Patent US4232459A successfully refreshed from Google Patents.
Patent US3840381A successfully refreshed from Google Patents.
US3840381A
Expired / Lapsed
US
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Titanium coated pigments
Assignee: Nikon Kogen Kogyo Co Ltd
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Filing: 1972-07-12
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Granted: 1974-10-08
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Expires: 1992-07-12
Abstract
Abstract A composite nacreous pigment exhibiting a high degree of pearly luster is made by uniformly coating transparent to translucent thin platelets of single crystals of barium sulfate with a homogeneous transparent to translucent thin film of titanium dioxide formed by the hydrolysis in aqueous media of titanium tetrachloride, a water-soluble titanium ester or a water-soluble titanium salt. The hydrous titanium hydroxide film attached to the surface of the barium sulfate crystal is heated to a high temperature to convert the film to titanium dioxide. The pigment thus prepared can be dispersed, if desired, in a transparent or semi transparent light-transmitting medium. The thickness of the individual crystals can be controlled to provide a white lustrous product or a lustrous product colored by optical interference phenomena.
Inventors
- 👤 A Watanabe
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 21:34
CPC Classifications
C; C09; C09C; C09C1/00; C09C1/0015; C09C1/0021; C01; C01F; C01F11/00; C01F11/46; C01F11/462; C09C1/0018; C01P; C01P2004/00; C01P2004/20; C01P2004/60; C01P2004/61; C09C2200/00; C09C2200/10; C09C2200/1087; C09C2200/30; C09C2200/301; C09C2200/302; C09C2220/00; C09C2220/10
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
21 words
A METHOD OF MAKING A HIGHLY LUSTROUS NACREOUS PIGMENT CONSISTING ESSETIALLY OF SUBSTANTIALLY UNIFORM CRYSTALLINE PLATELETS, THE INDIVIDUAL PLATELETS CONSISTING OF:
Claim 2
Independent Claim
21 words
A METHOD OF MAKING A HIGHLY LUSTROUS NACREOUS PIGMENT CONSISTING ESSETIALLY OF SUBSTANTIALLY UNIFORM CRYSTALLINE PLATELETS, THE INDIVIDUAL PLATELETS CONSISTING OF:
Claim 3
Dependent Claim
22 words
A SUBSTRATE OF TRANSPARENT TO TRANSLUCENT SINGLE CRYSTALS OF BARIUM SULFATE HAVING A DIAMETER OF 5-200U AND A THICKNESS OF 0.05-1.0U, AND
Claim 4
Dependent Claim
22 words
A SUBSTRATE OF TRANSPARENT TO TRANSLUCENT SINGLE CRYSTALS OF BARIUM SULFATE HAVING A DIAMETER OF 5-200U AND A THICKNESS OF 0.05-1.0U, AND
Claim 5
Dependent Claim
163 words
A UNIFORM TRANSPARENT TO TRANSLUCENT OUTER COATING OF TITANIUM DIOXIDE ATTACHED TO SAID BARIUM SULFATE CRYSTAL, THE TICKNESS OF SAID OUTER COATING BEING 500-20,000 A, SAID PIGMENT BEING MADE BY THE STEPS COMPRISING: A. ADDING SUBSTANTIALLY UNIFORM BARIUM SULFATE CRYSTALS, PREPARED FROM A DILUTE AQUEOUS SOLUTION HAVING A BARIUM SALT CONCENTRATION OF LESS THAN 0.1 MOLE PER LITER TO AN ACIDIC AQUEOUS SOLUTION OF TITANIUM TETRACHLORIDE, A TITANIUM ESTER OR A TITANIUM SALT, THE CONCENTRATION OF THE TITANIUM COMPOUND BEING BETWEEN 5-60 PER CENT BY WEIGHT, BASED ON THE WEIGHT OF THE HYDROLYSIS SOLUTION, B. MAINTAINING THE RESULTING SOLUTION AT A TEMPERATURE BETWEEN 20*C. AND THE BOILING POINT OF THE SOLUTION FOR A TIME SUFFICIENT TO EFFECT HYDROLYSIS AND TO ATTACH TO THE SURFACE OF THE BARIUM SULFATE CRYSTALS A HYDROUS COATING OF TITANIUM OXIDE HAVING A THICKNESS BETWEEN 500-20,000 A, AND C. DRYING AND CALCINING THE RESULTING CRYSTALS TO CONVERT THE HYDROUS TITANIUM OXIDE TO A LUSTROUS THIN FILM OF TITANIUM DIOXIDE.
Claim 6
Dependent Claim
163 words
A UNIFORM TRANSPARENT TO TRANSLUCENT OUTER COATING OF TITANIUM DIOXIDE ATTACHED TO SAID BARIUM SULFATE CRYSTAL, THE TICKNESS OF SAID OUTER COATING BEING 500-20,000 A, SAID PIGMENT BEING MADE BY THE STEPS COMPRISING: A. ADDING SUBSTANTIALLY UNIFORM BARIUM SULFATE CRYSTALS, PREPARED FROM A DILUTE AQUEOUS SOLUTION HAVING A BARIUM SALT CONCENTRATION OF LESS THAN 0.1 MOLE PER LITER TO AN ACIDIC AQUEOUS SOLUTION OF TITANIUM TETRACHLORIDE, A TITANIUM ESTER OR A TITANIUM SALT, THE CONCENTRATION OF THE TITANIUM COMPOUND BEING BETWEEN 5-60 PER CENT BY WEIGHT, BASED ON THE WEIGHT OF THE HYDROLYSIS SOLUTION, B. MAINTAINING THE RESULTING SOLUTION AT A TEMPERATURE BETWEEN 20*C. AND THE BOILING POINT OF THE SOLUTION FOR A TIME SUFFICIENT TO EFFECT HYDROLYSIS AND TO ATTACH TO THE SURFACE OF THE BARIUM SULFATE CRYSTALS A HYDROUS COATING OF TITANIUM OXIDE HAVING A THICKNESS BETWEEN 500-20,000 A, AND C. DRYING AND CALCINING THE RESULTING CRYSTALS TO CONVERT THE HYDROUS TITANIUM OXIDE TO A LUSTROUS THIN FILM OF TITANIUM DIOXIDE.
