WO2006028696A1 - Pigments traites en surface - Google Patents

Pigments traites en surface Download PDF

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Publication number
WO2006028696A1
WO2006028696A1 PCT/US2005/029910 US2005029910W WO2006028696A1 WO 2006028696 A1 WO2006028696 A1 WO 2006028696A1 US 2005029910 W US2005029910 W US 2005029910W WO 2006028696 A1 WO2006028696 A1 WO 2006028696A1
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Prior art keywords
pigment
titanium dioxide
weight
pigments
inorganic
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PCT/US2005/029910
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English (en)
Inventor
Daniel H. Craig
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Kerr-Mcgee Chemical Llc
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Publication of WO2006028696A1 publication Critical patent/WO2006028696A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3669—Treatment with low-molecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

Definitions

  • This invention relates to inorganic pigments with improved surface treatments.
  • the pigments of this invention are useful as opacifiers and colorants in the manufacture of products produced in many industries, including in coatings and coated goods, in plastics and articles made from plastics, and in paper and paper goods.
  • inorganic pigments such as titanium dioxide
  • pigments are generally handled in the form of a finely divided powder.
  • titanium dioxide the most widely used white pigment in commerce today due to its ability to confer high opacity when formulated into end-use products, is handled in the form of a finely divided powder.
  • titanium dioxide powders are inherently dusty and frequently exhibit poor powder flow characteristics during the handling of the powder itself, especially during formulation, compounding, and manufacture of end-use products. While free-flowing powders with low dust properties can be obtained through known manufacturing practices, these powders usually exhibit reduced opacifying properties.
  • chemical modification of titanium dioxide pigment surfaces has been the preferred approach to achieving the desired balance of pigment opacity and flow characteristics.
  • titanium dioxide pigments can be improved by exposure to certain inorganic treatments, for example, depositing inorganic metal oxide and/or metal hydroxide coatings on the surface of the titanium dioxide.
  • Certain other chemical modifications of titanium dioxide pigment surfaces are also known to improve pigment performance, including helping to reduce the tendency of a pigment to adsorb moisture and improving its gloss characteristics, particularly in coatings.
  • improved pigment dispersion characteristics results in improved thermoplastics processing and uniformity of color.
  • Organic chemical treatment of the pigment surface has also become the preferred method for achieving desired performance enhancements in cosmetics compositions, in paper and in inks, wherein the uniformity of pigment dispersion is critical.
  • the most advantageous chemical composition for surface treatment in general will be dependent on the particular end use to which the titanium dioxide is put.
  • hydrophobic organic compounds have frequently been the surface treatments of choice, due to their known ability to enhance pigment/polymer compatibility and to decrease thermoplastic polymer melt viscosity.
  • many patents have been issued disclosing methods for improving titanium dioxide pigments wherein a hydrophobic organic compound is deposited onto the pigment surface prior to its incorporation into such end use materials as plastics, as well as in coatings, inks and paper.
  • U.S. Patent 3,015,573 discloses titanium dioxide pigments having adsorbed thereon a small amount of the water-soluble salt of a tertiary amine with an organic acid of low water solubility, wherein substantially improved dispersibility in surface coating compositions is said to be achieved.
  • U.S. Patent 3,172,772 discloses a method for improving the gloss properties of titanium dioxide pigments, comprising the treatment of a hydrous oxide treated titanium dioxide with specified levels of either benzoic or para-aminobenzoic acid and an organic amine.
  • U.S. Patent 3,506,466 discloses a titanium dioxide pigment of either anatase or rutile modification with or without a coating of inorganic substances, which is treated with a salt of a water-soluble alkanolamine and an oxycarboxylic acid and milled in a fluid energy mill to provide improved properties in coating compositions.
  • U.S. Patent 3,728,142 describes an inorganic pigment such as titanium dioxide which is described as being made more readily dispersible in plastics by coating with an alkyd resin of specified composition.
  • U.S. Patent 3,754,956 discloses improved wetting and dispersion characteristics of titania pigments in plastics by treating the pigment with from 0.1-60.0 percent by weight of a polylactone having terminal hydroxy groups.
