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US4095993A Expired / Lapsed US ⏱️ 0.0 years remaining

Method for preparing polycrystalline fibrous TiO2 pigment

Assignee: NL Chemicals Inc
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Filing: 1977-03-18
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Granted: 1978-06-20
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Expires: 1997-03-18
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Abstract

Abstract A polycrystalline, fibrous rutile TiO 2 pigmentary material having good optical properties and retention in paper, and exceptionally high tinting strength in latex paint systems is prepared by treating a substantially sulfate-free hydrous TiO 2 , prior to calcination, with a mineralizing complex comprising alkali metal and alkaline earth metal salts, a compound of boron and a rutile promoter sol, and calcining the treated hydrous TiO 2 at temperatures in the ranges of from 812°-865° C. followed by washing to remove the calcium ions, milling, hydroclassification and drying; or optionally by a postcalcination treatment for imparting optimum pigmentary properties.

Inventors

  • 👤 John P. Preston

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 03:40
CPC Classifications
C; C09; C09C; C09C1/00; C09C1/36; C09C1/3607; C01; C01P; C01P2004/00; C01P2004/10; C01P2004/54; C01P2004/60; C01P2004/61; C01P2004/62; C01P2006/00; C01P2006/60

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 272 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition wherein the individual fibers have a cross-section dimension in the range of from 0.04 to 0.3 millimicrons and a ratio of length to cross-section in the range of from 1.5 to about 25 comprising the steps of: hydrolyzing a titaniium sulfate-iron-sulfate solution to form a titania hydrate, filtering, bleaching and washing said hydrate to remove the soluble iron salts therefrom, said bleached hydrate being substantially iron-free but containing from 5% to 15% H 2 SO 4 associated with said hydrate, slurrying said hydrate and treating said hydrate with a sufficient amount of an ammoniacal agent selected from the group consisting of ammonia, ammonia hydroxide and ammonium carbonate to neutralize the titania hydrate slurry to a pH of from 5 to 11, washing said titania hydrate to remove the soluble salts therefrom and retaining no more than about 2% SO 3 in said hydrate, calculated on a TiO 2 basis, adding to the washed substantially sulfate-free TiO 2 hydrate a mineralizing complex consisting essentially of a potassium salt in an amount from 0.0 to 2.0% calculated as K 2 O, and calcium salt in an amount from 1.0 to 6.0% calculated as CaO, a compound of boron in an amount from 0.5 to 2.0% calculated as B 2 O 3 and rutile promoter sol in an amount of about 6.0%, all percentages based on the weight of TiO 2 , calcining the treated hydrate at temperatures in the range of from 812° to 865° C., washing the calcine to remove calcium ions, milling the calcine and optionally hydroclassifying and finishing the milled calcine.
Claim 2
Dependent Claim 272 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition wherein the individual fibers have a cross-section dimension in the range of from 0.04 to 0.3 millimicrons and a ratio of length to cross-section in the range of from 1.5 to about 25 comprising the steps of: hydrolyzing a titaniium sulfate-iron-sulfate solution to form a titania hydrate, filtering, bleaching and washing said hydrate to remove the soluble iron salts therefrom, said bleached hydrate being substantially iron-free but containing from 5% to 15% H 2 SO 4 associated with said hydrate, slurrying said hydrate and treating said hydrate with a sufficient amount of an ammoniacal agent selected from the group consisting of ammonia, ammonia hydroxide and ammonium carbonate to neutralize the titania hydrate slurry to a pH of from 5 to 11, washing said titania hydrate to remove the soluble salts therefrom and retaining no more than about 2% SO 3 in said hydrate, calculated on a TiO 2 basis, adding to the washed substantially sulfate-free TiO 2 hydrate a mineralizing complex consisting essentially of a potassium salt in an amount from 0.0 to 2.0% calculated as K 2 O, and calcium salt in an amount from 1.0 to 6.0% calculated as CaO, a compound of boron in an amount from 0.5 to 2.0% calculated as B 2 O 3 and rutile promoter sol in an amount of about 6.0%, all percentages based on the weight of TiO 2 , calcining the treated hydrate at temperatures in the range of from 812° to 865° C., washing the calcine to remove calcium ions, milling the calcine and optionally hydroclassifying and finishing the milled calcine.
Claim 3
Dependent Claim 29 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 1 wherein the milled calcine is hydroclassified to remove particles greater than 3 to 3.5 microns.
Claim 4
Dependent Claim 56 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 2 wherein the hydroclassified fibrous TiO 2 is finished by coating the fibrous TiO 2 with a hydrous oxide selected from the group consisting of TiO 2 , SiO 2 , Al 2 O 3 and mixtures thereof, followed by drying and micronizing.
Claim 5
Dependent Claim 30 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 1 wherein the potassium salt is selected from the group consisting of potassium sulfate and potassium chloride.
Claim 6
Dependent Claim 22 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 1 wherein the calcium salt is hydrous calcium chloride.
Claim 7
Dependent Claim 32 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 1 wherein the compound of boron is selected from the group consisting of hydrous sodium borate and boric acid.
Claim 8
Dependent Claim 29 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 3 wherein the hydroclassified fibrous TiO 2 is coated with 3% Al 2 O 3 .
Claim 9
Dependent Claim 39 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 3 wherein the hydroclassified fibrous TiO 2 is coated with from 1 to 4% SiO 2 and from 2 to 3% Al 2 O 3 .
Claim 10
Dependent Claim 33 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 3 wherein the hydroclassified fibrous TiO 2 is coated with 1% TiO 2 and 2% Al 2 O 3 .
Claim 11
Dependent Claim 30 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 1 wherein a flocculating agent is added to the ball milled calcine to form a calcine floc.
Claim 12
Dependent Claim 21 words
Process for producing a fibrous, polycrystalline, rutile TiO 2 composition according to claim 10 wherein the flocculating agent is formic acid.

References Cited (Backward Citations)

US2143851A Cited
US3088840A Cited
US3862297A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-06-19 1981-12-19 1982-06-20 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-06-19 1985-12-19 1986-06-20 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-06-19 1989-12-19 1990-06-20 $7700.00 Window Closed / Lapsed

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