WO2004041930A1 - 難燃性塩化ビニル系樹脂組成物およびその成形体 - Google Patents
難燃性塩化ビニル系樹脂組成物およびその成形体Info
- Publication number
- WO2004041930A1 WO2004041930A1 PCT/JP2003/014052 JP0314052W WO2004041930A1 WO 2004041930 A1 WO2004041930 A1 WO 2004041930A1 JP 0314052 W JP0314052 W JP 0314052W WO 2004041930 A1 WO2004041930 A1 WO 2004041930A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- vinyl chloride
- flame
- weight
- compound
- resin composition
- Prior art date
Links
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000011342 resin composition Substances 0.000 title claims abstract description 43
- 239000005078 molybdenum compound Substances 0.000 claims abstract description 55
- 229920005989 resin Polymers 0.000 claims abstract description 53
- 239000011347 resin Substances 0.000 claims abstract description 53
- 150000002752 molybdenum compounds Chemical class 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000002845 discoloration Methods 0.000 claims abstract description 42
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 150000007514 bases Chemical class 0.000 claims abstract description 36
- 238000001125 extrusion Methods 0.000 claims abstract description 32
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 29
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 21
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 20
- 238000007654 immersion Methods 0.000 claims abstract description 14
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 6
- 150000003606 tin compounds Chemical class 0.000 claims abstract description 5
- 239000000779 smoke Substances 0.000 claims description 60
- 238000000465 moulding Methods 0.000 claims description 55
- 239000003063 flame retardant Substances 0.000 claims description 45
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 44
- 239000002667 nucleating agent Substances 0.000 claims description 26
- 239000010459 dolomite Substances 0.000 claims description 25
- 229910000514 dolomite Inorganic materials 0.000 claims description 25
- 239000011248 coating agent Substances 0.000 claims description 21
- 238000000576 coating method Methods 0.000 claims description 17
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 16
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 7
- 150000003672 ureas Chemical class 0.000 claims description 5
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical class NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 150000002734 metacrylic acid derivatives Chemical class 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 2
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 claims description 2
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims 2
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 claims 1
- -1 poly(vinyl chloride) Polymers 0.000 abstract description 24
- 239000010457 zeolite Substances 0.000 abstract description 21
- 229910021536 Zeolite Inorganic materials 0.000 abstract description 20
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 20
- 239000003795 chemical substances by application Substances 0.000 abstract description 12
- 239000011777 magnesium Substances 0.000 abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 abstract description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011162 core material Substances 0.000 abstract description 5
- 229920000915 polyvinyl chloride Polymers 0.000 abstract description 5
- 239000004800 polyvinyl chloride Substances 0.000 abstract description 5
- 230000003449 preventive effect Effects 0.000 abstract description 4
- 239000003086 colorant Substances 0.000 abstract description 3
- 230000000391 smoking effect Effects 0.000 abstract 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 45
- 238000011156 evaluation Methods 0.000 description 44
- 239000003381 stabilizer Substances 0.000 description 36
- 238000000354 decomposition reaction Methods 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 26
- 239000000126 substance Substances 0.000 description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 19
- 150000001875 compounds Chemical class 0.000 description 18
- 239000002904 solvent Substances 0.000 description 18
- 239000011609 ammonium molybdate Substances 0.000 description 16
- 235000018660 ammonium molybdate Nutrition 0.000 description 16
- 229940010552 ammonium molybdate Drugs 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 14
- 238000006116 polymerization reaction Methods 0.000 description 14
- 239000000654 additive Substances 0.000 description 12
- 230000008033 biological extinction Effects 0.000 description 10
- 150000002611 lead compounds Chemical class 0.000 description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 9
- 230000008859 change Effects 0.000 description 8
- 239000000383 hazardous chemical Substances 0.000 description 8
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 8
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 8
- 238000003466 welding Methods 0.000 description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 7
- 229910052750 molybdenum Inorganic materials 0.000 description 7
- 239000011733 molybdenum Substances 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 230000032798 delamination Effects 0.000 description 6
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 235000012438 extruded product Nutrition 0.000 description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- FCSHMCFRCYZTRQ-UHFFFAOYSA-N N,N'-diphenylthiourea Chemical compound C=1C=CC=CC=1NC(=S)NC1=CC=CC=C1 FCSHMCFRCYZTRQ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 239000012760 heat stabilizer Substances 0.000 description 4