  • U.S. Patent 3,825,438 discloses a process for coating titanium dioxide pigment with at least one hydrous metal oxide by precipitating, in a slurry process, a hydrous oxide on to the pigment in the presence of an alcohol and/or a carboxylic acid, each of which contains at least two or more hydroxy groups.
  • U.S. Patent 3,925,095 describes free-flowing dispersible inorganic pigment or filler compositions containing, as dispersion aids, hydroxyalkylated alkylenediamines.
  • U.S. Patent 3,947,287 discloses stable aqueous pigment dispersions comprising a water- soluble surfactant which is a reaction product of a polyhydroxyl compound with specified amounts of, sequentially, propylene oxide and ethylene oxide per equivalent of hydroxyl.
  • U.S. Patent 4,056,402 describes water-dispersible dry, non-dusting pigment compositions which develop good strength and color values in waterborne industrial finish systems, wherein the pigment compositions contain specified ratios of pigment, nonionic dispersing agents, and at least one water soluble nonionic cellulose ether.
  • U.S. Patent 4,127,421 discloses an aqueous process for production of non-dusting granular lead chromate-containing pigments via agitation in the presence of a friable low molecular weight hydrocarbon resin and a cationic surfactant.
  • the granules are useful as colorants for air-drying enamels coating systems and plastics.
  • U.S. Patent 4,156,616 describes dispersions of inorganic and organic pigments containing an alkylene oxide adduct on long-chain aliphatic amines and an anionic surfactant having an aliphatic radical of 3 to 40 carbon atoms which are readily incorporated into hydrophilic or hydrophobic media, yielding, paints of high tinctorial strength and purity of shade.
  • U.S. Patent 4,235,768 discloses an improved aqueous production process for readily dispersible titanium dioxide pigments comprising the homogeneous coating of a titanium dioxide pigment with an organic carboxyl group-containing polymer. The pigment products are described as dispersing very easily into organic binders.
  • U.S. Patent 4,375,520 describes a procedure for the densification of particulate materials comprising treatment of particles, including pigments, with a composition comprising a liquid polymeric substance, such as soybean oil, and a solid low molecular weight polymer, such as polyethylene vinyl acetate copolymer, resulting in the production of clean dustless uniform beads.
  • a composition comprising a liquid polymeric substance, such as soybean oil, and a solid low molecular weight polymer, such as polyethylene vinyl acetate copolymer, resulting in the production of clean dustless uniform beads.
  • U.S. Patent 4,375,989 claims a titanium dioxide pigment, comprising a coating of an inorganic substance, the total amount of the inorganic coating, expressed as oxide being at maximum about 0.5% of the weight of the pigment, and further comprising a coating of an organic substance selected from the group comprising large-molecule fatty acids and their salts, organic silicon compounds, such as dimethylpolysiloxane, alcohols and polyalcohols.
  • U.S. Patent 4,464,203 discloses highly concentrated, dust-free, solid and readily dispersible inorganic or organic pigment formulations containing sequential propylene oxide and ethylene oxide addition products of alkyleneamines which are useful for pigmenting printing inks, surface coatings, and printing pastes for textiles.
  • U.S. Patent 4,563,221 discloses a particulate titanium dioxide having an organic coating of isostearic acid, dodecylbenzene sulfonic acid and a cationic emulsifying agent of a fatty alkyl amine. After such treatment the pigment does not require milling in a fluid energy mill and is easily dispersible in plastics media.
  • U.S. Patent 4,599,114 describes the treatment of titanium dioxide and other pigments with a surfactant compound consisting of the reaction product of a diamine, a carboxylic acid, and a fatty acid, to enhance the performance of the pigment in paints, plastics, paper making compositions, and reinforced plastic composite compositions.
  • U.S. Patent 4,752,340 describes titanium dioxide pigments characterized by improved gloss developing and dispersibility properties in surface coating vehicles and reduced tendencies to adsorb moisture.
