Patent US4670243A successfully refreshed from Google Patents.
US4670243A
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Method of precipitating metal titanate powders
Assignee: Vibrantz Corp
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Filing: 1986-06-30
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Granted: 1987-06-02
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Expires: 2006-06-30
Abstract
Abstract A titanium acylate solution is produced by adding glacial acetic acid to tetra-isopropyl titanate. Distilled water is then added until the solution clears, and a high grade alkaline-earth metal carbonate, such as BaCO 3 , SrCO 3 or CaCO 3 , or a combination thereof, is added and agitated until the earth-metal dissolves and the solution again becomes clear. An alkaline hydroxide, such as NaOH, is added until the pH of the solution reaches 13 or 10 above, and causes crystals of an earth-metal titanate to form in the solution. The solution is thereafter filtered to produce an alkaline-earth metal titanate filter cake which is then dried and washed to produce the desired powder. At no time during the process is it necessary to apply any external heat to the solution. The heat of reaction is sufficient.
Inventors
- 👤 James M. Wilson
- 👤 Dana L. Coller
- 👤 Subramaniam Venkataramani
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 07:28
CPC Classifications
C; C01; C01G; C01G23/00; C01G23/003; C01G23/006; C01P; C01P2002/00; C01P2002/70; C01P2002/72; C01P2002/76; C01P2002/80; C01P2002/88; C01P2004/00; C01P2004/01; C01P2004/03; C01P2004/60; C01P2004/62; C01P2006/00; C01P2006/12; C01P2006/32; C01P2006/33; C01P2006/36
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
89 words
A method of producing alkaline earth-metal titanates in powder form, comprising preparing an acidic titanium acylate solution, adding to said acidic solution a water insoluble alkaline earth-metal carbonate and causing the alkaline earth-metal ions from the carbonate to solubilize in the acidic solution, thereafter adding an alkaline hydroxide to raise the pH of the solution to 13 or above, and to precipitate alkaline earth-metal titanate crystals in the solution, and filtering said crystals from the solution to produce a filter cake comprising an alkaline earth-metal titanate in powder form.
Claim 2
Independent Claim
89 words
A method of producing alkaline earth-metal titanates in powder form, comprising preparing an acidic titanium acylate solution, adding to said acidic solution a water insoluble alkaline earth-metal carbonate and causing the alkaline earth-metal ions from the carbonate to solubilize in the acidic solution, thereafter adding an alkaline hydroxide to raise the pH of the solution to 13 or above, and to precipitate alkaline earth-metal titanate crystals in the solution, and filtering said crystals from the solution to produce a filter cake comprising an alkaline earth-metal titanate in powder form.
Claim 3
Dependent Claim
44 words
A method as defined in claim 1 in which said solution is not subjected to any heat, other than the heat of reaction generated as the result of the preparation of said titanium acylate solution, and any subsequent reactions caused by the additions thereto.
Claim 4
Dependent Claim
27 words
A method as defined in claim 1, wherein said alkaline earth-metal carbonate is selected from the group consisting of Ba, Sr and Ca carbonates and combinations thereof.
Claim 5
Dependent Claim
23 words
A method as defined in claim 1, wherein said titanium acylate solution is prepared by mixing a tetra-alkyl titanate with glacial acetic acid.
Claim 6
Dependent Claim
13 words
A method as defined in claim 4, wherein tetra-alkyl titanate is tetra-isopropyl titanate.
Claim 7
Dependent Claim
32 words
A method as defined in claim 1, including washing drying and heating the filter cake to a range of 900°-1000° C. to cause its crystalline structure to change from cubic to tetragonal.
Claim 8
Independent Claim
103 words
A method of producing alkaline-earth metal titanate in powder form, comprising mixing titanium alkoxide and an acid to form an titanium acylate solution, adding to said acidic solution water and a water insoluble alkaline-earth metal carbonate in quantities sufficient to cause the alkaline-earth metal in the carbonate to dissolve in the acidic solution, thereafter adding an alkaline hydroxide to the solution to raise the solution pH to 13 or above, and to precipitate alkaline-earth metal titanate crystals in the solution, filtering the crystals from the solution to produce a filter cake, and drying and washing the cake to produce the the desired powder.
Claim 9
Independent Claim
103 words
A method of producing alkaline-earth metal titanate in powder form, comprising mixing titanium alkoxide and an acid to form an titanium acylate solution, adding to said acidic solution water and a water insoluble alkaline-earth metal carbonate in quantities sufficient to cause the alkaline-earth metal in the carbonate to dissolve in the acidic solution, thereafter adding an alkaline hydroxide to the solution to raise the solution pH to 13 or above, and to precipitate alkaline-earth metal titanate crystals in the solution, filtering the crystals from the solution to produce a filter cake, and drying and washing the cake to produce the the desired powder.
Claim 10
Dependent Claim
26 words
A method as defined in claim 7, including mixing said titanium alkoxide with acetic acid in ratios of approximately 1:2 to form said titanium acylate solution.
Claim 11
Dependent Claim
14 words
A method as defined in claim 8, wherein said titanium alkoxide is tetra-isopropyl titanate.
Claim 12
Dependent Claim
25 words
A method as defined in claim 7, wherein said carbonate is selected from the group consisting of Ba, Sr, and Ca carbonates and mixtures thereof.
Claim 13
Independent Claim
132 words
A method of producing alkaline earth-metal titanate chemical powders by direct precipitation from a chemical reaction product produced without the application of any heat other than that generated by the heat of reaction, comprising mixing water, glacial acetic acid and an organic titanium compound in ratios of approximately 1:3:1.5 to form a clear, acidic titanium acylate solution, mixing a water insoluble alkaline earth-metal carbonate in the acidic solution effectively to dissolve the alkaline earth-metal of the carbonate in the solution, thereafter adding an alkaline hydroxide to said mixture in quantities sufficient to raise the solution pH to 13 or above, and to cause alkaline earth-metal titanate crystals to form in the solution, and filtering said crystals from the solution to form a filter cake comprising an alkaline earth-metal titanate in powder form.
Claim 14
Independent Claim
132 words
A method of producing alkaline earth-metal titanate chemical powders by direct precipitation from a chemical reaction product produced without the application of any heat other than that generated by the heat of reaction, comprising mixing water, glacial acetic acid and an organic titanium compound in ratios of approximately 1:3:1.5 to form a clear, acidic titanium acylate solution, mixing a water insoluble alkaline earth-metal carbonate in the acidic solution effectively to dissolve the alkaline earth-metal of the carbonate in the solution, thereafter adding an alkaline hydroxide to said mixture in quantities sufficient to raise the solution pH to 13 or above, and to cause alkaline earth-metal titanate crystals to form in the solution, and filtering said crystals from the solution to form a filter cake comprising an alkaline earth-metal titanate in powder form.
Claim 15
Dependent Claim
28 words
A method as defined in claim 11, wherein said alkaline-earth metal titanate carbonate is selected from the group consisting of Ba, Sr, and Ca carbonates and mixtures thereof.
Claim 16
Dependent Claim
15 words
A method as defined in claim 11, wherein said titanium compound is a tetra-alkyl titanate.
Claim 17
Dependent Claim
13 words
A method as defined in claim 13, wherein said alkaline hydroxide is NaOH.
Claim 18
Dependent Claim
19 words
A method as defined in claim 11, wherein said alkaline-earth metal carbonate includes BaCO 3 and SrCO 3 .
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-06-01 | 1990-12-01 | 1991-06-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-06-01 | 1994-12-01 | 1995-06-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-06-01 | 1998-12-01 | 1999-06-02 | $7700.00 | Window Closed / Lapsed |