- 235000019359 magnesium stearate Nutrition 0.000 description 4
- 230000008520 organization Effects 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- CBXWGGFGZDVPNV-UHFFFAOYSA-N so4-so4 Chemical compound OS(O)(=O)=O.OS(O)(=O)=O CBXWGGFGZDVPNV-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- FULZLIGZKMKICU-UHFFFAOYSA-N N-phenylthiourea Chemical compound NC(=S)NC1=CC=CC=C1 FULZLIGZKMKICU-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 235000012255 calcium oxide Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 229910001701 hydrotalcite Inorganic materials 0.000 description 3
- 229960001545 hydrotalcite Drugs 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000454 talc Substances 0.000 description 3
- 229910052623 talc Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000002341 toxic gas Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229920000388 Polyphosphate Polymers 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical compound [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical class C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- FMXPXIONARXTLI-UHFFFAOYSA-N methane;1,3,5-triazine-2,4,6-triamine Chemical compound C.NC1=NC(N)=NC(N)=N1.NC1=NC(N)=NC(N)=N1 FMXPXIONARXTLI-UHFFFAOYSA-N 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000001205 polyphosphate Substances 0.000 description 2
- 235000011176 polyphosphates Nutrition 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 239000012463 white pigment Substances 0.000 description 2
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 2
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 2
- BHTBHKFULNTCHQ-UHFFFAOYSA-H zinc;tin(4+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Sn+4] BHTBHKFULNTCHQ-UHFFFAOYSA-H 0.000 description 2
- HQEMUQNZGCZHHN-UHFFFAOYSA-N (3-nitrophenyl)thiourea Chemical compound NC(=S)NC1=CC=CC([N+]([O-])=O)=C1 HQEMUQNZGCZHHN-UHFFFAOYSA-N 0.000 description 1
- ZJLRWLYVCHKHMM-UHFFFAOYSA-N (4-aminophenyl)thiourea Chemical compound NC(=S)NC1=CC=C(N)C=C1 ZJLRWLYVCHKHMM-UHFFFAOYSA-N 0.000 description 1
- PAWSVPVNIXFKOS-IHWYPQMZSA-N (Z)-2-aminobutenoic acid Chemical compound C\C=C(/N)C(O)=O PAWSVPVNIXFKOS-IHWYPQMZSA-N 0.000 description 1
- ZBBLRPRYYSJUCZ-GRHBHMESSA-L (z)-but-2-enedioate;dibutyltin(2+) Chemical compound [O-]C(=O)\C=C/C([O-])=O.CCCC[Sn+2]CCCC ZBBLRPRYYSJUCZ-GRHBHMESSA-L 0.000 description 1
- PXDTZJRKXYJXTL-UHFFFAOYSA-N 1,1-dibenzyl-3-(2-phenylethyl)thiourea Chemical compound C=1C=CC=CC=1CN(CC=1C=CC=CC=1)C(=S)NCCC1=CC=CC=C1 PXDTZJRKXYJXTL-UHFFFAOYSA-N 0.000 description 1
- FPZXQVCYHDMIIA-UHFFFAOYSA-N 1,1-diphenylthiourea Chemical compound C=1C=CC=CC=1N(C(=S)N)C1=CC=CC=C1 FPZXQVCYHDMIIA-UHFFFAOYSA-N 0.000 description 1
- BPXVHIRIPLPOPT-UHFFFAOYSA-N 1,3,5-tris(2-hydroxyethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound OCCN1C(=O)N(CCO)C(=O)N(CCO)C1=O BPXVHIRIPLPOPT-UHFFFAOYSA-N 0.000 description 1
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 description 1
- FYBHEPNLHXGWJV-UHFFFAOYSA-N 1,3-bis(2-hydroxyethyl)thiourea Chemical compound OCCNC(=S)NCCO FYBHEPNLHXGWJV-UHFFFAOYSA-N 0.000 description 1
- SSTJIFMUJKCEAB-UHFFFAOYSA-N 1,3-di(docosyl)thiourea Chemical compound CCCCCCCCCCCCCCCCCCCCCCNC(=S)NCCCCCCCCCCCCCCCCCCCCCC SSTJIFMUJKCEAB-UHFFFAOYSA-N 0.000 description 1
- KAJICSGLHKRDLN-UHFFFAOYSA-N 1,3-dicyclohexylthiourea Chemical compound C1CCCCC1NC(=S)NC1CCCCC1 KAJICSGLHKRDLN-UHFFFAOYSA-N 0.000 description 1
- LRDWZYFXZNDIRZ-UHFFFAOYSA-N 1,3-dioctadecylthiourea Chemical compound CCCCCCCCCCCCCCCCCCNC(=S)NCCCCCCCCCCCCCCCCCC LRDWZYFXZNDIRZ-UHFFFAOYSA-N 0.000 description 1
- XYAKDKSYCSTBMN-UHFFFAOYSA-N 1-(4-chlorophenyl)-3-phenylthiourea Chemical compound C1=CC(Cl)=CC=C1NC(=S)NC1=CC=CC=C1 XYAKDKSYCSTBMN-UHFFFAOYSA-N 0.000 description 1
- JMKRMQGOPWYOGL-UHFFFAOYSA-N 1-(4-methoxyphenyl)-3-phenylthiourea Chemical compound C1=CC(OC)=CC=C1NC(=S)NC1=CC=CC=C1 JMKRMQGOPWYOGL-UHFFFAOYSA-N 0.000 description 1
- OROCFDLTBPBLFS-UHFFFAOYSA-N 1-ethyl-3-phenylthiourea Chemical compound CCNC(=S)NC1=CC=CC=C1 OROCFDLTBPBLFS-UHFFFAOYSA-N 0.000 description 1
- HAZJTCQWIDBCCE-UHFFFAOYSA-N 1h-triazine-6-thione Chemical compound SC1=CC=NN=N1 HAZJTCQWIDBCCE-UHFFFAOYSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- KLLLJCACIRKBDT-UHFFFAOYSA-N 2-phenyl-1H-indole Chemical compound N1C2=CC=CC=C2C=C1C1=CC=CC=C1 KLLLJCACIRKBDT-UHFFFAOYSA-N 0.000 description 1
- MDAYOTNXXTVAMM-VRHVFUOLSA-N 3-[(z)-3-aminobut-2-enoyl]oxybutyl (z)-3-aminobut-2-enoate Chemical compound C/C(N)=C/C(=O)OC(C)CCOC(=O)\C=C(\C)N MDAYOTNXXTVAMM-VRHVFUOLSA-N 0.000 description 1
- PDQICKRFOKDJCH-UHFFFAOYSA-N 6-amino-2-(dodecanoylamino)hexanoic acid Chemical compound CCCCCCCCCCCC(=O)NC(C(O)=O)CCCCN PDQICKRFOKDJCH-UHFFFAOYSA-N 0.000 description 1
- 239000004801 Chlorinated PVC Substances 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- PDQAZBWRQCGBEV-UHFFFAOYSA-N Ethylenethiourea Chemical compound S=C1NCCN1 PDQAZBWRQCGBEV-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- FLVIGYVXZHLUHP-UHFFFAOYSA-N N,N'-diethylthiourea Chemical compound CCNC(=S)NCC FLVIGYVXZHLUHP-UHFFFAOYSA-N 0.000 description 1
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical compound C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 description 1