  • Said titanium dioxide pigments comprise pigmentary titanium dioxide particles having deposited thereon a treating agent comprising at least one amine salt of a polyprotic acid having pKal value greater than about 2.5 and a water solubility at 20° C. of at least 2.0 weight percent and an alkanolamine having a pKbl greater than about 4.4.
  • U.S. Patent 4,762,523 claims permanently non-dusting inorganic or organic pigment preparations produced by a process comprising thoroughly mixing a moist press cake of the pigment with from 0.5 to 10% of a long-chain polyester surfactant produced by condensation of at least one saturated or unsaturated aliphatic ⁇ -hydroxycarboxylic acid with at least 4 carbon atoms between the hydroxy group and the carboxy group and a total of at least 9 carbon atoms including the carboxy group or by condensing the at least one hydroxycarboxylic acid with a carboxylic acid lacking hydroxy substitution, then drying the surfactant-containing mixture; adding an essentially non-volatile liquid selected from the group consisting of mineral oil and molten wax to the dried mixture in an amount of 2-25%; and applying intensive stress to the liquid-containing mixture until the pigment is wetted by the liquid and the flowable granulate results.
  • a long-chain polyester surfactant produced by condensation of at least one saturated or unsaturated aliphatic ⁇ -hydroxycar
  • U.S. Patent 4,863,800 discloses a pigment material, the surfaces of which are treated with a saturated fatty acid triglyceride having an iodine value of not more than 5.
  • the treated material which is used in cosmetics, has strong water repellency, feels smooth, and adheres well to the skin.
  • U.S. Patent 4,909,853 claims pigment preparations consisting essentially of an organic pigment and/or carbon black and a surfactant selected from the group consisting of sulfosuccinic acid ester series, alkylbenzenesulfonate series and mixtures thereof, which have been dried, after wet comminution, by spray- or freeze-drying from an aqueous medium, and which are useful for pigmenting thermoplastics.
  • U.S. Patent 4,923,518 discloses chemically inert pigmentary zinc oxide compositions, useful in producing UV light stable polymeric resin compositions and prepared by wet treatment of chemically reactive zinc oxide base pigments.
  • U.S. Patent 4,935,063 discloses inorganic fillers or pigments having simultaneous reinforcing effect and stabilizing effect on organic polymers, obtained by bringing the inorganic filler or pigment into contact with a solution, in an inert organic solvent, of a sterically hindered amine comprising one or more alkoxysilane groups, maintaining the mixture at higher than ambient temperature for a period of at least 0.5 hours, removing the solvent, and recovering the stabilizing filler or pigment.
  • U.S. Patent 4,986,853 discloses lamina-shaped pearlescent pigment preparations of improved flowability, wherein the starting pigments have been coated with preferably 0.2-20% by weight of a saturated monocarboxylic acid having preferably 10-26 carbon atoms or of a cyclohexanone condensate resin.
  • U.S. Patent 5,228,912 teaches the surface treatment of platelet-shaped pigments, such as mica and metal oxide-coated mica, with a polyacrylate or polymethacrylate and water-soluble salts thereof, for improved dispersibility in printing ink systems.
  • U.S. Patent 5,260,353 and U.S. Patent 5,362,770 describe a method of increasing the hydrophobicity of solid materials, such as titanium dioxide and other particulate property modifiers, and polymeric compositions containing the hydrophobic particulate property modifiers.
  • the method comprises the steps of: (a) metal ion activating the surface of a solid substrate material to provide reactive metal sites on the surface and (b) chemically bonding a surfactant to the surface at the reactive metal sites.
  • U.S. Patent 5,266,622 discloses stable aqueous dispersions of fillers and/or pigments, useful as paper coating compounds, which contain a dispersant combination comprising a water- soluble polymer, a non-ionic alkylene oxide adduct, an organosulfonate, sulfate or phosphate, and anionic sulfosuccinate.
  • U.S. Patent 5,288,320 discloses titanium dioxide carrying on its surface an ester or partial ester of an organic hydroxy compound containing 1 to 6 hydroxy groups and an aliphatic saturated Ci 0 to C 22 monocarboxylic acid, for use in plastic masterbatches.
