# US 5,700,318 A · Durable pigments for plastic > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,700,318 A - Document ID: US5700318A - Status: Granted - Kind: A - Application number: 08/632,993 - Filed: 1996-04-16 - Granted: 1997-12-23 - Earliest claimed: 1996-04-16 - Assignees: Kerr-McGee Chemical Corporation - Inventors: John R. Brand; Kelly A. Green - Web page: https://patentgrep.com/patent/US5700318A ## CPC - C09C 1/3661: {Coating} - C09C 3/063: {Coating} - C01P 2004/51: Particles with a specific particle size distribution - C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer - C01P 2004/82: two phases having the same anion, e.g. both oxidic phases - C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values - C01P 2006/90: Other properties not specified above - Y10T 428/2991: Coated - C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS} - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract Improved alumina-coated inorganic pigments having a first coating of boehmite alumina, a second coating of amorphous alumina, and a third coating of boehmite alumina which exhibit good durability, dispersibility, and optical properties in plastic compositions are disclosed. Also disclosed is a process whereby an aqueous slurry of an alumina-containing inorganic pigment is milled to achieve a particular particle size distribution, a first coating of boehmite alumina is precipitated onto the pigment material within a first pH range, a second amount of an alumina coating agent is added to the aqueous slurry within a second pH range to obtain a second coating of amorphous alumina over the first boehmite alumina coating, and then the pH of the slurry is adjusted to a third pH range thus forming a third boehmite alumina coating over the second amorphous alumina coating. ## Claims ### Claim 1 An alumina-coated inorganic pigment comprising an inorganic pigment material containing at least about 0.75 percent alumina by weight based upon the weight of said pigment material having a first coating of predominantly boehmite alumina on said inorganic pigment, a second coating of predominantly amorphous alumina over said first coating, and a third coating of predominantly boehmite alumina over said second coating; said first coating being achieved in a discrete interval and said second and third coatings being achieved continuously. ### Claim 2 (depends on 1) The alumina-coated inorganic pigment of claim 1 wherein said inorganic pigment contains from about 0.75 percent to about 2 percent alumina by weight based upon the weight of said pigment. ### Claim 3 (depends on 2) The alumina-coated inorganic pigment of claim 2 wherein said pigment material contains from about 1 percent to about 1.5 percent alumina by weight based upon the weight of said pigment material. ### Claim 4 (depends on 3) The alumina-coated inorganic pigment of claim 3 wherein said pigment material contains about 1.3 percent alumina by weight based upon the weight of said pigment material. ### Claim 5 (depends on 1) The alumina-coated inorganic pigment of claim 1 wherein said pigment material is titanium dioxide containing at least about 0.75 wt % of alumina based on the weight of said pigment material. ### Claim 6 A process for preparing alumina-coated inorganic pigments comprising the steps of: (a) milling an aqueous slurry containing inorganic pigment material, wherein said pigment material contains at least about 0.75 percent alumina by weight based upon the weight of said pigment material, in the presence of a dispersing agent, to achieve a particle size distribution in said pigment material wherein no more than about 40 percent of said pigment particles are greater than 0.49 microns as measured by a Microtrac 9200 FRA; (b) removing the milling media from said aqueous slurry; (c) adding a first amount of an alumina coating agent to said slurry and adjusting the slurry pH to a level of at least about 1.5 to form a first coating of predominately boehmite alumina on said pigment; (d) digesting the slurry at a temperature of from about 50.degree. C. to about 70.degree. C. for a time of from about 5 to about 60 minutes; (e) increasing the pH of the slurry to a level within the range of from about 2.5 to about 5; (f) adding a second aamount of an alumina coating agent to the slurry with concurrent addition of a pH adjusting agent to form a second coating of predominately amorphous alumina over said first coating while maintaining the pH of the slurry within a range of from about 5 to about 7; (g) digesting the slurry at a temperature of from about 50.degree. C. to about 70.degree. C. for a time of from about 10 to about 90 minutes; (h) adjusting the pH of the slurry to a level within the range of from about 6 to about 9 and digesting said slurry at a temperature of from about 50.degree. C. to about 70.degree. C. for a time of from about 5 to about 60 minutes to form a third coating of predominately boehmite alumina on said pigment and over said second coating; (i) recovering said alumina coated pigment to provide a plastics grade pigment. ### Claim 7 (depends on 6) The process of claim 6 wherein said pigment material in step (a) contains from about 1 percent to about 1.5 percent alumina by weight based upon the weight of said pigment material. ### Claim 8 (depends on 7) The process of claim 7 wherein said pigment material contains about 1.3 percent alumina by weight based upon the weight of said pigment material. ### Claim 9 (depends on 6) The process of claim 6 wherein said pigment material is titanium dioxide containing at least about 0.75 wt % alumina based on the weight of said pigment material. ### Claim 10 (depends on 6) The process of claim 6 wherein a second aamount of a dispersing agent is added in step (c). ### Claim 11 (depends on 10) The process of claim 10 wherein said dispersing agent in steps (a) and (c) is selected from the group consisting of