NZ714909B2 - Polystyrene-phenolic foam composites - Google Patents
Polystyrene-phenolic foam composites Download PDFInfo
- Publication number
- NZ714909B2 NZ714909B2 NZ714909A NZ71490914A NZ714909B2 NZ 714909 B2 NZ714909 B2 NZ 714909B2 NZ 714909 A NZ714909 A NZ 714909A NZ 71490914 A NZ71490914 A NZ 71490914A NZ 714909 B2 NZ714909 B2 NZ 714909B2
- Authority
- NZ
- New Zealand
- Prior art keywords
- composite
- expandable
- polystyrene
- expanded
- microspheres
- Prior art date
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- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 239000006260 foam Substances 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 108
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000004005 microsphere Substances 0.000 claims abstract description 74
- 239000002245 particle Substances 0.000 claims abstract description 69
- 229920002223 polystyrene Polymers 0.000 claims abstract description 68
- 239000004793 Polystyrene Substances 0.000 claims abstract description 61
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 60
- 229920003987 resole Polymers 0.000 claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 49
- 239000004416 thermosoftening plastic Substances 0.000 claims abstract description 48
- 239000004794 expanded polystyrene Substances 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 230000002378 acidificating Effects 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000004604 Blowing Agent Substances 0.000 claims description 23
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 14
- 229920001568 phenolic resin Polymers 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 13
- 239000005011 phenolic resin Substances 0.000 claims description 13
- 150000002148 esters Chemical class 0.000 claims description 11
- LGXVIGDEPROXKC-UHFFFAOYSA-N 1,1-Dichloroethene Chemical compound ClC(Cl)=C LGXVIGDEPROXKC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003380 propellant Substances 0.000 claims description 10
- 229920000103 Expandable microsphere Polymers 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 150000007524 organic acids Chemical class 0.000 claims description 7
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 5
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-Vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims description 4
- OYUNTGBISCIYPW-UHFFFAOYSA-N 2-chloroprop-2-enenitrile Chemical compound ClC(=C)C#N OYUNTGBISCIYPW-UHFFFAOYSA-N 0.000 claims description 4
- GYCMBHHDWRMZGG-UHFFFAOYSA-N 2-cyanopropene-1 Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 claims description 4
- RVBFWXYFXKDVKG-UHFFFAOYSA-N 2-ethoxyprop-2-enenitrile Chemical compound CCOC(=C)C#N RVBFWXYFXKDVKG-UHFFFAOYSA-N 0.000 claims description 4
- 229920001567 Vinyl ester Polymers 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 4
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 24
- 239000000463 material Substances 0.000 description 23
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 21
- 235000010338 boric acid Nutrition 0.000 description 21
- 239000004327 boric acid Substances 0.000 description 19
- 239000007788 liquid Substances 0.000 description 19
- 241001438449 Silo Species 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 16
- 229910052799 carbon Inorganic materials 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- OFBQJSOFQDEBGM-UHFFFAOYSA-N pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000007664 blowing Methods 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 230000000717 retained Effects 0.000 description 6
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 238000007792 addition Methods 0.000 description 5
- 150000001299 aldehydes Chemical class 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 150000002484 inorganic compounds Chemical class 0.000 description 5
- 229910010272 inorganic material Inorganic materials 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 239000003607 modifier Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 229920002456 HOTAIR Polymers 0.000 description 4
- QWTDNUCVQCZILF-UHFFFAOYSA-N Isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 235000005985 organic acids Nutrition 0.000 description 4
- 239000011369 resultant mixture Substances 0.000 description 4
- 150000004756 silanes Chemical class 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N Barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 230000003750 conditioning Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000008079 hexane Substances 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002989 phenols Chemical class 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000000454 talc Substances 0.000 description 3
- 229910052623 talc Inorganic materials 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- PZZYQPZGQPZBDN-UHFFFAOYSA-N Aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L Barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L Barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229960003563 Calcium Carbonate Drugs 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N Isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000005187 foaming Methods 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
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- 239000003365 glass fiber Substances 0.000 description 2
- 150000008282 halocarbons Chemical class 0.000 description 2
- 239000001282 iso-butane Substances 0.000 description 2
- NHTMVDHEPJAVLT-UHFFFAOYSA-N isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L mgso4 Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N n-heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
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- 125000001424 substituent group Chemical group 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- ZZXDRXVIRVJQBT-UHFFFAOYSA-N 2,3-dimethylbenzenesulfonic acid Chemical compound CC1=CC=CC(S(O)(=O)=O)=C1C ZZXDRXVIRVJQBT-UHFFFAOYSA-N 0.000 description 1
- IKBFHCBHLOZDKH-UHFFFAOYSA-N 2-chloroethyl(triethoxy)silane Chemical compound CCO[Si](CCCl)(OCC)OCC IKBFHCBHLOZDKH-UHFFFAOYSA-N 0.000 description 1
- CASYTJWXPQRCFF-UHFFFAOYSA-N 2-chloroethyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCl CASYTJWXPQRCFF-UHFFFAOYSA-N 0.000 description 1
- PZTIZDBYLCQIEI-UHFFFAOYSA-N 2-chloroethyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(CCCl)OCC PZTIZDBYLCQIEI-UHFFFAOYSA-N 0.000 description 1
- SGFSMOHWPOFZQW-UHFFFAOYSA-N 2-chloroethyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCl SGFSMOHWPOFZQW-UHFFFAOYSA-N 0.000 description 1
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- JPUCXJPPHJORGK-UHFFFAOYSA-N 2-chloroethyl-methoxy-dimethylsilane Chemical compound CO[Si](C)(C)CCCl JPUCXJPPHJORGK-UHFFFAOYSA-N 0.000 description 1
- IULJSGIJJZZUMF-UHFFFAOYSA-N 2-hydroxybenzenesulfonic acid Chemical compound OC1=CC=CC=C1S(O)(=O)=O IULJSGIJJZZUMF-UHFFFAOYSA-N 0.000 description 1
- FXBOKASTQKMONI-UHFFFAOYSA-N 2-methyl-5-(2-methylphenoxy)benzenesulfonic acid Chemical compound CC1=CC=CC=C1OC1=CC=C(C)C(S(O)(=O)=O)=C1 FXBOKASTQKMONI-UHFFFAOYSA-N 0.000 description 1
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- 239000001095 magnesium carbonate Substances 0.000 description 1
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- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- KVBGVZZKJNLNJU-UHFFFAOYSA-N naphthalene-2-sulfonic acid Chemical compound C1=CC=CC2=CC(S(=O)(=O)O)=CC=C21 KVBGVZZKJNLNJU-UHFFFAOYSA-N 0.000 description 1
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052904 quartz Inorganic materials 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000001603 reducing Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000003014 reinforcing Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- 239000004616 structural foam Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 1
- KQBSGRWMSNFIPG-UHFFFAOYSA-N trioxane Chemical compound C1COOOC1 KQBSGRWMSNFIPG-UHFFFAOYSA-N 0.000 description 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 1
- 229940105963 yttrium fluoride Drugs 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/22—Thermoplastic resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
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- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J2333/20—Homopolymers or copolymers of acrylonitrile
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2339/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2339/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08J2339/08—Homopolymers or copolymers of vinyl-pyridine
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with monohydric phenols
- C08J2361/10—Phenol-formaldehyde condensates
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/02—Homopolymers or copolymers of hydrocarbons
- C08J2425/04—Homopolymers or copolymers of styrene
- C08J2425/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2461/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2461/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2461/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with monohydric phenols
- C08J2461/10—Phenol-formaldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
- C08J9/232—Forming foamed products by sintering expandable particles
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
- C08J9/236—Forming foamed products using binding agents
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/35—Composite foams, i.e. continuous macromolecular foams containing discontinuous cellular particles or fragments
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
Abstract
Polystyrene-phenolic foam composites and precursor compositions comprising expandable polystyrene particles, phenolic resole resin, expandable thermoplastic microspheres, and acidic catalyst are disclosed. The composites exhibit excellent flame resistance properties and may be suitably prepared in standard expanded polystyrene processing equipment. tandard expanded polystyrene processing equipment.
