Patent US4970253A successfully refreshed from Google Patents.
US4970253A
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Thermoplastic plasticized polyvinylbutyral molding composition
Assignee: Clariant Produkte Deutschland GmbH
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Filing: 1987-11-03
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Granted: 1990-11-13
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Expires: 2007-11-03
Abstract
Abstract Thermoplastic plasticized polyvinylbutyral molding compositions, in particular films of improved tensile strength and reduced tackiness are prepared by acetalization of polyvinyl alcohol, capable of association, in the associated state with n-butyraldehyde in aqueous phase in the presence of an acid catalyst and, if appropriate, of an organic sulfonic acid having an emulsifying action, after-treatment of the polyvinylbutyral under acetalization conditions at an elevated temperature in the presence of an organic sulfonic acid having 8 to 30 C atoms and having an emulsifying action, isolation and/or purification of the polyvinylbutyral and, if appropriate, admixture of conventional additives and mixing of the product, which may have been dried, with up to 40% by weight of plasticizer, relative to the polymer/plasticizer mixture, and molding, the plasticizers employed being esters of phthalic acid with C 6 -C 10 -alcohols and/or esters of adipic acid with C 6 -C 10 -alcohols. Use of the films for the manufacture of laminated glass, and laminated glass containing the films as the joining layer.
Inventors
- 👤 Hans Dieter Hermann
- 👤 Kurt Fock
- 👤 Klaus Fabian
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 16:40
CPC Classifications
B; B32; B32B; B32B17/00; B32B17/06; B32B17/10; B32B17/10005; B32B17/1055; B32B17/10761; B32B17/10605; C; C08; C08F; C08F8/00; C08F8/48
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
247 words
A process for preparing thermoplastic plasticized polyvinylbutyral molding composition which comprises the following steps: (1) acetalizing polyvinyl alcohol with n-butyraldehyde in aqueous phase with an acid catalyst, (2) aftertreating obtained polyvinylbutyral under acetalization conditions in aqueous phase at an elevated temperature with an emulsifier, (3) isolating and purifying the resulting polyvinylbutyral, and (4) mixing the thus obtained polyvinylbutyral with plasticizer, wherein the polyvinylalcohol employed is one which has less than 0.5% by weight of vinyl acetate units, and its aqueous solution has been cooled to a temperature below 20° C., acetalizing is initially conducted at a temperature below 20° C. and is subsequently effected at a temperature of from 20° to above 40° C., to obtain polyvinylbutyral the aftertreating emulsifier is an organic sulfonic acid having from 8 to 30 C atoms or a salt thereof, the aftertreating is effected at from 50° to 70° C. for from 0.5 to 10 hours to obtain a polyvinylbutyral having a residual vinyl alcohol content of from 15 to 21% by weight, the plasticizer is at least one member selected from the group consisting of (a) an ester of phthalic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols and (b) an ester of adipic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols, and the amount of plasticizer is from 20 to 40% by weight, relative to the weight of the polymer/plasticizer mixture.
Claim 2
Dependent Claim
247 words
A process for preparing thermoplastic plasticized polyvinylbutyral molding composition which comprises the following steps: (1) acetalizing polyvinyl alcohol with n-butyraldehyde in aqueous phase with an acid catalyst, (2) aftertreating obtained polyvinylbutyral under acetalization conditions in aqueous phase at an elevated temperature with an emulsifier, (3) isolating and purifying the resulting polyvinylbutyral, and (4) mixing the thus obtained polyvinylbutyral with plasticizer, wherein the polyvinylalcohol employed is one which has less than 0.5% by weight of vinyl acetate units, and its aqueous solution has been cooled to a temperature below 20° C., acetalizing is initially conducted at a temperature below 20° C. and is subsequently effected at a temperature of from 20° to above 40° C., to obtain polyvinylbutyral the aftertreating emulsifier is an organic sulfonic acid having from 8 to 30 C atoms or a salt thereof, the aftertreating is effected at from 50° to 70° C. for from 0.5 to 10 hours to obtain a polyvinylbutyral having a residual vinyl alcohol content of from 15 to 21% by weight, the plasticizer is at least one member selected from the group consisting of (a) an ester of phthalic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols and (b) an ester of adipic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols, and the amount of plasticizer is from 20 to 40% by weight, relative to the weight of the polymer/plasticizer mixture.
Claim 3
Dependent Claim
14 words
A process which comprises molding the molding composition prepared as claimed in claim 1.
