 wt%; at least about 0.33 wt%; at least about 0.34 wt%; at least about 0.35 wt%; at least about 0.36 wt%; at least about 0.37 wt%; at least about 0.38 wt%; at least about 0.39 wt%; at least about 0.40 wt%; at least about 0.41 wt%; at least about 0.42 wt%; at least about 0.43 wt%; at least about 0.44 wt%; at least about 0.45 wt%; at least about 0.46 wt%; at least about 0.47 wt%; at least about 0.48 wt%; or at least about 0.49 wt%, all based on the weight of the treated inorganic particle. In some aspects, the organic treatment consists essentially of glycerol, and the organic treatment is present in an amount of less than 0.5 wt%; at most about 0.49 wt%; at most about 0.48 wt%; at most about 0.47 wt%; at most about 0.46 wt%; at most about 0.45 wt%; at most about 0.44 wt%; at most about 0.43 wt%; at most about 0.42 wt%; at most about 0.41 wt%; at most about 0.4 wt%; at most about 0.39 wt%; at most about 0.38 wt%; at most about 0.37 wt%; at most about 0.36 wt%; at most about 0.35 wt%; or at most about 0.3 wt%, all based on the weight of the treated inorganic particle.
[0045] A mixture of siliconate and glycercol, or a mixture of siliconate and polyol where the polyol is selected from H-(O-CH2CH2)n-OH and / or C(H)x(OH)y(R1OH)z as defined above, and where z=3-4, may be present in an amount of about 0.01 to about 1 wt%, about 0.1 to about 1 wt%, or about 0.3 to about 0.5 wt% of the treated inorganic particle. In some aspects, the mixture is present in an amount of at least about 0.01 wt%; at least about 0.05 wt%; at least about 0.1 wt%; at least about 0.15 wt%; at least about 0.2 wt%; at least about 0.25 wt%; at least about 0.3 wt%; at least about 0.31 wt%; at least about 0.32 wt%; at least about 0.33 wt%; at least about 0.34 wt%; at least about 0.35 wt%; at least about 0.36 wt%; at least about 0.37 wt%; at least about 0.38 wt%; at least about 0.39 wt%; at least about 0.40 wt%; at least about 0.41 wt%; at least about 0.42 wt%; at least about 0.43 wt%; at least about 0.44 wt%; at least about 0.45 wt%; at least about 0.46 wt%; at least about 0.47 wt%; at least about 0.48 wt%; or at least about 0.49 wt%, all based on the weight of the treated inorganic particle. In some aspects, the mixture is present in an amount of at most about 1 wt%; at most about 0.9 wt%; at most about 0.8 wt%;TI0009-W001 at most about 0.7 wt%; at most about 0.6 wt%; at most about 0.55 wt%; at most about 0.54 wt%; at most about 0.53 wt%; at most about 0.52 wt%; at most about 0.51 wt%; at most about 0.5 wt%; at most about 0.49 wt%; at most about 0.48 wt%; at most about 0.47 wt%; at most about 0.46 wt%; at most about 0.45 wt%; at most about 0.44 wt%; at most about 0.43 wt%; at most about 0.42 wt%; at most about 0.41 wt%; at most about 0.4 wt%; at most about 0.39 wt%; at most about 0.38 wt%; at most about 0.37 wt%; at most about 0.36 wt%; at most about 0.35 wt%; or at most about 0.3 wt%, all based on the weight of the treated inorganic particle.
[0046] In some aspects, a siliconate may comprise an alkali metal salt of alkyl and / or aryl siliconate. In some aspects, a siliconate may comprise a sodium and / or potassium salt of alkyl and / or aryl siliconates. In some aspects, a siliconate may comprise R2-Si(OM)3, wherein M is independently alkali metal (preferably Na, K) or H, R2is linear or branched C1-C18 alkyl or aryl, and at least one M must be alkali metal. In some aspects, a siliconate may be selected from sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof. In some aspects, a suitable siliconate may have one or more of the following formulae:wherein R = alkyl (C1-C18); aryl.
[0047] A siliconate may be present in an amount of about 0.01 to about 1 wt%, about 0.1 to about 1 wt%, about 0.3 wt% to about 1 wt%, about 0.01 wt% to about 0.7 wt%, about 0.1 wt% to about 0.7 wt%, about 0.3 wt% to about 0.7 wt%, about 0.01 wt% to about 0.4 wt%, about 0.1 wt% to about 0.4 wt%, about 0.01 wt% toTI0009-W001 about 0.5 wt%, about 0.1 wt% to about 0.5 wt%, about 0.3 wt% to about 0.4 wt%, or about 0.3 to about 0.5 wt% of the treated inorganic particle.
[0048] In some aspects, the organic treatment does not include trimethylolpropane. In some aspects, the organic treatment does not include trimethylolethane.
[0049] The organic surface treatment may be applied to the inorganic particle by conventional means, such as by mixing the inorganic particle with the organic treatment compound in either solution or solid form, followed by drying and milling of the particles. In some aspects, the organic treatment is present in an amount of about 0.01 wt% to about 1 wt%, about 0.1 wt% to about 1 wt%, about 0.3 wt% to about 1 wt%, about 0.01 wt% to about 0.7 wt%, about 0.1 wt% to about 0.7 wt%, about 0.3 wt% to about 0.7 wt%, about 0.01 wt% to about 0.4 wt%, about 0.1 wt% to about 0.4 wt%, about 0.3 wt% to about 0.5 wt%, or about 0.3 wt% to about 0.4 wt% of the treated inorganic particle.
[0050] In some aspects, the treated inorganic particle does not comprise an amine-based dispersant. In some aspects, the treated inorganic particle does not comprise a polymeric dispersant. In other words, in some aspects, no amine-based dispersant and / or no polymeric dispersant is / are used to form the treated inorganic particle itself, for example, during the inorganic oxide formation or organic treatment steps.
[0051] The organic treatment may be contacted with the inorganic particles at various points along the process. For example, the organic treatment may be contacted with the aqueous inorganic particle slurry. This could occur before or after wet milling, when wet milling is employed. In this instance, the organic treatment is then dried quickly to disperse the organic material on the particle surfaces. In another aspect, the organic treatment may be contacted with the dried inorganic particles. In this instance, the organic treatment may be added during the drying process, or it may be added after the inorganic particle exit the dryer. In another aspect, the organic treatment is contacted with the milled inorganic particles as the inorganic particles exit the steam mill, such that the temperature is elevated. When the organic treatment is added to the dried inorganic particles or milled inorganic particles, the heat of the steam from steam milling causes quick drying of the organic treatment on the inorganic particles.TI0009-W001Particle Size
[0052] In some aspects, a treated inorganic particle may have a mean particle size of about 100 nm to about 500 nm, or about 200 nm to about 350 nm. The term “mean particle size” is intended to mean the mathematical mean of a sample of particles having a particle size distribution. It can be measured in dilute aqueous dispersions with a particle size analyzer, such as Horiba LA-300 Particle Size Analyzer.Slurry Composition / Coating Composition
[0053] Treated inorganic particles and pigments may be added to coating compositions and / or slurry compositions. The term “slurry composition” is hereby used to denote compositions made from the previously formed treated inorganic particles by combining the treated inorganic particles with additional components. The composition is different than that of the aqueous inorganic particle slurry described in the process for making the treated inorganic particle.
[0054] For example, titanium dioxide pigments may be added to coating compositions for imparting whiteness and / or opacity to the finished article. Treated inorganic particles as described herein may be added to water-borne and / or solvent-borne coating compositions.
[0055] Coating compositions and slurry compositions which include treated inorganic particles as described herein may also include additional desired components. A slurry composition may include treated inorganic particles, water, and dispersant. Additional components in the slurry compositions or coating compositions include, but are not limited to, pH modifiers, biocides, or defoamers.
[0056] The slurry compositions can be used as another mechanism for incorporating the treated inorganic particles into their intended application. A slurry composition may be made by mixing the hydrophobic inorganic particles with water and optional additives with a mechanical mixer. A mechanical dispersing aid, such as zirconia beads or other solid particles, may be added during mixing and later removed.
