US4138375A
Expired / Lapsed
US
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Process for the production of pulverulent, pourable elastomer-filler mixtures optionally containing plasticizer oil
Assignee: Huels AG
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Filing: 1977-11-30
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Granted: 1979-02-06
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Expires: 1997-11-30
Abstract
Abstract Pourable elastomer-filler mixtures, optionally containing plasticizer oil, are prepared by an improved process, the process comprising mixing an aqueous emulsion of an elastomer solution with an aqueous dispersion of a filler(s); introducing this mixture into water containing a precipitant(s); precipitating the elastomer-filler mixture while simultaneously removing the elastomer solvent by distillation; separating the thus-precipitated elastomer-filler mixture from the water; and drying the elastomer mixture under constant agitation; and the improvement comprising:
Inventors
- 👤 Gerhard Berg, deceased
- 👤 Karl-Heinz Nordsiek
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 03:52
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/20; C08J3/205; C08J3/21; C08J3/215; C08J2321/00
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
298 words
In a process for the production of pulverulent, pourable elastomer-filler mixtures, optionally containing plasticizer oil, by mixing an aqueous emulsion of an elastomer solution with an aqueous dispersion of filler; introducing this mixture into water containing a precipitant; precipitating the elastomer-filler mixture while simultaneously removing the elastomer solvent by distillation; separating the thus-precipitated elastomer-filler mixture from the water; and drying the elastomer mixture under continuous agitation; the improvement which comprises: emulsifying the elastomer solution in water in the presence of: (a) 0.01-1.0% by weight of an anionic emulsifier, based on the amount of the elastomer solution; (b) 0.001-0.1% by weight of an ionic protective colloid, based on the amount of the elastomer solution; and (c) 0.001-0.1% by weight of a nonionic protective colloid, based on the amount of the elastomer solution; combining the thus-stabilized solution-emulsion with an aqueous dispersion of filler, said dispersion having a pH of > 7, and containing 0.01-5% by weight, based on the amount of filler, of a tenside or a mixture of tensides, which when combined with components (a) through (c) of the elastomer emulsion do not result in a reduction of the surface activity of either the components (a) through (c) or the tensides, to obtain a homogeneous mixture stable with respect to storage and agitation; and introducing this mixture into a precipitating bath, the pH of which is set at 1.0-5.0 by the addition of precipitants selected from acids, metallic salts subject to acidic hydrolysis in water and mixtures thereof, the temperature of which is above the azeotropic boiling point of the elastomer solvent and water, and which contains an amount of sodium silicate, based on the total elastomer content, such that, at the pH values of the precipitating bath, 0.001-20% by eight of colloidally dissolved silicic acid is produced therefrom.
Claim 2
Dependent Claim
298 words
In a process for the production of pulverulent, pourable elastomer-filler mixtures, optionally containing plasticizer oil, by mixing an aqueous emulsion of an elastomer solution with an aqueous dispersion of filler; introducing this mixture into water containing a precipitant; precipitating the elastomer-filler mixture while simultaneously removing the elastomer solvent by distillation; separating the thus-precipitated elastomer-filler mixture from the water; and drying the elastomer mixture under continuous agitation; the improvement which comprises: emulsifying the elastomer solution in water in the presence of: (a) 0.01-1.0% by weight of an anionic emulsifier, based on the amount of the elastomer solution; (b) 0.001-0.1% by weight of an ionic protective colloid, based on the amount of the elastomer solution; and (c) 0.001-0.1% by weight of a nonionic protective colloid, based on the amount of the elastomer solution; combining the thus-stabilized solution-emulsion with an aqueous dispersion of filler, said dispersion having a pH of > 7, and containing 0.01-5% by weight, based on the amount of filler, of a tenside or a mixture of tensides, which when combined with components (a) through (c) of the elastomer emulsion do not result in a reduction of the surface activity of either the components (a) through (c) or the tensides, to obtain a homogeneous mixture stable with respect to storage and agitation; and introducing this mixture into a precipitating bath, the pH of which is set at 1.0-5.0 by the addition of precipitants selected from acids, metallic salts subject to acidic hydrolysis in water and mixtures thereof, the temperature of which is above the azeotropic boiling point of the elastomer solvent and water, and which contains an amount of sodium silicate, based on the total elastomer content, such that, at the pH values of the precipitating bath, 0.001-20% by eight of colloidally dissolved silicic acid is produced therefrom.
Claim 3
Dependent Claim
40 words
The improvement of claim 1, wherein the elastomer solution is a solution of polybutadiene, a polyisoprene, copolymers of butadiene and styrene, EPM or EPDM polymers produced of solution polymerization, polyalkenamers produced by the ring-opening polymerization of cycloolefins or mixtures thereof.
Claim 4
Dependent Claim
27 words
The improvement of claim 2 wherein the elastomer solution is a solution of a polybutadiene or a copolymer of butadiene and styrene dissolved in an aliphatic solvent.
Claim 5
Dependent Claim
29 words
The improvement of claim 3, wherein the elastomer solution is a solution of polybutadiene or a copolymer of butadiene and styrene each having a vinyl group content of 10-70%.