Description
POLYSTYRENE-PHENOLIC FOAM COMPOSITES
FIELD
The present disclosure relates to polystyrene-phenolic foam composites
and to particulate compositions suitable for preparing the composites. The foam
composites possess advantageous properties particularly, although not
exclusively, useful in insulation and fire resisting applications.
BACKGROUND
Polystyrene foam slabs or forms are widely used for thermal and acoustic
insulation in building construction. The conventional process for the production of
a polystyrene foam slab or form is as follows:
1. Expandable polystyrene is supplied from the manufacturer in
particulate form graded for particle size. This particulate polystyrene has a
proportion of blowing agent such as pentane dissolved in it.
2. The particles are exposed to heat, usually by steam, in a fluidised
bed. As the particles pass from the bottom of the fluidised bed to the top, they
soften and as the pentane is lost from solid solution, the released gas causes the
softened polystyrene particles to expand up to fifty times their original volume.
The particles become approximately spherical with a very low density. The
expanded polystyrene particles are collected at the top of the bed. The particles
still contain a small amount of pentane after this primary expansion process.
3. The dry particles are introduced into moulds the walls of which are
penetrated by many small apertures. The dry particles may then be compressed.
Steam is introduced into the vessel containing the polystyrene particles. The
polystyrene particles soften and the residual pentane is released. In this second
stage the volume expansion of the charge is contained by the mould walls forcing
the particles together and fusing them to form a single, lightweight mass of
expanded polystyrene foam.
4. If the mould is in the form of a block, the blocks of expanded
polystyrene are subsequently sliced into slabs. These slices may be used as the
cores of insulating walls or panels.
A disadvantage of polystyrene foams is their high propensity to burn and/or
melt in a fire leading to the loss of structural strength. In contrast, foams with a
16567571_1 (GHMatters) P37447NZPC
phenolic resin matrix, that is phenolic foams, as a class of materials, are known
for their excellent fire resistance and thermal properties, but their commercial
potential in many fields of application is impeded due to their poor structural
properties characterised by high brittleness and friability.
It would be desirable to identify new foam products and compositions that
address one or more of the above limitations.
SUMMARY
There is provided a particulate composition comprising:
(a) expandable polystyrene particles;
(b) reactive phenolic resole resin;
(c) expandable thermoplastic microspheres; and
(d) acidic catalyst.
The particulate composition possesses excellent handling qualities, being
substantially flowable. The advantageous flowability enables ease of transfer and
manipulation of the particles during manufacturing operations. Furthermore,
although the resole resin is highly reactive it is present in the particulate
composition in a latent state and may be suitably activated so as to induce curing.
The reactive phenolic resole resin may be present in the particulate
composition in a partially cured state.
‘Partially cured state’ as used herein means that the phenolic resole resin
may not have been subjected to temperatures above 80°C, or above 70°C. Also,
the phenolic resole resin may not been subjected to temperatures above 80°C, or
not above 70°C, for more than 1 hour. Alternatively, the phenolic resole resin may
not have been subjected to temperatures above 80°C, or not above 70°C, for
more than 0.5 hour.
The particulate composition may be substantially dry. As used in this
context the term ‘substantially’ means that the particulate composition contains
less than 10% by weight water based on the total weight of the composition and
water, or less than 7% by weight water, or less than 5% by weight water, or less
than 3% by weight water, or less than 1% by weight water, or 0% water. The
particulate composition may also be tack-free.
The reactive phenolic resole resin may be substantially insoluble in
16567571_1 (GHMatters) P37447NZPC
water.
The particulate composition as disclosed herein may have any one or
any combination of the above disclosed features.
The particulate composition may further comprise a filler, and particularly
a reinforcing filler. A range of fillers is available. One or more fillers may be used
depending on the characteristics required of the end product. Suitable, non
limiting fillers include particulate silica, talc, kaolin, clay and titanium dioxide,
glass fiber, nanocomposites and nanoparticles. Inorganic compounds, particularly
particulate inorganic compounds, may be utilised. The filler may be present in
amounts of 0.5-60% by weight, or 1-20% by weight, or 2-15% by weight, based
on the total weight of the particulate composition.
The properties of the particulate filler may be suitably modified by
treatment with one or more agents, for example to modify the surface properties
of the filler. Such treatment may, for example, reduce the solubility of soluble
fillers in a liquid, particularly an aqueous liquid. The selection of the modifying
agent(s) will depend on the desired characteristics of the filler. A preferred class
of modifying agents includes silanes.
The filler may have a particle size between 0.1 mm and 5 mm, or
between 0.5 mm and 2 mm. The particulate filler may be granular boric acid.
Granular boric acids of particle size of about 1 mm are suitable. The granular
boric acid may be treated with a silane to yield a silane coated granular boric
acid. The silane serves to reduce the water solubility of the boric acid.
The particulate composition may be prepared by combining expandable
polystyrene particles, phenolic resole resin, thermoplastic expandable
microspheres, and, optionally, filler in the presence of an acidic catalyst.
At least one of the constituents of the particulate composition may be
provided in the form of an aqueous solution, dispersion or suspension. During the
process of forming the particulate composition, which may involve partial curing,
at least some of the water may be removed from the composition, with the result
that the particulate composition becomes substantially dry so that it is free flowing
and easily transferable. As used in this context the term ‘substantially’ means that
the particulate composition contains less than 10% by weight water based on the
16567571_1 (GHMatters) P37447NZPC
total weight of the composition and water, or less than 7% by weight water, or
less than 5% by weight water, or less than 3% by weight water, or less than 1%
by weight water, or 0% water.
Expandable Polystyrene Particles
The expandable polystyrene particles may have an average particle size
between 0.1 and 5 mm, or between 0.5 and 3 mm, or between 0.5 and 1.5 mm,
or between 0.7 and 1.0 mm.
The density of the expandable polystyrene particles may be between 5
3 3 3 3
and 20 kg/m or between 7 and 18 kg/m , or between 9 kg/m and 14
kg/m ,
kg/m .
The expandable polystyrene particles may contain at least one blowing
agent. The preferred polystyrene blowing agent comprises liquid physical
blowing agents, which are volatile liquids and which produce a blowing gas
through vaporisation of the blowing agent or through decomposition of the
blowing agent when heated.
The amount of blowing agent present in the expandable polystyrene
particles may be between 1 and 12% by weight, or between 2 and 10% or
between 4 and 8%.
Numerous blowing agents suitable for use are well known in the art. The
blowing agent may be a liquid having an atmospheric pressure boiling point
between -50° and 100° C, or between 0° and 50° C.