- GMEHFXXZSWDEDB-UHFFFAOYSA-N N-ethylthiourea Chemical compound CCNC(N)=S GMEHFXXZSWDEDB-UHFFFAOYSA-N 0.000 description 1
- WCUQNDYMZCICMD-UHFFFAOYSA-N N.[O--].[Mg++] Chemical compound N.[O--].[Mg++] WCUQNDYMZCICMD-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical class OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 206010047289 Ventricular extrasystoles Diseases 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 125000005250 alkyl acrylate group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- RLKBOGLIOLFMEK-NSCUHMNNSA-N amino (e)-but-2-enoate Chemical compound C\C=C\C(=O)ON RLKBOGLIOLFMEK-NSCUHMNNSA-N 0.000 description 1
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- 229910001038 basic metal oxide Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 150000001565 benzotriazoles Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- BIOOACNPATUQFW-UHFFFAOYSA-N calcium;dioxido(dioxo)molybdenum Chemical compound [Ca+2].[O-][Mo]([O-])(=O)=O BIOOACNPATUQFW-UHFFFAOYSA-N 0.000 description 1
- NWXHSRDXUJENGJ-UHFFFAOYSA-N calcium;magnesium;dioxido(oxo)silane Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O NWXHSRDXUJENGJ-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 description 1
- KRGNPJFAKZHQPS-UHFFFAOYSA-N chloroethene;ethene Chemical group C=C.ClC=C KRGNPJFAKZHQPS-UHFFFAOYSA-N 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- UQLDLKMNUJERMK-UHFFFAOYSA-L di(octadecanoyloxy)lead Chemical compound [Pb+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O UQLDLKMNUJERMK-UHFFFAOYSA-L 0.000 description 1
- 229910052637 diopside Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000004312 hexamethylene tetramine Chemical class 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000013003 hot bending Methods 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002475 indoles Chemical class 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229940070765 laurate Drugs 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- VYQMZUUUGRXQHR-UHFFFAOYSA-N magnesium;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Mg+2].[Ti+4] VYQMZUUUGRXQHR-UHFFFAOYSA-N 0.000 description 1
- 229940049920 malate Drugs 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-L malate(2-) Chemical compound [O-]C(=O)C(O)CC([O-])=O BJEPYKJPYRNKOW-UHFFFAOYSA-L 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229960004011 methenamine Drugs 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GUSFEBGYPWJUSS-UHFFFAOYSA-N pentaazanium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O GUSFEBGYPWJUSS-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229940116351 sebacate Drugs 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052645 tectosilicate Inorganic materials 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical class C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2666/00—Composition of polymers characterized by a further compound in the blend, being organic macromolecular compounds, natural resins, waxes or and bituminous materials, non-macromolecular organic substances, inorganic substances or characterized by their function in the composition
- C08L2666/66—Substances characterised by their function in the composition
- C08L2666/84—Flame-proofing or flame-retarding additives
Definitions
- the present invention provides a vinyl chloride resin composition having excellent flame retardancy, molding processability, discoloration resistance, and other various properties, and a hard resin obtained by molding this composition by various molding methods. And a molded article.
- the vinyl chloride resin composition has excellent flame retardancy because it contains chlorine in the molecule, and various inorganic additives can be added in a wide content, so that a wide range of mechanical properties, heat resistance, Formability and weather resistance can be realized.
- Molded articles of the vinyl chloride resin composition having such properties are used for transporting equipment inside and outside of aircraft such as aircraft, ships, and vehicles; building interior and exterior materials; furniture; It is widely used as daily necessities; housing materials for home appliances and electronic devices; parts for semiconductor devices.
- the vinyl chloride resin composition is exposed to a temperature higher than the heat resistance temperature, such as in a fire, etc., it emits a large amount of smoke due to chlorine in the molecule and contains chlorine gas and hydrogen chloride gas. Generates toxic gas. For this reason, attempts have been made to suppress the generation of toxic gases by using inorganic additives, and the types and amounts of inorganic additives have been studied.
- Japanese Patent Application Laid-Open No. 11-181204 discloses a method for producing vinyl chloride resin that satisfies the FM standard (a standard based on the evaluation criteria defined by the mutual insurance organization ⁇ Factory Mutual System >>). It discloses a flame-retardant vinyl chloride resin molded article obtained by adding calcium carbonate, talc, and a chlorine-trapping compound to form a desired shape.
- this molded product has the effect of improving flame retardancy, it has the effect of suppressing the generation of toxic gas.
- the results are not sufficient, the thermal stability during molding is poor, and the additives are poorly dispersed, which causes agglomerates in the molded body, making the appearance unsatisfactory.
