# US 8,772,366 B2 · Phenolic foam > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,772,366 B2 - Document ID: US8772366B2 - Status: Granted - Kind: B2 - Application number: 13/603,889 - Filed: 2012-09-05 - Published: 2013-03-21 - Granted: 2014-07-08 - Earliest claimed: 2005-09-08 - Assignees: Kingspan Holdings (IRL) Limited - Applicants: Vincent Coppock; Ruud Zeggelaar; Hiroo Takahashi; Toshiyuki Kato - Inventors: Vincent Coppock; Ruud Zeggelaar; Hiroo Takahashi; Toshiyuki Kato - Web page: https://patentgrep.com/patent/US8772366B2 ## CPC - C08J 9/145: {only chlorine as halogen atoms} - C08J 9/0066: {Use of inorganic compounding ingredients} - C08J 9/149: {Mixtures of blowing agents covered by more than one of the groups C08J9/141 - C08J9/143} - C08L 71/08: Polyethers derived from hydroxy compounds or from their metallic derivatives (C08L71/02 takes precedence) - C08J 2203/14: Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons - C08J 2203/142: Halogenated saturated hydrocarbons, e.g. H3C-CF3 - C08J 2361/06: of aldehydes with phenols - C08J 2361/10: Phenol-formaldehyde condensates - Y10T 428/249953: Composite having voids in a component [e.g., porous, cellular, etc.] - Y10T 442/647: Including a foamed layer or component - 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) - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract A phenolic foam is made by foaming and curing a foamable phenolic resin composition that comprises a phenolic resin, a blowing agent, an acid catalyst and an inorganic filler. The blowing agent comprises a blend of chlorinated aliphatic hydrocarbon containing 2 to 5 carbon atoms and an aliphatic hydrocarbon containing from 3 to 6 carbon atoms mixed in a ratio of 60/40 to 5/5 parts by weight. The inorganic filler is at least one selected from a metal hydroxide, a metal oxide, a metal carbonate and a metal powder. The phenolic foam has a pH of 5 or more and a water uptake less than 1 kg/m2. A phenolic foam with a higher pH value compared with conventional phenolic foam reduces corrosion risk when in contact with metallic materials. The phenolic foam maintains excellent long-term stable thermal insulation performance, low water uptake and fire resistance performance and by using the said blowing agent, does not harm the environment as an ozone or global warming depleting material. ## Claims ### Claim 1 A composition for forming, when foamed and cured, a phenolic foam product with a pH of 5 or more, a closed cell content of 90% or more, and an aged thermal conductivity of 0.025 W/m·K or less when measured at a mean temperature of 10° C. after heat aging for 175±5 days at 70±2° C. in accordance with the procedure specified in European Standard EN13166: 2001, Annex C, Section C.4.2.3, the composition comprising: a phenolic resin, a blowing agent, an acid curing catalyst to initiate polymerization of the phenolic resin, an inorganic filler, a plasticiser and an organic modifier for co-reacting with the phenolic resin; wherein the blowing agent comprises isopropyl chloride and at least one hydrocarbon of butane, pentane, hexane and their isomers in a weight ratio of from 60:40 to 95:5; the inorganic filler consists of a metal hydroxide or metal carbonate with an ionic equilibrium solubility (Ksp) less than 10−8 when measured at 25° C.; and the plasticiser has a molecular structure containing both an ester backbone and a hydroxyl group. ### Claim 2 (depends on 1) The composition as claimed in claim 1 wherein the filler consists of a metal carbonate selected from calcium carbonate, barium carbonate, or zinc carbonate. ### Claim 3 (depends on 1) The composition as claimed in claim 1 wherein the filler consists of calcium carbonate. ### Claim 4 (depends on 1) The composition as claimed in claim 1 wherein the phenolic resin comprises phenol groups and aldehyde groups in a molar ratio of phenol groups to aldehyde groups in the range 1:1 to 1:3. ### Claim 5 (depends on 1) The composition as claimed in claim 1 wherein the phenolic resin comprises phenol groups and aldehyde groups in a molar ratio of phenol groups to aldehyde groups in the range of from 1:1.5 to 1:2.5. ### Claim 6 (depends on 1) The composition as claimed in claim 1 wherein the phenolic resin has a weight average molecular weight of from 400 to 3,000. ### Claim 7 (depends on 1) The composition as claimed in claim 1 wherein the phenolic resin has a weight average molecular weight of from 700 to 2,000. ### Claim 8 (depends on 1) The composition as claimed in claim 1 wherein the blowing agent is present in an amount of 1 to 20 parts by weight per 100 parts by weight of phenolic resin. ### Claim 9 (depends on 1) The composition as claimed in claim 1 wherein the blowing agent comprises 75% or more is isopropyl chloride. ### Claim 10 (depends on 1) The composition as claimed in claim 1 wherein the hydrocarbon is iso-pentane and is present as 15% by weight of the blowing agent. ### Claim 11 (depends on 1) The composition as claimed in claim 1 wherein the blowing agent blend