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Process for manufacturing a stable titanyl sulfate solution

Assignee: NL Chemicals Inc
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Filing: 1980-09-19
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Granted: 1981-06-23
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Expires: 2000-09-19
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Abstract

Abstract A process is provided for the manufacture of a stable titanyl sulfate solution by diluting a reaction mixture containing iron sulfate and titanyl sulfate with a material selected from water, a titanyl sulfate solution, and mixtures thereof. The titanyl sulfate solution may be recovered or processed to provide titanium dioxide hydrate which may be calcined to provide titanium dioxide pigment.

Inventors

  • 👤 Joseph L. Waldman
  • 👤 Edgar Klein
  • 👤 Achim Kulling
  • 👤 Joseph A. Rahm

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 03:05
CPC Classifications
C; C01; C01G; C01G23/00; C01G23/04; C01G23/047; C01G23/053; C22; C22B; C22B34/00; C22B34/10; C22B34/12; C22B34/1236; C22B34/124; C22B34/125; C01G23/008

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 201 words
A process for preparing a stable titanyl sulfate solution, which comprises: (1) reacting a titaniferous bearing material in an amount between about 10% and about 400% above the stoichiometric amount of material necessary to react with sulfuric acid to provide titanyl sulfate with a dilute sulfuric acid solution having a concentration between about 25% and about 60% by weight, based upon the total weight of said solution, at a temperature below about 140° C.; (2) cooling the resulting reaction mixture to a temperature below about 110° C. without precipitating the titanyl sulfate to produce a reaction mixture containing dissolved titanyl sulfate; (3) diluting the reaction mixture containing titanyl sulfate with a sufficient amount of a diluent material selected from the group consisting of water, titanyl sulfate solution, and mixtures thereof, to produce a reaction mixture having the following properties in the absence of undissolved solids: an iron to titanium dioxide weight ratio of about 0.5-1.2:1.0, a titanium dioxide content of about 120 to about 180 grams per liter, a specific gravity of about 1.4 to about 1.8, and an active sulfuric acid to titanium dioxide mole ratio of about 1.4-1.9:1; (4) separating undissolved solids and obtaining a stable titanyl sulfate solution.
Claim 2
Dependent Claim 201 words
A process for preparing a stable titanyl sulfate solution, which comprises: (1) reacting a titaniferous bearing material in an amount between about 10% and about 400% above the stoichiometric amount of material necessary to react with sulfuric acid to provide titanyl sulfate with a dilute sulfuric acid solution having a concentration between about 25% and about 60% by weight, based upon the total weight of said solution, at a temperature below about 140° C.; (2) cooling the resulting reaction mixture to a temperature below about 110° C. without precipitating the titanyl sulfate to produce a reaction mixture containing dissolved titanyl sulfate; (3) diluting the reaction mixture containing titanyl sulfate with a sufficient amount of a diluent material selected from the group consisting of water, titanyl sulfate solution, and mixtures thereof, to produce a reaction mixture having the following properties in the absence of undissolved solids: an iron to titanium dioxide weight ratio of about 0.5-1.2:1.0, a titanium dioxide content of about 120 to about 180 grams per liter, a specific gravity of about 1.4 to about 1.8, and an active sulfuric acid to titanium dioxide mole ratio of about 1.4-1.9:1; (4) separating undissolved solids and obtaining a stable titanyl sulfate solution.
Claim 3
Dependent Claim 26 words
The process of claim 1 wherein the diluent is a titanyl sulfate solution having a weight ratio of iron to titanium dioxide of less than 0.4:1.0.
Claim 4
Dependent Claim 16 words
The process of claim 1 wherein the dilution is performed prior to separating the undissolved solids.
Claim 5
Dependent Claim 37 words
The process of claim 1 wherein dilution is performed by using said diluent materials at a temperature less than the temperature of the reaction mixture to inhibit hydrolytic nucleation of titanyl sulfate present in the reaction mixture.
Claim 6
Dependent Claim 262 words