Claim 7
Dependent Claim
163 words
a uniform transparent to translucent outer coating of titanium dioxide attached to said barium sulfate crystal, the thickness of said outer coating being 500-20,000 A, said pigment being made by the steps comprising: a. adding substantially uniform barium sulfate crystals, prepared from a dilute aqueous solution having a barium salt concentration of less than 0.1 mole per liter to an acidic aqueous solution of titanium tetrachloride, a titanium ester or a titanium salt, the concentration of the titanium compound being between 5-60 per cent by weight, based on the weight of the hydrolysis solution, b. maintaining the resulting solution at a temperature between 20*C. and the boiling point of the solution for a time sufficient to effect hydrolysis and to attach to the surface of the barium sulfate crystals a hydrous coating of titanium oxide having a thickness between 500-20,000 A, and c. drying and calcining the resulting crystals to convert the hydrous titanium oxide to a lustrous thin film of titanium dioxide.
Claim 8
Dependent Claim
163 words
a uniform transparent to translucent outer coating of titanium dioxide attached to said barium sulfate crystal, the thickness of said outer coating being 500-20,000 A, said pigment being made by the steps comprising: a. adding substantially uniform barium sulfate crystals, prepared from a dilute aqueous solution having a barium salt concentration of less than 0.1 mole per liter to an acidic aqueous solution of titanium tetrachloride, a titanium ester or a titanium salt, the concentration of the titanium compound being between 5-60 per cent by weight, based on the weight of the hydrolysis solution, b. maintaining the resulting solution at a temperature between 20*C. and the boiling point of the solution for a time sufficient to effect hydrolysis and to attach to the surface of the barium sulfate crystals a hydrous coating of titanium oxide having a thickness between 500-20,000 A, and c. drying and calcining the resulting crystals to convert the hydrous titanium oxide to a lustrous thin film of titanium dioxide.
Claim 9
Dependent Claim
29 words
Method according to claim 1 in which the pH of the hydrolysis solution is adjusted by adding up to 5 per cent by weight of a strong mineral acid.
Claim 10
Dependent Claim
28 words
Method according to claim 1 in which the thickness of the outer coating of titanium dioxide is between 500-1,000 A and the product is a white lustrous pigment.
Claim 11
Dependent Claim
28 words
Method according to claim 1 in which the thickness of the outer coating of titanium dioxide is between 2,000-20,000 A and the product is an iridescent lustrous pigment.
Claim 12
Dependent Claim
21 words
Method according to claim 1 in which the temperature of hydrolysis is between 70*C. and the boiling point of the solution.
Claim 13
Dependent Claim
17 words
Method according to claim 1 in which the product is dried at 75*-300*C. and calcined at 700*-1,100*C.
Claim 14
Dependent Claim
23 words
Method according to claim 1 wherein the barium sulfate crystals have a diameter of 10-125 Mu and a thicknEss of 0.05-0.7 Mu .
Claim 15
Dependent Claim
85 words
Method according to claim 1 wherein the ultimate concentration of the solution in which the barium sulfate crystals are formed is controlled to a concentration of less than 0.1 mole per liter by admixing substantially stoichiometric quantities of a barium salt solution having a concentration of 0.1-0.7 mole per liter and an alkali metal or ammonium sulfate solution having a concentration of 0.1-0.7 mole per liter in a sufficient volume of an ammonium sulfate solution having a concentration of less than 0.01 mole per liter.
Claim 16
Dependent Claim
94 words
A highly lustrous nacreous pigment consisting essentially of substantially uniform nacreous crystalline platelets, the individual platelets consisting of (1) a substrate of transparent to translucent single crystals of barium sulfate originating from a dilute aqueous solution having a barium salt concentration of less than 0.1 mole per liter, said single crystals having a diameter of 5-200 microns and a thickness of 0.05 to 1 micron, and (2) a uniform transparent to translucent outer coating of titanium dioxide attached to each of said barium sulfate crystals, the thickness of the outer coating being 500-20,000 angstroms.
Claim 17
Dependent Claim
94 words
A highly lustrous nacreous pigment consisting essentially of substantially uniform nacreous crystalline platelets, the individual platelets consisting of (1) a substrate of transparent to translucent single crystals of barium sulfate originating from a dilute aqueous solution having a barium salt concentration of less than 0.1 mole per liter, said single crystals having a diameter of 5-200 microns and a thickness of 0.05 to 1 micron, and (2) a uniform transparent to translucent outer coating of titanium dioxide attached to each of said barium sulfate crystals, the thickness of the outer coating being 500-20,000 angstroms.
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-10-07 | 1978-04-08 | 1978-10-08 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-10-07 | 1982-04-08 | 1982-10-08 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-10-07 | 1986-04-08 | 1986-10-08 | $7700.00 | Window Closed / Lapsed |