[0057] Dispersants useful in the slurry composition include any that aid in dispersing those applications, including but not limited to, amines; phosphates; carboxylic acids; di or tri carboxylic acids; phosphonates; phosphonate based carboxyic acids; polymeric dispersants; polyhydric alcohols; and mixtures thereof.TI0009-W001Specific compounds may include, but are not limited to, potassium pyrophosphate; tetrapotassium pyrophosphate; sodium hexametaphosphate; sodium, potassium, or ammonium polyphosphate; aliphatic carboxylic acid; citric acid; polyhydroxy alcohols; polyacrylates; alcohol amines such as 1-amino-2-ethanol, 2-amino-1- ethanol, 1-amino-2-propanol, 2-amino-2-methyl-1 -propanol, diethanolamine, diisopropanolamine, 2-methylamino-1 -ethanol, monoisopropanolamine, or triethanolamine; 2-amino-2-methyl-1 ,3-propanediol; 2-amino-2-ethyl-1 ,3- propanediol; tris(hydroxymethyl)aminomethane; triethanolamine; N-butyl- diethanolamine; dimethylglucamine; phosphate carboxyic acids; salts of phosphate carboxylic acids; hydroxyl carboxylic acids; salts of hydroxyl carboxylic acids; polyacrylic acid; polyacrylic acid copolymers; salts of polyacrylic acid and polyacrylic acid copolymers; maleic acid copolymers; salts of maleic acid copolymers; trimethylolpropane; ditrimethylolpropane; glycerol; diglycerol; pentaerythritol; mannitol; and mixtures thereof. Some dispersants are commercially available under the tradenames TAMOL, DISPERBYK, and STRODEX, such as Tamol™ 681 , Tamol™ 165, Tamol™ 1124, Tamol™ 963, Tamol™ 731A, Disperbyk™-190, Disperbyk™-199,or Strodex™ PK-90. The dispersants or other additives may compose up to about 5% by weight of the total weight of the slurry composition. In one aspect, the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles; in another aspect, the slurry composition comprises at most 0.2 g dispersant / 100 g treated inorganic particles; and in another aspect, the slurry composition comprises at most 0.1 g dispersant / 100 g treated inorganic particles. In one aspect, the slurry composition comprises at least 0.005 g dispersant / 100 g treated inorganic particles; in another aspect, the slurry composition comprises at least 0.01 g dispersant / 100 g treated inorganic particles; and in another aspect, the slurry composition comprises at least 0.02 g dispersant / 100 g treated inorganic particles. In one aspect, the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles; in another aspect, a dispersant demand of at most 0.2 g dispersant / 100 g treated inorganic particles; and in another aspect, a dispersant demand of at most 0.1 g dispersant / 100 g treated inorganic particles. In one aspect, the slurry composition comprises a dispersant and has a dispersant demand of at least 0.005 g dispersant / 100 g treated inorganic particles; in another aspect, a dispersant demand of at least 0.01 g dispersant / 100 g treated inorganic particles;TI0009-W001 and in another aspect, a dispersant demand of at least 0.02 g dispersant / 100 g treated inorganic particles. Dispersant demand is determined by forming a slurry composition and identifying the minimum amount of added dispersant that forms the lowest apparent viscosity.
[0058] In one aspect, the coating composition provides a scats value of at most 30; in another aspect, at most 20; in another aspect, at most 15; in another aspect, at most 10. In another aspect, the treated inorganic particle provides a scats value of at most 30; in another aspect, at most 20; in another aspect, at most 15; in another aspect, at most 10. The scats value is determined by mixing the treated inorganic particle with a solvent-borne alkyd coating base having 65% by weight alkyd resin, based on the total weight of the solvent-borne alkyd coating base, to form a mixture having 70.3% by weight treated inorganic particle, based on the total weight of the mixture; diluting the mixture with additional solvent-borne alkyd coating base such that the treated inorganic particle is 33.1 % by weight treated inorganic particle, based on the total weight of the mixture; forming a paint film with an autoscraper; and using a Hegman gauge to read the number of scats.
[0059] Coating compositions may comprise an "alkyd coating," which is understood to mean a conventional liquid coating based on alkyd resins, typically a paint, clear coating, or stain. The alkyd resins are complex branched and crosslinked polyesters containing unsaturated aliphatic acid residues.
[0060] Coating compositions may comprise a "urethane coating," which is understood to mean a conventional liquid coating based on Type I urethane resins, typically a paint, clear coating, or stain. Urethane coatings typically contain the reaction product of a polyisocyanate, usually toluene diisocyanate, and a polyhydric alcohol ester of drying oil acids. Urethane coatings are classified by ASTM D16 into five categories. Type I urethane coatings contain a minimum of 10% by weight of a pre-reacted autoxidizable binder, characterized by the absence of significant amounts of free isocyanate groups. These are also known as uralkyds, urethane- modified alkyds, oil-modified urethanes, urethane oils, or urethane alkyds. Type I urethane coatings are the largest volume category of polyurethane coatings and include paints, clear coatings, or stains. The cured coating for a Type I urethane coating is formed by air oxidation and polymerization of the unsaturated drying oil residue in the binder.TI0009-W001
[0061] Coating compositions may comprise an "unsaturated polyester coating," which is understood to mean a conventional liquid coating based on unsaturated polyester resins, dissolved in monomers and containing initiators and catalysts as needed, typically as a paint, clear coating, stain, or gel coat formulation.
[0062] Coating compositions may comprise "water-dispersed coatings," which are understood to mean surface coatings intended for the decoration or protection of a substrate, comprising essentially an emulsion, latex, or suspension of a film-forming material dispersed in an aqueous phase, and optionally containing surfactants, protective colloids and thickeners, pigments and extender pigments, preservatives, fungicides, freeze-thaw stabilizers, antifoam agents, agents to control pH, coalescing aids, and other ingredients. Water-dispersed coatings are exemplified by, but not limited to, pigmented coatings such as latex paints, unpigmented coatings such as wood sealers, stains, and finishes, coatings for masonry and cement, and water-based asphalt emulsions. For latex paints the film forming material is a latex polymer of acrylate acrylic, styrene acrylic, vinyl-acrylic, vinyl, or a mixture thereof. Such water-dispersed coating compositions are described by C. R. Martens in "Emulsion and Water-Soluble Paints and Coatings" (Reinhold Publishing Corporation, New York, NY, 1965).
[0063] Coating compositions may comprise water-borne coating compositions such as latex coating compositions, e.g. acrylic, styrene acrylic, vinyl acetate, ethylene vinyl acetate, polyurethane, alkyd dispersion etc; and / or solvent based coating compositions such as alkyd coating compositions; urethane coating compositions; and unsaturated polyester coating compositions, acrylic, styrene- acrylic compositions typically a paint, clear coating, or stain. These coatings may be applied to a substrate by spraying, applying with a brush or roller or electrostatically, such as pigment coatings, etc. These coating compositions are described in Outlines of Paint Technology (Halstead Press, New York, NY, Third edition, 1990) and Surface Coatings Vol. I, Raw Materials and Their Usage (Chapman and Hall, New York, NY, Second Edition, 1984).
[0064] Coating compositions may comprise a "coating base," which is understood to mean a liquid formulation of a water-dispersed coating, an epoxy polymer coating, an alkyd coating, a Type I urethane coating, or an unsaturated polyester coating, which is later applied to a substrate for the purpose of creating a lasting film on said surface. The coating base includes those solvents, pigments, fillers, andTI0009-W001 functional additives found in a conventional liquid coating. For example, the coating base formulation may include a polymer resin and pigment dispersed in water, where the polymer resin is an acrylic polymer latex, vinyl-acrylic polymer, vinyl polymer, Type I urethane polymer, alkyd polymer, epoxy polymer, or unsaturated polyester polymer, or mixtures thereof.
[0065] In one aspect, a coating base is a water-dispersed coating in the form of an aqueous acrylic latex paint. The coating base includes those solvents, pigments, fillers, and functional additives found in a conventional liquid coating. Typically, the coating base may include a resin compound from 10 to 60% by weight, from 0.1 to 80% by weight of functional additives including pigments, fillers, and other additives, and the balance of the coating base composition is water or solvent. For an architectural coating, the resin compound is in an amount of about 30 to 60% by weight, functional additives including pigments, extenders, fillers, and other additives are in an amount of 0.1 to 60% by weight, with the balance being water or solvent.
[0066] In addition to the treated inorganic particles as described herein, coating compositions may include pigments such as rutile and anatase TiC>2, clays such as kaolin clay, asbestos, calcium carbonate, zinc oxide, chromium oxide, barium sulfate, iron oxide, tin oxide, calcium sulfate, talc, mica, silicas, dolomite, zinc sulfide, antimony oxide, zirconium dioxide, silicon dioxide, cadmium sulfide, cadmium selenide, lead chromate, zinc chromate, nickel titanate, diatomaceous earth, glass fibers, glass powders, glass spheres, MONASTAL Blue G (C.l. Pigment Blue 15), molybdate Orange (C.l. Pigment Red 104), Toluidine Red YW (C.l. Pigment 3)-process aggregated crystals, Phthalo Blue (C.l. Pigment Blue 15)- cellulose acetate dispersion, Toluidine Red (C.l. Pigment Red 3), Watchung Red BW (C.l. Pigment Red 48), Toluidine Yellow GW (C.l. Pigment Yellow 1), MONASTRAL Blue BW (C.I. Pigment Blue 15), MONASTRAL Green BW (C.I. Pigment Green 7), Pigment Scarlet (C.l. Pigment Red 60), Auric Brown (C.l.Pigment Brown 6), MONASTRAL Green G (C.l. Pigment Green 7), MONASTRAL Maroon B, MONASTRAL Orange, and Phthalo Green GW 951 . Such a pigment may be part of the coating base formulation, or may be added subsequently.TI0009-W001Polymer Compositions
[0067] Treated inorganic particles and pigments may be added to polymer compositions to impart a number of properties, including opacity, whiteness, or lightblocking power. Polymer compositions may include a polymer, the treated inorganic particles, and optional other additives. The present invention includes a process of making a polymer composition comprising producing a treated inorganic particle and contacting the treated inorganic particle with a polymer.