- Japanese Patent Application Laid-Open No. 2000-226683 discloses that metal hydroxide is 4 to 60 parts by weight based on 100 parts by weight of vinyl chloride resin.
- a flame-retardant vinyl chloride resin molded article containing 2 to 40 parts by weight of a zinc stannate-based flame retardant and 20 to 150 parts by weight of a plasticizer has been proposed.
- this molded product has a problem that the softening temperature of the extruded product is lowered even though the flame retardancy, the thermal stability at the time of extrusion and the appearance are good.
- the molybdenum compound is used in an amount of 0.1 to 2.5 parts by weight (0.05 to 5 (1.5 parts by weight), and a flame-retardant vinyl chloride resin composition to which vinyl chloride is added is disclosed in Japanese Patent Application Laid-Open No. 2002-284948.
- a vinyl chloride resin composition has been proposed in which a molybdenum compound is at least 1 part by weight, a hydroxide compound is at least 1 part by weight, and titanium oxide is at least 3 parts by weight, and the total of these is 8 to 25 parts by weight.
- vinyl chloride resin compositions are used as a material for semiconductor cleaning tanks requiring cleaning with hot water or as a material for peripheral components thereof, because of their stable hot water cleaning properties (the disadvantages such as discoloration even in contact with hot water). It is difficult to satisfy flame retardancy o
- the present invention has sufficient flame retardancy, thermal stability at the time of molding processing, and other various properties, and has a good appearance and a high softening temperature when formed into a molded product, and uses a lead compound. Stable and sufficient hot water discoloration resistance without solvent It is an object of the present invention to provide a flame-retardant vinyl chloride resin composition and a hard molded product obtained by molding the composition by various molding methods. Summary of the Invention
- the flame-retardant vinyl chloride resin composition of the present invention comprises 100 parts by weight of a vinyl chloride resin
- At least one smoke suppressant selected from a zinc compound, a molybdenum compound, and a tin compound; 0.05 to 10 parts by weight; and
- composition further comprises a polyalkyl methacrylate as a processing aid
- At least one kind of polyalkyl acrylates in an amount of 0.1 to 10 parts by weight.
- the smoke suppressant is a molybdenum compound, which contains 0.05 to 8 parts by weight of the molybdenum compound, and further contains 0.1 to 3 parts by weight of the basic compound. You may.
- the composition of the present invention is characterized in that the smoke suppressant comprises a basic compound or a basic compound and titanium oxide as a nucleating agent, and the nucleating agent is surface-coated with a molybdenum compound. It may contain 0.1 to 8 parts by weight of a smoke suppressant, and in this case, the above-mentioned processing aid may not be contained.
- the molybdenum compound is 5 to 50% by weight based on the total amount of the surface coating smoke suppressant.
- the flame-retardant vinyl chloride-based resin composition according to the present invention preferably has a decomposition time of at least 15 min according to a dynamic thermal stability evaluation method using a plastmill.
- the molded article is formed by extrusion molding the above flame-retardant vinyl chloride resin composition, calender press molding (refers to a molding technique in which press molding is performed subsequent to calender molding; the same applies hereinafter), or continuous extrusion press molding (for extrusion molding). Continued And press molding. The same applies hereinafter).
- the molded product preferably has a color difference of three values of -0.5 to 0.5 before and after immersion in warm water in a warm water discoloration test at 60 ° C for 48 hours.
- the hard composition of the present invention has an average calorific value (AHRR) measured according to ASTM E 1354 of eSkWZm 2 or less and an average extinction volume (ASEA: 1 g of a molded body in a fixed space). and when the amount of light is interrupted, the value in terms of the volume of the hypothesis with a certain smoke density (density), becomes the higher smoke density is higher larger volume) or less 800 m 2 / g Yes, it is preferable that the Piccat softening temperature measured according to JISK 7206 B method load 49.03 N is 70 ° C or more.
- the vinyl chloride resin in the present invention includes, in addition to homopolymers such as polyvinyl chloride and chlorinated polyvinyl chloride, vinyl chloride-vinyl acetate copolymers, vinyl chloride-ethylene copolymers, vinyl chloride-acrylyl copolymers, and the like. Copolymers can also be used, and soft or hard polymers having a degree of polymerization of about 400 to 1400 are suitable.
- the smoke suppressant added to these vinyl chloride resins is at least one selected from zinc compounds, molybdenum compounds, and tin compounds, and among them, zinc compounds and molybdenum compounds are preferable.
- Examples of the zinc compound include zinc borate, zinc oxide, zinc hydroxystannate, zinc stannate, zincite, and the like.
- molybdenum compounds include molybdenum oxide, molybdenum trioxide, molybdic acid, ammonium molybdate, ammonium octamolybdate, zinc molybdate, calcium molybdate, calcium zinc molybdate, sodium molybdate, molybdenum disulfide, Melamine molybdate and the like can be mentioned.
- tin compound examples include tin oxide. These smoke suppressants may be used by adding these compounds as they are to the above-mentioned vinyl chloride resin, or may be added by coating with other additives.
- additives to be coated with these smoke suppressants include inorganic substances such as calcium carbonate and talc.
- inorganic substances such as calcium carbonate and talc.
- an aluminum-based or magnesium-based metal hydroxide or zeolite blended as an essential component in the present invention together with these smoke suppressants may be coated with the smoke suppressant before use.
- the smoke suppressant as described above has an effect of promoting carbonization of the vinyl chloride resin composition at the time of combustion and reducing the amount of smoke, and the flame retardancy of the molded article by the vinyl chloride resin composition of the present invention. It contributes to the effect of improving the properties.