Examples of blowing agents include organic compounds such as
hydrocarbons, halogenated hydrocarbons, alcohols, ketones and ethers. Specific
examples of hydrocarbon blowing agents include propane, butane, pentane, iso-
pentane and hexane. Pentane is an exemplary blowing agent.
The expandable polystyrene particles may be derived from styrene
polymers that are commonly used for preparing polystyrene particles that are to
be blown to form polystyrene foam particles. As well as using styrene as the sole
monomer other addition polymerisable monomers may be used and such
copolymers are embraced by the term polystyrene in this specification. Styrene is
always present as the major component of the polystyrene polymer.
16567571_1 (GHMatters) P37447NZPC
The expandable polystyrene particles may be unexpanded or partially
expanded polystyrene particles or mixtures thereof. The expandable polystyrene
particles may be partially expanded.
The expandable polystyrene particles may be modified by the addition
of one or more additives, such as flame retardants, smoke suppressants,
antistatic agents, flowability improvers, foaming modifiers, and other additives
commonly found or used in expandable polystyrene particles. For example, the
expandable polystyrene particles may be coated or impregnated with carbon or
graphite.
Phenolic Resole Resin
Base-catalysed phenol-formaldehyde resins made with a formaldehyde
to phenol ratio of greater than one (usually around 1.5) are termed resoles. The
phenolic resole resin present in the particulate composition may be derived from
a reactive phenolic resole resin having a viscosity of between 500-4,000cP at a
temperature of 25°C, or between 1000-3000cP at a temperature of 25°C. The
reactive phenolic resole present in the particulate composition may have a water
content of 2-7% by weight based on the total weight of the reactive phenolic
resole resin and water, or water content of 3-6% by weight based on the total
weight of the reactive phenolic resole resin and water. The reactive phenolic
resole resin may have a free phenol content of less than 25% by weight relative
to the total weight of the reactive phenolic resole resin and water, or less than
% by weight, or less than 18% by weight. The free phenol content may be
between 10% and 20% by weight, or between 14% and 18% by weight. The
reactive phenolic resole resin may have a free formaldehyde content of less than
3% by weight, or less than 1% by weight relative to the total weight of the reactive
phenolic resole resin and water. The reactive phenolic resole resin may have a
pH of 7 or less, or a pH of 6.6 or less. The reactive phenolic resole resin may
have any one or any combination of the above disclosed features.
Expandable Thermoplastic Microspheres
The expandable thermoplastic microspheres may have an average
particle size from between 1 and 100 microns, or from between 2 and 50 microns,
or from between 5 and 20 microns. The expandable thermoplastic microspheres
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may be derived from unexpanded or partially expanded microspheres or a
mixture thereof, and comprise a thermoplastic polymer shell made of a
homopolymer or copolymer. Mixtures of different thermoplastic microspheres may
be utilised.
The thermoplastic polymer shell of the thermoplastic microspheres may
be derived from monomers selected from the group consisting of acrylonitrile,
methacrylonitrile, α-chloroacrylonitrile, α-ethoxyacrylonitrile, fumaroacrylonitrile,
crotoacrylonitrile, acrylic esters, methacrylic esters, vinyl chloride, vinylidene
chloride, vinylidene dichloride, vinyl pyridine, vinyl esters, and derivatives or
mixtures thereof.
The thermoplastic polymer shell may be derived from at least vinylidene
chloride monomer.
The expandable microspheres may contain a propellant encapsulated
within the thermoplastic polymer shell. The microspheres may expand by heating
above the boiling point of the propellant and above the softening point of the
polymer shell.
The propellant may be a volatile liquid trapped within the polymer shell.
Suitable propellants include various short chain alkanes and short chain
isoalkanes such as, but not limited to, isopentane, isobutane, n-butane, hexane,
heptane, isooctane, petroleum ether and pentane or mixtures thereof.
Suitable thermoplastic microspheres may begin to soften in the range
70-100°C, or 85-95°C, and maximum expansion may occur in the range of 100-
150°C, or 115-125°C.
The expandable thermoplastic microspheres may be provided in the
form of an aqueous dispersion and then added to form the particulate
composition as this aqueous dispersion. The amount of expandable microspheres
in the aqueous dispersion may be between 2 and 60% by weight based on the
total weight of the aqueous dispersion, or between 5 and 40% by weight based
on the total weight of the dispersion, or between 10 and 25% by weight based on
the total weight of the dispersion.
The expandable microspheres may be combined with one or more
fillers prior to mixing with the other components to form the particulate
16567571_1 (GHMatters) P37447NZPC
composition. Preferably an aqueous dispersion of expandable microspheres is
treated with the particulate filler. If required, the filler may be pre-treated with a
suitable modifying agent.
Acidic Catalyst
The acidic catalyst may be a strong inorganic or organic acid or their
esters. Strong organic acids include sulphonic acids and their esters including
benzene sulphonic acid, toluene sulphonic acid, phenol sulphonic acid, xylene
sulphonic acid, β-naphthalene sulphonic acid, α-naphthalene sulphonic acid,
esters thereof and mixtures thereof. The acids may further include weak inorganic
acids and their esters, either alone or in admixture. The acids that may be
employed still further include mixtures of two or more of strong organic acids;
mixtures of two or more of esters of strong organic acids; mixtures of two or more
of weak inorganic acids; and mixtures of two or more of esters of weak inorganic
acids, as well as mixtures of different acids or their esters. Suitable catalysts are
phosphate esters and blends of phosphoric acid with strong organic acids such
as para-toluene sulphonic acid or any other sulphonic acid or its ester. Mixtures of
any two or more of the acids and/or esters can also be used.
Other Components
Other components may be included in the composition to improve
particular physical properties or to reduce costs. These may be added to one or
more of the expandable polystyrene, the phenolic resole resin or the
thermoplastic microspheres or at any stage of mixing these components to form
the particulate composition. For example, fire retardants containing, for example,
chlorine, bromine, boron, phosphorous or ammonia, especially ammonium
phosphate may be added to improve fire resistance. Expandable graphite can
also be usefully employed. The graphite expands when exposed to high
temperatures as encountered in a fire.
One or more surfactants may also be present in the composition.
Suitable surfactants include silicone polyethers particularly silicone glycol
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copolymers. Water repellents, such as silicon containing aqueous emulsions may
also be added to control or reduce water absorption.
One or more of the constituents of the particulate composition may be
treated with other additives and/or modifiers. For example they may be treated
with a thermal conductivity modifier such as carbon, particularly an aqueous
dispersed carbon. The thermoplastic microspheres may be treated with a thermal
conductivity modifier such as carbon, particularly an aqueous dispersed carbon
prior to combining with the other components of the particulate composition.
As described above, the particulate composition as herein disclosed
comprises a phenolic resole resin that may be cured.
There is also provided a polystyrene-phenolic foam composite formed
by curing the phenolic resole resin as disclosed herein, in the presence of an
acidic catalyst, expandable polystyrene particles and expandable thermoplastic
microspheres, and, optionally, a filler. The composite may be characterised by the
expanded polystyrene and/or the expanded thermoplastic microspheres being, at
least in part, solubilised and/or mixed in the cured phenolic resin. The expanded
polystyrene and/or the expanded thermoplastic microspheres may also be, at
least in part, chemically reacted with the cured phenolic resin to form covalent
bonds.
