US3929707A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for the production of pourable, pulverulent rubber-filler mixtures
Assignee: Huels AG
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Filing: 1974-06-27
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Granted: 1975-12-30
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Expires: 1994-06-27
Abstract
Abstract In a process for preparing discrete, finely divided, tack-free, pourable, powdery, filler-containing elastomer particles from an admixture of (a) an aqueous elastomer emulsion comprising (i) a solution of elastomer dissolved in a volatile, inert organic solvent having a boiling point below 100*C, (ii) an elastomer emulsifying amount of an alkylamine oxyalkylate surfactant, and (iii) water; and (b) an aqueous suspension or dispersion of a solid, finely divided elastomer filler, which comprises gradually introducing said admixture into an aqueous alkali silicate solution containing 2-20 moles of SiO2 per mole of said alkylamine oxyalkylate while maintaining said silicate solution at an acidic pH of 0.1-7 and simultaneously evaporating said volatile organic solvent to form said filler-containing elastomer particles, the improvement which comprises: EMPLOYING SAID ADMIXTURE OF (A) AND (B) IN THE FORM OF A STABLE, AQUEOUS EMULSION CONTAINING AN EMULSION-STABILIZING AMOUNT OF AN IONIC, WATER SOLUBLE PROTECTIVE COLLOID AND HAVING AN ALKALINE PH of 7-14.
Inventors
- 👤 Gerhard Berg
- 👤 Karl-Heinz Nordsiek
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 21:15
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/20; C08J3/205; C08J3/21; C08J3/215; C08J2321/00
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
175 words
IN A PROCESS FOR PREPARING DICRETE, FINELY DIVIDED, TACK FREE, POURABLE, POWDERY, FILLER-CONTAINING ELASTOMER PARTICLE FROM AN ADMIXTURE OF (A) AN AQUEOUS ELASTOMER EMULSION COMPRISING (I) A SOLUTION OF ELASTOMER DISSOLVED IN A VOLATILE INERT ORGANIC SOLVENT HAVING A BOILING POINT BELOW 100*C, (II) AN ELASTOMER EMULSIFYING AMOUNT OF ABOUT 0.05-2% BY WEIGHT, BASED ON THE ELASTOMER SOLUTION, OF AN ALKYLAMINE OXYALKYLATE SURFACTANT, AND (III) WATER; AND (B) AN AQUEOUS SUSPENSION OR DISPERSION OF A SOLID, FINELY DIVIDED ELASTOMWER FILLER, WHICH COMPRISES GRADUALLY INTRODUCING SAID ADMIXTURE INTO AN AQUEOUS ALKALI SILICATE SOLUTION CONTAINING 2-20 MOLES OF SIO2 PER MOLE OF SAID ALKYLAMINE OXYALKYLATE WHILE MAINTAINING SAID SILICATE SOLUTION AT AN ACIDIC PH OF 0.1-7 AND SIMULTANEOUSLY EVAPORATING SAID VOLATILE ORGANIC SOLVENT TO FORM SAID FILLER-CONTAINING ELASTOMER PARTICLES, THE IMPROVEMENT WHICH COMPRISES: EMPLOYING SAID ADMIXTURE OF (A) AND (B) IN THE FORM OF A STABLE AQUEOUS EMULSION CONTAINING AN EMULSION-STABILIZING AMOUNT OF ABOUT 0.001-0.5% BY WEIGHT, BASED ON THE ELASTOMER SOLUTION, OF AN IONIC, WATER SOLUBLE PROTECTIVE COLLOID, SAID STABLE EMULSION HAVING AN ALKALINE PH OF
Claim 2
Dependent Claim
175 words
IN A PROCESS FOR PREPARING DICRETE, FINELY DIVIDED, TACK FREE, POURABLE, POWDERY, FILLER-CONTAINING ELASTOMER PARTICLE FROM AN ADMIXTURE OF (A) AN AQUEOUS ELASTOMER EMULSION COMPRISING (I) A SOLUTION OF ELASTOMER DISSOLVED IN A VOLATILE INERT ORGANIC SOLVENT HAVING A BOILING POINT BELOW 100*C, (II) AN ELASTOMER EMULSIFYING AMOUNT OF ABOUT 0.05-2% BY WEIGHT, BASED ON THE ELASTOMER SOLUTION, OF AN ALKYLAMINE OXYALKYLATE SURFACTANT, AND (III) WATER; AND (B) AN AQUEOUS SUSPENSION OR DISPERSION OF A SOLID, FINELY DIVIDED ELASTOMWER FILLER, WHICH COMPRISES GRADUALLY INTRODUCING SAID ADMIXTURE INTO AN AQUEOUS ALKALI SILICATE SOLUTION CONTAINING 2-20 MOLES OF SIO2 PER MOLE OF SAID ALKYLAMINE OXYALKYLATE WHILE MAINTAINING SAID SILICATE SOLUTION AT AN ACIDIC PH OF 0.1-7 AND SIMULTANEOUSLY EVAPORATING SAID VOLATILE ORGANIC SOLVENT TO FORM SAID FILLER-CONTAINING ELASTOMER PARTICLES, THE IMPROVEMENT WHICH COMPRISES: EMPLOYING SAID ADMIXTURE OF (A) AND (B) IN THE FORM OF A STABLE AQUEOUS EMULSION CONTAINING AN EMULSION-STABILIZING AMOUNT OF ABOUT 0.001-0.5% BY WEIGHT, BASED ON THE ELASTOMER SOLUTION, OF AN IONIC, WATER SOLUBLE PROTECTIVE COLLOID, SAID STABLE EMULSION HAVING AN ALKALINE PH OF
Claim 3
Dependent Claim
16 words
A process according to claim 1, wherein said stable aqueous emulsion has a pH of 10-13.