A process for producing titanium dioxide from a titanyl sulfate solution, which comprises: (1) reacting a titaniferous bearing material in an amount between about 10% and about 400% above the stoichiometric amount of titaniferous bearing material necessary to react with sulfuric acid to provide titanyl sulfate with a dilute sulfuric acid solution having a concentraton between about 25% and about 60% by weight, based upon the total weight of said solution, at a temperature below about 140° C.; (2) cooling the resulting reaction mixture to a temperature below about 110° C. without precipitating titanyl sulfate to produce a reaction mixture containing dissolved titanyl sulfate; (3) diluting the reaction mixture containing titanyl sulfate with a sufficient amount of a diluent material selected from the group consisting of water, titanyl sulfate solution, and mixtures thereof to produce a reaction mixture having the following properties in the absence of undissolved solids, an iron to titanium dioxide weight ratio of about 0.7-1.1:1.0, a titanium dioxide content of about 120 to about 180 grams per liter, a specific gravity of about 1.4 to about 1.8, and an active sulfuric acid to titanium dioxide mole ratio of about 1.4-1.9:1.0; (4) separating undissolved solids from the reaction mixture to provide a solution of iron sulfate and titanyl sulfate; (5) removing iron sulfate from said solution of iron sulfate and titanyl sulfate to produce a solution of titanyl sulfate; (6) hydrolyzing said titanyl sulfate to provide a titanium dioxide hydrate, and spent sulfuric acid solution; (7) calcining said titanium dioxide hydrate to provide titanium dioxide; and (8) recovering titanium dioxide.
Claim 7
Dependent Claim 262 words
A process for producing titanium dioxide from a titanyl sulfate solution, which comprises: (1) reacting a titaniferous bearing material in an amount between about 10% and about 400% above the stoichiometric amount of titaniferous bearing material necessary to react with sulfuric acid to provide titanyl sulfate with a dilute sulfuric acid solution having a concentraton between about 25% and about 60% by weight, based upon the total weight of said solution, at a temperature below about 140° C.; (2) cooling the resulting reaction mixture to a temperature below about 110° C. without precipitating titanyl sulfate to produce a reaction mixture containing dissolved titanyl sulfate; (3) diluting the reaction mixture containing titanyl sulfate with a sufficient amount of a diluent material selected from the group consisting of water, titanyl sulfate solution, and mixtures thereof to produce a reaction mixture having the following properties in the absence of undissolved solids, an iron to titanium dioxide weight ratio of about 0.7-1.1:1.0, a titanium dioxide content of about 120 to about 180 grams per liter, a specific gravity of about 1.4 to about 1.8, and an active sulfuric acid to titanium dioxide mole ratio of about 1.4-1.9:1.0; (4) separating undissolved solids from the reaction mixture to provide a solution of iron sulfate and titanyl sulfate; (5) removing iron sulfate from said solution of iron sulfate and titanyl sulfate to produce a solution of titanyl sulfate; (6) hydrolyzing said titanyl sulfate to provide a titanium dioxide hydrate, and spent sulfuric acid solution; (7) calcining said titanium dioxide hydrate to provide titanium dioxide; and (8) recovering titanium dioxide.
Claim 8
Dependent Claim 48 words
The process of claim 5 wherein the titanyl sulfate solution employed for diluting the reaction mixture is a titanyl sulfate solution recovered after removing ferrous sulfate but prior to hydrolyzing said titanyl sulfate solution, said diluent having a weight ratio of iron to titanium dioxide less than 0.4:1.0.
Claim 9
Dependent Claim 16 words
The process of claim 5 wherein the dilution is performed prior to separating the undissolved solids.
Claim 10
Dependent Claim 39 words
The process of claim 5 wherein the dilution is performed by using said diluent materials at a temperature less than the temperature of the reaction mixture to inhibit hydrolytic nucleation of the titanyl sulfate present in the reaction mixture.

References Cited (Backward Citations)

US1338473A Cited
US1504671A Cited
US1504669A Cited
US1504670A Cited
US2617724A Cited
US3071439A Cited
US3760058A Cited
US3647414A 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) 1984-06-22 1984-12-22 1985-06-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-06-22 1988-12-22 1989-06-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-06-22 1992-12-22 1993-06-23 $7700.00 Window Closed / Lapsed

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