Patent US3922240A successfully refreshed from Google Patents.
US3922240A
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Process for the production of pourable, pulverulent rubber-filler mixtures
Assignee: Huels AG
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Filing: 1974-05-17
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Granted: 1975-11-25
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Expires: 1994-05-17
Abstract
Abstract In a process for preparing discrete, finely divided, tack-free, pourable, powdery, filler-containing elastomer particles, optionally containing mineral oil plasticizer, by combining an aqueous suspension of a filler with a solution of elastomer dissolved in a volatile, inert organic solvent having a boiling point below 100*C, converting the unstable mixture thereby produced into a stable emulsion and precipitating and drying the mixture wherein a solid filler is suspended in water, a solution of elastomer, is introduced into this suspension with the formation of an unstable pseudo-emulsion, this unstable pseudoemulsion is converted into a stable, aqueous emulsion by the addition of a combination of a quaternary ammonium salt surfactant with a non-ionic, water-soluble, protective colloid, while stirring, this stable emulsion is introduced into an aqueous alkali silicate solution containing 2-20 moles of SiO2 per mole of said quaternary ammonium salt while maintaining said silicate solution at a pH of 7-14, and the filler containing elastomer is precipitated in a finely divided form with simultaneous removal by distillation of the elastomer solvent and is separated from water and dried.
Inventors
- 👤 Gerhard Berg
- 👤 Karl-Heinz Nordsiek
- 👤 Egge Barnstedt
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 19:47
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/20; C08J3/205; C08J3/21; C08J3/215; C08J2321/00
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
148 words
IN A PROCESS FOR PREPARING DISCRETE, FINELY DIVIDED, TACKFREE, POURABLE, POWDERY, FILLER-CONTAINING ELASTOMER PARTICLES FROM AN ADMIXTURE OF (A) AN AQUEOUS ELASTOMER EMULSION COMPRISING (I) A SOLUTION OF VULCANIZABLE ELASTOMER DISSOLVED IN A VOLATILE, INERT ORGANIC SOLVEN, (II) AN ELASTOMER EMULSIFYING AMOUNT OF QUATERNARY AMMONIUM SALT CATIONIC SURFACTANT AND (III) WATER; AND (B) AN AQUEOUS SUSPENSION OR DISPERSION OF A SOLID, FINELY DIVIDED ELASTOMER FILLER, WHICH PROCESS COMPRISES GRADUALLY INTRODUCING SAID ADMIXTURE INTO AN AQUEOUS ALKALI SILICATE SOLUTION CONTAINING 0.5-20 MOLES OF SIO2 PER MOLE OF SAID QUATERNARY AMMONIUM SALT WHILE MAINTAINING SAID SILICATE SOLUTION AT PH OF 7-14 AND SIMULTANEOUSLY EVAPORATING SAID VOLATILE ORGANIC SOLVENT TO FORM SAID FILLER-CONTAINING ELASTOMER PARTICLES, THE IMPROVEMENT WHICH COMPRISES: ADMIXING (I) AND (II) WITH (B) TO FORM AN UNSTABLE PSEUDOEMULSION AND CONVERTING THE RESULTANT PSEUDO-EMULSION INTO A STABLE EMULSION BY ADMIXING (II) AND A WATER SOLUBLE CELLULOSE DERIVATIVE PROTECTIVE COLLOID THEREWITH.
Claim 2
Dependent Claim
148 words
IN A PROCESS FOR PREPARING DISCRETE, FINELY DIVIDED, TACKFREE, POURABLE, POWDERY, FILLER-CONTAINING ELASTOMER PARTICLES FROM AN ADMIXTURE OF (A) AN AQUEOUS ELASTOMER EMULSION COMPRISING (I) A SOLUTION OF VULCANIZABLE ELASTOMER DISSOLVED IN A VOLATILE, INERT ORGANIC SOLVEN, (II) AN ELASTOMER EMULSIFYING AMOUNT OF QUATERNARY AMMONIUM SALT CATIONIC SURFACTANT AND (III) WATER; AND (B) AN AQUEOUS SUSPENSION OR DISPERSION OF A SOLID, FINELY DIVIDED ELASTOMER FILLER, WHICH PROCESS COMPRISES GRADUALLY INTRODUCING SAID ADMIXTURE INTO AN AQUEOUS ALKALI SILICATE SOLUTION CONTAINING 0.5-20 MOLES OF SIO2 PER MOLE OF SAID QUATERNARY AMMONIUM SALT WHILE MAINTAINING SAID SILICATE SOLUTION AT PH OF 7-14 AND SIMULTANEOUSLY EVAPORATING SAID VOLATILE ORGANIC SOLVENT TO FORM SAID FILLER-CONTAINING ELASTOMER PARTICLES, THE IMPROVEMENT WHICH COMPRISES: ADMIXING (I) AND (II) WITH (B) TO FORM AN UNSTABLE PSEUDOEMULSION AND CONVERTING THE RESULTANT PSEUDO-EMULSION INTO A STABLE EMULSION BY ADMIXING (II) AND A WATER SOLUBLE CELLULOSE DERIVATIVE PROTECTIVE COLLOID THEREWITH.
