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US3635671A Expired / Lapsed US ⏱️ 0.0 years remaining

Continuous preparation of titanium dioxide seed suspensions

Assignee: Dow Chemical Co
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Filing: 1970-05-07
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Granted: 1972-01-18
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Expires: 1990-05-07
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Abstract

Abstract A continuous process is provided for preparing an opalescent seed suspension of colloidal TiO2 particles, i.e. seed suspension. In this method a stream of an aqueous feed solution having certain chloride, titanium, hydrogen and multivalent ion concentrations is conducted through a heating zone where it is heated to a temperature of between 80* to 125* C. and then the stream is continuously conducted through a reaction zone while maintaining the temperature of the stream within said range. The total period of time (reaction time) during which the stream is maintained within said temperature range is from about 1 to about 30 minutes. The heating and reaction zones are designed and the flow rate of the stream is controlled to prevent back mixing of portions of the flowing stream which differ substantially as to the degree of reaction attained therein.

Inventors

  • 👤 Elmer C Tveter

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 13:27
CPC Classifications
B; B82; B82Y; B82Y30/00; C; C01; C01G; C01G23/00; C01G23/04; C01G23/047; C01G23/053; C01G23/0536; C01P; C01P2004/00; C01P2004/60; C01P2004/64; C01P2006/00; C01P2006/60

