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US4784794A Expired / Lapsed US ⏱️ 0.0 years remaining

High-dispersion sol or gel of monoclinic zirconia supermicrocrystals and production of the same

Assignee: Nissan Chemical Corp
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Filing: 1987-01-14
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Granted: 1988-11-15
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Expires: 2007-01-14
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Abstract

Abstract Disclosed herein is a high-dispersion sol of monoclinic zirconia supermicrocrystals which is translucent and contains monoclinic zirconia supermicrocrystals of uniform size and a rodlike shape or ellipsoidal shape having a diameter or width smaller than 100 Å, at a concentration higher than 0.1 mol/liter. The sol is produced by preparing a clear or sherbetlike mixture of water and zirconyl chloride or an aqueous solution of a zirconium salt of hydroxide and hydrochloric acid, subjecting the mixture or the aqueous solution to hydrothermal treatment in a sealed container at more than 130° C. for more than 24 hours, to give a white pasty product, diluting the pasty product with water so that the concentration decreases below 1 mol/liter as zirconium, adjusting the pH to 3 to 7, and finally concentrating the diluted product.

Inventors

  • 👤 Etsuro Kato

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-04 11:11
CPC Classifications
C; C01; C01G; C01G25/00; C01G25/02; C01P; C01P2004/00; C01P2004/10; C01P2004/12; C01P2004/30; C01P2004/51; C01P2004/52; C01P2006/00; C01P2006/60

Claims Analysis

Total Claims: 21
Claim 1
Independent Claim 54 words
A high-dispersion product which comprises: a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 2
Dependent Claim 54 words
A high-dispersion product which comprises: a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 3
Dependent Claim 14 words
The high-dispersion product as defined in claim 1, wherein said product is a sol.
Claim 4
Dependent Claim 14 words
The high-dispersion product as defined in claim 1, wherein said product is a gel.
Claim 5
Dependent Claim 169 words
A process for producing a high-dispersion product which is a sol or gel of monoclinic zirconia microcrystals which comprises: adding water to hydrated salt crystal composed mainly of zirconyl chloride in an amount of 400 ml or less per 1 gram atom of zirconium so as to produce a mixture; subjecting said mixture to hydrothermal treatment in a sealed container at more than 130° C. for more than 24 hours to produce a white pasty product; diluting said white pasty product with water so that the zirconium concentration decreases below 1 mol/liter to produce a diluted product; adjusting the pH of said diluted product to 3 to 7; and concentrating said diluted product to obtain a high-dispersion product which comprises a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 6
Dependent Claim 169 words
A process for producing a high-dispersion product which is a sol or gel of monoclinic zirconia microcrystals which comprises: adding water to hydrated salt crystal composed mainly of zirconyl chloride in an amount of 400 ml or less per 1 gram atom of zirconium so as to produce a mixture; subjecting said mixture to hydrothermal treatment in a sealed container at more than 130° C. for more than 24 hours to produce a white pasty product; diluting said white pasty product with water so that the zirconium concentration decreases below 1 mol/liter to produce a diluted product; adjusting the pH of said diluted product to 3 to 7; and concentrating said diluted product to obtain a high-dispersion product which comprises a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 7
Dependent Claim 13 words
The process as defined in claim 4, wherein a high-dispersion sol is produced.
Claim 8
Dependent Claim 13 words
The process as defined in claim 4, wherein a high-dispersion gel is produced.
Claim 9
Dependent Claim 25 words
The process as defined in claim 4, wherein said water is in an amount of 40 to 350 ml per 1 gram atom of zirconium.
Claim 10
Dependent Claim 25 words
The process as defined in claim 4, wherein said mixture is subjected to hydrothermal treatment at 180° to 270° C. for 1 to 10 days.
Claim 11
Dependent Claim 25 words
The process as defined in claim 4, wherein said white pasty product is diluted so that the zirconium concentration decreases to 0.1 to 0.5 mol/liter.
Claim 12
Dependent Claim 35 words
The process as defined in claim 4, wherein said obtained high-dispersion product is a sol and wherein said sol is concentrated by heating in the range of 80° to 100° C. to produce a gel.
Claim 13
Dependent Claim 179 words
A process for producing a high-dispersion product which is a sol or gel of monoclinic zirconia microcrystals which comprises: subjecting to hydrothermal treatment in a sealed container an aqueous solution which contains more than 1.5 mol/liter of zirconium salt or hydroxide based on zirconium concentration and having such a composition as to produce more than 3 mol/liter of hydrochloric acid after hydrolysis, said hydrothermal treatment being conducted at more than 130° C. for more than 24 hours so as to produce a white pasty product; diluting said white pasty product with water so that the zirconium concentration decreases below 1 mol/liter to produce a diluted product; adjusting the pH of said diluted product to 3 to 7; and concentrating said diluted product to obtain a high dispersion product which comprises a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 14
Dependent Claim 179 words
A process for producing a high-dispersion product which is a sol or gel of monoclinic zirconia microcrystals which comprises: subjecting to hydrothermal treatment in a sealed container an aqueous solution which contains more than 1.5 mol/liter of zirconium salt or hydroxide based on zirconium concentration and having such a composition as to produce more than 3 mol/liter of hydrochloric acid after hydrolysis, said hydrothermal treatment being conducted at more than 130° C. for more than 24 hours so as to produce a white pasty product; diluting said white pasty product with water so that the zirconium concentration decreases below 1 mol/liter to produce a diluted product; adjusting the pH of said diluted product to 3 to 7; and concentrating said diluted product to obtain a high dispersion product which comprises a sol or gel of isolated monoclinic zirconia microcrystals dispersed in an aqueous solution without agglomeration at a concentration of 0.1 to 1 mol/liter, wherein said monoclinic zirconia microcrystals have uniform size, and a diameter or width smaller than 100 angstroms, and wherein said sol or gel is translucent.
Claim 15
Dependent Claim 13 words
The process as defined in claim 11, wherein a high-dispersion sol is produced.
Claim 16
Dependent Claim 13 words
The process as defined in claim 11, wherein a high-dispersion gel is produced.
Claim 17
Dependent Claim 42 words
The process as defined in claim 11, wherein said aqueous solution contains 1.5 to 7 mol/liter of zirconium salt or hydroxide based on zirconium concentration and has such a composition as to produce 3 to 9 mol/liter of hydrochloric acid after hydrolysis.
Claim 18
Dependent Claim 37 words
The process as defined in claim 14, wherein said zirconium salt comprises a member selected from the group consisting of zirconyl chloride, zirconium carbonate, zirconium nitrate, zirconium sulfate, zirconium acetate, and mixtures of two or more thereof.
Claim 19
Dependent Claim 23 words
The process as defined in claim 11, wherein said hydrothermal treatment is conducted at 180° to 270° C. for 1 to 10 days.
Claim 20
Dependent Claim 25 words
The process as defined in claim 11, wherein said white pasty product is diluted so that the zirconium concentration decreases to 0.1 to 0.5 mol/liter.
Claim 21
Dependent Claim 35 words
The process as defined in claim 11, wherein said obtained high-dispersion product is a sol and wherein said sol is concentrated by heating in the range of 80° to 100° C. to produce a gel.

References Cited (Backward Citations)

US2984628A Cited
US3110681A Cited
US3282857A Cited
US3259585A Cited
US3442817A Cited
US3645910A Cited
US4664894A Cited
US4619817A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1991-11-15 1992-05-16 1992-11-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1995-11-15 1996-05-16 1996-11-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1999-11-15 2000-05-16 2000-11-15 $7700.00 Window Closed / Lapsed

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