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US4390641A Expired / Lapsed US ⏱️ 0.0 years remaining

Flame-retardant benzylic-ether phenolic modified foam and method of preparing same

Assignee: LINAMAR MACHINE Ltd
•
Filing: 1982-01-04
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Granted: 1983-06-28
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Expires: 2002-01-04
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Abstract

Abstract A method of preparing a flame-retardant benzylic-ether phenolic modified foam product and the resulting foam product produced thereby, which method comprises reacting and mixing benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of from about 400 to 600, with from about 50 to 150 parts by weight of a boric-acid catalyst to each 100 parts of the resin, optionally in the presence of melamine, to form a resin prepolymer, and, thereafter, reacting the prepolymer so formed, in the presence of a blowing agent and an organometal catalyst, with a methylene diisocyanate in an exothermic reaction, to provide a nonfriable, substantially closed-cell, flame-retardant benzylic-ether phenolic modified foam product characterized by substantially acid methylene linkages in the resulting thermosetting foam product.

Inventors

  • 👤 Stuart B. Smith

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 20:18
CPC Classifications
C; C08; C08G; C08G18/00; C08G18/06; C08G18/28; C08G18/40; C08G18/54; C08G18/542; C08G2110/00; C08G2110/0025; C08G2110/0041; C08G2110/005; C08G2110/0058