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 22 words
The process as defined in claim 1 wherein the titanium dioxide particles range in size from about 0.002 to about 0.020 micron.
Claim 2
Dependent Claim 28 words
The process as defined in claim 1 wherein the titanium concentration in said stream of aqueous feed solution ranges from about 0.3 to about 0.42 gram-atoms per liter.
Claim 3
Dependent Claim 39 words
The process as defined in claim 1 wherein said hydrogen concentration in said stream of aqueous feed solution is such that twice the titanium concentration plus the hydrogen concentration ranges from about 0.36 to about 0.6 gram-atoms per liter.
Claim 4
Dependent Claim 45 words
The process as defined in claim 1 wherein the stream of aqueous feed solution is heated to a temperature of from about 85* to about 100* C. and maintained at said temperature for from about 5 to about 20 minutes to form said seed suspension.
Claim 5
Dependent Claim 216 words
A continuous process for preparing an opalescent seed suspension of colloidal titanium dioxide particles which comprises: a. heating a stream of an aqueous feed solution having a titanium concentration at the maximum of about 0.6 gram-atoms per liter, a chloride to titanium gram-mole ratio of at least 1.8, a hydrogen concentration such that twice the titanium concentration plus the hydrogen concentration at the maximum is about 1.2 gram-atoms per liter and not more than 0.1 gram-atoms per liter of multivalent anions to a temperature of from about 80* C. to about 125* C. while flowing said stream upwardly in laminar flow, said flow characterized as having a Reynolds number of less than about 2,100, through a substantially vertical heating zone to form a heated feed solution; b. conducting the flowing stream of heated solution at a temperature of from about 80* to about 125* C. through a reaction zone, said stream being maintained at said temperature for a total period of from about 1 to about 30 minutes, at a flow rate adjusted to prevent bulk back-mixing of reacted portions of the flowing stream containing titanium dioxide particles with the unreacted portion of the flowing stream which does not contain said titanium dioxide particles; and c. continuously removing said titanium dioxide particles from said reaction zone.
Claim 6
Dependent Claim 93 words
The process as defined in claim 6 wherein said stream of heated feed solution from said heating zone is conducted at a temperature not greater than the temperature of the stream from the heating zone downwardly in laminar flow through a substantially vertical reaction zone to form said seed suspension said reaction zone being characterized as designed to prevent bulk back-mixing of portions of the stream which differ substantially as to the degree of reaction attained therein and said laminar flow is characterized as having a Reynolds number of less than about 2,100.
Claim 7
Dependent Claim 80 words
The process as defined in claim 6 wherein said stream of heated feed solution is conducted at said temperature through a reaction zone having a sufficiently restricted cross-sectional area such that at the volume flow rate of the stream turbulent flow characterized as having a Reynolds number of greater than about 2,100 results, thereby forming said seed suspension while preventing bulk back-mixing of portions of said stream differing substantially as to the degree of completion of the reaction attained therein.
Claim 8
Dependent Claim 38 words
The process as defined in claim 1 including continuously mixing a stream of a concentrated aqueous solution with a stream of water in a mixing zone in turbulent flow in proportions required to form said aqueous feed solution.
Claim 9
Dependent Claim 34 words
The process as defined in claim 9 wherein said concentrated aqueous feed solution contains at least about 4.2 gram-atoms per liter of titanium and a chloride to titanium gram-mole ratio of at least 2.
Claim 10
Dependent Claim 190 words
A continuous process for preparing an opalescent seed suspension of colloidal titanium dioxide particles which comprises: a. mixing a stream of concentrated aqueous solution, containing at least about 4.2 gram-atoms per liter of titanium and a chloride to titanium gram-mole ratio of at least 2 and having a temperature of less than about 70* C., with a sufficient quantity of a stream of water having a temperature of from about 80* to 140* C. to provide a heated flowing stream of aqueous feed solution having a temperature of from about 80* to about 125* C., the flow of said stream being characterized by an average Reynolds number of greater than about 2,100; b. conducting said heated stream at said temperature through a reaction zone, said stream being maintained at said temperature for a total period of from about 1 to about 30 minutes, at a flow rate adjusted to prevent bulk back-mixing of reacted portions of the flowing stream containing titanium dioxide particles with the unreacted portion of the flowing stream which does not contain said titanium dioxide particles; and c. continuously removing said seed suspension from said reaction zone.
Claim 11
Dependent Claim 205 words
A continuous process for preparing an opalescent seed suspension of colloidal titanium dioxide particles which comprises: a. heating a stream of an aqueous feed solution having a titanium concentration at the maximum of about 0.6 gram-atoms per liter, a chloride to titanium gram-mole ratio of at least 1.8, a hydrogen concentration such that twice the titanium concentration plus the hydrogen concentration at the maximum is about 1.2 gram-atoms per liter and not more than 0.1 gram-atoms per liter of multivalent anions, by flowing said stream through a heating zone in turbulent flow, said flow characterized as having a Reynolds number of greater than about 2,100, to a temperature of from about 80* to about 125* C; b. conducting the flowing stream of heated solution at a temperature of from about 80* to about 125* C. through a reaction zone, said stream being maintained at said temperature for a total period of from about 1 to about 30 minutes, at a flow rate adjusted to prevent bulk back-mixing of reacted portions of the flowing stream containing titanium dioxide particles with the unreacted portion of the flowing stream which does not contain said titanium dioxide particles; and c. continuously removing said seed suspension from said reaction zone.
Claim 12
Dependent Claim 54 words
The process as defined in claim 11 wherein the heated stream of aqueous feed solution is flowed downwardly in laminar flow characterized as having a Reynolds number of less than about 2,100 through a substantially vertical reaction zone, while maintained at a temperature not greater than the temperature thereof when entering the reaction zone.
Claim 13
Dependent Claim 64 words
The process as defined in claim 12 wherein said stream of heated feed solution at said temperature is conducted through said reaction zone in turbulent flow characterized as having a Reynolds number of greater than about 2,100 so that back-mixing of portions of the flowing stream which differ substantially as to the degree of reaction attained therein is avoided, thereby forming said seed suspension.
Claim 14
Dependent Claim 71 words
The process as defined in claim 12 wherein said stream of heated reaction solution at said temperature is conducted downwardly in laminar flow characterized as having a Reynolds number of less than about 2,100 through a substantially vertical reaction zone to form said seed suspension, said reaction zone being designed to prevent bulk back-mixing of portions of the flowing stream which differ substantially as to the degree of reaction attained therein.

References Cited (Backward Citations)

US1758528A Cited
US2337215A Cited
US2285486A Cited
US2480869A Cited
US2452390A Cited
US2511218A Cited
US2519389A Cited
US3329484A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1975-01-17 1975-07-19 1976-01-18 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1979-01-17 1979-07-19 1980-01-18 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1983-01-17 1983-07-19 1984-01-18 $7700.00 Window Closed / Lapsed

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