  • U.S. Patent 5,567,754 claims pigmentary materials, such as titanium dioxide, having deposited thereon a partial ester polyol and unsaturated monocarboxylic acid treating agent corresponding to the formula R(OH)xCOOR', wherein R is an alkyl or aryl radical containing from about 2 to about 20 carbon atoms, R' is an unsaturated alkyl radical containing from about 6 to about 20 carbon atoms, and x is a number from about 2 to about 6.
  • Such treating agents are described as improving the dispersibility of the pigments in thermoplastic resins and enabling the production of thermoplastic concentrates comprising a high percentage of treated inorganic pigment dispersed in a thermoplastic resin.
  • U.S. Patent 5,643,592 discloses finely-divided particulate additives for polymers with a surface coating comprised of a compound selected from the group consisting of esters of difunctional C 6 -C 40 aliphatic and aromatic carboxylic acids and triesters of phosphoric acid.
  • the preferred additive compositions are described as especially useful in the manufacture of synthetic fibers.
  • U.S. Patent 5,733,365 describes a process for preparing a low-dusting, free-flowing pigment possessing good processibility and dispersibility in plastics concentrates, wherein a monovalent salt of a dialkyl ester of sulfosuccinic acid treating agent is deposited onto the pigment surface.
  • thermoplastic concentrates comprising an inorganic pigment dispersed in a thermoplastic resin and having deposited thereon a dialkyl sulfosuccinate treating agent, said dialkyl sulfo succinate treating agent being deposited in a dry-treating operation without the presence of aqueous metal ions in an amount ranging from about 0.1 percent to about 5 percent by weight.
  • U.S. Patent 5,908,498 describes a process for preparing a low-dusting, free-flowing pigment possessing good processibility and dispersibility in plastics concentrates, wherein a monovalent salt of a dialkyl ester of sulfosuccinic acid treating agent is deposited onto the pigment surface under a specified set of treatment conditions.
  • U.S. Patent 5,910,213 discloses a pigmentary material comprising particulate titanium dioxide treated with a polymeric hindered amine stabilizer, and which can be incorporated into a polymeric composition resulting in reduced degradation of the composition.
  • the stabilizing effect of the hindered amine is greater than the effect observed when titanium dioxide and hindered amine stabilizer are separately added to a composition.
  • U.S. Patent 6,139,617 claims titanium dioxide pigments which exhibit improved gloss developing and dispersibility properties in surface coating vehicles and reduced dispersant requirements, said pigments comprising pigmentary titanium dioxide particles having deposited thereon a treating agent comprising the reaction product of at least one monoprotic acid selected from the group consisting of dimethylolpropionic acid and dimethylolbutanoic acid and an amine.
  • U.S. Patent 6,544,328 describes a process for preparing an improved pigment which is readily dispersible in paints and plastics concentrates, using specific surface active agents to coat the pigment.
  • Preferred surface active agents are ethoxylated sorbitan derivatives and non- ethoxylated or ethoxylated mono- and diglycerides.
  • U.S. Patent Application Publication No. US 2003/0029359 Al describes improved particulate inorganic pigments and processes for preparing such inorganic pigments, which have enhanced dispersibility in plastic materials.
  • the processes comprise coating the particulate inorganic pigment with a complex mixture of partially and totally polysaturated and unsaturated fatty acid esters and derivatives thereof.
  • U.S. Patent 4,183,843 discloses an improved process for dispersing inorganic fillers in a polyester resin wherein the improvement comprises coating the filler with 0.05 to 1.0 percent, based on weight of the filler, of a polar phosphate ester surfactant containing acid groups and polar ether groups.
  • U.S. Patent 4,186,028 describes improved fluid aqueous pigment dispersions, including titanium dioxide dispersions, using a phosphonocarboxylic acid or salt thereof as a dispersion aid.
  • U.S. Patent 4,209,430 discloses improved inorganic pigments, such as pigmentary titanium dioxide, made by treating such pigments with a treating agent comprising the reaction product of a phosphorylating agent and a polyene.