Claims Analysis

Total Claims: 21
Claim 1
Independent Claim 185 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of greater than about 200, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a weak acid catalyst at a pH of from about 4.0 to 6.5, to form a benzylic-ether phenol resin prepolymer; and (b) reacting the prepolymer, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, with from about 50 to 200 parts by weight of a methylene diphenyl polyisocyanate in an exothermic reaction, to provide for the further heat and acid condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to produce a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.
Claim 2
Independent Claim 185 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of greater than about 200, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a weak acid catalyst at a pH of from about 4.0 to 6.5, to form a benzylic-ether phenol resin prepolymer; and (b) reacting the prepolymer, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, with from about 50 to 200 parts by weight of a methylene diphenyl polyisocyanate in an exothermic reaction, to provide for the further heat and acid condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to produce a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.
Claim 3
Dependent Claim 13 words
The method of claim 1 wherein the weak acid catalyst comprises boric acid.
Claim 4
Dependent Claim 25 words
The method of claim 1 wherein the weak acid catalyst comprises from about 50 to 120 parts by weight of a powdered boric acid catalyst.
Claim 5
Dependent Claim 13 words
The method of claim 1 wherein the blowing agent comprises a liquid fluorocarbon.
Claim 6
Dependent Claim 15 words
The method of claim 1 wherein the organometal catalyst comprises a fatty acid tin catalyst.
Claim 7
Dependent Claim 20 words
The method of claim 1 wherein the reaction is carried out at a pH of from about 5.0 to 5.7.
Claim 8
Dependent Claim 13 words
The method of claim 1 wherein the methylene diphenyl polyisocyanate comprises toluene diisocyanate.
Claim 9
Dependent Claim 20 words
The method of claim 1 wherein the benzylic-ether phenol-formaldehyde resin has a hydroxyl number ranging from about 400 to 600.
Claim 10
Dependent Claim 28 words
The method of claim 1 which includes mixing the benzylic-ether phenol-formaldehyde resin and weak acid catalyst to form the prepolymer for a period of at least 6 hours.
Claim 11
Dependent Claim 23 words
The method of claim 1 which includes adding sufficient melamine to react with substantially all of the free formaldehyde of the phenolic-formaldehyde resin.
Claim 12
Dependent Claim 27 words
The method of claim 1 which includes adding from about 1 to 5 parts by weight of melamine per 100 parts of the resin to the prepolymer.
Claim 13
Dependent Claim 19 words
The method of claim 1 wherein the methylene diphenyl polyisocyanate has an average functionality of from 2.4 to 3.2.
Claim 14
Dependent Claim 29 words
The method of claim 1 wherein the weak acid catalyst is selected from the group consisting of oxalic acid, citric acid, tartaric acid and boric acid, and combinations thereof.
Claim 15
Dependent Claim 77 words
The method of claim 1 wherein the benzylic-ether-phenol formaldehyde resin has the structural formula: ##STR4## wherein R is a hydrogen or a phenolic substituent meta to the phenolic hydroxyl group, the sum of m and n is at least 2 and the ratio of m to n is at least 1, and X is an end group from the group consisting of hydrogen and methylol, the molar ratio of said methylol-to-hydrogen end groups being at least 1.
Claim 16
Dependent Claim 24 words
The method of claim 1 which includes reacting the resin with the weak acid catalyst at a temperature of less than about 100° F.
Claim 17
Dependent Claim 24 words
The method of claim 1 which includes adding an amine reactive with formaldehyde to the prepolymer to react with free formaldehyde in the prepolymer.
Claim 18
Independent Claim 191 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of from about 400 to 600, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a boric acid catalyst at a temperature of less than about 100° F. and a pH of from about 4.0 to 6.5, to form a benzylic-ether phenol resin prepolymer; and (b) reacting, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, the prepolymer with from about 50 to 200 parts by weight of a methylene diphenyl diisocyanate in an exothermic reaction, to provide the further condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to provide a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.
Claim 19
Independent Claim 191 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of from about 400 to 600, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a boric acid catalyst at a temperature of less than about 100° F. and a pH of from about 4.0 to 6.5, to form a benzylic-ether phenol resin prepolymer; and (b) reacting, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, the prepolymer with from about 50 to 200 parts by weight of a methylene diphenyl diisocyanate in an exothermic reaction, to provide the further condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to provide a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.
Claim 20
Independent Claim 229 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of from about 400 to 600, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a boric acid catalyst at a temperature of less than about 100° F. and a pH of from about 4.0 to 6.5, and with a sufficient amount of melamine to react with substantially all of the free formaldehyde of the phenolic-formaldehyde resin and mixing the resin, melamine and weak acid catalyst for a period of about 6 to 24 hours, to form a benzylic-ether phenol resin prepolymer; and (b) reacting, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, the prepolymer with from about 50 to 200 parts by weight of a methylene diphenyl diisocyanate in an exothermic reaction, to provide the further condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to produce a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.
Claim 21
Independent Claim 229 words
A method of preparing a nonfriable, closed-cell, benzylic-ether phenol-formaldehyde modified thermosetting foam product characterized by a low flame spread and smoke properties, which method comprises: (a) reacting, under substantially anhydrous conditions, 100 parts of a benzylic-ether phenol-formaldehyde resin, having a hydroxyl number of from about 400 to 600, with from about 50 to 150 parts by weight per 100 parts of the benzylic-ether phenol-formaldehyde resin in the presence of a boric acid catalyst at a temperature of less than about 100° F. and a pH of from about 4.0 to 6.5, and with a sufficient amount of melamine to react with substantially all of the free formaldehyde of the phenolic-formaldehyde resin and mixing the resin, melamine and weak acid catalyst for a period of about 6 to 24 hours, to form a benzylic-ether phenol resin prepolymer; and (b) reacting, in the presence of a blowing amount of a blowing agent to form a foamable mass, and a catalytic amount of an organometallic catalyst, which is not affected by the pH of the prepolymer, the prepolymer with from about 50 to 200 parts by weight of a methylene diphenyl diisocyanate in an exothermic reaction, to provide the further condensation of the phenolic resin prepolymer and the reaction of the isocyanate with the prepolymer, to produce a low-friability, substantially closed-cell, phenolic modified thermosetting foam product composed substantially of acid methylene linkages.

References Cited (Backward Citations)

US2608536A Cited
US3242107A Cited
US3485797A Cited
US4046721A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1986-06-27 1986-12-27 1987-06-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1990-06-27 1990-12-27 1991-06-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1994-06-27 1994-12-27 1995-06-28 $7700.00 Window Closed / Lapsed

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