# US 11,898,020 B2 · Phenolic foam and method of manufacture thereof

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- Number: US 11,898,020 B2
- Document ID: US11898020B2
- Status: Granted
- Kind: B2
- Application number: 17/264,664
- Filed: 2019-07-29
- Published: 2021-07-29
- Granted: 2024-02-13
- Earliest claimed: 2018-07-30
- Assignees: Kingspan Holdings (IRL) Limited
- Applicants: Kingspan Holdings (IRL) Limited
- Inventors: Vincent Coppock; Lynne Ripley; Ruud Zeggelaar
- Web page: https://patentgrep.com/patent/US11898020B2

## CPC

- C08J 9/0023: {containing oxygen}
- C08J 9/141: {Hydrocarbons}
- C08L 61/06: of aldehydes with phenols
- C08J 9/0033: {containing sulfur}
- C08J 9/0038: {containing phosphorus}
- C08J 9/0061: {characterized by the use of several polymeric components}
- C08J 9/0066: {Use of inorganic compounding ingredients}
- C08J 9/144: {containing carbon, halogen and hydrogen only}
- C08J 2201/026: Crosslinking before of after foaming
- C08J 2203/142: Halogenated saturated hydrocarbons, e.g. H3C-CF3
- C08J 2203/162: Halogenated unsaturated hydrocarbons, e.g. H2C=CF2
- C08J 2205/052: Closed cells, i.e. more than 50% of the pores are closed
- C08J 2361/04: Condensation polymers of aldehydes or ketones with phenols only
- C08J 2361/10: Phenol-formaldehyde condensates
- C08J 2467/02: Polyesters derived from dicarboxylic acids and dihydroxy compounds (C08J2467/06 takes precedence)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)

## Abstract

A thermal insulating phenolic foam and method of manufacture thereof is provided. A phenolic foam is formed by foaming and curing a phenolic resin composition that comprises a phenolic resin, an acid catalyst, a blowing agent comprising a hydrocarbon having 6 carbon atoms or less, and an alkoxy alcohol. The resulting foam has low thermal conductivity and has excellent long term thermal stability.

## Claims

### Claim 1

A phenolic foam formed by foaming and curing a phenolic resin foamable composition that comprises a phenolic resin, a surfactant, an acid catalyst, a blowing agent comprising a hydrocarbon having 6 carbon atoms or less, and an alkoxy alcohol either (a) having the formula:
wherein n is 0 to 4, and wherein R is a C1 to C6 aliphatic chain, R1 is H or alkyl, or (b) being selected from the group consisting of:
propylene glycol monomethyl ether, propylene glycol monoethyl ether,
propylene glycol monopropyl ether, propylene glycol monobutyl ether,
propylene glycol monopentyl ether, propylene glycol monohexyl ether,
dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether,
dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether,
dipropylene glycol monopentyl ether, dipropylene glycol monohexyl ether
tripropylene glycol monomethyl ether, tripropylene glycol monoethyl ether,
tripropylene glycol monopropyl ether, tripropylene glycol monobutyl ether,
tripropylene glycol monopentyl ether and tripropylene glycol monohexyl ether;
wherein the foam has a closed cell content of 85% or more as determined according to ASTM D6226, and a density of from 10 kg/m3 or more and 100 kg/m3 or less as measured according to BS EN 1602:2013.

### Claim 2 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic resin has a water content in the range of from 7.5 wt % to 16 wt % based on the total weight of the phenolic resin foamable composition.

### Claim 3 (depends on 1)

The phenolic foam as claimed in claim 1, wherein n is 0, 1 or 2.

### Claim 4 (depends on 1)

The phenolic foam as claimed in claim 1, wherein R1 is H, or C1 to C6 alkyl.

### Claim 5 (depends on 1)

The phenolic foam as claimed in claim 1, wherein R is selected from the group comprising methyl, ethyl, propyl, butyl, pentyl, hexyl and isomers thereof.

### Claim 6 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the alkoxy alcohol is present in an amount of from 0.5 to 15 parts by weight per 100 parts by weight of phenolic resin.

### Claim 7 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the hydrocarbon comprising 6 carbons atoms or less is one or more compounds selected from the group comprising butane, pentane, hexane, n-butane, isobutane, cyclobutane, n-pentane, isopentane, cyclopentane and cyclohexane, and isomers thereof.

### Claim 8 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the blowing further comprises a halogenated hydrocarbon comprising 6 carbon atoms or less, a hydrofluoroolefin, or a combination thereof.

### Claim 9 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the blowing agent further comprises propyl chloride, dichloroethane, or isomers thereof.

### Claim 10 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the blowing agent further comprises a hydrofluoroolefin selected from the group consisting of 1-chloro-3,3,3-trifluoropropene, 1,3,3,3-tetrafluoropropene, 2,3,3,3-tetrafluoropropene and 1,1,1,4,4,4-hexafluoro-2-butene.

### Claim 11 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the blowing agent is present in an amount of from 1 to 20 parts by weight per 100 parts by weight of phenolic resin.

### Claim 12 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic resin has a molar ratio of phenol groups to aldehyde groups in the range of from 1:1 to 1:3.

### Claim 13 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic resin has a weight average molecular weight of from 700 to 2000.

### Claim 14 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the pH of the foam is 4 or more.

### Claim 15 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the density of the foam is of from 10 to 60 kg/m3.

### Claim 16 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic foam has a compressive strength of from 80 kPa to 220 kPa.

### Claim 17 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic foam has an aged thermal conductivity 0.025 W/m·K or less when measured at a mean temperature of 10° C. after heat ageing for 175±5 days at 70±2° C., in accordance with the procedure specified in European Standard BS EN 13166:2012.

### Claim 18 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the phenolic foam has an aged thermal conductivity in the range of from 0.025 W/m·K to 0.016 W/m·K when measured at a mean temperature of 10° C. after heat ageing for 175±5 days at 70±2° C., in accordance with the procedure specified in European Standard BS EN 13166:2012.

### Claim 19 (depends on 1)

The phenolic foam as claimed in claim 1, wherein the viscosity of the phenolic resin, including the surfactant and alkoxy alcohol is in the range of from 2500 to 7000 mPa·s at 25° C. as measured using a Brookfield viscometer (model DV-II+Pro) with a controlled temperature water bath, maintaining the sample temperature at 25° C., with spindle number S29 rotating at 20 rpm.

### Claim 20

A method for manufacturing a phenolic foam comprising the steps of:
foaming and curing a foamable composition comprising:
a phenolic resin, a surfactant, an acid catalyst, a blowing agent comprising a hydrocarbon having 6 carbon atoms or less, and an alkoxy alcohol either (a) having the formula:
wherein n is 0 to 4, and wherein R is a C1 to C6 aliphatic chain, R1 is H or alkyl, or (b) being selected from the group consisting of:
propylene glycol monomethyl ether, propylene glycol monoethyl ether,
propylene glycol monopropyl ether, propylene glycol monobutyl ether,
propylene glycol monopentyl ether, propylene glycol monohexyl ether,
dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether,
dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether,
dipropylene glycol monopentyl ether, dipropylene glycol monohexyl ether
tripropylene glycol monomethyl ether, tripropylene glycol monoethyl ether,
tripropylene glycol monopropyl ether, tripropylene glycol monobutyl ether,
tripropylene glycol monopentyl ether and tripropylene glycol monohexyl ether;
the foam has a closed cell content of 85% or more as determined according to ASTM D6226, and a density of from 10 kg/m3 or more and 100 kg/m3 or less as measured according to BS EN 1602:2013.