- the amount of the smoke suppressant is too small, the above effects cannot be obtained.On the other hand, if the amount is too large, not only the physical properties of the molded article are deteriorated, but also there is a concern that poor dispersion may appear in the molded article.
- the amount is 0.05 to 10 parts by weight based on 100 parts by weight of the vinyl chloride resin.
- the behavior of decomposition and degradation of vinyl chloride resin at the temperature is indicated by the start of de-HCI in the processing temperature range up to 220 ° C, and the temperature range around 220 ° C to 70 ° C. HCI desorption proceeds, and the main chain is cut or carbon burns in a temperature range of, for example, 450 ° C or more.
- decomposition in the temperature range up to 220 ° G which is the forming temperature range
- low-temperature decomposition the temperature range of 450 ° C or higher at which main chain breakage and carbon combustion occur.
- high-temperature decomposition is referred to as low-temperature decomposition.
- the molybdenum compound works well as a high-temperature decomposition accelerator, and promptly progresses carbonization in a temperature range in which the main chain is cut or carbon burns.
- a molded article made of a vinyl chloride resin composition to which the molybdenum compound is not added carbonization of the molded article is not promoted in this temperature range.
- a flame retardant is incorporated, good flame retardancy cannot be exhibited.
- the addition amount of the molybdenum compound having a good high-temperature decomposition promoting action is 0.01 to 1 with respect to 100 parts by weight of the vinyl chloride resin, that is, the addition amount of the above-mentioned smoke suppressant. Although it may be 0 parts by weight, preferably vinyl chloride resin 10 The amount is 0.05 to 8 parts by weight, more preferably 0.5 to 5 parts by weight, based on 0 parts by weight. If the amount is too small, good high-temperature decomposition promoting action cannot be exhibited, and if the amount is too large, defects of poor dispersion occur in the molded product, and a high-quality molded product cannot be obtained.
- the molybdenum compound is preferably used in a liquid form rather than a powder form in order to obtain a high-quality molded article without poor dispersion.
- a high-quality molded product can be obtained by mixing and using or by performing uniform mixing at the compounding stage.
- molybdenum compound molybdenum oxide, molybdenum trioxide, molybdic acid, ammonium molybdate, ammonium dimolybdate, ammonium heptamolybdate, ammonium octamolybdate, ammonium decamolybdate, zinc molybdate, Calcium phosphate, zinc calcium molybdate, potassium molybdate, sodium molybdate, molybdenum disulfide, phosphomolybdate, potassium phosphomolybdate, calcium phosphomolybdate, zinc phosphomolybdate, ⁇ melamine molybdate can be used. These can be used alone or as a mixture of two or more of them in an appropriate combination.
- molybdenum compounds may be used in combination with a flame retardant aid, and examples of the flame retardant aid include molybdenum oxide, tin oxide, zinc oxide, vanadium oxide, ammonium polyphosphate, and phosphate esters. These flame retardant aids are used alone or in combination of two or more.
- molybdenum compounds may be added to the above-mentioned vinyl chloride resin as it is, or may be added by coating with other additives.
- other additives those usually added to a vinyl chloride resin may be used, and talc, silica, titanium oxide and the like are preferable among them.
- the present inventors pursued a method of suppressing a decrease in the Mo valence of the molybdenum compound, and as a result, a method of neutrally controlling the hydrogen ion concentration in the molded body during immersion in warm water has been developed. It has been found that discoloration can be stably prevented.
- the vinyl chloride-based resin tends to be acidic due to the HCI removal reaction accompanying thermal degradation during the molding process in the above-mentioned processing temperature range.
- the organotin-based stabilizer to be added to the vinyl chloride-based resin is a laurate-based, malate-based, or mercaptide-based stabilizer, and is typified by lauric acid, maleic acid, thioglycolic acid, and the like.
- the stabilizer itself has acidity because it is synthesized with an acidic substance.
- a basic compound is blended in the present invention as the above-mentioned regulator of hydrogen ion concentration.
- the hydrogen ion concentration (pH) in the aqueous solution after the hot water discoloration test under the conditions of 60 ° C and 48 hours was adjusted to 5.5 to 8.5, Therefore, stable hot water discoloration resistance is ensured.
- the basic compound is compounded to prevent discoloration due to immersion in warm water.
- the basic compound also has an action as a low-temperature decomposition inhibitor, and the compounding of the molybdenum compound promotes decomposition even at a low temperature, that is, at a processing temperature range, and results in resin burning and satisfactory appearance.
- This compound is compounded to prevent the formation of a molded body, or to prevent corrosion of a molding machine due to a minute amount of hydrochloric acid generated by decomposition in this low temperature range.
- the compounding amount of the basic compound having such an action is too large, it is related to the hydrogen ion concentration, but the heat stability is deteriorated, and the molded article is satisfactory. If the amount is too small, good hot water discoloration resistance cannot be obtained.Therefore, 0.1 to 3 parts by weight, preferably 0.5 to 5 parts by weight, per 100 parts by weight of the vinyl chloride resin. 2 parts by weight.
- Examples of the basic compound include alkali metal oxides and hydroxides; basic salts of carbonic acid, sulfuric acid, sulfurous acid, phosphoric acid, and phosphorous acid; beryllium oxide, magnesium oxide, calcium oxide, strontium oxide, and oxide.