[0068] The dispersibility of the treated inorganic particle in polymer can be measured by screen pack dispersion (Ti count), as defined by particle retention on a 500 mesh screen of a composition containing 50 weight % treated inorganic particles in polyethylene. The present invention also includes a polymer composition containing the treated inorganic particles and the polymer composition using treated inorganic particles made by the process described above. In one aspect, the treated inorganic particles of the present invention have a screen pack dispersion (Ti count) of at most 100; in another aspect, a Ti count of at most 90; in another aspect, a Ti count of at most 80; and in another aspect, a Ti count of at most 70.
[0069] Polymers suitable for use in this invention include melt processible polymers, such as thermoplastics or thermoplastic elastomers. By “melt- processable,” it is meant a polymer that can be extruded or otherwise converted into shaped articles through a stage that involves obtaining the polymer in a molten state. Polymers may also be high molecular weight, meaning they have a melt index value of 0.01 to 50, typically from 2 to 10 as measured by ASTM method D1238-98.
[0070] Polymers include, but are not limited to, polymers of ethylenically unsaturated monomers; copolymers of ethylene and at least one olefin; vinyl polymers; polyvinyl esters; polystyrenes; acrylic homopolymers; acrylic copolymers; phenolic polymers; alkyd polymers; amino resins; epoxy resins; polyoxyethylenes; polyamides; polyurethanes; phenoxy resins; polysulfones; polycarbonates; polyesters; polyethers; acetal resins; polyimides; polyoxyethylenes; elastomers; natural or synthetic polymers of diene monomers; and mixtures thereof. Elastomers may include natural or synthetic rubbers. Diene polymers may include grafted copolymers, random copolymers, block copolymers, or blended polymers.
[0071] Ethylenically unsaturated monomer polymers include polyolefins such as polyethylene homopolymers or copolymers, polypropylene homopolymers or copolymers, and many others. Ethylene copolymers may include copolymers withTI0009-W001C3-C6 olefins, including but not limited to propylene or butylene. Low density polyethylene (LDPE), ultra-low density polyethylene (ULDPE), medium density polyethylene (MDPE), high density polyethylene (HDPE), and linear low density polyethylene (LLDPE) are all examples. Vinyl polymers include, for example, polyvinyl chloride. Specific polypropylene homopolymers include but are not limited to atactic polypropylene homopolymer, isotactic polypropylene homopolymer, and syndiotactic polypropylene homopolymer, for example, HIPP (highly isotactic polypropylene) or HCPP (highly crystalline polypropylene). Polyesters may include, for example, polyethylene terephthalate) or other common polyesters. When polyethylene or polypropylene copolymers are used, the polymer is typically a copolymer of polyethylene or polypropylene with an a-olefin comonomer. Examples of a-olefins include, but are not limited to, 1 -butene, 1 -hexene, 1 -octene, 4-methyl- 1 -pentene, vinyl acetate, methyl acrylate, ethyl acrylate, acrylic acid, or mixtures thereof. Other suitable polypropylene copolymers include impact copolymers produced by the addition of a copolymer such as ethylene-propylene rubber (EPR), ethylene-propylene-diene monomer (EPDM), polyethylene, or plastomers to a polypropylene homopolymer or polypropylene random copolymer.
[0072] A wide variety of additives may be present in the polymer composition as necessary, desirable or conventional. Such additives include polymer processing aids (e.g., fluoropolymers, fluoroelastomers, etc.), catalysts, initiators, antioxidants (e.g., hindered phenol such as butylated hydroxytoluene), blowing agents, stabilizers (e.g., hydrolytic stabilizers, radiation stabilizers, thermal stabilizers, or ultraviolet light stabilizers such as hindered amine light stabilizers or “HALS”), ultraviolet ray absorbers, organic pigments including tinctorial pigments, plasticizers, antiblocking agents (e.g. clay, talc, calcium carbonate, silica, silicone oil, and the like), anti-static agents, leveling agents, flame retardants, anti-cratering additives, optical brighteners, adhesion promoters, colorants, dyes or pigments, delustrants, fillers, fire retardants, lubricants, reinforcing agents (e.g., glass fiber and flakes), anti-slip agents, slip agents (e.g., talc or anti-block agents), and other additives.
[0073] Any process for contacting the polymer and treated inorganic particle may be used, for example melt compounding. Packages or other articles may be made after the formation of a masterbatch. The term masterbatch is used herein to describe a mixture of treated inorganic particles and / or fillers (including TiC particles) (collectively called solids), melt processed at high solids to resin loadingsTI0009-W001(generally 50 - 70 wt% by weight of the total masterbatch) in high shear compounding machinery such as Banbury mixers, continuous mixers or twin screw mixers, which are capable of providing enough shear to fully incorporate and disperse the solids into the melt processable resin. The resultant melt processable resin product highly loaded with solids is termed a masterbatch, and is typically subsequently diluted or “letdown” by incorporation of additional virgin melt processable resin in plastic production processes. The letdown procedure is accomplished in the desired processing machinery utilized to make the final consumer article, whether it is sheet, film, bottle, package or another shape. The amount of virgin resin utilized and the final solids content is determined by the use specifications of the final consumer article.Paper Articles
[0074] The treated inorganic particles may also be combined with paper pulp or paper pulp slurry to form paper articles. The treated inorganic particles may be added to the paper pulp as a dry treated inorganic particle or as a treated inorganic particle slurry. Paper articles include, but are not limited to, decor paper or paper laminates. Such paper articles may be used in applications such as desk tops, countertops, floor surfacing, wall panels, cabinetry, laminate furniture, etc. Paper pulp may include, for example, long fiber pulps or short fiber pulps such as coniferous wood pulp, hardwood pulp such as eucalyptus, cotton fibers, or mixtures thereof.
[0075] Additional materials may also be present in the paper article or paper slurry. For example, fillers, additives, and / or polymer material may be present. The paper slurry may also include a liquid carrier such as water, organic solvent, or a mixture thereof. Some examples of fillers include talcum, zinc oxide, kaolin, calcium carbonate, or mixtures thereof. Examples of polymer material include, but are not limited to, cationic polymers such as chlorohydroxypropyl trimethyl ammonium chloride, glycidyl trimethyl ammonium chloride, polyamide / polyamine epichlorohydrin resins, other polyamine derivatives or polyamide derivatives, cationic polyacrylates, modified melamine formaldehyde resins, cationized starches, diallyl phthalates, epoxide resins, urea formaldehyde resins, urea-acrylic acid ester copolyesters, melamine formaldehyde resins, melamine phenol formaldehyde resins, phenol formaldehyde resins, poly(meth)acrylates and / or unsaturatedTI0009-W001 polyester resins, or mixtures thereof. Additives include, but are not limited to, retention aids, wet-strength aids, sizing agents, fixing agents, pigments, dyes, optical brighters, dispersants, or mixtures thereof. Combinations of additives are commonly used.Benefits
[0076] Inorganic particles such as TiC pigments are typically small particles (such as around 0.25 microns) that must be ground prior to use in coatings or plastics. Inorganic particles in this size regime can re-agglomerate and be difficult to disperse in the downstream applications.
[0077] Treated inorganic particles of the present invention have surprisingly been found to overcome these difficulties while also minimizing dispersant demand. By modifying the surface of an inorganic particle with an organic treatment as described herein that can be applied upstream or downstream of the micronization process, treated inorganic particles of the present invention may demonstrate desirable dispersion in water-borne and solvent-borne applications, while requiring less dispersant than traditional treated inorganic particles. Such treated inorganic particles may also demonstrate improved dispersion in polymer compositions.EXAMPLES
[0078] Samples were prepared according to the descriptions below.TEST METHODSDispersibility in Solvent-Borne Paint (Scats and Fineness)
[0079] In solvent-borne paint, the dispersibility of TiC>2 pigment was evaluated by the low-shear dispersion test in an alkyd resin system. The “scats” are the visible defects detected on the paint surface due to the presence of a big agglomerate. A method for measuring “scats” is disclosed in U.S. 7,639,862, which is incorporated by reference herein. A well-dispersed TiO? pigment should have a low “scats” number, such as lower than 15, or lower than 10.
[0080] 190 grams of in-house solvent-borne alkyd paint masterbatch was poured into a 1000 ml “tri-pour” beaker in a water-jacketed pot. Paint masterbatch was composed of resin and solvent at 65% solids by weight of the masterbatch. The disperser was equipped with a 3” Cowles blade that was lowered to a fixed position from the bottom of the pot. The mill was started, and the speed was adjusted toTI0009-W0011750 rpm. During the grinding, 450 grams of Tit pigment was added within the first 30 seconds of a one-minute total mixing.
[0081] With the impeller running, the spatula was used to scrape off the pigment on the agitator carefully. The mill was stopped, and the beaker sidewall was scraped. A paper towel wet with a solvent was used to clean the residual pigment that may remain on the inside wall of the beaker.
[0082] After the premix, the grinding was then performed for 5 minutes at 1750 rpm. Upon completion of the grind, 106 grams of the ground base was poured into an unlined pint can containing 119 grams of solvent-based resin. The can was capped and shaken for 10 minutes. The paint was stood for 10 minutes before the reading.
[0083] A Hegman gauge was used to read the number of scats, which is defined by the number of spots (larger particles) observed in between the fineness line to the zero in the Hegman gauge. The Fineness line is defined as a point where the pattern forms a line across the gauge width.
