US4275041A
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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
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 02:09
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.
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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 |