US3846347A
Expired / Lapsed
US
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Rigid foams from polyurethane and methods and compositions for use in their preparation
Assignee: Witco Corp
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Filing: 1970-09-21
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Granted: 1974-11-05
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Expires: 1990-09-21
Abstract
Abstract A stable, highly branched polyurethane prepolymer which is in liquid form is prepared by the conversion of polyether/polyols having at least four hydroxyl groups to a polyurethane by reaction with an excess of a urethane-forming reactant such as a polyisocyanate. The said excess functions as a solvent for the prepolymer and in this dissolved, stable form the prepolymer can be converted to rigid foams which have K factors of about 0.14 and below 0.22 and which have closed cell contents of about 90 percent, the cells being fine, uniform cells. In the conversion to the foams the prepolymer is reacted with additional polyether/polyol, this being a polymeric hydroxy compound prepared by reacting a compound containing four or more hydroxyl groups with an alkylene oxide, such as propylene oxide. The foaming is effected in the presence of a blowing agent which consists of a volatile, halogenated lower alkane containing chlorine and fluorine atoms. The iscoyanato content of the prepolymer is about 22 percent to about 30 percent and the final polyurethane has its molecular weight made up to an extent of about 65 percent to about 80 percent by the said polymeric hydroxy compound. Since the foaming is effected without the use of water, the nitrogen atoms in the reaction go substantially to form urethane linkages. The polyether/polyol is represented by such materials as the propylene oxide adducts of sorbitol or sucrose while the urethane forming reactant is represented by such a material as toluene diisocyanate and the blowing agent by such a material as monofluorotrichloromethane. The stability of the prepolymers and their liquid form afford ready shipment of the various components for the foams over long distances and storage for substantial time lengths.
Inventors
- 👤 K Satterly
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 16:16
CPC Classifications
C; C08; C08G; C08G18/00; C08G18/06; C08G18/28; C08G18/40; C08G18/48; C08G18/4895; C08G18/08; C08G18/10; C08G18/4829; C08G2110/00; C08G2110/0008; C08G2110/0016; C08G2110/0025; C08G2110/0041; C08G2110/005; C08G2110/0058; C08G2110/0083
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
139 words
A STABLE, HIGHLT BRANCHED PREPOLYMER WHICH IS A POLYURETHANE AND IS IN LIQUID FORM, BEING DISSOLVED IN A SOLVENT COMPRISING A REACTIVE ORGANIC POLYISOCYANATE, SAID PREPOLYMER BEING CAPABLE OF BEING PLACED INTO THE FORM OF A RIGID FOAM WHICH HAS A K FACTOR VLAUE OF LESS THAN 0.22 AND WHICH FOAM HAS A CLOSED CELL CONTENT OF ABOUT 90 PERCENT, THE CELLS BEING FINE, UNIFORM CELLS, SAID PREPOLYMER COMPRISING THE REACTION PRODUCT OF AN EXCESS OF POLYISOCYANATE AND A POLYMERIC HYDROXY COMPOUND WHICH COMPOUND IS A POLYALKYLENE OXIDE BEING THE ADDITION PRODUCT OF AN HYDROXY COMPOUND HAVING AT LEAST THREE CARBON ATOMS WITH A HYDROXY COMPOUND HAVING AT LEAST SIX HYDROXYL GROUPS, AND SAID PREPOLYMER CONTAINING REACTIVE ORGANIC KPOLYISCYANATE CONTRIBUTING TO THE PRESENCE OF UNCHANGED ISOCYANATO GROUPS REACTIVE TO FURTHER POLYMERIZATION THE SAID REACTIVE POLYISOCYANATE ACTING AS SAID SOLVENT.
Claim 2
Dependent Claim
139 words
A STABLE, HIGHLT BRANCHED PREPOLYMER WHICH IS A POLYURETHANE AND IS IN LIQUID FORM, BEING DISSOLVED IN A SOLVENT COMPRISING A REACTIVE ORGANIC POLYISOCYANATE, SAID PREPOLYMER BEING CAPABLE OF BEING PLACED INTO THE FORM OF A RIGID FOAM WHICH HAS A K FACTOR VLAUE OF LESS THAN 0.22 AND WHICH FOAM HAS A CLOSED CELL CONTENT OF ABOUT 90 PERCENT, THE CELLS BEING FINE, UNIFORM CELLS, SAID PREPOLYMER COMPRISING THE REACTION PRODUCT OF AN EXCESS OF POLYISOCYANATE AND A POLYMERIC HYDROXY COMPOUND WHICH COMPOUND IS A POLYALKYLENE OXIDE BEING THE ADDITION PRODUCT OF AN HYDROXY COMPOUND HAVING AT LEAST THREE CARBON ATOMS WITH A HYDROXY COMPOUND HAVING AT LEAST SIX HYDROXYL GROUPS, AND SAID PREPOLYMER CONTAINING REACTIVE ORGANIC KPOLYISCYANATE CONTRIBUTING TO THE PRESENCE OF UNCHANGED ISOCYANATO GROUPS REACTIVE TO FURTHER POLYMERIZATION THE SAID REACTIVE POLYISOCYANATE ACTING AS SAID SOLVENT.