There is also provided a polystyrene-phenolic foam composite
comprising:
(a) expanded polystyrene;
(b) cured phenolic resole resin; and
(c) expanded thermoplastic microspheres.
There is also provided a polystyrene-phenolic foam composite
comprising:
(a) expanded polystyrene;
(b) cured phenolic resole resin; and
(c) expanded thermoplastic microspheres.
wherein the expanded polystyrene and/or the expanded thermoplastic
microspheres are, at least in part, solubilised and/or mixed in the cured phenolic
resin.
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There is also provided a polystyrene-phenolic foam composite
comprising:
(a) expanded polystyrene;
(b) cured phenolic resole resin; and
(c) expanded thermoplastic microspheres;
wherein the composite has a specific mass loss rate @ 50kW/m , measured
according to ISO 17554, of less than 8 g/m .s, or less than 6 g/m .s, or less than
4 g/m .s, or less than 2 g/m .s.
There is also provided a polystyrene-phenolic foam composite
comprising:
(a) expanded polystyrene;
(b) cured phenolic resole resin; and
(c) expanded thermoplastic microspheres;
wherein the composite exhibits insulation failure times, according to AS1530.4,
for a 100 mm thick panel, of greater than 30 minutes, or greater than 20 minutes,
or greater than 10 minutes.
The foam composites as disclosed herein may comprise from 20 to 80
wt.% of (a), from 20 to 60 wt.% of (b) and from 0.5 to 5 wt.% of (c) based on the
total weight of the composites, or the composites comprises from 35 to 65 wt.% of
(a), from 25 to 50 wt.% of (b) and from 1.5 to 5 wt.% of (c) based on the total
weight of the composites.
The foam composites as disclosed herein may advantageously possess
low interstitial volume. While not wishing to be bound by theory it is believed that
solubilisation and/or mixing of the polystyrene and/or thermoplastic microsphere
phases in the phenolic phase accounts, at least in part, for the low interstitial
volume. The interstitial volume may be 5% or less, or 3% or less, or 1% or less, or
0.5% or less, or 0.3% or less.
The foam composites as disclosed herein may advantageously possess
low water absorption in accordance with ASTM C272 (Standard Test Method for
Water Absorption of Core Materials for Sandwich Constructions). The water
absorption of the foam composites may be 8% by volume or less, or 7% by
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volume or less, or 5% by volume or less. The water absorption may also be
between 4 and 8% by volume, or between 5 and 7% by volume.
The foam composites as disclosed herein possess excellent physical
and chemical properties. They are highly fire resistant and the cured phenolic
resole resin is not rigid and brittle but is, conversely, tough and resilient in nature.
The polystyrene-phenolic foam composites may further comprise one
or more fillers or treated fillers, as hereinbefore described.
Expanded Polystyrene
The expanded polystyrene may be derived from expandable
polystyrene particles having an average particle size from between 0.1 and 5 mm,
or between 0.5 and 3 mm, or between 0.5 and 1.5 mm.
The expandable polystyrene particles may contain at least one blowing
agent. The preferred polystyrene blowing agent comprises liquid physical
blowing agents, which are volatile liquids which produce a blowing gas through
vaporisation of the blowing agent or through decomposition of the blowing agent
when heated.
Numerous blowing agents suitable for use are well known in the art.
Ideally, the blowing agent should be a liquid having an atmospheric pressure
boiling point between -50° and 100° C, or between 0° and 50° C.
Examples of blowing agents include organic compounds such as
hydrocarbons, halogenated hydrocarbons, alcohols, ketones and ethers. Specific
examples of hydrocarbon blowing agents include propane, butane, pentane,
isopentane and hexane. Pentane is a preferred blowing agent.
The expandable polystyrene particles as used herein are derived from
styrene polymers that are commonly used for preparing polystyrene particles that
are to be blown to form polystyrene foam particles. As well as using styrene as
the sole monomer other addition polymerisable monomers may be used and such
copolymers are embraced by the term polystyrene in this specification. Styrene is
always present as the major component of the polystyrene polymer.
The expandable polystyrene particles as used herein may be
unexpanded or partially expanded polystyrene particles or mixtures thereof. This
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enables relatively high levels of expanded polystyrene to be incorporated into the
final foam composite.
The expandable polystyrene particles as used herein may be modified
by the addition of one or more additives, such as flame retardants, smoke
suppressants, antistatic agents, flowability improvers, foaming modifiers, and
other additives commonly found or used in expandable polystyrene particles.
Cured Phenolic Resole Resin
The cured phenolic resole resin may be formed from the phenolic
resole resin, as disclosed herein, through the application of heat. Steam is a
preferred source of heat and the preferred curing treatment.
Expanded Thermoplastic Microspheres
The expanded thermoplastic microspheres are derived from
expandable thermoplastic microspheres having an average particle size from
between 1 and 100 microns, or from between 2 and 50 microns, or from between
and 20 microns. The expanded thermoplastic microspheres may be derived
from unexpanded or partially expanded microspheres or a mixture thereof, and
comprise a thermoplastic polymer shell made of a homopolymer or copolymer.
The thermoplastic polymer shell of the thermoplastic microspheres is
derived from monomers selected from the group consisting of acrylonitrile,
methacrylonitrile, α-chloroacrylonitrile, α-ethoxyacrylonitrile, fumaroacrylonitrile,
crotoacrylonitrile, acrylic esters, methacrylic esters, vinyl chloride, vinylidene
chloride, vinylidene dichloride, vinyl pyridine, vinyl esters, and derivatives or
mixtures thereof.
The thermoplastic polymer shell may be derived from vinylidene
chloride monomer.
The expandable microspheres may contain a propellant encapsulated
within the thermoplastic polymer shell. The microspheres may expand by heating
above the boiling point of the propellant and above the softening point of the
polymer shell.
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The propellant may be a volatile liquid trapped within the polymer shell.
Suitable propellants include various short chain alkanes and short chain
isoalkanes such as, but not limited to, isopentane, isobutane, n-butane, hexane,
heptane, isooctane, petroleum ether and pentane or mixtures thereof.
Suitable thermoplastic microspheres may begin to soften in the
temperature range of 70-100°C, or 85-95°C and maximum expansion may occur
in the temperature range of 100-150°C, or 115-125°C.
Other Components
Other components may be included in the foam composites, such as
those described in relation to prior art polystyrene foams and as disclosed
hereinbefore in respect of particulate compositions.
Properties of the Foam Composites
A feature of the composites is the plasticisation and physical and/or
chemical interaction of the cured phenolic resole resin with the thermoplastic shell
of the microspheres and/or with the polystyrene particles. The phenolic resin may
solubilise, and/or mix, and/or cross-link with the thermoplastic
homopolymer/copolymer of the microspheres and/or polystyrene particles and, as
a result, a composite product is formed. When the composite is exposed to a heat
source it advantageously maintains its structural integrity.
The solubilisation and/or mixing and/or chemical interaction may
account for, at least in part, the low interstitial volume and low water absorption of
the foam composites.
Where physical interaction occurs this may be in the form of polymer
entanglement which may form an interpenetrating polymer network.