[0084] The paint sample was placed at the deep end of the groove of the gauge. The auto-scraper was activated, and an in-house image processing program took and analyzed a picture. The program reported the Fineness and the average number of scats. A lower scats number, typically below 15, or in some aspects below 10, is considered a well-dispersed paint.Dispersibility in Water-Borne Paint (Gloss)
[0085] In water-borne paint, the dispersibility of TiC>2 pigment was evaluated by the low-shear gloss test in an acrylic resin system.
[0086] 573 grams of in-house water-borne paint masterbatch was loaded into a one-quart stainless steel beaker attached to a disperser. The disperser with a 2” Cowles blade was started, and the speed was adjusted to 300 rpm. 177 grams of TiC>2 pigment was added as fast as possible while maintaining the vortex. The grinding was stopped at 3 minutes, and an aliquot of sample (about 15 grams) was collected. The grinding was restarted with an agitation speed of 700 rpm for 5 minutes, and an aliquot sample was collected. The grinding was restarted with an agitation speed of 1500 rpm for another 5 minutes, and an aliquot sample was collected. Finally, the grinding was restarted with an agitation speed of 3000 rpm for 15 minutes, and an aliquot of sample was collected.TI0009-W001
[0087] Drawdown samples were made with the collected samples on 5.5” x 11 .24” x 0.01” black PVC panels with an automatic drawdown machine and a film applicator. The gloss of the overnight dried panels was then measured with a BYK- Gardner Gloss meter. The reported gloss at 85 degrees is the average of three readings taken from the top, middle, and bottom of each panel.
[0088] The higher gloss, typically above 80, denoted a well-dispersed paint.Dispersant Demand
[0089] TiO2 pigment (1031 .8 g) was charged into a mixture of water (242 g), defoamer 2210 (1.6 g), and 2-amino-2-methyl-1 -propanol, 5% aqueous solution (0.5 g) in a 1 -liter stainless steel pot. The pot was placed in a disperser equipped with a Cowles blade with a diameter of 50 mm rotating at 1500 rpm. The dispersant (Tamol™ 1124 or other dispersants) was added slowly, the mixture was allowed to equilibrate, and the torque was recorded. The apparent viscosity was calculated from the torque with following equations:Apparent Viscosity = calculated viscosity based on the torque input from the instrument in (centipoise) d = diameter of the blade (cm) rps = agitator speed (rotation per second) p = density of the mixture (kg / L)NReynoids = Reynolds numberNpower = Power numberTorque = measured torque (Ft.lbs)
[0090] The dispersion titration was carried on until the minimum torque was observed and extended until the increase in torque was observed. The apparent viscosity was plotted against amount of dispersant active content, and the dispersant demand value was the lowest amount of dispersant active content (g / 100 g pigment) that corresponds to the minimum apparent viscosity. “Active content” is the amount of active dispersant compound present in the dispersant compositionTI0009-W001 and can generally be determined based on the solids content of the dispersant composition. Lower dispersant demand indicates a desirable scenario where a formulation can have the desired performance using less material.Screen Pack Dispersion in Polyethylene Melt
[0091] Dispersion analyses, as defined by particle retention on a 500 mesh screen, were performed on 50 weight % polyethylene (NA206, Equistar) masterbatch concentrates (Parrel Banbury BR1600 produced) containing the particles of interest. Said concentrates were extruded (500 g; Killion % inch single screw extruder, Cedar Grove, N.J.) through a sandwich of fine mesh, metal wire screens (30, 60, 500, 60, 60, 60 mesh) which were then separated, and the magnitude of particles (Ti count) retained on the 500 mesh screen was determined using x-ray fluorescence (9200 Series Portable Analyzer, Texas Nuclear Corp., Austin, Tex.). A lower Ti count indicates fewer large particle agglomerates and better dispersibility in polymer.Surface Treatment Analysis and Weight % Organic Treatment
[0092] Percentages of surface compounds were reported on a weight basis. Silica and alumina were analyzed by X-ray fluorescence spectroscopy (XRF) based on oxide compound content. Oxide content of titanium dioxide powder samples was measured using an X-ray wavelength dispersive spectrometer with flow and scintillation detectors, such as the Malvern Panalytical Zetium Spectrometer. Pellet specimens for analysis were formed in a Carver Model C3912 pellet press with a 35mm inner diameter steel mold. A Somar film was placed into the mold and enough sample to completely cover the film circle was added (1 -4g), followed with enough reagent grade boric acid on top of the sample to fill the mold. Pellets were then formed using 10,000 to 20,000 psig, held for 10-30 seconds. The Somar film was removed after pressing. Matrix matched calibration standards were employed to establish calibration curves for measurement of AI2O3 and SiC .
[0093] Amounts of Carbon (%C), in % by weight of the particle, were measured using a LECO Series 844 carbon analyzer (LECO Corporation, St. Joseph, Ml). The % by weight of organic treatment, based on the total particle weight, was calculated using the %C as measured by elemental analysis and the known molecular weight of the organic treatment compound. If multiple organic compounds were present,TI0009-W001 elemental analysis was completed after each sequential organic treatment to give the %C of each organic compound present.Sample A - TiCh treated with silica, alumina, and glycerol
[0094] The in-process TiC>2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiO2 particle. The slurry (208 kg, 28% by weight solids TiCh particle content, based on the total slurry weight; 2.76% by weight alumina and 3.09% by weight silica, based on the total particle weight) was filtered with a filter press and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, the glycerol (Gly) solution was injected into the micronizer. The flow rate of the glycerol was adjusted to achieve 0.17 % by weight carbon of the micronized TiC>2. Alumina and silica content was measured at 2.76% by weight and 3.09% by weight, respectively, based on the total particle weight. As described in further detail below, the micronized TiC>2 exhibits a gloss of 85.4 (measured at 85°) after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the low “scats” number of 2. The required dispersant to achieve minimum viscosity was 0.2331 g / 100 g of pigment, which is significantly lower than Comparative Sample 1.Sample B - TiCh treated with silica, alumina, and pentaerythritol
[0095] The in-process TiC slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC>2 particle. The slurry (208 kg, 28% by weight solids TiO2 particle content, based on the total slurry weight; 2.76% by weight alumina and 3.09% by weight silica, based on the total particle weight) was filtered with a filter press and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer.Pentaerythritol solution was sprayed into the dryer discharge to target the %C of 0.11 . The dryer discharge was then micronized with superheated steam as the grinding fluid. Alumina and silica content was measured at 2.76% by weight and 3.09% by weight, respectively, based on the total particle weight. As described in further detail below, the micronized TiC>2 exhibits a gloss of 82.5 (measured at 85°)TI0009-W001 after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the low “scats” number of 0.9. The required dispersant to achieve minimum viscosity was 0.1633 g / 100 g of pigment, which is significantly lower than Comparative Sample 1.Sample C - TiC>2 treated with silica, alumina, and sodium methyl siliconate
[0096] The in-process TiO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC>2 particle. The TiC>2 slurry (208 kg, 28% by weight solids TiC>2 particle content, based on the total slurry weight; 2.89% by weight alumina and 3.17% by weight silica, based on the total particle weight) was heated to 90°C, and the pH was adjusted to 7 before the simultaneous addition of 4.7 kg sodium methyl siliconate (MeSil; DOW OFS- 0772) and HCI. HCI flow was adjusted to maintain the pH of the TiO2 slurry. The slurry was cured for 1 hour and cooled down before being sent to a filter press. The obtained filtered cake was dried in a flash dryer and micronized with superheated steam without any further additives. The micronized sample contains 0.06% by weight carbon, 2.75% by weight AI2O3, and 3.42% by weight SiO2, based on the total particle weight. As described in further detail below, the micronized TiO2 exhibits a gloss of 83.8 (measured at 85°) after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the low “scats” number of 4.13. The required dispersant to achieve minimum viscosity was 0.06 g / 100 g of pigment, which is significantly lower than Comparative Sample 1.Sample D - TiOz treated with silica, alumina, reduced amount of methyl siliconate, and a reduced amount of TMP
[0097] The in-process TiC slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC particle. The TiC>2 slurry (208 kg, 28% by weight solids TiC>2 particle content, based on the total slurry weight; 3.08% by weight alumina and 3.42% by weight silica, based on the total particle weight) was heated to 90°C, and the pH was adjusted to 7 before the simultaneous addition of 0.93 kg sodium methyl siliconate (DOW OFS-0772) and HCI. HCI flow was adjusted to maintain the pH of the TiO2 slurry. The slurry wasTI0009-W001 cured for 1 hour and cooled down before being sent to a filter press. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, the TMP solution was injected into the micronizer. The flow rate of the TMP was adjusted to achieve 0.10% carbon of the micronized TiC . The micronized sample contains 0.117% by weight carbon, 3.08% by weight AI2O3, and 3.42% by weight SiO2, based on the treated inorganic particle weight. As described in further detail below, the micronized TiCh exhibits a gloss of 81 .6 (measured at 85°) after being ground for 5 min at 700 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the “scats” number of 4.76. The required dispersant to achieve minimum viscosity was 0.195 g / 100 g of pigment, which is significantly lower than Comparative Sample 1.Sample E - TiCh treated with silica, alumina, reduced amount of methyl siliconate, and glycerol
[0098] The in-process TO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiO? particle. The TiO2 slurry (208 kg, 28% by weight solids TiO2 particle content, based on the total slurry weight; 3.08% by weight alumina and 3.42% by weight silica, based on the total particle weight) was heated to 90°C, and the pH was adjusted to 7 before the simultaneous addition of 0.93 kg sodium methyl siliconate (DOW OFS-0772) and HCI. HCI flow was adjusted to maintain the pH of the TiO2 slurry. The slurry was cured for 1 hour and cooled down before being sent to a filter press. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. Glycerol was sprayed into the dryer discharge during micronizing to achieve 0.14% carbon of the micronized TiO2. As described in further detail below, the micronized sample contains 0.14% by weight carbon, 3.08% by weight AI2O3, and 3.42% by weight SiO2, based on the particle weight. The micronized TiC>2 exhibits a gloss of 80.5 (measured at 85°) after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the “scats” number of 8.8. The required dispersant to achieve minimumTI0009-W001 viscosity was 0.1585 g / 100 g of pigment, which is significantly lower than Comparative Sample 1.Comparative Sample 1 (Comp. 1)
[0099] The in-process TiCb slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC particle. The slurry (208 kg, 28% by weight solids TiC particle content, based on the total slurry weight; 2.8% by weight alumina and 3.11 % by weight silica, based on the total particle weight) was filtered with a filter press and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, the TMP solution was injected into the micronizer. The flow rate of the TMP was adjusted to achieve 0.20% by weight carbon of the micronized TiC>2. Silica and alumina content was measured at 2.8% by weight and 3.1 1 % by weight, respectively, based on the particle weight. As described in further detail below, the micronized TiC>2 exhibits a gloss of 76.7 (measured at 85°) after being ground for 5 min at 700 rpm in a waterborne acrylic paint system. The sample was also dispersed well in solvent-borne alkyd paint, as indicated by the low “scats” number of 2. The required dispersant to achieve minimum viscosity was 0.3397 g / 100 g of pigment.Comparative Sample 2 (Comp. 2)
[0100] The in-process T1O2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC>2 particle. The slurry (208 kg, 28% by weight solids TiC>2 particle content, based on the total slurry weight; 2.92% by weight alumina and 3.09% by weight silica, based on the total particle weight) was filtered with a filter press and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. Alumina and silica content was measured at 2.92% by weight and 3.09% by weight, respectively, based on particle weight. As described in further detail below, the micronized TiC>2 cannot achieve a gloss of >80 (measured at 85°) after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sampleTI0009-W001 cannot disperse well in solvent-borne alkyd paint, as indicated by the high “scats” number of 83.5. The dispersant demand test was not performed because the sample cannot be well dispersed in the paint application.
