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US4268422A Expired / Lapsed US ⏱️ 0.0 years remaining

Titanium dioxide hydrate of a particular structure and process of manufacture thereof

Assignee: Kronos Titan GmbH
•
Filing: 1979-04-23
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Granted: 1981-05-19
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Expires: 1999-04-23
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Abstract

Abstract A novel titanium dioxide hydrate is provided whose structure exhibits X-ray diffraction peaks at 24.6±0.4° and 48±0.4°, and which is suitable as an adsorbent material. A process for preparing the novel titanium dioxide hydrate also is provided which includes hydrolyzing a specific titanium sulfate solution and thereafter flocculating colloidal titanium dioxide hydrate by the addition of a monobasic acid and recovering the titanium dioxide hydrate.

Inventors

  • 👤 Heinrich Becker
  • 👤 Edgar Klein
  • 👤 Franz Rosendahl
  • 👤 Helmut Weber

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 03:36
CPC Classifications
C; C22; C22B; C22B60/00; C22B60/02; C22B60/0204; C22B60/0217; C22B60/0252; C22B60/0265; C22B60/0273; B; B01; B01J; B01J20/00; B01J20/02; B01J20/06; C01; C01G; C01G23/00; C01G23/04; C01G23/047; C01G23/053; C01P; C01P2002/00; C01P2002/70; C01P2002/72