The foam composites are resilient or semi-resilient and non-friable
compared to other structural foams. Densities may be produced in the range 10-
50 kg/m3, preferably 10-40 kg/m , more preferably 10-30 kg/m depending on
formulation and additives. Despite the apparently flammable microsphere and
polystyrene content, the foam composites are highly resistant to temperature and
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fire, likely in part due to the solubilisation and/or mixing and/or chemical
interaction of the polymer shell of the microspheres and/or the polystyrene by the
phenolic resin. Desirable flame stability is also observed whereas conventional
phenolic foams and resin are often subject to spalling/punking.
The advantageous fire resistance is surprising. It is believed that the
thermoplastic microspheres and polystyrene particles become thermosetting and
therefore char on exposure to heat. This contrasts to thermoplastic resins which
melt on heating.
There is also provided a composite block comprising the foam
composite as disclosed herein.
There is also provided a panel or a sheet comprising the foam
composite as disclosed herein.
The blocks, panels and/or sheets find advantageous use in applications
requiring thermal and/or acoustic insulation, for example, in construction.
There is also provided a construction material comprising the blocks,
panels and/or sheets as disclosed herein.
Throughout this specification, use of the terms “comprises” or
“comprising” or grammatical variations thereon shall be taken to specify the
presence of stated features, integers, steps or components but does not preclude
the presence or addition of one or more other features, integers, steps,
components or groups thereof not specifically mentioned.
For the sake of brevity, only certain ranges are explicitly disclosed
herein. However, ranges from any lower limit may be combined with any upper
limit to recite a range not explicitly recited, as well as, ranges from any lower limit
may be combined with any other lower limit to recite a range not explicitly recited,
in the same way, ranges from any upper limit may be combined with any other
upper limit to recite a range not explicitly recited.
DETAILED DESCRIPTION
It will now be convenient to describe the disclosure with reference to
particular embodiments and examples. These embodiments and examples are
illustrative only and should not be construed as limiting upon the scope of the
disclosure. It will be understood that variations upon the described disclosure as
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would be apparent to the skilled addressee are within the scope of the disclosure.
Similarly, the present disclosure is capable of finding application in areas that are
not explicitly recited in this document and the fact that some applications are not
specifically described should not be considered as a limitation on the overall
applicability of the disclosure.
Thermoplastic Microspheres
When thermoplastic microspheres are heated, the polymeric shell
gradually softens, and the liquid within the shell begins to gasify and expand.
When the heat is removed, the shell stiffens and the microsphere remains in its
expanded form. When fully expanded, the volume of the microspheres increases
more than 40 times. Significant density reductions can be achieved with even a
small concentration of, for example, 3% thermoplastic microspheres by weight.
The most obvious benefit of the hollow microsphere is the potential to reduce part
weight, which is a function of density. Compared to traditional mineral-based
additives, such as calcium carbonate, gypsum, mica, silica and talc, hollow
microspheres have much lower densities. Typical loadings are 1.5-5% by weight,
which can equate to 25% or more by volume.
The expandable thermoplastic microspheres suitable for preparing the
compositions and foam composites as disclosed herein may be utilised in various
forms. They may be in the form of a slurry dispersed in water or they may be
utilised in dry form. Aqueous dispersions are preferred. Suitable microspheres are
supplied by AkzoNobel under the trade mark Expancel®.
Phenolic Resole Resin
A phenolic resole resin suitable for curing, that is, to form a partially
cured or substantially completely cured resin as disclosed herein, may be
produced by the base-catalysed condensation reaction of a molar excess of an
aldehyde, with a substituted or unsubstituted phenol. Preferred substituted
phenols are those in which the substituent does not impede the condensation of
the phenol(s) with the aldehyde(s). Suitable substituents include halogens or a
hydroxy, alkyl or an aryl group. Unsubstituted phenol is most preferred. Suitable
aldehydes are formaldehyde (including oligomers/polymers such as trioxane),
furfural, sugars and cellulose hydrolysates. A preferred aldehyde is formaldehyde.
16567571_1 (GHMatters) P37447NZPC
In one embodiment the molar ratio of aldehyde to phenol is from 1.4 to 1.8:1, for
example, about 1.6:1. In a preferred method the temperature at which the
phenolic resole resin is prepared should not exceed 65°C, for example no more
than 60°C±2°C or no more than about 60°C. This limiting temperature of 65°C is
preferably maintained while the basic catalyst is active, that is, until the basic
catalyst is neutralised. This limiting temperature allows the maximum substitution
of the phenol aromatic ring by reactive methylol (-CH OH) groups and results in
only low molecular weight development in the polymer. Water may then be
optionally distilled off to the preferred specification. Due to the resulting low
molecular weight (preferably less than 1000 Daltons), the reactive phenolic resole
resin is highly soluble in water without phase separation and remains sufficiently
reactive to cross-link under dilute aqueous conditions.
Suitable alkaline condensation catalysts are ammonia, ammonium
hydroxide, sodium hydroxide, potassium hydroxide and barium hydroxide.
Sodium hydroxide is a preferred catalyst.
The phenolic resole resin may be produced from phenol with a molar
excess of formaldehyde in the presence of sodium hydroxide as a condensation
catalyst.
Conventional phenolic resins are produced by carefully increasing the
temperature to around 60±2°C and holding there for a period of about 1 hour,
after which the temperature is increased to around 80°C for a further period of 2-4
hours. The two stages essentially are:
(1) Ring Substitution at 60°C by formaldehyde into the phenol aromatic ring;
(2) Condensation Polymerisation at 80°C to increase molecular weight.
In contrast, the present reactive phenolic resole resin may be obtained,
for example, by only heating to no more than 65°C, for example, no more than
60±2°C or no more than about 60°C for a period of about 5 hours or until an
intermediate viscosity of 13.5-14.5 centiStokes at 25°C is reached for the reaction
mixture. This leads to maximum substitution by methylol (-CH OH) groups in
ortho-, meta- and para- positions of the aromatic ring and only low molecular
weight build. The mixture is then neutralised with an acid such as para-toluene
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sulphonic acid to a pH of less than 7, or 5.5-6.6, or about 6 and most of the
process and reaction water may then be distilled off under vacuum down to a
level of around 2-7%, resulting in a highly reactive material.
Fillers
The particulate composition and/or the phenolic composites as
disclosed herein may comprise one or more fillers. Suitable, non limiting fillers
include inorganic compounds, particularly particulate inorganic compounds.
Preferred fillers include elemental metal selected from the group
consisting of metals of Groups I, II, III and IV, transition metals or the like of the
periodic table, oxides or complex oxides of these metals, salts of these metals,
such as fluorides, carbonates, sulfates, silicates, hydroxides, chlorides, sulfites,
and phosphates of these metals, and composites of these salts of metals.
Preferably used are metal oxides such as amorphous silica, quartz, alumina,
titania, zirconia, barium oxide, yttrium oxide, lanthanum oxide, and ytterbium
oxide, silica-based complex oxides such as silica-zirconia, silica-titania, silica-
titania-barium oxide, and silica-titania-zirconia, glass such as borosilicate glass,
glass fibres, aluminosilicate glass, or fluoroaluminosilicate glass, metal fluorides
such as barium fluoride, strontium fluoride, yttrium fluoride, lanthanum fluoride,
and ytterbium fluoride; inorganic carbonates such as calcium carbonate,
magnesium carbonate, strontium carbonate, and barium carbonate; and metal
sulfates such as magnesium sulfate and barium sulfate. Other suitable fillers
include particulate silica, talc, kaolin, clay, nanocomposites and nanoparticles.