[0101] Particle size distribution (“PSD”) of the samples was analyzed as follows: TiC>2 (20 grams) was added into a beaker containing 80 ml of dispersing solution (tetra potassium pyrophosphate, 0.4 g / L in water). It was stirred and sonicated with a fixed setting and fed into the Horiba LA-300 for PSD analysis. The PSD results were reported in the form of D50, which is the micron size with a cumulative mass greater than 50% (median).
[0102] The properties of the samples are included in Table 1 .Table 1 : Properties of Prepared SamplesExample 1 - Dispersibility in Solvent-Borne Paint
[0103] Table 2 shows the scats count for various TiC>2 samples. The results show that the samples including an organic treatment provide comparable or superior effectiveness for dispersion as compared to a particle with traditional treatment (Comparative Samples 1 and 2).TI0009-W001Table 2: Scats Counts for Tested SamplesExample 2 - Dispersibility in Water-Borne Paint
[0104] As shown in Table 3, the samples including an organic treatment provide comparable or superior effectiveness for dispersion as compared to a particle with traditional treatment (Comparative Samples 1 and 2).Table 3: Gloss Measurements for Tested SamplesExample 3 - Dispersant Demand
[0105] The dispersant demand data of the various samples with Tamol™ 1124 dispersant is shown in Table 4 and in Figure 1 . The results show that the samples including an organic treatment according to the invention require significantly less dispersant as compared to a particle with traditional treatment (Comparative Samples 1 and 2).TI0009-W001Table 4: Dispersant Demand for Tested Samples
[0106] As shown above, Comparative Sample 2 cannot disperse well in solvent- borne alkyd paint, as indicated by the high scats number of 83.5. Therefore, the dispersant demand test was not performed for Comparative Sample 2.Sample F
[0107] The in-process TiOs slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiO? particle. The slurry (28% by weight solids TiO2 particle content, based on the total slurry weight; 3.12% by weight silica and 2.38% by weight alumina, based on the total particle weight) was filtered and washed to remove the salt. Subsequently, glycerol was added before spray drying the material. The flow rate of glycerol was adjusted to achieve 0.15 % by weight carbon based on the total TiC>2 weight. The dryer discharge was then micronized with superheated steam as the grinding fluid. The required dispersant to achieve minimum viscosity was 0.04 g / 100 g of pigment, which is significantly lower than Comparative Sample 3.Comparative Sample 3
[0108] The in-process TiO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC>2 particle. The slurry (28% by weight solids TiO2 particle content, based on the total slurry weight; 3.05% by weight silica and 2.36% by weight alumina, based on the total particle weight) was filtered and washed to remove the salt. Subsequently, TMP solution was added before spray drying the material. The flow rate of TMP was adjusted to achieve 0.20 % by weight carbon based on the total Tit weight. The dryer discharge was then micronized with superheated steam as the grinding fluid.TI0009-W001Silica and alumina content was measured at 3.05% by weight and 2.36% by weight, respectively, based on the total weight of the particle. The required dispersant to achieve the minimum viscosity was 0.11 g / 100 g of pigment.Example 4 - Dispersant Demand of Sample F and Comparative Sample 3
[0109] Two additional samples were prepared according to the compositions listed in Table 5 and tested according to the Test Methods above.Table 5: Sample Compositions
[0110] The dispersant demand for each sample was tested with several different dispersants according to the dispersant demand test. The results are shown in Table 6.Table 6: Dispersant Demand for Tested Samples
[0111] It is clearly shown that the glycerol treated sample (Sample F) has significantly lower dispersant demand for each tested dispersant compared to the TMP-treated sample (Comparative 3).Sample G
[0112] The in-process TiO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiO? particle. The slurry (28% by weight solids TiO2 particle content, based on the total slurry weight; 3.01 % by weight silica and 2.66% by weight alumina, based on the total particle weight) was filtered and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, theTI0009-W001 triethylene glycol (TEG) solution was injected into the micronizer. The flow rate of the TEG was adjusted to achieve 0.20 % by weight carbon based on the weight of the micronized TiO2. Silica and alumina content was measured at 3.01 % by weight and 2.66% by weight respectively, based on the total particle weight. As described in further detail below, the micronized TiO? exhibits a gloss of 83.8 (measured at 85°) after being ground for 5 minutes at 1500 rpm in a waterborne acrylic paint system. The sample also dispersed well in the solvent-borne alkyd paint, as indicated by the low “scats” number of 2.4. The required dispersant to achieve minimum viscosity was 0.073 g / 100 g of pigment, which is significantly lower than the Comparative Sample 4.Comparative Sample 4
[0113] The in-process TiO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiO2 particle. The slurry (28% by weight solids TiO2 particle content, based on the total slurry weight; 2.97% by weight silica and 2.73% by weight alumina, based on the total particle weight) was filtered and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, the trimethylolpropane (TMP) solution was injected into the micronizer. The flow rate of TMP was adjusted to achieve 0.20 % by weight carbon based on the total TiO2 weight. The dryer discharge was then micronized with superheated steam as the grinding fluid. Silica and alumina content was measured at 2.97% by weight and 2.73% by weight, respectively, based on the particle weight. As described in further detail below, the micronized TiO2 exhibits a gloss of 84.2 (measured at 85°) after being ground for 5 min at 1500 rpm in a waterborne acrylic paint system. The sample dispersed well in solvent-borne alkyd paint, as indicated by the low “scats” number of 1 .6. The required dispersant to achieve the minimum viscosity was 0.21 g / 100 g of pigment.TI0009-W001Table 7: Sample CompositionsTable 8: Scats and Dispersant Demand
[0114] It is clearly shown that the TEG treated sample (Sample G) has significantly lower dispersant demand for each tested dispersant compared to the TMP-treated sample (Comparative 4).Sample H
[0115] The in-process TiO2 slurry sample was collected at the tank outlet after the inorganic surface treatment of silica and alumina. Silica and alumina content of the particles was formed by wet treatment of silica then alumina on a core TiC>2 particle. The slurry (28% by weight solids TiO2 particle content, based on the total slurry weight; 3.02% by weight silica and 2.8% by weight alumina, based on the total particle weight) was filtered and washed to remove the salt. Subsequently, the filtered cake was obtained and dried in a flash dryer. The dryer discharge was then micronized with superheated steam as the grinding fluid. During the grinding, glycerol solution was injected into the micronizer. The flow rate of glycerol was adjusted to achieve 0.143% by weight carbon based on the total TiO2 weight, which indicates 0.366% by weight organic material on the surface, based on the total weight of the particle.Example 5 - Screen Pack of Sample H and Comparative Sample 4
[0116] The samples from Sample H and Comparative Sample 4 were tested according to the Screen Pack Test. The particles of Sample H exhibited a Ti count of 55 in the screen pack dispersion test, which was significantly lower than the Ti count of the Comparative 4 Sample.TI0009-W001Table 9: Pigment Dispersion Performance in Polyethylene Melt
Claims
TI0009-W001CLAIMSWhat is claimed is:
1. A treated inorganic particle comprising an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
2. The treated inorganic particle of claim 1 , wherein the inorganic particle comprises an inorganic oxide pigment.
3. The treated inorganic particle of claim 1 , where the inorganic particle comprises an inorganic oxide selected from TiO2, AI2O3, SiO2, ZnO, SrTiOs, BaSC , PbCOs, BaTiOs, Ce20s, CaCOs, ZrO2, or mixtures thereof.