comprises isopropyl chloride and iso-pentane in a weight ratio of from 60:40 to 95:5. ### Claim 12 (depends on 1) The composition as claimed in claim 1 wherein the blowing agent blend comprises isopropyl chloride and iso-pentane in a weight ratio of from 65:35 to 90:10. ### Claim 13 (depends on 1) The composition as claimed in claim 1 wherein the blowing agent blend comprises isopropyl chloride and iso-pentane in a weight ratio of from 70:30 to 85:15. ### Claim 14 (depends on 1) The composition as claimed in claim 1 wherein the acid catalyst is present in an amount of 5 to 25 parts by weight per 100 parts by weight of phenolic resin. ### Claim 15 (depends on 14) The composition as claimed in claim 14 wherein the acid catalyst comprises at least one of benzenesulphonic acid, para-toluene sulphonic acid, xylene sulphonic, naphthalene sulphonic acid, ethylbenzene sulphonic acid and phenol sulphonic acid. ### Claim 16 (depends on 1) The composition as claimed in claim 1 wherein the inorganic filler is present in an amount of from 1 to 20 parts by weight per 100 parts by weight of phenolic resin. ### Claim 17 (depends on 1) The composition as claimed in claim 1 wherein the plasticiser is present in an amount of 0.1 to 20 parts by weight per 100 parts by weight of phenolic resin. ### Claim 18 (depends on 1) The composition as claimed in claim 1 wherein the plasticiser is present in an amount of 5 parts by weight per 100 parts by weight of phenolic resin, and the plasticiser comprises a polyester polyol that is the reaction product of a polybasic carboxylic acid selected from a dibasic to a tetra basic carboxylic acid with a polyhydric alcohol selected from a dihydric to a pentahydric alcohol. ### Claim 19 (depends on 18) The composition as claimed in claim 18 wherein the polyester polyol has a number average molecular weight of 250 to 350 and a weight average molecular weight of 400 to 550. ### Claim 20 (depends on 18) The composition as claimed in claim 18 wherein the polybasic carboxylic acid used to synthesise the polyester polyol comprises at least one of phthalic acid, isophthalic acid, terephthalic acid, naphthalene-2,3-dicarboxylic acid, naphthalene-1,4-dicarboxylic acid and naphthalene-2,6-dicarboxylic acid. ### Claim 21 (depends on 18) The composition as claimed in claim 18 wherein the polybasic carboxylic acid used to synthesise the polyester polyol comprises one or more of phthalic acid, isophthalic acid, or terephthalic acid. ### Claim 22 (depends on 18) The composition as claimed claim 18 wherein the polyhydric alcohol used to synthesis the polyester polyol comprises at least one of ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, 1,4-butane diol, 1,5-pentane diol, 1,6-hexane diol and neopentyl glycol. ### Claim 23 (depends on 22) The composition as claimed in claim 22 wherein the polyhydric alcohol used to synthesise the polyester polyol comprises one or more of diethylene glycol, propylene glycol, dipropylene glycol, 1,4-butane diol. ### Claim 24 (depends on 1) The composition as claimed in claim 1 comprising a surfactant for the phenolic resin and the surfactant is present in an amount of 1 to 6 parts by weight per 100 parts by weight of phenolic resin. ### Claim 25 (depends on 24) The composition as claimed in claim 24, wherein the surfactant is a castor oil-ethylene oxide adduct wherein more than 20 moles but less than 40 moles of ethylene oxide are added per 1 mole of castor oil. ### Claim 26 (depends on 1) The composition as claimed in claim 1 wherein the modifier is a compound having an amino group and said modifier is present in an amount of 1 to 10 parts by weight per 100 parts by weight of phenolic resin. ### Claim 27 (depends on 26) The composition as claimed in claim 26 wherein the compound having an amino group is selected from urea, dicyandiamide and melamine. ### Claim 28 (depends on 27) The composition as claimed in claim 27 wherein the modifier comprises approximately 5 parts by weight of urea. ### Claim 29 (depends on 1) The composition as claimed in claim 1 wherein the density of phenolic foam is from 10 to 100 kg/m3. ### Claim 30 (depends on 1) The composition as claimed in claim 1 wherein the density of the phenolic foam is from 10 to 45 kg/m3. ### Claim 31 (depends on 1) The composition as claimed in claim 1 wherein the phenolic foam has a closed cell content of 95.5% or more. ### Claim 32 (depends on 1) The composition as claimed in claim 1 wherein the phenolic foam has a limiting oxygen index of 30% or more. ### Claim 33 (depends on 1) The composition as claimed in claim 1 wherein the phenolic foam has a water uptake of less than 0.9 kg/m2. ### Claim 34 (depends on 1) The composition as claimed in claim 1 wherein the phenolic foam has a facing on at least one surface thereof, wherein the facing comprises at least one of glass fibre-non woven fabric, spun bonded-non woven fabric, aluminium foil, bonded-non woven fabric, metal sheet, metal foil, ply wood, calcium silicate-board, plaster board, paper product, and wooden board.