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 22 words
δTitanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6±0.4° and 48±0.4°.
Claim 2
Dependent Claim 22 words
δTitanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6±0.4° and 48±0.4°.
Claim 3
Dependent Claim 50 words
A mixture of titanium dioxide hydrates, which, calculated as TiO 2 and related to the total quantity of TiO 2 , contains more than 20% δ titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° C. and 48°±0.4° C.
Claim 4
Dependent Claim 50 words
A mixture of titanium dioxide hydrates, which, calculated as TiO 2 and related to the total quantity of TiO 2 , contains more than 20% δ titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° C. and 48°±0.4° C.
Claim 5
Dependent Claim 131 words
A process for producing δ titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° and 48°±0.4°, and mixtures of titanium dioxide hydrates containing at least 20% of said δ titanium dioxide hydrate which comprises: hydrolyzing a titanium sulfate solution by heating to form colloidal δ titanium dioxide hydrate, said solution containing up to 150 g/l TiO 2 , and having a molar ratio of TiO 2 to free sulphuric acid between 1:1 and 1:2, and a bivalent iron content between 0 and 1 gram Fe per gram TiO 2 ; removing the colloidal δ titanium dioxide hydrate by flocculation by the adding of a monobasic acid or its salt; and separating the flocculated δ titanium dioxide hydrate from the solution.
Claim 6
Dependent Claim 131 words
A process for producing δ titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° and 48°±0.4°, and mixtures of titanium dioxide hydrates containing at least 20% of said δ titanium dioxide hydrate which comprises: hydrolyzing a titanium sulfate solution by heating to form colloidal δ titanium dioxide hydrate, said solution containing up to 150 g/l TiO 2 , and having a molar ratio of TiO 2 to free sulphuric acid between 1:1 and 1:2, and a bivalent iron content between 0 and 1 gram Fe per gram TiO 2 ; removing the colloidal δ titanium dioxide hydrate by flocculation by the adding of a monobasic acid or its salt; and separating the flocculated δ titanium dioxide hydrate from the solution.
Claim 7
Dependent Claim 173 words
A process for preparing δ titanium dioxide hydrate and mixtures of titanium dioxide hydrates containing at least 20% δ titanium dioxide hydrate wherein said δ titanium dioxide hydrate has an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° and 48°±0.4°, which comprises: hydrolyzing a titanium sulfate solution by heating in the presence of nuclei of titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kθ rays which exhibit main peaks at 2θ=24.6°±0.4° and 48°±0.4° to form colloidal δ titanium dioxide hydrate, said solution containing 120 to 250 g/l TiO 2 , having a molar ratio of TiO 2 to free sulfuric acid between 1:1 and 1:2 and a bivalent iron content between 0 and 1 gram Fe per gram TiO 2 ; removing the colloidal δ titanium dioxide hydrate by flocculation by the addition of a monobasic acid or its salt; and separating the flocculated δ titanium dioxide hydrate together with precipitated titanium dioxide hydrate consisting essentially of anatase hydrate from the solution.
Claim 8
Dependent Claim 173 words
A process for preparing δ titanium dioxide hydrate and mixtures of titanium dioxide hydrates containing at least 20% δ titanium dioxide hydrate wherein said δ titanium dioxide hydrate has an X-ray diffraction diagram taken by means of Cu-Kα rays which exhibits main peaks at 2θ=24.6°±0.4° and 48°±0.4°, which comprises: hydrolyzing a titanium sulfate solution by heating in the presence of nuclei of titanium dioxide hydrate having an X-ray diffraction diagram taken by means of Cu-Kθ rays which exhibit main peaks at 2θ=24.6°±0.4° and 48°±0.4° to form colloidal δ titanium dioxide hydrate, said solution containing 120 to 250 g/l TiO 2 , having a molar ratio of TiO 2 to free sulfuric acid between 1:1 and 1:2 and a bivalent iron content between 0 and 1 gram Fe per gram TiO 2 ; removing the colloidal δ titanium dioxide hydrate by flocculation by the addition of a monobasic acid or its salt; and separating the flocculated δ titanium dioxide hydrate together with precipitated titanium dioxide hydrate consisting essentially of anatase hydrate from the solution.
Claim 9
Dependent Claim 51 words
Process according to claims 3 or 4, characterized in that the titanium dioxide hydrate, which after the addition of the monobasic acid or its salts is present in the solution in a flocculated form, is removed and washed and then neutralized with alkali or ammonia and once more washed and/or dried.
Claim 10
Dependent Claim 45 words
Process in accordance with claims 3 or 4, characterized in that the titanium dioxide hydrate, which after the addition of the monobasic acid or its salts is present in the solution in a flocculated form, is thickened by sedimentation before being separated from the solution.
Claim 11
Dependent Claim 41 words
Process according to claims 3 or 4, characterized in that, before separation of the titanium dioxide hydrate which after the addition of a monobasic acid or its salts is present in the solution in a flocculated form, a flocculant is added.
Claim 12
Dependent Claim 28 words
Process according to claims 3 or 4, characterized in that, after its separation from the solution, the titanium dioxide hydrate or the titanium dioxide hydrate mixture is granulated.
Claim 13
Dependent Claim 57 words
Process in accordance with claims 3 or 4, characterized in that, solid inorganic or organic substances insoluble in acids are added to the titanium dioxide hydrate or the titanium dioxide hydrate mixture at a quantity of up to 70% by weight related to the resulting total mixture and that the total mixture thus obtained is then dried.
Claim 14
Dependent Claim 34 words
The process of claim 3 or 4 wherein precipitated titanium dioxide hydrate consisting essentially of anatase hydrate is removed from the hydrolyzed solution prior to removing the colloidal δ titanium dioxide hydrate by flocculation.
Claim 15
Dependent Claim 26 words
The process of claim 3 or 4 wherein the monobasic acid or its salt is added to the solution in amounts of 1.5 to 8 moles/liter.
Claim 16
Dependent Claim 21 words
The process of claim 3 or 4 wherein the separated material is washed with water to remove iron and other impurities.
Claim 17
Dependent Claim 26 words
The process of claim 3 or 4 wherein hydrolysis of the titanium sulfate solution is conducted in the presence of a trivalent titanium as a reductant.

References Cited (Backward Citations)

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US2333660A Cited
US2448683A Cited
US3211528A Cited
US3582275A Cited
US3567480A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-05-18 1984-11-17 1985-05-19 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-05-18 1988-11-17 1989-05-19 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-05-18 1992-11-17 1993-05-19 $7700.00 Window Closed / Lapsed

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