  • the treated pigments are useful in thermoplastic formulations and provide the additional benefit of suppressing yellowing in thermoplastic polyolefins containing a phenolic antioxidant and titanium dioxide.
  • U.S. Patent 4,357,170 and U.S. Patent 4,377,417 disclose titanium dioxide pigments treated to suppress yellowing in polymers, the treating composition comprising an organophosphate/alkanolamine addition product or a combination of an organophosphate/alkanolamine addition product and a polyol, respectively.
  • U.S. Patent 5,318,625 and U.S. Patent 5,397,391 disclose, respectively, thermoplastic pigment concentrates and pigments of improved dispersibility in thermoplastic resins, wherein an inorganic pigment such as titanium dioxide has an organophosphate triester treatment deposited thereon.
  • U.S. Patent 5,837,049 describes a pigment, extender or filler, the particles of which are coated with an alkylphosphonic acid or ester thereof.
  • the treated inorganic solid is particularly useful for preparing polymer compositions such as masterbatches.
  • U.S. Patent 6,713,543 describes a unique treatment for pigments which uses certain organo-phosphoric acids and/or their salts, resulting in improved physical and chemical qualities, including lacing resistance, improved dispersion and decreased chemical reactivity when these treated pigments are incorporated into polymeric matrices.
  • inorganic pigments treated with at least one N-acyl amino acid or a salt thereof selected from the N-acyl neutral and acidic aminosulfonic and alkylaminosulfonic acids and the salts thereof possess improved processibility and dispersibility in thermoplastic materials, and impart improved properties to thermoplastic compositions containing said surface-treated pigments.
  • N-acyl amino acids contemplated by the instant invention comprise especially N- acyl aminosulfonic and alkylaminosulfonic acids wherein the acyl group derives from animal-, vegetable- or petroleum-origin fatty acids, the amino acid moiety contains at least two and up to twelve carbon atoms, and the amino group is a primary or secondary amine.
  • Surface treatments of the inorganic pigments according to the present invention can be accomplished with the acids or with neutralized, salt forms of the acids or with combinations of these materials.
  • N-acyl sarcosines and N-acyl taurines (and the salts based thereon) wherein the acyl group derives from an animal- or vegetable-origin fatty acid and contains from six to twenty-two carbon atoms.
  • the surface treating materials based on N-acyl sarcosines and N-acyl taurines wherein the acyl groups contain from twelve to twenty carbon atoms, for example, N-lauroyl sarcosine and sodium N-cocoyl-N-methyl taurate.
  • the amount of N-acyl aminosulfonic or alkylaminosulfonic acids or salts thereof added as a surface treatment according to the instant invention will be an amount of such materials sufficient to provide a treated inorganic particulate-containing thermoplastic resin with improved processing properties over that of a thermoplastic resin composition derived from the corresponding untreated inorganic particulate, preferably being incorporated on the inorganic particulate in an amount ranging from 0.1 to 5 weight percent of one or more such materials, based on the weight of the inorganic particulate. More preferred is an N-acyl aminosulfonic or alkylaminosulfonic acid and/or salt content of from 0.25 percent to 2.5 percent, based on the weight of the inorganic particulate. Most preferably, the surface treated inorganic particulate will use from 0.5 percent to 1.5 percent of these materials, based on the weight of the inorganic particulate.
  • the pigment surface treatments identified by the present invention can be accomplished using any of the known methods of treating pigment surfaces, such as deposition in a fluid energy mill, applying the treating agent to the dry pigment by mixing or spraying, or through the drying of pigment slurries containing said treating agent.
  • Inorganic pigments improved by the instant invention include any of the particulate inorganic pigments known in the surface coatings and plastics industries.
  • white opacifying pigments such as titanium dioxide, basic carbonate white lead, basic sulfate white lead, basic silicate white lead, zinc sulfide, zinc oxide; composite pigments of zinc sulfide and barium sulfate, antimony oxide and the like; white extender pigments such as calcium carbonate, calcium sulfate, china and kaolin clays, mica, diatomaceous earth; and colored pigments such as iron oxide, lead oxide, cadmium sulfide, cadmium selenide, lead chromate, zinc chromate, nickel titanate and chromium oxide.
