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US3840382A Expired / Lapsed US ⏱️ 0.0 years remaining

Silica pigment and elastomer-silica pigment masterbatches and production processes relating thereto

Assignee: Individual
•
Filing: 1972-07-17
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Granted: 1974-10-08
•
Expires: 1992-07-17
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Abstract

Abstract As indicated at (A) through (D-6) of the drawings, the invention first produces an aqueously wet silica pigment composition (D-1) which in the embodiments is treated with oleophilic material (B) and/or reactant (C). The so treated compositions (D-1) are suitable for masterbatching with elastomer in solvent dispersion (E)-(FIG. 1) or aqueous dispersion (E'')-(FIG. 2) with or without prior reduction or removal of free water (D-2). The silica pigment composition (D-2) is blended (at D-3) with carbon black pigment and/or processing oil (M) and, with adjusted water content, these combinations are formable into pigment beads (via D-4, D-5, D-6). The overall process curbs the losses of pigments in the masterbatching and promotes uniformity of product, The silica pigment compositions (D-1), and especially (D-3) when beaded, constitute pigment materials useful for the compounding of rubber.

Inventors

  • 👤 O Burke

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 16:28
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/20; C08J3/22; C08K; C08K3/00; C08K3/34; C08K3/36

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 179 words
A PROCESS FOR PREPARING PIGMENT COMPOSITION WHICH COMPRISES, IN COMBINATION: A. PROVIDING 10 WEIGHT PARTS, DRY BASIS, OF AQUEOUSLY WET HYDRATED SILICA PIGMENT PRECIPITATE WHICH HAS A BOUND ALKALI CONTENT IN THE RANGE OF 0.1 TO 10 PERCENT BY WEIGHT AS NA2O; WHICH HAS BEEN PREPARED BY PRECIPIPITATION FROM AN AQUEOUS SOLUTION OF ALKALI METAL SILICATE WITH THE AID OF CARBON DIOXIDE; AND WHICH HAS CONTINUOUSLY BEEN MAINTAINED IN AN AQUEOUSLY WET STATE WITHOUT HAVING BEEN DRIED THEREFROM AFTER ITS PRECIPITATION; B. PRIVIDING FROM 0.1 TO 2 WEIGHT PARTS, DRY BASIS, OF OLEOPHILIC MATERIAL SELECTED FROM THE CLASS CONSISTING OF THE MEMBERS OF THE FOLLOWING GROUPS: (1) THE OLEOPHILIC AMINES; (II) THE OLEOPHILIC CARBOXYLIC ACIDS AND THEIR ALKALI METAL AND AMMONIUM SALTS; (III) THE OLEOPHILIC CARBOXYLIC ACID SALTS OF ALUMINUM, ZINC, THE ALKALINE EARTH METALS, AND SUCH WITH AMONIUM HYDROXIDE; (IV) THE OLEOPHILIC AMINE CARBOXYLATES; (V) THE OLEOPHILIC QUATERNARY AMMONIUM COMPOUNDS, (Vi) THE OLEOPHILIC HYDROXY COMPOUNDS; (VII) THE COMBINATIONS OF 2 OR MORE MEMBERS OF THE FOREGOING GROUPS; AND FROM 0 TO 1 WEIGHT PART OF POLYOL DRY BASIS;
Claim 2
Dependent Claim 179 words
A PROCESS FOR PREPARING PIGMENT COMPOSITION WHICH COMPRISES, IN COMBINATION: A. PROVIDING 10 WEIGHT PARTS, DRY BASIS, OF AQUEOUSLY WET HYDRATED SILICA PIGMENT PRECIPITATE WHICH HAS A BOUND ALKALI CONTENT IN THE RANGE OF 0.1 TO 10 PERCENT BY WEIGHT AS NA2O; WHICH HAS BEEN PREPARED BY PRECIPIPITATION FROM AN AQUEOUS SOLUTION OF ALKALI METAL SILICATE WITH THE AID OF CARBON DIOXIDE; AND WHICH HAS CONTINUOUSLY BEEN MAINTAINED IN AN AQUEOUSLY WET STATE WITHOUT HAVING BEEN DRIED THEREFROM AFTER ITS PRECIPITATION; B. PRIVIDING FROM 0.1 TO 2 WEIGHT PARTS, DRY BASIS, OF OLEOPHILIC MATERIAL SELECTED FROM THE CLASS CONSISTING OF THE MEMBERS OF THE FOLLOWING GROUPS: (1) THE OLEOPHILIC AMINES; (II) THE OLEOPHILIC CARBOXYLIC ACIDS AND THEIR ALKALI METAL AND AMMONIUM SALTS; (III) THE OLEOPHILIC CARBOXYLIC ACID SALTS OF ALUMINUM, ZINC, THE ALKALINE EARTH METALS, AND SUCH WITH AMONIUM HYDROXIDE; (IV) THE OLEOPHILIC AMINE CARBOXYLATES; (V) THE OLEOPHILIC QUATERNARY AMMONIUM COMPOUNDS, (Vi) THE OLEOPHILIC HYDROXY COMPOUNDS; (VII) THE COMBINATIONS OF 2 OR MORE MEMBERS OF THE FOREGOING GROUPS; AND FROM 0 TO 1 WEIGHT PART OF POLYOL DRY BASIS;
Claim 3
Dependent Claim 17 words
A process as claimed in claim 1, wherein g. following step (f) the pigment composition is dried.
Claim 4
Dependent Claim 19 words
A process as claimed in claim 1, wherein g. following step (f) the pigment composition is beaded and dried.