Claim 3
Dependent Claim
49 words
A process according to claim 1, wherein the quaternary ammonium salt surfactant is a compound of the formula (NR1R2R3R4) X wherein R1, R2, R3 and R4 are each alkyl of 1-20 carbon atoms or aralkyl of 6-20 carbon atoms and X is chlorine, bromine, sulfate or lower alkyl sulfate.
Claim 4
Dependent Claim
27 words
A process according to claim 1, wherein the protective colloid is a water-soluble cellulose derivative selected from the group consisting of methylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, hydroxyethylmethylcellulose and carboxymethylcellulose.
Claim 5
Dependent Claim
25 words
A process according to claim 2, wherein the quaternary ammonium salts are utilized in an amount of 0.01-2.0% by weight based on the elastomer solution.
Claim 6
Dependent Claim
40 words
A process according to claim 2, wherein the quaternary ammonium salt is selected from the group consisting of lauryldimethylbenzylammonium chloride, cetyltrimethylammonium bromide, lauryldimethylethylammonium ethyl sulfate, alkyl (C12 to C16)-trimethylammonium bromide, coconut-dimethylbenzyl-ammonium chloride, cetyldimethylbenzylammonium chloride, cetyldimethylethylammonium ethyl sulfate and distearyldimethyl-ammonium chloride.
Claim 7
Dependent Claim
27 words
A process according to claim 3, wherein the watersoluble cellulose derivative is used in amounts of between 0.001 and 0.5% by weight based on the elastomer solution.
Claim 8
Dependent Claim
24 words
A process according to claim 1, wherein the elastomer is a polybutadiene having a vinyl group content of 8-60% obtained by lithium-based catalyst polymerization.
Claim 9
Dependent Claim
22 words
A process according to claim 7, wherein the polybutadiene is obtained by adiabatic polymerization and has a vinyl group content of 25-60%.
Claim 10
Dependent Claim
41 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 11
Dependent Claim
19 words
A process according to claim 9, wherein the copolymer is one obtained by adiabatic polymerization of butadiene and styrene.
Claim 12
Dependent Claim
23 words
A process according to claim 10, wherein the elastomer is a block copolymer of butadiene with up to 60% by weight of styrene.
Claim 13
Dependent Claim
23 words
A process according to claim 9, wherein the elastomer is a random copolymer of butadiene with up to 40% by weight of styrene.
Claim 14
Dependent Claim
15 words
A process according to claim 1, wherein the elastomer is an EPM or EPDM copolymer.
Claim 15
Dependent Claim
17 words
A process according to claim 1, wherein the pH of the stable filler-water-elastomer solution emulsion is 3-7.
Claim 16
Dependent Claim
27 words
A process according to claim 1, characterized in that the precipitant employed is an aqueous sodium silicate solution in molar ratios of Na2O:SiO2 of 2:1 to 1:4.
Claim 17
Dependent Claim
15 words
A process according to claim 1, further comprising adding vulcanization ingredients to the stable emulsion.
Claim 18
Dependent Claim
17 words
A process according to claim 1, further comprising adding a mineral oil plasticizer to the stable emulsion.
References Cited (Backward Citations)
US3846365A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-11-24 | 1979-05-26 | 1979-11-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-11-24 | 1983-05-26 | 1983-11-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-11-24 | 1987-05-26 | 1987-11-25 | $7700.00 | Window Closed / Lapsed |