Claim 3
Dependent Claim
18 words
A composition in accordance with claim 1 in which the polymeric hydroxy compound comprises a poly(alkylene oxide) sorbitol.
Claim 4
Dependent Claim
18 words
A composition in accordance with claim 1 in which the polymeric hydroxy compound comprises a poly(propylene oxide) sorbitol.
Claim 5
Dependent Claim
21 words
A composition in accordance with claim 1 in which the polymeric hydroxy compound comprises a polyalkylene oxide derived from a biose.
Claim 6
Dependent Claim
21 words
A composition in accordance with claim 1 in which the polymeric hydroxy compound comprises a polypropylene oxide derived from a biose.
Claim 7
Dependent Claim
24 words
A composition in accordance with claim 1 in which the molecular weight of the polymeric hydroxy compound is between about 400 and about 1,200.
Claim 8
Dependent Claim
27 words
A composition in accordance with claim 1 in which said polymeric hydroxy compound contributes about 20 percent to about 27 percent of the weight of said prepolymer.
Claim 9
Dependent Claim
40 words
A prepolymer in accordance with claim 1 which is capable by further polymerization of forming a second polyurethane in which said polymeric hydroxy compound contributes about 65 percent to about 80 percent of the molecular weight of said second polyurethane.
Claim 10
Dependent Claim
196 words
A process for the formation of a stable, highly branched prepolymer which is a polyurethane and is in liquid form being dissolved in a solvent comprising a reactive organic polyisocyanate and which prepolymer in said form is capable of being further polymerized to form a high molecular weight polyurethane, which is capable of forming a rigid foam having a K factor less than 0.22, and which has a closed cell content of about 90 percent, the cells being fine, uniform cells, which process comprises mixing and reacting a polymeric hydroxy compound, being a polyalkylene oxide which is the addition product of an alkylene oxide having at least three carbon atoms with a hydroxy compound having at least six hydroxyl groups, thus being highly branched, with an organic, polyfunctional urethane-forming reactant being an organic polyisocyanate the ratio of said polymeric hydroxy compound to said reactant being such that there is an excess of urethane-forming reactant groups in the resultant prepolymer reactive to further polymerization which polymerization effects the formation of said higher molecular polyurethane in which about 65 percent to about 80 percent of the molecular weight is derived from the said highly branched polymeric hydroxy compound.
Claim 11
Dependent Claim
196 words
A process for the formation of a stable, highly branched prepolymer which is a polyurethane and is in liquid form being dissolved in a solvent comprising a reactive organic polyisocyanate and which prepolymer in said form is capable of being further polymerized to form a high molecular weight polyurethane, which is capable of forming a rigid foam having a K factor less than 0.22, and which has a closed cell content of about 90 percent, the cells being fine, uniform cells, which process comprises mixing and reacting a polymeric hydroxy compound, being a polyalkylene oxide which is the addition product of an alkylene oxide having at least three carbon atoms with a hydroxy compound having at least six hydroxyl groups, thus being highly branched, with an organic, polyfunctional urethane-forming reactant being an organic polyisocyanate the ratio of said polymeric hydroxy compound to said reactant being such that there is an excess of urethane-forming reactant groups in the resultant prepolymer reactive to further polymerization which polymerization effects the formation of said higher molecular polyurethane in which about 65 percent to about 80 percent of the molecular weight is derived from the said highly branched polymeric hydroxy compound.
Claim 12
Dependent Claim
15 words
A process in accordance with claim 9 in which said reactant is an organic diisocyanate.
Claim 13
Dependent Claim
19 words
A process in accordance with claim 9 in which the said polymeric hydroxy compound comprises a poly(alkylene oxide) sorbitol.
Claim 14
Dependent Claim
22 words
A process in accordance with claim 9 in which the said polymeric hydroxy compound comprises a polyalkylene oxide derived from a biose.
Claim 15
Dependent Claim
21 words
A process in accordance with claim 9 in which said polymeric hydroxy compound comprises a polypropylene oxide derived from a biose.
Claim 16
Dependent Claim
37 words
A process in accordance with claim 9 in which the said urethane-forming reactant is an organic diisocyanate and there is present in the prepolymer product an excess isocyanato content of about 22 percent to about 30 percent.
