US5280049A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Molded cellular crosslinked vinyl lactam polymer gel and method of preparation
Assignee: ISP Investments LLC
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Filing: 1993-08-09
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Granted: 1994-01-18
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Expires: 2013-08-09
Abstract
Abstract This invention relates to a foamed, cellular crosslinked vinyl lactam polymer and to a formed rigid product obtained therefrom having dimensional stability and a high Tg above 150° C. The invention also relates to the method of preparing said molded cellular polymer.
Inventors
- 👤 Philip F. Wolf
- 👤 Susan Y. Tseng
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 09:26
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/26; C08F; C08F226/00; C08F226/06; C08J2339/00; C08J2339/04; C08J2339/06
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
275 words
The process of producing the foamed cellular 0.1 to 10% crosslinked lactam polymer in a rigid, molded form which comprises (1) forming a uniform liquid mixture of (a) between about 10 and about 30 wt. % of a polymerizable reactant containing at least 55% N-vinyl lactam monomer; (b) between about 0.01 and about 10.0 wt. % crosslinking agent; (c) between about 60 and about 90 wt. % solvent and (d) between about 0.1 and about 5 wt. % of a free radical initiator having a decomposition temperature below the boiling point of said solvent; (2) introducing said mixture into a dish or mold; (3) in the absence of agitation and in an inert atmosphere, heating the mixture to between about 50° and about 80° C. for a period of from about 2 to about 5 hours to begin polymerization without displacement of the solvent medium, and then raising the temperature to between about 100° and about 145° C. for an additional period of from about 0.5 to about 3 hours or until a constant viscosity is reached to complete the crosslinking of the polymer; (4) recovering the crosslinked polymer in the form of a shaped rubbery intermediate and digesting said intermediate in water to swell the polymer and to extract and remove soluble monomer, linear polymer and other residuals in the aqueous phase; (5) recovering a clear, formed, crosslinked vinyl lactan polymer hydrogel from water and (6) freeze drying said hydrogel for a period of from about 2 to about 70 hours at a critical temperature of between -85° C. and -40° C. to produce a white, cellular foamed product of crosslinked N-vinyl lactam polymer.
Claim 2
Dependent Claim
275 words
The process of producing the foamed cellular 0.1 to 10% crosslinked lactam polymer in a rigid, molded form which comprises (1) forming a uniform liquid mixture of (a) between about 10 and about 30 wt. % of a polymerizable reactant containing at least 55% N-vinyl lactam monomer; (b) between about 0.01 and about 10.0 wt. % crosslinking agent; (c) between about 60 and about 90 wt. % solvent and (d) between about 0.1 and about 5 wt. % of a free radical initiator having a decomposition temperature below the boiling point of said solvent; (2) introducing said mixture into a dish or mold; (3) in the absence of agitation and in an inert atmosphere, heating the mixture to between about 50° and about 80° C. for a period of from about 2 to about 5 hours to begin polymerization without displacement of the solvent medium, and then raising the temperature to between about 100° and about 145° C. for an additional period of from about 0.5 to about 3 hours or until a constant viscosity is reached to complete the crosslinking of the polymer; (4) recovering the crosslinked polymer in the form of a shaped rubbery intermediate and digesting said intermediate in water to swell the polymer and to extract and remove soluble monomer, linear polymer and other residuals in the aqueous phase; (5) recovering a clear, formed, crosslinked vinyl lactan polymer hydrogel from water and (6) freeze drying said hydrogel for a period of from about 2 to about 70 hours at a critical temperature of between -85° C. and -40° C. to produce a white, cellular foamed product of crosslinked N-vinyl lactam polymer.
Claim 3
Dependent Claim
35 words
The process of claim 1 wherein the freeze drying step is effected at a temperature of between about -80° C. and about -50° C. for a period of from about 5 to about 10 hours.
Claim 4
Dependent Claim
10 words
The process of claim 1 wherein component (a) is N-vinylpyrrolidone.
Claim 5
Dependent Claim
11 words
The process of claim 1 wherein component (a) is N-vinyl caprolactam.
Claim 6
Dependent Claim
14 words
The process of claim 1 wherein component (a) is a N-vinylpyrrolidone/N-vinyl caprolactam monomer mixture.
Claim 7
Dependent Claim
14 words
The process of claim 1 wherein component (a) is a N-vinylpyrrolidone/vinyl acetate monomer mixture.
Claim 8
Dependent Claim
14 words
The process of claim 1 wherein component (a) is a N-vinylpyrrolidone/acrylic acid monomer mixture.
Claim 9
Dependent Claim
11 words
The process of claim 1 wherein component (b) is 1-vinyl-3(E)ethylene pyrrolidone.
Claim 10
Dependent Claim
10 words
The process of claim 1 wherein component (b) is ethylene-bis(N-vinylpyrrolidone).
Claim 11
Dependent Claim
10 words
The process of claim 1 wherein component (b) is divinylimidazolidone.
Claim 12
Dependent Claim
10 words
The process of claim 1 wherein component (c) is water.
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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) | 1997-01-17 | 1997-07-19 | 1998-01-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2001-01-17 | 2001-07-19 | 2002-01-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2005-01-17 | 2005-07-19 | 2006-01-18 | $7700.00 | Window Closed / Lapsed |