Other inorganic compounds such as boric acid may be utilised as a filler.
The filler may be present in amounts of 0.5-60% by weight, or 1-20% by
weight, or 2-15% by weight, based on the total weight of the particulate
composition.
The filler may have a particle size between 0.1 mm and 5 mm, or
between 0.5 mm and 2 mm. The filler may be granular boric acid. Granular boric
acids of particle size of about 1 mm are suitable.
Modified Fillers
Often it is advantageous to treat fillers with a modifiying agent so as to
modify the surface properties of the filler. For example fillers may be modified with
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agents so as to change the fillers solubility properties. Suitable modifiying agents
are well known in the art. One preferred class of modifying agents are silanes.
One class of silanes are haloalkylsilanes examples of which are 3-
chloropropyltrimethoxysilane, 3-chloropropyltriethoxysilane,
3-chloropropyltripropoxysilane, chloropropylmethyldimethoxysilane,
chloropropylmethyldiethoxysilane, chloropropyldimethylethoxysilane,
chloropropyldimethylmethoxysilane, chloroethyltrimethoxysilane,
chloroethyltriethoxy-silane, chloroethylmethyldimethoxysilane,
chloroethylmethyldiethoxysilane, chloroethyldimethylmethoxysilane,
chloroethyldimethylethoxysilane, chloromethyltriethoxy-silane,
chloromethyltrimethoxysilane, chloromethylmethyl-dimethoxysilane,
chloromethylmethyldiethoxysilane, chloro-methyldimethylmethoxysilane or
chloromethyldimethylethoxysilane.
Granular boric acid may be treated with one or more of the above silanes so as to
reduce the solubility of the boric acid in water.
Materials and Process
In an exemplary embodiment a preblend of the following components
as described herein may be prepared. After combining the components the
preblend may be stored for future use. The specific gravity of the mixture may be
in the range 1.4 to 1.7. Continuous slow agitation during the manufacturing
process may be utilised.
Preblend %.w/w
Expandable thermoplastic microspheres 9.3%
Boric acid 56.0%
Carbon dispersion 15.6%
Surfactant 0.4%
Acidic catalyst 18.7%
The preblend may be combined with reactive phenolic resole to form a
reactive liquid matrix in the exemplary proportions shown below. This liquid matrix
may have a shelf life of between 4 and 10 minutes at about 20°C after which time
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exothermic cross linking may occur. The rate of cross linking is temperature
dependent.
Liquid matrix %.w/w
Reactive phenolic resole 76%
Preblend 24%
The liquid matrix may be used to coat partially expanded polystyrene
particles in the exemplary proportions (and exemplary ranges) shown below.
Foam composite %.w/w
Partially expanded polystyrene 45% (25% to 65%)
Liquid Matrix 55% (35% to 70%)
Coating
Coating may be performed in a batch mixer such as a ribbon type mixer.
The components may also be blended in a continuous process by preparing the
liquid matrix immediately prior to coating partially expanded polystyrene particles.
A stream of partially expanded polystyrene particles may be introduced
into, for example, a rotating drum beneath liquid matrix feed streams such that
the liquid matrix is drizzled over the surface of the moving partially expanded
polystyrene particles. Rotation of the drum may facilitate even distribution of the
matrix evenly over the surfaces of the partially expanded polystyrene particles.
The absence of any form of strakes or mixing impellors in the rotating
drum may advantageously eliminate the matrix coming into contact with other
surfaces, and potential adherence to parts of the mixer.
Conditioning (B-Staging) to form particulate composition
Conditioning may conveniently be performed in, for example, a rotating
drum. Air heated to between, for example, 45°C and 60°C may be passed
through the drum and the coating material may progressively lose free water and
may initiate cross linking and bond development between the partially expanded
polystyrene and the matrix.
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During the conditioning process the product characteristic may change
from a wet free flowing high viscosity fluid to a sticky plastic, and finally to discrete
clumps of lightly adhering mixture.
Coated product exiting the drum may drop on to a mesh conveyor belt or
tray. The belt may be fully enclosed in a heated chamber with suitable means of
passing air heated to between, for example, 45°C and 60°C over the coated
product. The size and speed of the belt or tray may be such that the coated
product remains as an undisturbed 100mm thick layer for about 45 mins duration.
Discharge off the belt into a grizzly feeder or combination of granulator
and sizing mesh may be required to break down the aggregated material into
discrete coated grains ready for conveying into storage prior to composite
formation.
Composite formation
Clamshell style vacuum assisted expanded polystyrene block moulding
equipment may be suitable for processing the coated product into blocks. Coated
product may be allowed to come to equilibrium in a fully vented storage space
where the temperature preferably does not exceed 20°C for between 4hrs and
48hrs from coating. Air transport may be used to convey material to standard
block moulder filling guns via a de-dusting station to remove any fines generated
during the coated product handling processes.
A standard expandable polystyrene block making cycle may be
employed with maximum steam pressure being for example about 2 bar and
utilising gentle cross steaming with vacuum assistance. Polishing of mould
surfaces may be utilised so as to minimise mechanical keying of the matrix to the
mould surface thereby facilitating clean ejection of the finished block.
Fire Resistance Testing
Fire resistance may be tested in terms of integrity and insulation.
Integrity
Integrity may be defined as the ability of an element of construction
to resist the passage of flames and hot gases from one space to another when
tested in accordance with AS1530.4. Failure of integrity criteria is deemed to
occur when continuous flaming occurs on the non-exposed side of the test
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specimen, or when cracks, fissures and other openings through which hot flames
and gases can pass through are present.
Insulation
Insulation may be defined as the ability of an element of
construction to maintain a temperature on the surface that is not exposed to a
heat source, below the limits specified, when tested in accordance with Australian
Standard AS1530.4 (Fire Resistance Test to Building Material). Failure for
insulation criteria is deemed to have occurred when the temperature rise of the
non exposed side exceeds predetermined thresholds.
Panels prepared from composites according to the present
disclosure achieve 30 mins insulation for 100 mm thick panels when tested
according to AS1530.4.
EXAMPLES
The following example utilised the components as set out in Table
1. The weights of the thermoplastic microspheres and the carbon dispersion
include water present in the materials.
Example 1
Table 1
Material % w/w
Expanded 69.7
polystyrene
(Lambdapor 753p)
Phenolic resole resin 23.2
Thermoplastic 1.74
microspheres
(Expancel® 820
SLU40)
Treated boric acid 3.48
Aqueous carbon 0.46
dispersion
16567571_1 (GHMatters) P37447NZPC
Catalyst (p-toluene 1.39
sulphonic acid)
Preparation of microsphere composition
Particulate boric acid was treated with 3-
chloropropyltrimethoxysilane followed by heating the mixture to 70°C for 30mins.
A microsphere composition comprising expandable thermoplastic
microspheres, coated boric acid, carbon dispersion and catalyst was prepared by
mixing the components in a plough-share mixer for 5 mins. The resultant blend
was then sieved through a vacuum assisted Buchner funnel fitted with 1mm
aperture square mesh.