- Basic metal oxides such as barium, silicon oxide, aluminum oxide, and zinc oxide
- basic inorganic pigments such as lime carbonate, ultramarine, barium sulfate, and precipitated barium sulfate
- dolomite compounds Compounds: Urea derivatives such as urea, thiourea, N, N'-diphenylthiourea; yS-aminocrotonate, N-lauroyl lysine, tris (2-hydroxyethyl) isocyanurate, tris (epoxypropyl) isocyanurate, etc.
- Aminocarboxylic acid derivatives Indoles such as 2-phenylindole; N, N'-diphenylethylene Polyamines such as n-diamine, diethylene triamine, hexamethylene tetramine; amine derivatives such as phenyl ⁇ -naphthylamine, aldol-l-naphthylamine, 6-ethoxy-2,2,4-trimethyl-l, 2-dihydroquinoline; Benzotriazoles such as 2'-hydroxyphenyl) benzotriazole; hindered amine derivatives such as bis (2,2,6,6-tetramethylpyridinyl) 14-sebacate; hydrazine derivatives; thiocarbamine derivatives; metals Organic compounds such as stones; Among them, urea derivatives, aminocarboxylic acid derivatives, dolomite derivatives, and metal stones are preferred from the viewpoint of compatibility with vinyl chloride resins and the like.
- urea derivative examples include a thiourea derivative represented by the following general formula. Specific examples of the urea derivative represented by this general formula include the following.
- R 2 NR 3 1-Ethyl-3-phenylthiourea, 1,3-Diphenylthiourea, 1,3-Diethylthiourea, 1-Ethyl-3-p-cloth phenylthiourea, 1-Ethyl-3- (2-hydroxyethylurea Thiol) thiourea, 1- (2-thiazolyl) -3 1-phenylthiourea, 1,3-distearylthiourea, 1,3-dibehenylthiourea, 1-ethylthiourea, 11-p-bromophenyl 3-phenylthiourea, 1- (2-thiophenyl) -1-3-phenylthiourea, 1,3-bis (2-hydroxyethyl) thiourea, 1-1 p-aminophenyl-1-3-phenyl Ruthiourine, 1-p-nitrophenyl-13-phenylthiourea, 1-p-hydroxyphenyl-13-pheny
- aminocarboxylic acid derivatives include, for example, 1,3-butanediol bis (3-aminocrotonate), methyl- ⁇ -aminocrotonate, 1,4-butane-bis-yS-aminocrotonate, 2,6 —Dimethyl-3,5-methoxycarbodehydropyridine, 6-amino-1,3-dimethylperacyl and the like.
- Examples of the metal stone include, for example, a general formula M (OOCR) n (where M is a metal such as Ba, C a, AI, or Mg, R is suaric acid, lauric acid, or 2-ethylhexo) And barium stearate and magnesium stearate as typical examples.
- M a metal such as Ba, C a, AI, or Mg
- R is suaric acid, lauric acid, or 2-ethylhexo
- barium stearate and magnesium stearate as typical examples.
- dolomite compound widely naturally occurring, wall material, dolomite used in the iron making resistant fire or the like, i.e., dolomite (M g C 0 3 'C a CO 3), magnesia Quicklime (Mg0 ⁇ Ca0), slaked lime (Mg0 (OH) 2 ⁇ Ca (0H) 2 ), etc .; its chemical composition is a double salt of calcium carbonate and magnesium carbonate Synthetic dolomite (weight ratio of magnesium to calcium is 5: 95-95: 5 in terms of MgO: CaO); or the natural or synthetic dolomite is calcined, slaked, etc.
- dolomite M g C 0 3 'C a CO 3
- Mg0 ⁇ Ca0 magnesia Quicklime
- its chemical composition is a double salt of calcium carbonate and magnesium carbonate
- Synthetic dolomite weight ratio of magnesium to calcium is 5: 95-
- Dolomite cement lightly-burned dolomite, deadly-burned dolomite, dolomite clinker, digested dolomite, dolomite plaster, synthetic magdro-clinker, which is obtained by adding water to lightly-burned dolomite ; more Akerumanaito (C a 2 M g S i 2 O 7), diopside [C a M g (S i 0 3) 2 ], as various slag, mixing ratio of the Karushiu arm and magnesium above Doromai Natural minerals and synthetic double salts in the same range as the above can be modified. These dolomite compounds may be used alone or in an appropriate combination.
- Two or more kinds may be used as a mixture.
- dolomite compounds may have been subjected to a surface treatment.
- the surface treatment agent include organic acids, organic acid metal salts, and polyhydric alcohol compounds. They may be used, or two or more of them may be mixed and used in an appropriate combination.
- the above basic compound is particularly preferably sedimentable barium sulfate which has the same pigment properties as titanium oxide and has excellent chemical resistance.
- the present invention provides a molybdenum compound as a coating material, which is coated with a basic compound or a nucleating agent comprising a mixture of a basic compound and titanium oxide with the coating material as a smoke-proofing agent.
- the smoke suppressant as a whole can be neutralized so that the valence of molybdenum does not change.
- titanium oxide used as a nucleating agent instead of or in combination with the above basic compound, either anatase type or rutile type titanium oxide may be used, but in terms of light stability, Rutile titanium oxide is preferred.
- Titanium oxide may be surface-treated similarly to the above-mentioned dolomite-based compound.
- Examples of the surface-treating agent include AI—Si, AI—Si, and AI—Si— Zr-based treatment agents and the like.