4. The treated inorganic particle of claim 1 , wherein the inorganic particle comprises a TiO2 particle.
5. The treated inorganic particle of claim 1 , wherein the inorganic particle comprises a TiC pigment.
6. The treated inorganic particle of any of the preceding claims, wherein the polyol comprises propylene glycol, H-(O-CH2CH2)n-OH, and / or C(H)x(OH)y(R1OH)z , wherein n =1-4, x=0-1 , y=0-1 , z=2-4, such that x+y+z=4, and R1=CI-C3 alkylene.
7. The treated inorganic particle of any of the preceding claims, wherein the polyol comprises a diol without an alkyl branch, a triol without an alkyl branch, a tetraol without an alkyl branch, or combinations thereof.
8. The treated inorganic particle of any of the preceding claims, wherein the polyol comprises glycerol, triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof.TI0009-W0019. The treated inorganic particle of any of the preceding claims, wherein the siliconate comprises an alkali metal salt of alkyl and / or aryl siliconate.
10. The treated inorganic particle of any of claims 1-8, wherein the siliconate comprises R2-Si(OM)3, wherein M is independently alkali metal or H, R2is linear or branched Ci-Cis alkyl or aryl, and at least one M comprises alkali metal.11 . The treated inorganic particle of any of claims 1-8, wherein the siliconate comprises sodium and / or potassium salt of alkyl and / or aryl siliconates.
12. The treated inorganic particle of any of claims 1-8, wherein the siliconate comprises sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof.
13. The treated inorganic particle of any of claims 1-8, wherein the siliconate comprises:O' Na+ / K+R - S / r — O' Na .VKNa+ / K+ / OHR - S / r- — O' Na+ / K+O' Na+ / K+orOHR - S / i- — OHO' Na+ / K+or combinations thereof, wherein R = alkyl (Ci-Cis); aryl.
14. The treated inorganic particle of any of the preceding claims, wherein the mean particle size is about 100 nm to about 500 nm.
15. The treated inorganic particle of any of the preceding claims, wherein the organic treatment is present in an amount of about 0.3 wt% to about 0.4 wt% of the treated inorganic particle.TI0009-W00116. The treated inorganic particle of any of the preceding claims, wherein the silica is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
17. The treated inorganic particle of any of the preceding claims, wherein the silica is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
18. The treated inorganic particle of any of the preceding claims, wherein the alumina is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
19. The treated inorganic particle of any of the preceding claims, wherein the alumina is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
20. The treated inorganic particle of any of the preceding claims, wherein the polyol is present in an amount of about 0.01 to about 1 wt% of the treated inorganic particle.21 . The treated inorganic particle of any of the preceding claims, wherein the polyol is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
22. The treated inorganic particle of any of the preceding claims, wherein the polyol is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
23. The treated inorganic particle of any of the preceding claims, wherein the siliconate is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
24. The treated inorganic particle of any of the preceding claims, wherein the siliconate is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
25. The treated inorganic particle of any of the preceding claims, wherein the siliconate is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
26. The treated inorganic particle of any of the preceding claims, wherein the organic treatment comprises a polyol and a siliconate.TI0009-W00127. The treated inorganic particle of any of the preceding claims, wherein the organic treatment does not comprise trimethylolpropane.
28. The treated inorganic particle of any of the preceding claims, wherein the treated inorganic particle does not comprise an amine-based dispersant.
29. The treated inorganic particle of any of the preceding claims, wherein the treated inorganic particle does not comprise a polymeric dispersant.
30. A slurry composition comprising a treated inorganic particle of any of the preceding claims, water, and dispersant.31 . A coating composition comprising a treated inorganic particle of any of the preceding claims.
32. A solvent-borne coating composition comprising a treated inorganic particle of any of the preceding claims.
33. A water-borne coating composition comprising a treated inorganic particle of any of the preceding claims.
34. A treated inorganic particle comprising an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1) silica, (2) alumina, and (3) an organic treatment consisting essentially of glycerol, and wherein the organic treatment is present in an amount of at least about 0.1 wt% and less than 0.5 wt% of the treated inorganic particle.
35. The treated inorganic particle of claim 34, wherein the inorganic particle comprises an inorganic oxide pigment.
36. The treated inorganic particle of claim 34, where the inorganic particle comprises an inorganic oxide selected from TiC , AI2O3, SiC>2, ZnO, SrTiOs, BaSO4, PbCOs, BaTIOs, Ce20s, CaCOs, ZrO2, or mixtures thereof.
37. The treated inorganic particle of claim 34, wherein the inorganic particle comprises a TiC>2 particle.
38. The treated inorganic particle of claim 34, wherein the inorganic particle comprises a TiC pigment.
39. The treated inorganic particle of claims 34-38, wherein the mean particle size is about 100 nm to about 500 nm.TI0009-W00140. The treated inorganic particle of claims 34-39, wherein the organic treatment is present in an amount of about 0.3 wt% to about 0.46 wt% of the treated inorganic particle.41 . The treated inorganic particle of claims 34-40, wherein the silica is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
42. The treated inorganic particle of claim 41 , wherein the silica is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
43. The treated inorganic particle of claims 34-42, wherein the alumina is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
44. The treated inorganic particle of claim 43, wherein the alumina is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
45. The treated inorganic particle of claims 34-44, wherein the organic treatment does not comprise trimethylolpropane.
46. The treated inorganic particle of claims 34-45, wherein the treated inorganic particle does not comprise an amine-based dispersant.
47. The treated inorganic particle of claims 34-46, wherein the treated inorganic particle does not comprise a polymeric dispersant.
48. A slurry composition comprising a treated inorganic particle of claims 34-47, water, and dispersant.
49. A coating composition comprising a treated inorganic particle of claims 34-47.
50. A solvent-borne coating composition comprising a treated inorganic particle of claims 34-47.51 . A water-borne coating composition comprising a treated inorganic particle of claims 34-47.
52. A treated inorganic particle comprising an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1) silica, (2) alumina, and (3) an organic treatment comprising a polyol, siliconate, mixture of siliconate and glycerol, or mixture of siliconate and polyol, a. wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle, andTI0009-W001 b. wherein the polyol comprises propylene glycol, H-(O-CH2CH2)n-OH, and / or C(H)x(OH)y(R1OH)z, where n =1-4, x=0-1 , y=0-1 , z=3-4, such that x+y+z=4, andR1=Ci-Cs alkylene.
53. The treated inorganic particle of claim 52, wherein the inorganic particle comprises an inorganic oxide pigment.
54. The treated inorganic particle of claim 52, where the inorganic particle comprises an inorganic oxide selected from TiO2, AI2O3, SiC>2, ZnO, SrTiOs, BaSO4, PbCOs, BaTiOs, Ce2O3, CaCOs, ZrO2, or mixtures thereof.
55. The treated inorganic particle of claim 52, wherein the inorganic particle comprises a TiO2 particle.
56. The treated inorganic particle of claim 52, wherein the inorganic particle comprises a TiO2 pigment.
57. The treated inorganic particle of claims 52-56, wherein the polyol comprises triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof.
58. The treated inorganic particle of claims 52-57, wherein the siliconate is present and comprises an alkali metal salt of alkyl and / or aryl siliconate.
59. The treated inorganic particle of claims 52-58, wherein the siliconate is present and comprises R2-Si(OM)3, wherein M is independently alkali metal or H, R2is linear or branched C1-C18 alkyl or aryl, and at least one M comprises alkali metal.
60. The treated inorganic particle of claims 52-59, wherein the siliconate is present and comprises sodium and / or potassium salt of alkyl and / or aryl siliconates.61 . The treated inorganic particle of claims 52-60, wherein the siliconate is present and comprises sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof.TI0009-W00162. The treated inorganic particle of claims 52-61 , wherein the siliconate is present and comprises:or combinations thereof, wherein R = alkyl (Ci-Cis); aryl.
63. The treated inorganic particle of claims 52-62, wherein the mean particle size is about 100 nm to about 500 nm.
64. The treated inorganic particle of claims 52-63, wherein the organic treatment is present in an amount of about 0.3 wt% to about 0.4 wt% of the treated inorganic particle.