Preparation of the particulate composition
Polystyrene was expanded to a density of 18kg/m and retained in a
silo for 11 hrs. The partially expanded polystyrene was fed into a mixing head at a
rate of 68 litres/min. The phenolic resole resin was pumped into the mixing head
at a rate of 0.68kg/min. The microsphere composition was pumped into the
mixing head at a rate of 0.208kg/min.
A multi stream nozzle fed a curtain of phenolic resin and
microsphere composition over the moving polystyrene particles at a temperature
between 15°C and 30°C.
After approximately 3 minutes the resultant mixture was fed into a
second rotating drum with a hot air curtain blowing over the mix. The air
temperature was maintained between 50°C and 75°C with a transit time of 10
mins.
The discharge was transferred to a fluid bed and held at 35°C for up
to 45 minutes. This material was then fed via air transport to a cloth silo, where it
was held for 24 hours.
Preparation of polystyrene/phenolic composite
The material was then removed from the silo by suction and blown
into a block moulder silo and drained down to fill a block mould. Once the mould
was filled, a steam cycle was commenced which yielded the completed
composite within 10 mins.
16567571_1 (GHMatters) P37447NZPC
Example 2
Preparation of microsphere composition
Particulate boric acid was treated with 3-
chloropropyltrimethoxysilane followed by heating the mixture to 70°C for 30mins.
A microsphere composition comprising expandable thermoplastic
microspheres, coated boric acid, and carbon dispersion was prepared by mixing
the components in a plough-share mixer for 5 mins. The resultant blend was then
sieved through a vacuum assisted Buchner funnel fitted with 1mm aperture
square mesh.
Preparation of the particulate composition
Polystyrene was expanded to a density of 18kg/m and retained in
a silo for 11hrs. The partially expanded polystyrene was fed into a mixing head at
a rate of 68 litres/min. The phenolic resole resin was pumped into the mixing
head at a rate of 0.68kg/min. The microsphere composition was pumped into the
mixing head at a rate of 0.167kg/min.
A multi stream nozzle fed a curtain of phenolic resin and
microsphere composition over the moving polystyrene particles in a mixer at a
temperature between 15°C and 30°C. Catalyst was added to the mixture at the
mixer discharge at a rate of 0.0488kg/min.
After approximately 3 minutes the resultant mixture was fed into a
second rotating drum with a hot air curtain blowing over the mix. The air
temperature was maintained between 50°C and 75°C with a transit time of 10
mins.
The discharge was transferred to a fluid bed and held at 35°C for
up to 45 minutes. This material was then fed via air transport to a cloth silo, where
it was held for 24 hours.
Preparation of polystyrene/phenolic composite
The material was then removed from the silo by suction and blown
into a block moulder silo and drained down to fill a block mould. Once the mould
was filled, a steam cycle was commenced which yielded the completed
composite within 10 mins.
16567571_1 (GHMatters) P37447NZPC
In an alternate experiment the material from the silo was used to fill
multiple sheet moulds and the moulds were subsequently steamed for 10 mins to
produce completed sheets.
Example 3
Preparation of microsphere composition
Particulate boric acid was treated with 3-
chloropropyltrimethoxysilane followed by heating the mixture to 70°C for 30mins.
The material was sieved and the fraction retained on BS#10 mesh discarded.
A microsphere composition comprising expandable thermoplastic
microspheres, carbon dispersion and catalyst was prepared by mixing the
components in a plough-share mixer for 5 mins.
Preparation of the particulate composition
Polystyrene was expanded to a density of 18kg/m and retained in
a silo for 11hrs. The partially expanded polystyrene was fed into a mixing head at
a rate of 68 litres/min. The phenolic resole resin was pumped into the mixing
head at a rate of 0.68kg/min. The microsphere composition was pumped into the
mixing head at a rate of 0.105kg/min. The treated boric acid was fed into the
mixing head at a rate of 0.102 kg/min.
A multi stream nozzle fed a curtain of phenolic resin and
microsphere composition over the moving polystyrene particles in a mixer at a
temperature between 15°C and 30°C.
After approximately 3 minutes the resultant mixture was fed into a
second rotating drum with a hot air curtain blowing over the mix. The air
temperature was maintained between 50°C and 75°C with a transit time of 10
mins.
The discharge was transferred to a fluid bed and held at 35°C for up
to 45 minutes. This material was then fed via air transport to a cloth silo, where it
was held for 24 hours.
Preparation of polystyrene/phenolic composite
The material was then removed from the silo by suction and blown
into a block moulder silo and drained down to fill a block mould. Once the mould
16567571_1 (GHMatters) P37447NZPC
was filled, a steam cycle was commenced which yielded the completed
composite within 10 mins.
In an alternate experiment the material from the silo was used to fill
multiple sheet moulds and the moulds were subsequently steamed for 10 mins to
produce completed sheets.
Example 4
Preparation of microsphere composition
Particulate boric acid was treated with 3-
chloropropyltrimethoxysilane followed by heating the mixture to 70°C for 30mins.
The material was sieved and the fraction retained on BS#10 mesh discarded.
A microsphere composition comprising expandable thermoplastic
microspheres, carbon dispersion and catalyst was prepared by mixing the
components in a plough-share mixer for 5 mins.
Preparation of the particulate composition
Polystyrene was expanded to a density of 18kg/m and retained in a
silo for 11hrs. The partially expanded polystyrene was fed into a mixing head at a
rate of 68 litres/min. The phenolic resole resin was pumped into the mixing head
at a rate of 0.68kg/min. The microsphere composition was pumped into the
mixing head at a rate of 0.105kg/min. The treated boric acid was fed into the
mixing head at a rate of 0.102 kg/min.
A multi stream nozzle fed a curtain of phenolic resin and
microsphere composition over the moving polystyrene particles in a mixer at a
temperature between 15°C and 30°C.
After approximately 3 minutes the resultant mixture was fed into a
second rotating drum with a hot air curtain blowing over the mix. The air
temperature was maintained between 50°C and 75°C with a transit time of 10
mins.
The discharge was transferred to a fluid bed and held at 35°C for up
to 45 minutes. This material was then fed via air transport to a cloth silo, where it
was held for 24 hours.
Preparation of polystyrene/phenolic composite
16567571_1 (GHMatters) P37447NZPC
The material was then removed from the silo by suction and blown
into a continuous tractor type moving belt panel press with our without using
facing steel sheets on two faces. The material in the press was steamed as it
progressed through the press to form completed sheets or completed insulated
panel sith steel, aluminium or other material facings. The continuous press was
moving a between 1 and 15 metres/min.
Table 2 indicates the formulations of other composites prepared as
Example 1.
Table 2
Run no. 1 2 3 4 5 6 7
Expanded
Polystyrene
%(w/w) 38.7 52.5 64.8 58.4 52.3 53.5 52.6
Phenolic
Resin %(w/w) 47.0 36.4 27.0 31.9 35.8 36.6 36.0
Thermoplastic
Microspheres
%(w/w) 3.5 2.7 2.0 2.4 3.6 1.5 2.7
Treated Boric
Acid %
(w/w) 7.0 5.5 4.0 4.8 5.4 5.5 5.4
Carbon
Dispersion
%(w/w) 0.9 0.7 0.5 0.6 0.7 0.7 0.7
Catalyst %
(w/w) 2.8 2.2 1.6 1.9 2.2 2.2 2.2
It was found that all of the composites had excellent physical
properties (low interstitial volume and low water absorption) demonstrating
advantage over a wide range of relative component amounts. The mechanical
properties of the composites were equivalent to expanded polystyrene.