Claim 4
Dependent Claim
18 words
A process according to claim 1, wherein the protective colloid is present in component (a) of the admixture.
Claim 5
Dependent Claim
24 words
A process according to claim 1, wherein the ionic protective colloid is an alkali metal polyacrylate having a molecular weight of 100,000 to 2,000,000.
Claim 6
Dependent Claim
22 words
A process according to claim 3, wherein the protective colloid is a sodium polyacrylate having a molecular weight of 200,000 to 1,500,000.
Claim 7
Dependent Claim
26 words
A process according to claim 5, wherein the protective colloid is used in amounts of between 0.005 and 0.1% by weight, based on the elastomer solution.
Claim 8
Dependent Claim
20 words
A process according to claim 1, wherein the elastomer solution (i) has a solution viscosity of 40-40,000 centipoises at 25*C.
Claim 9
Dependent Claim
21 words
A process according to claim 6, wherein said elastomer solution has a dissolved elastomer content of 5 to 25% by weight.
Claim 10
Dependent Claim
23 words
A process according to claim 1, wherein the elastomer is a polybutadiene having a vinyl group content of 8-60% by lithium-based catalyst polymerization.
Claim 11
Dependent Claim
22 words
A process according to claim 9, wherein the polybutadiene is obtained by adiabatic polymerization and has a vinyl group content of 25-60%.
Claim 12
Dependent Claim
42 words
A process according to claim 1, wherein the elastomer is a copolymer of butadiene with up to 60% by weight of styrene produced in the presence of a lithium based pOlymerization catalyst, wherein 8-30% of the butadiene is bound in the 1,2-position.
Claim 13
Dependent Claim
19 words
A process according to claim 11, wherein the copolymer is one obtained by adiabatic polymerization of butadiene and styrene.
Claim 14
Dependent Claim
23 words
A process according to claim 12, wherein the elastomer is a block copolymer of butadiene with up to 60% by weight of styrene.
Claim 15
Dependent Claim
23 words
A process according to claim 11, wherein the elastomer is a random copolymer of butadiene with up to 40% by weight of styrene.
Claim 16
Dependent Claim
15 words
A process according to claim 1, wherein the elastomer is an EPM or EPDM copolymer.
Claim 17
Dependent Claim
15 words
A process according to claim 1, wherein the stable aqueous emulsion further comprises vulcanization ingredients.
Claim 18
Dependent Claim
17 words
A process according to claim 1, wherein the aqueous stable emulsion further comprises a mineral oil plasticizer.
Claim 19
Dependent Claim
17 words
A process according to claim 17, wherein the mineral oil plasticizer is adsorbed onto carbon black particles.
Claim 20
Dependent Claim
18 words
A process according to claim 1, wherein the alkylamine oxyalkylate is at least one compound of the formula
Claim 21
Dependent Claim
90 words
A stable aqueous elastomer emulsion composition having a pH of 10-13 and consisting essentially of a. 5-25% by weight of an elastomer having a viscosity of 40-40, 000 centipoises selected from the group consisting of EPM, EPDM and butadiene elastomers dissolved in a volatile inert solvent having a boiling point below 100*C; b. 0.05-2.0% by weight, based on the elastomer solution, of an alkylamine oxyalkylate surfactant; and c. 0.001-0.5% by weight, based on the elastomer solution, of a water-soluble sodium polyacrylate protective colloid having molecular weight of 200,000 - 1,500,000.
Claim 22
Dependent Claim
90 words
A stable aqueous elastomer emulsion composition having a pH of 10-13 and consisting essentially of a. 5-25% by weight of an elastomer having a viscosity of 40-40, 000 centipoises selected from the group consisting of EPM, EPDM and butadiene elastomers dissolved in a volatile inert solvent having a boiling point below 100*C; b. 0.05-2.0% by weight, based on the elastomer solution, of an alkylamine oxyalkylate surfactant; and c. 0.001-0.5% by weight, based on the elastomer solution, of a water-soluble sodium polyacrylate protective colloid having molecular weight of 200,000 - 1,500,000.
Claim 23
Dependent Claim
12 words
A composition according to claim 20, further comprising a carbon black filler.
Claim 24
Dependent Claim
12 words
A composition according to claim 21, further comprising a mineral oil plasticizer.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-12-29 | 1979-06-30 | 1979-12-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-12-29 | 1983-06-30 | 1983-12-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-12-29 | 1987-06-30 | 1987-12-30 | $7700.00 | Window Closed / Lapsed |