  • titanium dioxide of either the anatase or rutile crystalline structure or some combination thereof.
  • the titanium dioxide pigment can have deposited thereon any of the inorganic metal oxide and/or metal hydroxide surface coatings known to the art, prior to treatment with the N-acyl aminosulfonic or alkylaminosulfonic acid and salt treating materials according to the instant invention.
  • polyolefins such as polyethylene and polypropylene
  • acrylic resins such as polymethylmethacrylate
  • polyester resins such as polyethylene or polybutylene terephthalate
  • polyamide resins such as polyamide resins
  • styrenic resins such as acrylonitrile-butadiene-styrene copolymer
  • poly(vinylchloride) polycarbonate resins and their
  • Particulate titanium dioxide pigment intermediate obtained from the vapor phase oxidation of titanium tetrachloride and containing 0.8% alumina in its crystalline lattice, was dispersed in water in the presence of 0.18% by weight (based on the pigment) of sodium hexametaphosphate dispersant and with sodium hydroxide sufficient to adjust the pH of the dispersion to a minimum value of 9.5, to provide an aqueous dispersion having a solids content of 35% by weight.
  • the resulting titanium dioxide slurry was sand milled, using a zircon sand-to- pigment weight ratio of 4 to 1, until a volume average particle size was achieved wherein greater than 90% of the particles were smaller than 0.63 microns, as determined utilizing a Microtrac XlOO Particle Size Analyzer (Microtrac Inc. Montgomeryville, PA).
  • the slurry was heated to 6O 0 C, acidified to a pH of 2.0 using concentrated sulfuric acid, then allowed to digest at 60 0 C for 30 minutes.
  • One thousand (1000) grams of the resulting pigment powder were thoroughly mixed with ten (10) grams of N-lauroyl sarcosine to achieve a pigment surface coating concentration of 1% by weight, based on titanium dioxide.
  • the dry powder mixture was subsequently roll milled for sixteen hours at room temperature, after which time the powder mixture was steam micronized, utilizing a steam to pigment weight ratio of five, with a steam injector pressure set at 1 MPa (146 psi) and micronizer ring pressure set at 800 kPa (118 psi).
  • the resulting treated pigment sample was evaluated in titanium dioxide/polyethylene concentrates, according to the following procedure:
  • the surface treated titanium dioxide produced according to the present invention and having no inorganic surface treatment coating thus demonstrates improved processibility and dispersibility, as indicated by the higher melt flow index value, the lower equilibrium torque value, and the lower maximum extruder processing pressure observed for the concentrate produced with the N-lauroyl sarcosine treated pigment versus the comparative example.
  • Particulate titanium dioxide pigment intermediate obtained from the vapor phase oxidation of titanium tetrachloride and containing 0.8% alumina in its crystalline lattice was dispersed in water in the presence of 0.18% by weight (based on pigment) of sodium hexametaphosphate dispersant, along with sufficient sodium hydroxide to adjust the pH of the dispersion to a minimum value of 9.5, to yield an aqueous dispersion with a solids content of 35% by weight.
  • the resulting titanium dioxide slurry was sand milled, using a zircon sand-to- pigment weight ratio of 4 to 1 , until a volume average particle size was achieved wherein more than 90% of the particles were smaller than 0.63 microns, as determined utilizing a Microtrac XlOO Particle Size Analyzer.
  • the slurry was heated to 6O 0 C, acidified to a pH of 2.0 using concentrated sulfuric acid, then treated with 1% alumina added as a 357 gram/liter aqueous sodium aluminate solution. During the addition of the sodium aluminate solution, the pH of the slurry was maintained between a value of 8.0 and 8.5 via the addition of sulfuric acid, prior to digestion for 15 minutes at 60°C.
  • the slurry pH was adjusted to a pH of 6.2 with additional sulfuric acid, followed by digestion for an additional 15 minutes at 6O 0 C, followed by a final adjustment of the slurry pH to 6.2.