- the coating amount of the molybdenum compound with respect to the nucleating agent is too small, the molybdenum compound does not provide the effect of promoting high-temperature decomposition (smoke prevention). Since a small connexion, is hot water discoloration and low-temperature degradation suppressing effect can not be obtained, while the total amount of the nucleating agent and the mode Ribuden compound, as a M o 0 3, 5 to 5 0 wt%, preferably 1 0-3 0 % By weight (molybdenum metal is suitably 1 to 20% by weight, preferably 5 to 10% by weight.
- the method for coating the nucleating agent with the molybdenum compound is not particularly limited. For example, it can be carried out by a method generally used for supporting various compounds on a carrier in the production of a catalyst or the like.
- a molybdenum compound or its precursor is dissolved in a solvent such as water in the presence of a nucleating agent, and then insolubilized by changing pH, coated on the nucleating agent, and dried.
- the coating is preferably performed using the technique described in US Pat. No. 3,726,694 or US Pat. No. 3,874,864.
- one or two or more aqueous solutions in which the nucleating agent is dispersed in advance are simultaneously or stepwise introduced into the concentrated aqueous solution of the molybdenum compound.
- the mixture is dried, calcined, and pulverized to remove aggregates generated in the drying step. It is done in a way.
- the amount of the surface coating smoke suppressant in which the above nucleating agent is coated with a molybdenum compound is too small, the effect of the molybdenum compound to prevent the smoke (accelerating high-temperature decomposition) is not exhibited, and if it is too large, the effect is saturated.
- the amount is preferably 0.1 to 8 parts by weight based on 100 parts by weight of the vinyl chloride resin.
- the molybdenum compound, basic compound, and titanium oxide are uniformly mixed simply by mixing the surface-coated smoke suppressant with the vinyl chloride resin.
- a uniform dispersion state can be obtained by a single substance. Dispersion of difficult molybdenum compounds becomes easy, and sufficient smoke prevention (high temperature decomposition promotion) effect can be obtained even with a small amount of molybdenum compounds.
- titanium oxide as a white pigment can be used together with a basic compound as a nucleating agent.
- a basic compound as a nucleating agent.
- a known flame retardant eg, phosphoric ester, condensed phosphate ester, orthophosphate ester, etc.
- a radical generator eg, peroxide, perchloric acid, etc.
- a cross-linking agent eg, a triazine thiol compound
- the amount of these known flame retardants used in combination is not particularly limited. However, if the amount is too large, poor dispersion and deterioration of thermal stability are caused as described above. , 10% by weight or less.
- the metal hydroxide added to the vinyl chloride-based resin together with the above-mentioned smoke suppressant is at least one selected from magnesium-based and aluminum-based metal hydroxides.
- zeolite added in place of or together with these metal hydroxides has a general formula of Mx / p [(AIO 2 ) x ⁇ (S i O 2 ) y] ZH 20
- M is a metal ion of valence p such as Ca, Mg, Na, K, etc.
- x + y is a tetrahedral number per unit cell and is an integer of 10 to 200
- X and y are 0 ⁇ x / y ⁇ 1.
- An integer satisfying the formula 1 and Z is an integer of 4 to 300, which is the number of moles of water molecules, can be preferably used.
- zeolites are one of the minerals belonging to the tectosilicate, and exist in natural and synthetic forms, and there are many types.
- the metal ions M in the synthetic form are Na and Ca.
- A-type zeolite can be preferably used.
- the above-mentioned metal hydroxide zeolite enhances the thermal stability of the vinyl chloride resin composition of the present invention, and requires molding processability, especially severe molding process conditions compared to the calender press method or extrusion method. It has the effect of improving the formability in the continuous extrusion press method.
- the content is 0.1 to 10 parts by weight, preferably 0.5 to 8 parts by weight based on 100 parts by weight of the polyvinyl chloride resin.
- a metal hydroxide known as a heat stabilizer for example, calcium hydroxide or hydrotalcite
- a heat stabilizer for example, calcium hydroxide or hydrotalcite
- the amount of these known heat stabilizers to be used in combination is not particularly limited. However, if the amount is too large, the above-mentioned poor dispersion is caused. Therefore, the amount of the above-mentioned magnesium-based or aluminum-based metal hydroxide or zeolite is added. Of these, the content is preferably 10% by weight or less.
- the processing aid in the present invention is at least one selected from polyalkyl methacrylates and polyalkyl acrylates, and preferably has a molecular weight of about 200,000 to 500,000, more preferably 500,000 to 300,000.
- the polyalkyl methacrylates include polymethyl methacrylate and polybutyl methacrylate, and the polyalkyl acrylates include polyethyl acrylate and polybutyl acrylate. And poly-2-ethylhexyl acrylate.
- alkyl methacrylates where the alkyl group is methyl or butyl
- the alkyl group is ethyl, butyl, or 2-ethyl
- processing aids are obtained by molding and processing the vinyl chloride resin composition of the present invention. It has the effect of eliminating poor dispersion of each additive in the molded article to be formed. That is, the flame-retardant vinyl chloride resin composition of the present invention is for hard molded articles, and does not contain a plasticizer or 5 parts by weight or less based on 100 parts by weight of the vinyl chloride resin. Due to the small amount, each additive may not be uniformly dispersed in the vinyl chloride resin. To solve this problem, a processing aid is added.
- the amount of the processing aid is 0.5 to 10 parts by weight, preferably 1.5 to 8 parts by weight, based on 100 parts by weight of the polyvinyl chloride resin.
- the basic compound or titanium oxide acts to disperse the molybdenum compound well. It is not necessary to mix it.