65. The treated inorganic particle of claims 52-64, wherein the silica is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
66. The treated inorganic particle of claim 65, wherein the silica is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
67. The treated inorganic particle of claims 52-66, wherein the alumina is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
68. The treated inorganic particle of claim 67, wherein the alumina is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
69. The treated inorganic particle of claims 52-68, wherein the polyol or glycerol is present in an amount of about 0.01 to about 1 wt% of the treated inorganic particle.TI0009-W00170. The treated inorganic particle of claim 69, wherein the polyol or glycerol is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.71 . The treated inorganic particle of claim 70, wherein the polyol or glycerol is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
72. The treated inorganic particle of claims 52-71 , wherein the siliconate is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
73. The treated inorganic particle of claim 72, wherein the siliconate is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
74. The treated inorganic particle of claim 72, wherein the siliconate is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
75. The treated inorganic particle of claims 52-74, wherein the organic treatment comprises a polyol and a siliconate.
76. The treated inorganic particle of claims 52-75, wherein the organic treatment does not comprise trimethylolpropane.
77. The treated inorganic particle of claims 52-76, wherein the treated inorganic particle does not comprise an amine-based dispersant.
78. The treated inorganic particle of claims 52-77, wherein the treated inorganic particle does not comprise a polymeric dispersant.
79. A slurry composition comprising a treated inorganic particle of claims 52-78, water, and dispersant.
80. A coating composition comprising a treated inorganic particle of claims 52-78.81 . A solvent-borne coating composition comprising a treated inorganic particle of claims 52-78.
82. A water-borne coating composition comprising a treated inorganic particle of claims 52-78.
83. A process of producing a treated inorganic particle comprising: a. producing an aqueous inorganic particle slurry having an inorganic particle with silica and alumina surface treatments;TI0009-W001 b. drying the aqueous inorganic particle slurry by flash drying or spray drying to form dried inorganic particles; c. steam milling the dried inorganic particles to form milled inorganic particles; and d. contacting the aqueous inorganic particle slurry, dried inorganic particles, or milled inorganic particles with an organic treatment, where the treated inorganic particle comprises an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
84. The process of claim 83, where the organic treatment is contacted with the aqueous inorganic particle slurry.
85. The process of claims 83-84, where the process further comprises a step of wet milling the aqueous inorganic particle before drying.
86. The process of claim 85, where the organic treatment is contacted with the aqueous inorganic particle slurry after wet milling.
87. The process of claim 85, where the organic treatment is contacted with the aqueous inorganic particle slurry before wet milling.
88. The process of claims 83 or 85, where the organic treatment is contacted with the dried inorganic particles.
89. The process of claim 88, where the organic treatment is contacted with the dried inorganic particles during the drying step.
90. The process of claim 83 or 85, where the organic treatment is contacted with the milled inorganic particles as the inorganic particles exit the steam mill, such that the temperature is elevated.91 . The process of claims 83-90, wherein the inorganic particle comprises an inorganic oxide pigment.TI0009-W00192. The process of claims 83-91 , where the inorganic particle comprises an inorganic oxide selected from TiC , AI2O3, SiC>2, ZnO, SrTiOs, BaSC>4, PbCOs, BaTiOs, Ce2O3, CaCOs, ZrO2, or mixtures thereof.
93. The process of claim 92, wherein the inorganic particle comprises a TiO2 particle.
94. The process of claim 92, wherein the inorganic particle comprises a TiC pigment.
95. The process of claims 83-94, wherein the polyol comprises propylene glycol, H- (O-CH2CH2)n-OH, and / or C(H)x(OH)y(R1OH)z, wherein n =1-4, x=0-1 , y=0-1 , z=2-4, such that x+y+z=4, and R1=CI-C3 alkylene.
96. The process of claims 83-95, wherein the polyol comprises a diol without an alkyl branch, a triol without an alkyl branch, a tetraol without an alkyl branch, or combinations thereof.
97. The process of claim 95, wherein the polyol comprises glycerol, triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof.
98. The process of claim 97, where the polyol comprises glycerol, and the organic treatment is present in an amount of at least about 0.10 wt% and less than 0.50 wt% of the treated inorganic particle.
99. The process of claim 95, where the organic treatment comprising a polyol, siliconate, mixture of siliconate and glycerol, or mixture of siliconate and polyol, where z=3-4.
100. The process of claims 83-99, wherein the siliconate comprises an alkali metal salt of alkyl and / or aryl siliconate.
101. The process of claims 83-100, wherein the siliconate comprises R2-Si(OM)3, wherein M is independently alkali metal or H, R2is linear or branched C1-C18 alkyl or aryl, and at least one M comprises alkali metal.TI0009-W001102. The process of claims 83-101 , wherein the siliconate comprises sodium and / or potassium salt of alkyl and / or aryl siliconates.
103. The process of claims 83-102, wherein the siliconate comprises sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof.
104. The process of claims 83-103, wherein the siliconate comprises:O’ Na+ / K+R - S / i- — O’ Na+. / KO’ Na+ / K+OHR - S / r- — O’ Na / KO’ Na+ / K+orOHR - S / r— OHO' Na+ / K+or combinations thereof, wherein R = alkyl (Ci-Cis); aryl.
105. The process of claims 83-104, wherein the mean particle size of the treated inorganic particle is about 100 nm to about 500 nm.
106. The process of claims 83-105, wherein the organic treatment is present in an amount of about 0.3 wt% to about 0.4 wt% of the treated inorganic particle.
107. The process of claims 83-106, wherein the silica is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
108. The process of claims 83-107, wherein the silica is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
109. The process of claims 83-108, wherein the alumina is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
110. The process of claims 83-109, wherein the alumina is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.TI0009-W001111. The process of claims 83-110, wherein the polyol is present in an amount of about 0.01 to about 1 wt% of the treated inorganic particle.
112. The process of claims 83-111 , wherein the polyol is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
113. The process of claims 112, wherein the polyol is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
114. The process of claims 83-113, wherein the siliconate is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
115. The process of claims 83-114, wherein the siliconate is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
116. The process of claims 83-115, wherein the siliconate is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
117. The process of claims 83-116, wherein the organic treatment comprises a polyol and a siliconate.
118. The process of claims 83-117, wherein the organic treatment does not comprise trimethylolpropane.
119. The process of claims 83-118, wherein the treated inorganic particle does not comprise an amine-based dispersant.
120. The process of claims 83-119, wherein the treated inorganic particle does not comprise a polymeric dispersant.121 . A slurry composition comprising a treated inorganic particle made by the process of claims 83-120, water, and dispersant.
122. A coating composition comprising a treated inorganic particle made by the process of claims 83-120.
123. A solvent-borne coating composition comprising a treated inorganic particle made by the process of claims 83-120.
124. A water-borne coating composition comprising a treated inorganic particle made by the process of claims 83-120.
125. A process of making a slurry composition comprising producing a treated inorganic particle according to claims 82-120 and contacting the treatedTI0009-W001 inorganic particle with water and an additive selected from at least one dispersant, pH modifier, biocide, or defoamer.
126. A process of producing a treated inorganic particle comprising: a. producing an aqueous inorganic particle slurry having an inorganic particle with silica and alumina surface treatments; b. drying the aqueous inorganic particle slurry to form dried inorganic particles; c. milling the dried inorganic particles to form milled inorganic particles; and d. contacting the aqueous inorganic particle slurry, dried inorganic particles, or milled inorganic particles with an organic treatment, where the treated inorganic particle comprises an inorganic particle having a surface and having a surface treatment on the inorganic particle surface, wherein the surface treatment comprises (1) silica, (2) alumina, and (3) an organic treatment comprising a polyol and / or siliconate, and wherein the organic treatment is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
127. The process of claim 126, where the organic treatment is contacted with the aqueous inorganic particle slurry.
128. The process of claims 126-127, where the process further comprises a step of wet milling the aqueous inorganic particle before drying.
129. The process of claim 128, where the organic treatment is contacted with the aqueous inorganic particle slurry after wet milling.
130. The process of claim 128, where the organic treatment is contacted with the aqueous inorganic particle slurry before wet milling.131 . The process of claims 129 or 130, where the organic treatment is contacted with the dried inorganic particles.
132. The process of claim 131 , where the organic treatment is contacted with the dried inorganic particles during the drying step.TI0009-W001133. The process of claim 129 or 130, where the organic treatment is contacted with the milled inorganic particles as the inorganic particles exit the mill, such that the temperature is elevated.
134. The process of claims 126-133, wherein the inorganic particle comprises an inorganic oxide pigment.
135. The process of claims 126-134, where the inorganic particle comprises an inorganic oxide selected from TiC , AI2O3, SiC>2, ZnO, SrTiOs, BaSO4, PbCOs, BaTiOs, Ce2O3, CaCOs, ZrCte, or mixtures thereof.
136. The process of claim 135, wherein the inorganic particle comprises a TiC>2 particle.
137. The process of claim 136, wherein the inorganic particle comprises a TiC>2 pigment.
138. The process of claims 126-137, wherein the polyol comprises propylene glycol, H-(O-CH2CH2)n-OH, and / or C(H)x(OH)y(R1OH)z , wherein n =1-4, x=0-1 , y=0-1 , z=2-4, such that x+y+z=4, and R1=CI-C3 alkylene.
139. The process of claims 126-138, wherein the polyol comprises a diol without an alkyl branch, a triol without an alkyl branch, a tetraol without an alkyl branch, or combinations thereof.