Claim 5
Dependent Claim 81 words
A process as claimed in claim 3, wherein step (f) is practiced in two parts, the pigment from one part of step (f) being supplied to step (g) in the still aqueously wet state, and the pigment from the other part of step (f) being at least partially dried and being supplied to step (g) in such dried state, the weight ratio of the wet and dried silica pigments being such as to provide a sufficient quantity of water for beading.
Claim 6
Dependent Claim 256 words
A pigment composition consisting essentially of the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated silica pigment, prior to its incorporation in the composition having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more membErs of the foregoing groups; c. from 0 to 1 weight part, dry basis, of polyol; d. from 0 to 150 weight parts of carbon black; and e. from 0 to 45 percent, based on the total of (c) and (d), of processing oil.
Claim 7
Dependent Claim 256 words
A pigment composition consisting essentially of the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated silica pigment, prior to its incorporation in the composition having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more membErs of the foregoing groups; c. from 0 to 1 weight part, dry basis, of polyol; d. from 0 to 150 weight parts of carbon black; and e. from 0 to 45 percent, based on the total of (c) and (d), of processing oil.
Claim 8
Dependent Claim 14 words
A pigment composition as claimed in claim 5, said composition being in beaded form.
Claim 9
Dependent Claim 258 words
A wet pigment composition consisting essentially of the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of aqueously wet hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated pigment, prior to its incorporation in the composition, having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, and the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; c. from 0 to 1 weight part of polyol dry basis; d. from 0 to 150 parts of carbon black; and e. from 0 to 45 percent, based on the total of (c) and (d), of processing oil.
Claim 10
Dependent Claim 258 words
A wet pigment composition consisting essentially of the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of aqueously wet hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated pigment, prior to its incorporation in the composition, having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, and the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; c. from 0 to 1 weight part of polyol dry basis; d. from 0 to 150 parts of carbon black; and e. from 0 to 45 percent, based on the total of (c) and (d), of processing oil.
Claim 11
Dependent Claim 300 words
A process for preparing pigment composition which comprises, in combination: a. providing 10 weight parts, dry basis, of aqueously wet hydrated silica pigment precipitate which has a bound alkali content in the range of 0.1 to 10 percent by weight as Na2O; which has been prepared by precipitation from an aqueous solution of alkali metal silicate with the aid of carbon dioxide; and which has continuously been maintained in an aqueously wet state without having been dried therefrom after its precipitation; b. providing from 0.1 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; and from 0 to 1 weight part of polyol dry basis; c. providing from 0 to 30 weight parts, dry basis, of carbon black; d. providing from 0 to 16 weight parts of processing oil; e. replacing from 0 to 100 percent of the alkalinity of the wet pigment provided in (a) by reaction with reactant selected from the class consisting of members of the following groups: Group (I) the water soluble salts of ammonium or zinc; Group (II) the water soluble salts of alkaline earth metals; Group (III) the water soluble acids; Group (IV) combinations of 2 or more members selected from Groups (I), (II) or (III); and f. combining the pigment providing by step (e) with the material provided by steps (b), (c) and (d) to provide tHe pigment composition.
Claim 12