  • the dispersion was filtered while hot, and the filtrate washed with an amount of 6O 0 C, pH 7.0 water equal in weight to the recovered pigment.
  • the washed filtrate was subsequently re-dispersed in water with agitation, in the presence of 0.35% by weight based on pigment of trimethylol propane, to achieve a concentration of less than 40% by weight of dispersed pigment.
  • the resulting pigment dispersion was spray dried using an APV Nordic PSD52 Spray Dryer, maintaining a dryer inlet temperature of approximately 28O 0 C, to yield a dry pigment powder.
  • One thousand (1000) grams of the resulting pigment powder were thoroughly mixed with ten (10) grams of N-lauroyl sarcosine to achieve a pigment surface coating concentration of 1% by weight based on titanium dioxide.
  • the dry powder mixture was subsequently roll milled for sixteen hours at room temperature, after which time the powder mixture was steam micronized at a steam to pigment weight ratio of five, with a steam injector pressure set at 1 MPa (146 psi) and micronizer ring pressure set at 800 kPa (1 18 psi).
  • the resulting finished pigment sample was evaluated in titanium dioxide/polyethylene concentrates, according to the following procedure:
  • the surface treated titanium dioxide produced according to the present invention and having deposited thereon an inorganic coating of 1% by weight of the pigment of alumina thus likewise demonstrates improved processibility and dispersibility, as indicated by the higher melt flow index value, the lower equilibrium torque value, and the lower maximum extruder processing pressure observed for the concentrate produced with the N-lauroyl sarcosine treated pigment versus the comparative example.
  • Particulate titanium dioxide pigment intermediate obtained from the vapor phase oxidation of titanium tetrachloride and containing 0.8% alumina in its crystalline lattice, was dispersed in water in the presence of 0.18% by weight (based on the pigment) of sodium hexametaphosphate dispersant and with sodium hydroxide sufficient to adjust the pH of the dispersion to a minimum value of 9.5, to provide an aqueous dispersion having a solids content of 35% by weight.
  • the resulting titanium dioxide slurry was sand milled, using a zircon sand-to- pigment weight ratio of 4 to 1, until a volume average particle size was achieved wherein greater than 90% of the particles were smaller than 0.63 microns, as determined utilizing a Microtrac XlOO Particle Size Analyzer (Microtrac Inc. Montgomeryville, PA).
  • the slurry was heated to 60°C, acidified to a pH of 2.0 using concentrated sulfuric acid, then allowed to digest at 60 0 C for 30 minutes.
  • One thousand (1000) grams of the resulting pigment powder were thoroughly mixed with ten (10) grams of sodium N-cocoyl-N-methyl taurate to achieve a pigment surface coating concentration of 1% by weight, based on titanium dioxide.
  • the dry powder mixture was subsequently roll milled for sixteen hours at room temperature, after which time the powder mixture was steam micronized, utilizing a steam to pigment weight ratio of five, with a steam injector pressure set at IMPa (146 psi) and micronizer ring pressure set at 80OkPa (1 18 psi).
  • the resulting treated pigment sample was evaluated in titanium dioxide/polyethylene concentrates, according to the following procedure:
  • the surface treated titanium dioxide produced according to the present invention and having no inorganic surface treatment coating thus demonstrates improved processibility and dispersibility, as indicated by the higher melt flow index value, the lower equilibrium torque value, and the lower maximum extruder processing pressure observed for the concentrate produced with the sodium N-cocoyl-N-methyl taurate treated pigment versus the comparative example.
  • Particulate titanium dioxide pigment intermediate obtained from the vapor phase oxidation of titanium tetrachloride and containing 0.8% alumina in its crystalline lattice was dispersed in water in the presence of 0.18% by weight (based on pigment) of sodium hexametaphosphate dispersant, along with sufficient sodium hydroxide to adjust the pH of the dispersion to a minimum value of 9.5, to yield an aqueous dispersion with a solids content of 35% by weight.
  • the resulting titanium dioxide slurry was sand milled, using a zircon sand-to- pigment weight ratio of 4 to 1, until a volume average particle size was achieved wherein more than 90% of the particles were smaller than 0.63 microns, as determined utilizing a Microtrac XlOO Particle Size Analyzer.