Claim 17
Dependent Claim
183 words
A rigid highly cross-linked, shrink stable polyurethane foam which is made from a polymer that is a polyurethane and in which foam substantially all of the cells of the foam are closed, the closed cell content being at least 90 percent the cells being fine uniform cells, and which foam comprises the reaction product of (a) and (b) as follows: (a) an arylene polyisocyanate aT least a part of which is a polyurethane in prepolymer form which prepolymer is derived from a polymeric hydroxy compound that is the addition product of an alkylene oxide that has at least three carbon atoms and a polyol having at least six hydroxy groups and (b) a polymeric polyoxyalkylene ether which is the addition product of an alkylene oxide having at least three carbon atoms with a highly branched polyol having at least six hydroxy groups, said foam having a K factor value of less than 0.22, said foam being formed using a volatile, halogenated, lower alkane containing chlorine and fluorine atoms as the sole blowing agent, thereby obtaining the said K factor of less than 0.22.
Claim 18
Dependent Claim
183 words
A rigid highly cross-linked, shrink stable polyurethane foam which is made from a polymer that is a polyurethane and in which foam substantially all of the cells of the foam are closed, the closed cell content being at least 90 percent the cells being fine uniform cells, and which foam comprises the reaction product of (a) and (b) as follows: (a) an arylene polyisocyanate aT least a part of which is a polyurethane in prepolymer form which prepolymer is derived from a polymeric hydroxy compound that is the addition product of an alkylene oxide that has at least three carbon atoms and a polyol having at least six hydroxy groups and (b) a polymeric polyoxyalkylene ether which is the addition product of an alkylene oxide having at least three carbon atoms with a highly branched polyol having at least six hydroxy groups, said foam having a K factor value of less than 0.22, said foam being formed using a volatile, halogenated, lower alkane containing chlorine and fluorine atoms as the sole blowing agent, thereby obtaining the said K factor of less than 0.22.
Claim 19
Dependent Claim
15 words
A rigid foam in accordance with claim 15 in which said polyol comprises a hexitol.
Claim 20
Dependent Claim
14 words
A rigid foam in accordance with claim 16 in which said hexitol comprises sorbitol.
Claim 21
Dependent Claim
19 words
A rigid foam in accordance with claim 15 in which said polyol comprises a polyol derived from a biose.
Claim 22
Dependent Claim
15 words
A rigid foam in accordance with claim 15 which contains therein a said blowing agent.
Claim 23
Dependent Claim
16 words
A rigid foam in accordance with claim 15 in which said blowing agent consists of monofluorotrichloromethane.
Claim 24
Dependent Claim
139 words
A liquid composition of matter comprising a mixture which comprises a blowing agent which consists of a volatile halogenated lower alkane containing chlorine and fluorine atoms admixed with a highly branched polyurethane which is reactive and which comprises the reaction product of an organic polyfunctional urethane-forming reactant being an organic polyisocyanate and a polymeric polyoxyalkylene ether which is the addition product of an alkylene oxide having at least three carbon atoms with a highly branched polyol having at least six hydroxyl groups, said reactive polyurethane being reactive to form a second but solid polyurethane which contains therein said halogenated alkane, said solid polyurethane being in the form of a rigid foam which has a K factor value of less than 0.22 and which foam has a closed cell content of about 90 percent, the cells being fine, uniform cells.
Claim 25
Dependent Claim
139 words
A liquid composition of matter comprising a mixture which comprises a blowing agent which consists of a volatile halogenated lower alkane containing chlorine and fluorine atoms admixed with a highly branched polyurethane which is reactive and which comprises the reaction product of an organic polyfunctional urethane-forming reactant being an organic polyisocyanate and a polymeric polyoxyalkylene ether which is the addition product of an alkylene oxide having at least three carbon atoms with a highly branched polyol having at least six hydroxyl groups, said reactive polyurethane being reactive to form a second but solid polyurethane which contains therein said halogenated alkane, said solid polyurethane being in the form of a rigid foam which has a K factor value of less than 0.22 and which foam has a closed cell content of about 90 percent, the cells being fine, uniform cells.
Claim 26
Dependent Claim
15 words
A composition of matter in accordance with claim 21 in which said polyol comprises sorbitol.
Claim 27
Dependent Claim
18 words
A composition of matter in accordance with claim 21 in which said polyol is derived from a biose.
Claim 28
Dependent Claim
16 words
A composition of matter in accordance with claim 21 in which said alkane consists of monofluorotrichloromethane.
Claim 29
Dependent Claim
16 words
A composition of matter in accordance with claim 21 in which said polyisocyanate comprises a diisocyanate.
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) | 1977-11-04 | 1978-05-06 | 1978-11-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-11-04 | 1982-05-06 | 1982-11-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-11-04 | 1986-05-06 | 1986-11-05 | $7700.00 | Window Closed / Lapsed |