Dependent Claim 300 words
A process for preparing pigment composition which comprises, in combination: a. providing 10 weight parts, dry basis, of aqueously wet hydrated silica pigment precipitate which has a bound alkali content in the range of 0.1 to 10 percent by weight as Na2O; which has been prepared by precipitation from an aqueous solution of alkali metal silicate with the aid of carbon dioxide; and which has continuously been maintained in an aqueously wet state without having been dried therefrom after its precipitation; b. providing from 0.1 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; and from 0 to 1 weight part of polyol dry basis; c. providing from 0 to 30 weight parts, dry basis, of carbon black; d. providing from 0 to 16 weight parts of processing oil; e. replacing from 0 to 100 percent of the alkalinity of the wet pigment provided in (a) by reaction with reactant selected from the class consisting of members of the following groups: Group (I) the water soluble salts of ammonium or zinc; Group (II) the water soluble salts of alkaline earth metals; Group (III) the water soluble acids; Group (IV) combinations of 2 or more members selected from Groups (I), (II) or (III); and f. combining the pigment providing by step (e) with the material provided by steps (b), (c) and (d) to provide tHe pigment composition.
Claim 13
Dependent Claim 27 words
A process as claimed in claim 8, wherein the quantities provided in steps (c) and (d) are respectively 0 parts and at least 5 parts by weight.
Claim 14
Dependent Claim 247 words
A pigment composition incorporating the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated silica pigment, prior to its incorporation in the composition having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; c. from 0 to 1 weight part, dry basis, of polyol; d. from 0 to 30 weight parts of carbon black; and e. from 0 to 16 weight parts of processing oil.
Claim 15
Dependent Claim 247 words
A pigment composition incorporating the following components, dry basis by weight, distributed throughout the composition: a. 10 weight parts, dry basis, of hydrated silica pigment which has been prepared by precipitation from an aqueous alkali metal silicate solution with the aid of carbon dioxide, said hydrated silica pigment, prior to its incorporation in the composition having had from 0 to 100 percent of its alkalinity replaced by reaction with reactant material selected from the class consisting of the members of the following groups: Group (I) the water soluble salts of aluminum or zinc; Group (II) the water soluble salts of the alkaline earth metals; Group (III) the water soluble acids; and Group (IV) combinations of 2 or more members selected from Groups (I), (II) and (III) of this class; b. from 0.01 to 2 weight parts, dry basis, of oleophilic material selected from the class consisting of the members of the following groups: (I) the oleophilic amines; (II) the oleophilic carboxylic acids and their alkali metal and ammonium salts; (III) the oleophilic carboxylic acid salts of aluminum, zinc, the alkaline earth metals, and such with ammonium hydroxide; (IV) the oleophilic amine carboxylates; (V) the oleophilic quaternary ammonium compounds; (VI) the oleophilic hydroxy compounds; (VII) the combinations of 2 or more members of the foregoing groups; c. from 0 to 1 weight part, dry basis, of polyol; d. from 0 to 30 weight parts of carbon black; and e. from 0 to 16 weight parts of processing oil.
Claim 16
Dependent Claim 26 words
A pigment composition as claimed in claim 10, the quantities of components (d) and (e) being respectively 0 parts and at least 5 parts, by weight.

References Cited (Backward Citations)

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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) 1977-10-07 1978-04-08 1978-10-08 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-10-07 1982-04-08 1982-10-08 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-10-07 1986-04-08 1986-10-08 $7700.00 Window Closed / Lapsed

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