phosphates, polyols and amines. ### Claim 12 (depends on 11) The process of claim 11 wherein said dispersing agent is sodium hexametaphosphate. ### Claim 13 (depends on 6) The process of claim 6 wherein said dispersing agent in step (a) is present in an aamount in the range of from about 0.05 percent to about 0.50 percent by weight based upon the weight of said pigment material. ### Claim 14 (depends on 13) The process of claim 13 wherein the aamount of said dispersing agent is about 0.15 percent by weight based upon the weight of said pigment material. ### Claim 15 (depends on 10) The process of claim 10 wherein said dispersing agent in step (c) is present in an aamount in the range of from about 0.05 percent to about 0.50 percent by weight based upon the weight of said pigment material. ### Claim 16 (depends on 15) The process of claim 15 wherein said dispersing agent is present in an aamount of about 0.30 percent by weight based upon the weight of said pigment material. ### Claim 17 (depends on 6) The process of claim 6 wherein from about 0.1 percent to about 20 percent of said pigment particles are 0.49 microns or less as measured by a Microtrac 9200 FRA. ### Claim 18 (depends on 17) The process of claim 17 wherein from about 5 percent to about 10 percent of said pigment particles are 0.49 microns or less. ### Claim 19 (depends on 18) The process of claim 18 wherein no more than about 7 percent of said pigment particles are 0.49 microns or less. ### Claim 20 (depends on 6) The process of claim 6 wherein the milling media of step (a) is sand. ### Claim 21 (depends on 6) The process of claim 6 wherein the temperature during steps c through h is maintained within the range of from about 50.degree. C. to about 70.degree. C. ### Claim 22 (depends on 21) The process of claim 21 wherein the temperature is maintained at about 60.degree. C. ### Claim 23 (depends on 6) The process of claim 6 wherein the alumina coating agent is an acidic or alkaline inorganic aluminum salt. ### Claim 24 (depends on 23) The process of claim 23 wherein said alumina coating agent is sodium aluminate. ### Claim 25 (depends on 6) The process of claim 6 wherein the amount of alumina coating agent added in step (c) is sufficient to provide said first coating in an amount within the range of from about 0.01 percent to about 1 percent boehmite alumina by weight based upon the weight of said pigment material. ### Claim 26 (depends on 25) The process of claim 25 wherein the alumina coating agent added in step (c) is sufficient to provide said first coating in an amount within the range of from about 0.2 percent to about 0.5 percent by weight based upon the weight of said pigment material. ### Claim 27 (depends on 26) The process of claim 26 wherein the alumina coating agent added is sufficient to provide said first coating in an amount of about 0.35 percent by weight based upon the weight of said pigment material. ### Claim 28 (depends on 6) The process of claim 6 wherein the alumina coating agent added in step (f) is sufficient to provide said second coating in an amount within a range of from about 0.2 percent to about 1.2 percent by weight based upon the weight of said pigment material. ### Claim 29 (depends on 28) The process of claim 28 wherein the alumina coating agent added is sufficient to provide said second coating in an aamount within a range of from about 0.5 percent to about 1.0 percent by weight based upon the weight of said pigment material. ### Claim 30 (depends on 29) The process of claim 29 wherein the alumina coating agent added is sufficient to provide said second coating in an aamount of about 0.75 percent by weight based upon the weight of said pigment material. ### Claim 31 (depends on 6) The process of claim 6 wherein the pH of said slurry during step (a) is about 10. ### Claim 32 (depends on 6) The process of claim 6 wherein the pH of said slurry in step (c) is adjusted to a level within the range of from about 1 to about 3. ### Claim 33 (depends on 32) The process of claim 32 wherein the pit of said slurry is adjusted to a level of about 1.5. ### Claim 34 (depends on 6) The process of claim 6 wherein the pH of said slurry in step (e) is adjusted to about 3. ### Claim 35 (depends on 6) The process of claim 6 wherein the pH of said slurry in step (f) is maintained at about 5.75. ### Claim 36 (depends on 6) The process of claim 6 wherein the pH of said slurry in step (h) is adjusted to a level within the range of from about 7 to about 9. ### Claim 37 (depends on 36) The process of claim 36 wherein the pH of said slurry is adjusted to about 8. ### Claim 38 (depends on 6) The process of claim 6 wherein the pH adjusting agent in steps (c) and (f) is a mineral acid. ### Claim 39 (depends on 38) The process of claim 38 wherein said pH adjusting agent is sulfuric acid. ### Claim 40 (depends on 6) The process of claim 6 wherein the pH adjusting agent in steps (e) and (h) is an alkali metal hydroxide base. ### Claim 41 (depends on 40) The process of claim 40 wherein said pH adjusting agent is sodium hydroxide. ### Claim 42 (depends on 6) The process of claim 6 wherein said slurry is digested in step (d) for from about 10 to about 45 minutes. ### Claim 43 (depends on 42) The process of claim 42 wherein said slurry is digested for about 15 minutes. ### Claim 44 (depends on 6) The process of claim 6 wherein said slurry is digested in step (g) for from about 20 to about 70 minutes. ### Claim 45 (depends on 44) The process of claim 44 wherein said slurry is digested for about 30 minutes. ### Claim 46 (depends on 6) The process of claim 6 wherein said slurry is digested in step (h) for from about 10 to about 45 minutes. ### Claim 47 (depends on 46) The process of claim 46 wherein said slurry is digested for about 15 minutes. ### Claim 48 (depends on 6) The process of claim 6 wherein said alumina coated pigment is recovered by filtering, drying and milling.