16567571_1 (GHMatters) P37447NZPC
Fire resistance testing
Test specimens consisted of insulated wall panels comprising foam
composites as prepared by the processes disclosed herein. The panels were 3.0
m high, 1.2 m or 0.6 m broad and had a thickness of 50 mm, 100 mm and 250
mm. A comparative test was performed with a 125 mm thick expanded
polystyrene panel. Tests were conducted in accordance with AS 1530.4 ‘Methods
for fire tests on building materials, components and structures, Part 4: Fire
resistance tests of elements of construction, Section 3 Walls – Vertical Separating
Elements’. The results are collected in Table 3.
Table 3
Material and thickness Insulation failure time
(minutes)
Inventive composite 50 mm 15
Inventive composite 100 mm 31
Inventive composite 250 mm 115
Comparative Polystyrene 125 mm 6
It is clear from the results that the composites disclosed herein
significantly outperform expanded polystyrene in fire resistance.
Tests were also conducted following ISO 17554. This is a small-scale
method for assessing the mass loss rate of essentially flat specimens exposed in
the horizontal orientation to controlled levels of radiant heating with an external
igniter under well-ventilated conditions. The mass loss rate is determined by
16567571_1 (GHMatters) P37447NZPC
measurement of the specimen mass and is derived numerically. Mass loss rate
can be used as an indirect measure of heat release rate.
Under the conditions of the test expanded polystyrene had an average
specific mass loss rate @ 50kW/m , over three tests, of 9.81 g/m .s, whereas the
composites disclosed herein had an average specific mass loss rate @ 50kW/m ,
over three tests, of 1.27 g/m .s. Accordingly, significantly slower combustion was
observed with the inventive composites.
16567571_1 (GHMatters) P37447NZPC
Claims (24)
1. A particulate composition comprising: (a) expandable polystyrene particles; (b) reactive phenolic resole resin; (c) expandable thermoplastic microspheres; and (d) acidic catalyst, wherein the reactive phenolic resole resin is present in the particulate composition in a partially cured state.
2. A composition according to claim 1 wherein the expandable polystyrene particles are partially expanded.
3. A composition according to claim 1 or claim 2 wherein the density of the expandable polystyrene particles is between 5 kg/m and 20 kg/m
4. A composition according to any one of claims 1 to 3 further comprising one or more fillers.
5. A composition according to claim 4 wherein the filler is present in an amount of 0.5 – 60% by weight based on the total weight of the composition.
6. A composition according to claim 5 wherein the filler is a surface treated filler.
7. A composition according to any one of claims 1 to 6 wherein the phenolic resole resin is derived from a reactive resole resin having one or more of the following properties: (a) a viscosity between 500 and 4,000 cP; (b) a water content between 2 and 7% by weight; (c) a free phenol content less than 25%; or 16567571_1 (GHMatters) P37447NZPC (d) a free formaldehyde content of less than 3%.
8. A composition according to any one of claims 1 to 7 wherein the expandable thermoplastic microspheres have an average particle size from between 1 and 50 microns and wherein the expandable microspheres contain a propellant encapsulated within a thermoplastic polymer shell.
9. A composition according to claim 8 wherein the thermoplastic polymer shell is derived from monomers selected from the group consisting of acrylonitrile, methacrylonitrile, α-chloroacrylonitrile, α-ethoxyacrylonitrile, fumaroacrylonitrile, crotoacrylonitrile, acrylic esters, methacrylic esters, vinyl chloride, vinylidene chloride, vinylidene dichloride, vinyl pyridine, vinyl esters, and derivatives or mixtures thereof.
10. A composition according to any one of claims 1 to 9 wherein the acidic catalyst is selected from a strong organic acid, an ester of a strong organic acid, a weak inorganic acid, an ester of a weak inorganic acid or mixtures thereof.
11. A polystyrene-phenolic foam composite comprising: (a) expanded polystyrene; (b) cured phenolic resole resin; and (c) expanded thermoplastic microspheres, wherein the composite has a density in the range 10-40 kg/m ; and wherein the composite exhibits an insulation failure time, according to AS1530.4, for a 100 mm thick panel, of greater than 10 minutes.
12. A composite according to claim 11 wherein the expanded polystyrene and/or the expanded thermoplastic microspheres are, at least in part, solubilised in the phenolic resin. 16567571_1 (GHMatters) P37447NZPC
13. A composite according to claim 11 or claim 12 wherein the composite comprises from 30 to 70 wt.% of (a), from 20 to 60 wt.% of (b) and from 0.5 to 5 wt.% of (c), based on the total weight of the composite.
14. A composite according to any one of claims 11 to 13 wherein the composite has an interstitial volume of less than 5%, preferably less than 1%, more preferably less than 0.5%.
15. A composite according to any one of claims 11 to 14 wherein the composite has a water absorption according to ASTM C272 of less than 8% by volume.
16. A composite according to any one of claims 11 to 15 wherein the specific mass loss rate @ 50kW/m , measured according to ISO 17554, is less than 8 g/m .s.
17. A composite according to any one of claims 11 to 16 wherein the composite exhibits an insulation failure time, according to AS1530.4, for a 100 mm thick panel, of greater than 20 minutes.
18. A composite according to any one of claims 11 to 17 wherein the composite exhibits an insulation failure time, according to AS1530.4, for a 100 mm thick panel, of greater than 30 minutes.
19. A composite according to any one of claims 11 to 18 wherein the expanded polystyrene particles are derived from expandable polystyrene particles having an average particle size from between 0.1 and 5 mm, the expandable polystyrene particles containing a blowing agent.
20. A composite according to any one of claims 11 to 19 wherein the expanded thermoplastic microspheres are derived from expandable thermoplastic microspheres having an average particle size from between 1 and 50 microns and wherein the expandable microspheres contain a propellant encapsulated within a thermoplastic polymer shell. 16567571_1 (GHMatters) P37447NZPC
21. A composite according to claim 20 wherein the thermoplastic polymer shell is derived from monomers selected from the group consisting of acrylonitrile, methacrylonitrile, α-chloroacrylonitrile, α-ethoxyacrylonitrile, fumaroacrylonitrile, crotoacrylonitrile, acrylic esters, methacrylic esters, vinyl chloride, vinylidene chloride, vinylidene dichloride, vinyl pyridine, vinyl esters, and derivatives or mixtures thereof.
22. A composite according to any one of claims 11 to 21 further comprising one or more fillers.
23. A composite according to claim 22 wherein the filler is a surface treated filler.
24. A composite block, panel or sheet for use in construction comprising the foam composite according to any one of claims 11 to 23. 16567571_1 (GHMatters) P37447NZPC 16567571_1 (GHMatters) P37447NZPC
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2013901615A AU2013901615A0 (en) | 2013-05-07 | Foam Composites | |
AU2013901615 | 2013-05-07 | ||
PCT/AU2014/050029 WO2014179842A1 (en) | 2013-05-07 | 2014-05-07 | Foam composites |
Publications (2)
Publication Number | Publication Date |
---|---|
NZ714909A NZ714909A (en) | 2020-09-25 |
NZ714909B2 true NZ714909B2 (en) | 2021-01-06 |
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