140. The process of claim 138, wherein the polyol comprises glycerol, triethylene glycol, diglycerol, propylene glycol, pentaerythritol, or combinations thereof.141 . The process of claim 140, where the polyol comprises glycerol, and the organic treatment is present in an amount of at least about 0.10 wt% and less than 0.50 wt% of the treated inorganic particle.
142. The process of claim 140, where the polyol consists essentially of glycerol, and the organic treatment is present in an amount of at least about 0.10 wt% and less than 0.50 wt% of the treated inorganic particle.TI0009-W001143. The process of claim 140, where the organic treatment comprising a polyol, siliconate, mixture of siliconate and glycerol, or mixture of siliconate and polyol, where z=3-4.
144. The process of claims 126-143, wherein the siliconate comprises an alkali metal salt of alkyl and / or aryl siliconate.
145. The process of claims 126-144, wherein the siliconate comprises R2-Si(OM)3, wherein M is independently alkali metal or H, R2is linear or branched C1-C18 alkyl or aryl, and at least one M comprises alkali metal.
146. The process of claims 126-145, wherein the siliconate comprises sodium and / or potassium salt of alkyl and / or aryl siliconates.
147. The process of claims 126-146, wherein the siliconate comprises sodium methyl siliconate, potassium methyl siliconate, potassium ethyl siliconate, sodium ethyl siliconate, potassium propyl siliconate, potassium benzyl siliconate, or combinations thereof.
148. The process of claims 126-147, wherein the siliconate comprises:O’ Na+ / K+R - S / i - O’ Na .7K .°' Na+ / K+OHR - S / r — O’ Na+ / K+O' Na+ / K+QrOHR - S / r— OHO' Na+ / K+or combinations thereof, wherein R = alkyl (C1-C18); aryl.
149. The process of claims 126-148, wherein the mean particle size of the treated inorganic particle is about 100 nm to about 500 nm.
150. The process of claims 126-149, wherein the organic treatment is present in an amount of about 0.3 wt% to about 0.4 wt% of the treated inorganic particle.TI0009-W001151 . The process of claims 126-150, wherein the silica is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
152. The process of claims 126-151 , wherein the silica is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
153. The process of claims 126-152, wherein the alumina is present in an amount of about 0.1 wt% to about 5 wt% of the treated inorganic particle.
154. The process of claims 126-153, wherein the alumina is present in an amount of about 1 wt% to about 5 wt% of the treated inorganic particle.
155. The process of claims 126-154, wherein the polyol is present in an amount of about 0.01 to about 1 wt% of the treated inorganic particle.
156. The process of claims 126-155, wherein the polyol is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
157. The process of claims 156, wherein the polyol is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
158. The process of claims 126-157, wherein the siliconate is present in an amount of about 0.01 wt% to about 1 wt% of the treated inorganic particle.
159. The process of claims 158, wherein the siliconate is present in an amount of about 0.1 wt% to about 1 wt% of the treated inorganic particle.
160. The process of claims 159, wherein the siliconate is present in an amount of about 0.3 wt% to about 0.5 wt% of the treated inorganic particle.
161. The process of claims 126-160, wherein the organic treatment comprises a polyol and a siliconate.
162. The process of claims 126-161 , wherein the organic treatment does not comprise trimethylolpropane.
163. The process of claims 126-162, wherein the treated inorganic particle does not comprise an amine-based dispersant.
164. The process of claims 126-163, wherein the treated inorganic particle does not comprise a polymeric dispersant.
165. The process of claims 126-164, wherein the drying step b is performed by flash drying or spray drying.TI0009-W001166. The process of claims 126-165, where the milling step c is performed by steam milling.
167. A slurry composition comprising a treated inorganic particle made by the process of claims 126-166, water, and dispersant.
168. A coating composition comprising a treated inorganic particle made by the process of claims 126-166.
169. A solvent-borne coating composition comprising a treated inorganic particle made by the process of claims 126-166.
170. A water-borne coating composition comprising a treated inorganic particle made by the process of claims 126-166.171 . A process of making a slurry composition comprising producing a treated inorganic particle according to claims 126-166 and contacting the treated inorganic particle with water and an additive selected from at least one dispersant, pH modifier, biocide, or defoamer.
172. A polymer composition comprising a polymer and the treated inorganic particle of claims 1-29.
173. The polymer composition of claim 172, where the polymer is a melt processible polymer.
174. The polymer composition of claims 172-173, where the polymer is selected from polymers of ethylenically unsaturated monomers; copolymers of ethylene and at least one olefin; vinyl polymers; polyvinyl esters; polystyrenes; acrylic homopolymers; acrylic copolymers; phenolic polymers; alkyd polymers; amino resins; epoxy resins; polyamides; polyurethanes; phenoxy resins; polysulfones; polycarbonates; polyesters; polyethers; acetal resins; polyimides; polyoxyethylenes; elastomers; natural or synthetic polymers of diene monomers; and mixtures thereof.
175. A process of making a polymer composition comprising producing a treated inorganic particle of claims 1-29 and contacting the treated inorganic particle with a polymer.
176. A polymer composition comprising a polymer and the treated inorganic particle of claims 34-47.TI0009-W001177. The polymer composition of claim 176, where the polymer is a melt processible polymer.
178. The polymer composition of claims 176-177, where the polymer is selected from polymers of ethylenically unsaturated monomers; copolymers of ethylene and at least one olefin; vinyl polymers; polyvinyl esters; polystyrenes; acrylic homopolymers; acrylic copolymers; phenolic polymers; alkyd polymers; amino resins; epoxy resins; polyamides; polyurethanes; phenoxy resins; polysulfones; polycarbonates; polyesters; polyethers; acetal resins; polyimides; polyoxyethylenes; elastomers; natural or synthetic polymers of diene monomers; and mixtures thereof.
179. A process of making a polymer composition comprising producing a treated inorganic particle of claims 34-47 and contacting the treated inorganic particle with a polymer.
180. A polymer composition comprising a polymer and the treated inorganic particle of claims 52-78.181 . The polymer composition of claim 180, where the polymer is a melt processible polymer.
182. The polymer composition of claims 180-181 , where the polymer is selected from polymers of ethylenically unsaturated monomers; copolymers of ethylene and at least one olefin; vinyl polymers; polyvinyl esters; polystyrenes; acrylic homopolymers; acrylic copolymers; phenolic polymers; alkyd polymers; amino resins; epoxy resins; polyamides; polyurethanes; phenoxy resins; polysulfones; polycarbonates; polyesters; polyethers; acetal resins; polyimides; polyoxyethylenes; elastomers; natural or synthetic polymers of diene monomers; and mixtures thereof.
183. A process of making a polymer composition comprising producing a treated inorganic particle of claims 52-78 and contacting the treated inorganic particle with a polymer.
184. A process of making a polymer composition comprising producing a treated inorganic particle by the process of claims 83-120 and contacting the treated inorganic particle with a polymer.TI0009-W001185. A process of making a polymer composition comprising producing a treated inorganic particle by the process of claims 126-166 and contacting the treated inorganic particle with a polymer.
186. The treated inorganic particles of claims 1-29, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
187. The treated inorganic particles of claims 34-47, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
188. The treated inorganic particles of claims 52-78, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
189. The process of claims 83-120, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
190. The process of claims 126-166, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
191. The polymer composition of claims 172-174, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
192. The polymer composition of claims 176-178, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
193. The polymer composition of claims 180-182, where the treated inorganic particles have a screen pack dispersion (Ti count) of at most about 100.
194. The slurry composition of claim 30, where the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles.
195. The slurry composition of claim 30, where the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles.
196. The slurry composition of claim 48, where the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles.
197. The slurry composition of claim 48, where the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles.
198. The slurry composition of claim 79, where the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles.TI0009-W001199. The slurry composition of claim 79, where the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles.
200. The slurry composition of claim 121 , where the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles.201 . The slurry composition of claim 121 , where the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles.
202. The slurry composition of claim 167, where the slurry composition comprises at most 0.3 g dispersant / 100 g treated inorganic particles.
203. The slurry composition of claim 167, where the slurry composition comprises a dispersant and has a dispersant demand of at most 0.3 g dispersant / 100 g treated inorganic particles.
204. The coating composition of claims 31-33, where the coating composition provides a scats value of at most 30.
205. The coating composition of claims 49-51 , where the coating composition provides a scats value of at most 30.
206. The coating composition of claims 80-82, where the coating composition provides a scats value of at most 30.
207. The coating composition of claims 122-124, where the coating composition provides a scats value of at most 30.
208. The coating composition of claims 168-170, where the coating composition provides a scats value of at most 30.
209. A paper article comprising the treated inorganic particles of claims 1-29 and a paper pulp.
210. A paper article comprising the treated inorganic particles of claims 34-47 and a paper pulp.211 . A paper article comprising the treated inorganic particles of claims 52-78 and a paper pulp.TI0009-W001212. The process of forming a paper article comprising producing a treated inorganic particle according to claims 83-120, and contacting the treated inorganic particles with a paper pulp.
213. The process of forming a paper article comprising producing a treated inorganic particle according to claims 126-166, and contacting the treated inorganic particles with a paper pulp.
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