Claim 6
Dependent Claim
30 words
The improvement of claim 4, wherein the elastomer solution is a solution of a polybutadiene or a copolymer of butadiene and styrene each having a vinyl group content of 20-60%.
Claim 7
Dependent Claim
31 words
The improvement of claim 1, wherein the anionic emulsifier (a) is present in the elastomer emulsion in an amount of 0.05-0.5% by weight, based on the amount of the elastomer solution.
Claim 8
Dependent Claim
31 words
The improvement of claim 1, wherein the anionic emulsifier (a) is an alkali metal salt of saturated or unsaturated C 12 - to C 18 -fatty acids or aromatic sulfonic acids.
Claim 9
Dependent Claim
32 words
The improvement of claim 1, wherein the ionic protective colloid (b) is present in the elastomer emulsion in an amount of 0.004-0.05% by weight, based on the amount of the elastomer solution.
Claim 10
Dependent Claim
15 words
The improvement of claim 1, wherein the ionic protective colloid (b) is a sodium polyacrylate.
Claim 11
Dependent Claim
15 words
The improvement of claim 9, wherein the sodium polyacrylate has a molecular weight of 100,000-2,000,000.
Claim 12
Dependent Claim
15 words
The improvement of claim 10, wherein the sodium polyacrylate has a molecular weight of 250,000-1,500,000.
Claim 13
Dependent Claim
32 words
The improvement of claim 1, wherein the nonionic protective colloid (c) is present in the elastomer emulsion in an amount of 0.004-0.05% by weight, based on the amount of the elastomer solution.
Claim 14
Dependent Claim
15 words
The improvement of claim 1, wherein the nonionic protective colloid (c) is a cellulose derivative.
Claim 15
Dependent Claim
17 words
The improvement of claim 13, wherein the nonionic protective colloid (c) is methylcellulose, carboxymethylcellulose, or a Tylose.
Claim 16
Dependent Claim
18 words
The improvement of claim 1, wherein the filler is carbon black, a mineral filler or a mixture thereof.
Claim 17
Dependent Claim
18 words
The improvement of claim 15, wherein the mineral filler is highly active silicic acid, kaolin, or ground slate.
Claim 18
Dependent Claim
43 words
The improvement of claim 15 wherein the amount of mineral filler in the mixture of elastomer emulsion and filler dispersion is between 20% by weight based on the weight of elastomer and 500 parts by weight per 100 parts by weight of elastomer.
Claim 19
Dependent Claim
43 words
The improvement of claim 17, wherein the amount of mineral filler in the mixture of elastomer emulsion and filler dispersion is between 30% by weight based on the weight of elastomer and 150 parts by weight per 100 parts by weight of elastomer.
Claim 20
Dependent Claim
43 words
The improvement of claim 1, wherein the amount of carbon black in the mixture of elastomer emulsion and filler dispersion is 20% by weight based on the weight of the elastomer to 400 parts by weight per 100 parts by weight of elastomer.
Claim 21
Dependent Claim
43 words
The improvement of claim 19, wherein the amount of carbon black in the mixture of elastomer emulsion and filler dispersion is 40% by weight based on the weight of the elastomer to 110 parts by weight per 100 parts by weight of elastomer.
Claim 22
Dependent Claim
21 words
The improvement of claim 1, wherein the filler dispersion contains 0.01-5% by weight, of tenside based on the quantity of filler.
Claim 23
Dependent Claim
33 words
The improvement of claim 1, wherein the precipitant is a water-soluble salt of a metal of Main Groups II or III, or Subgroups II or VIII of the Periodic Table of the Elements.
Claim 24
Dependent Claim
15 words
The improvement of claim 22, wherein a water-soluble aluminum salt is employed as the precipitant.
Claim 25
Dependent Claim
32 words
The improvement of claim 1, wherein the amount of silicic acid introduced into the precipitating bath by addition of sodium silicate is 1-10% by weight, based on the total amount of elastomer.
Claim 26
Dependent Claim
30 words
The improved process of claim 1, which further comprises adjusting the pH of the precipitating bath ot 5-9 after the precipitation of the elastomer-filler mixture and before the separation thereof.
Claim 27
Dependent Claim
13 words
The pulverulent, pourable elastomer-filler mixture prepared by the improved process of claim 1.
Claim 28
Dependent Claim
28 words
A method of preparing shaped rubber articles which comprises preparing a blend of elastomer and filler by the process of claim 1 and molding or extruding the blend.
Claim 29
Dependent Claim
18 words
A method of preparing shaped rubber articles which comprises shaping the pulverulent, pourable elastomer-filler mixture of claim 26.
References Cited (Backward Citations)
US3285869A
Cited
US3846365A
Cited
US3895035A
Cited
US3920604A
Cited
US3945978A
Cited
US3922240A
Cited
US3929707A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-02-05 | 1982-08-07 | 1983-02-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-02-05 | 1986-08-07 | 1987-02-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-02-05 | 1990-08-07 | 1991-02-06 | $7700.00 | Window Closed / Lapsed |