Claim 4
Dependent Claim
39 words
A process as claimed in claim 1 wherein the polyvinylbutyral obtained by step (3) has a viscosity (measured according to DIN 53015 at 23° C. on a 5% by weight solution in ethanol) of between 10 and 200 mPa.s.
Claim 5
Dependent Claim
27 words
A process as claimed in claim 1 wherein the polyvinylbutyral obtained by step (3) has a residual vinyl alcohol content of from 16 to 20% by weight.
Claim 6
Dependent Claim
37 words
A process as claimed in claim 1 wherein the emulsifier of step (2) comprises up to 1% by weight (based on the weight of the resulting polyvinylbutyral) of the organic sulfonic acid or of a salt thereof.
Claim 7
Dependent Claim
31 words
A process as claimed in claim 5 wherein step (2) is effected in the presence of 0.01 to 0.5% by weight of the organic sulfonic acid or of a salt thereof.
Claim 8
Dependent Claim
29 words
A process as claimed in claim 2, wherein the weight ratio of the plasticizer components is (a) : (b)=100 to 90:0 to 10 or 0 to 10:100 to 90.
Claim 9
Dependent Claim
23 words
A process as claimed in claim 2 which comprises molding the thermoplastic plasticized polyvinylbutyral molding composition to give a film of high strength.
Claim 10
Dependent Claim
12 words
A thermoplastic plasticizer polyvinylbutyral molding composition prepared as claimed in claim 1.
Claim 11
Dependent Claim
12 words
A high-strength thermoplastic plasticizer polyvinylbutyral film prepared as claimed in claim 8.
Claim 12
Dependent Claim
216 words
A process for preparing thermoplastic plasticized polyvinylbutyral molding composition which comprises the following steps: (1) cooling to a temperature below 20° C. an aqueous solution of polyvinyl alcohol having less than 0.5% by weight (based on the total weight of the polyvinyl alcohol) of vinyl acetate units, (2) initiating acetalization of the polyvinyl alcohol with n-butyraldehyde in aqueous phase with an acid catalyst while the aqueous solution is at temperature below 20° C., (3) continuing the aqueous-phase acid-catalyzed acetalization within a temperature range of from 20° to 40° C. to obtain polyvinylbutyral, (4) aftertreating the polyvinylbutyral under acetalization conditions in aqueous phase for from 0.5 to 10 hours within a temperature range of from 50° to 70° C. with an organic sulfonic acid emulsifier having from 8 to 30 C atoms, or a salt thereof, (5) isolating the resulting polyvinylbutyral, and (6) mixing the obtained isolated polyvinylbutyral with from 20 to 40% by weight, relative to the weight of the polymer/ plasticizer mixture, of plasticizer selected from the group consisting of (a) an ester of phthalic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols and (b) an ester of adipic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols.
Claim 13
Dependent Claim
216 words
A process for preparing thermoplastic plasticized polyvinylbutyral molding composition which comprises the following steps: (1) cooling to a temperature below 20° C. an aqueous solution of polyvinyl alcohol having less than 0.5% by weight (based on the total weight of the polyvinyl alcohol) of vinyl acetate units, (2) initiating acetalization of the polyvinyl alcohol with n-butyraldehyde in aqueous phase with an acid catalyst while the aqueous solution is at temperature below 20° C., (3) continuing the aqueous-phase acid-catalyzed acetalization within a temperature range of from 20° to 40° C. to obtain polyvinylbutyral, (4) aftertreating the polyvinylbutyral under acetalization conditions in aqueous phase for from 0.5 to 10 hours within a temperature range of from 50° to 70° C. with an organic sulfonic acid emulsifier having from 8 to 30 C atoms, or a salt thereof, (5) isolating the resulting polyvinylbutyral, and (6) mixing the obtained isolated polyvinylbutyral with from 20 to 40% by weight, relative to the weight of the polymer/ plasticizer mixture, of plasticizer selected from the group consisting of (a) an ester of phthalic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols and (b) an ester of adipic acid with a linear or branched C 6 -C 10 -alcohol or a mixture of such alcohols.
Claim 14
Dependent Claim
33 words
A process according to claim 11 which further comprises adding to the aqueous solution of step (1), prior to initiating acetalization, an organic sulfonic acid having an emulsifying action or a salt thereof.
Claim 15
Dependent Claim
22 words
A process according to claim 11 which further comprises adding dodecylbenzenesulfonate, to the aqueous solution of step (1) prior to initiating acetalization.
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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) | 1993-11-12 | 1994-05-14 | 1994-11-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-11-12 | 1998-05-14 | 1998-11-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-11-12 | 2002-05-14 | 2002-11-13 | $7700.00 | Window Closed / Lapsed |