  • the slurry was heated to 6O 0 C, acidified to a pH of 2.0 using concentrated sulfuric acid, then treated with 1% alumina added as a 357 gram/liter aqueous sodium aluminate solution.
  • the pH of the slurry was maintained between a value of 8.0 and 8.5 via the addition of sulfuric acid, prio ' r to digestion for 15 minutes at 60°C.
  • the slurry pH was adjusted to a pH of 6.2 with additional sulfuric acid, followed by digestion for an additional 15 minutes at 6O 0 C, followed by a final adjustment of the slurry pH to 6.2.
  • the dispersion was filtered while hot, and the filtrate washed with an amount of 60 0 C, pH 7.0 water equal in weight to the recovered pigment.
  • the washed filtrate was subsequently re-dispersed in water with agitation, in the presence of 0.35% by weight based on pigment of trimethylol propane, to achieve a concentration of less than 40% by weight of dispersed pigment.
  • the resulting pigment dispersion was spray dried using an APV Nordic PSD52 Spray Dryer, maintaining a dryer inlet temperature of approximately 280 0 C, to yield a dry pigment powder.
  • One thousand (1000) grams of the resulting pigment powder were thoroughly mixed with ten (10) grams of sodium N-cocoyl-N-methyl taurate to achieve a pigment surface coating concentration of 1% by weight based on titanium dioxide.
  • the dry powder mixture was subsequently roll milled for sixteen hours at room temperature, after which time the powder mixture was steam micronized at a steam to pigment weight ratio of five, with a steam injector pressure set at 1 MPa (146 psi) and micronizer ring pressure set at 800 kPa (1 18 psi).
  • the resulting finished pigment sample was evaluated in titanium dioxide/polyethylene concentrates, according to the following procedure:
  • the surface treated titanium dioxide produced according to the present invention and having deposited thereon an inorganic coating of 1% by weight of the pigment of alumina thus again demonstrates improved processibility and dispersibility, as indicated by the substantially lower maximum extruder processing pressure observed for the concentrate produced with the sodium N-cocoyl-N-methyl taurate treated pigment versus the comparative example.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

L'invention concerne des pigments inorganiques traités à l'aide d'au moins un acide aminé N-acylé ou à l'aide d'un sel de ce dernier sélectionné parmi les acides aminosulfoniques et alkylaminosulfoniques N-acylés acides et neutres et les sels de ces derniers. Lesdits pigments possèdent une aptitude au traitement et une dispersibilité améliorées dans des matières thermoplastiques et confèrent des propriétés améliorées aux compositions thermoplastiques contenant lesdits pigments traités en surface.
PCT/US2005/029910 2004-09-07 2005-08-22 Pigments traites en surface WO2006028696A1 (fr)

Applications Claiming Priority (2)

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US93500204A 2004-09-07 2004-09-07
US10/935,002 2004-09-07

Publications (1)

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WO2006028696A1 true WO2006028696A1 (fr) 2006-03-16

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PCT/US2005/029910 WO2006028696A1 (fr) 2004-09-07 2005-08-22 Pigments traites en surface

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WO (1) WO2006028696A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0139481A2 (fr) * 1983-09-22 1985-05-02 Ajinomoto Co., Inc. Modification de surface par application de lysines N-acylées
US4606914A (en) * 1981-10-26 1986-08-19 Miyoshi Kasei Co., Ltd. Cosmetic composition
EP0489657A1 (fr) * 1990-12-04 1992-06-10 The Mearl Corporation Pigments en forme de paillettes améliorés

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4606914A (en) * 1981-10-26 1986-08-19 Miyoshi Kasei Co., Ltd. Cosmetic composition
EP0139481A2 (fr) * 1983-09-22 1985-05-02 Ajinomoto Co., Inc. Modification de surface par application de lysines N-acylées
EP0489657A1 (fr) * 1990-12-04 1992-06-10 The Mearl Corporation Pigments en forme de paillettes améliorés

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