- a known processing aid for example, a methyl methacrylate-butyl acrylate-styrene copolymer: a molecular weight of 30
- the amount of the known processing aid is not particularly limited. However, if the amount is too large, the amount of shearing heat generated as described above increases. Of these, the content is preferably 10% by weight or less.
- the flame-retardant vinyl chloride resin composition of the present invention comprises a predetermined amount of a vinyl chloride resin, a smoke suppressant, a metal hydroxide / zeolite, a processing aid added as necessary, Of various additives (eg, smoke suppressants, heat stabilizers ⁇ metal hydroxides, etc. >>, coloring agents, etc.) using a Plender / Henschel mixer and the like, and can be uniformly mixed.
- various additives eg, smoke suppressants, heat stabilizers ⁇ metal hydroxides, etc. >>, coloring agents, etc.
- the moldability of the flame-retardant vinyl chloride resin composition of the present invention is based on whether or not the composition has excellent thermal stability.
- This thermal stability can be evaluated based on the decomposition time (for example, the time at which the torque starts to increase by 10% or more after heating to 200 ° G) by the dynamic thermal stability evaluation method using a plastmill. it can.
- the decomposition time for example, the time at which the torque starts to increase by 10% or more after heating to 200 ° G
- those having a decomposition time of 15 min or more are suitable. If it is shorter than 15 min, the stability during molding may be reduced.
- the upper limit of the decomposition time is not particularly limited, if it is too high, the carbonization during combustion is hindered, the smoke index becomes high, and the FM standard may not be satisfied. Degree.
- the flame-retardant vinyl chloride-based resin molded article of the present invention is obtained by extruding the above-mentioned twist-resistant vinyl chloride-based resin composition by extrusion molding, calender press molding, extrusion continuous press molding, or the like. It can be obtained by shaping into various forms such as pipe, pipe and irregular shapes.
- the calender press molding method is a molding method under mild conditions, so the strain generated in the composition during the calender molding is eliminated during the press molding, and the resulting molding is performed.
- the body (plate) is in an unstrained state, but when it is subjected to thermal processing to form housing materials for various home appliances and electronic devices, or parts for semiconductor devices, etc., from this plate, power The distortion during render molding is recovered, and a so-called glossy return phenomenon occurs in these various molded products.
- the calender press forming method since only a thin plate can be formed in the calender forming step, it is necessary to laminate a plurality of plates in the press forming step to obtain a plate having a desired thickness.
- the laminate itself, or the various molded articles obtained from the laminate as described above, may cause delamination when washed with a solvent or the like, and have poor solvent resistance.
- a plurality of plates obtained in the calender forming step are laminated in the press forming step to obtain a plate having a desired thickness.
- Has a certain degree of thickness fluctuation depending on the molding conditions, etc., and the thickness fluctuation caused by the conditions at the press molding stage etc. is synergistic with the thickness fluctuation, resulting in poor thickness accuracy. ing.
- Extrusion molding and continuous extrusion press molding are methods under severe conditions of high temperature and high pressure compared to force render press molding, so there is no such problem of gloss return as mentioned above.
- Extrusion can provide a plate of desired thickness, so there is no problem of delamination (solvent resistance).
- solvent resistance solvent resistance
- the continuous extrusion press forming method has not only the problem of gloss return and the problem of delamination (solvent resistance) but also the extruded plate is pressed after the extrusion, so that a waving phenomenon occurs. Further, it is possible to obtain an effect that a plate having a desired thickness can be obtained with high thickness accuracy, which cannot be obtained by the above two molding methods.
- the color difference ⁇ a value of the molded article of the present invention obtained by the above molding method before and after the hot water discoloration test under the conditions of 60 ° C and 48 hours shall be -0.5 to +0.5. is important.
- the color difference Aa 0.0, that is, that no discoloration occurs, but within this range, sufficient practicality is obtained.
- the color difference Aa ⁇ -0.5 or Aa> +0.5 discoloration occurs during use in molded products that come into contact with warm water constantly or frequently, such as semiconductor cleaning tanks ⁇ and peripheral members. It lacks practicality.
- the color difference occurs remarkably when a molybdenum compound is used as a smoke suppressant (high-temperature decomposition accelerator), and the color difference ⁇ a value falls within the range of 0.5 to 100.5. This can be achieved by adjusting the hydrogen ion concentration (pH) in the aqueous solution after the hot water discoloration test at 60 ° C for 48 hours to 5.5 to 8.5.
- the adjustment of the hydrogen ion concentration (pH) 5.5 to 8.5 can be easily and reliably realized by blending the basic compound and titanium oxide with the above-mentioned addition amount together with the molybdenum compound. .
- the molded article of the present invention also has excellent flame retardancy, and this flame retardancy can be evaluated using a cone calorimeter according to ASTM E1354.
- This evaluation is the flame-retardant characteristic evaluated by a combustion test using a cone calorimeter, and is the maximum value of the calorific value due to combustion per unit area and unit time (also described as the maximum calorific value, PHRR; Unit: kWZm 2 , Average value (Average heat value, also described as A HRR; Unit: kWZm 2 ), Total heat value (Total heat value, also referred to as THR) (Unit: MJ / m 2 ), average value of mass loss rate (also referred to as AMLR; unit: gZs e G ⁇ m 2 ), maximum value of extinction volume (maximum extinction volume, PS Also described as EA; unit: m 2 Zg), average value of extinction volume (average extinction volume, also described as AS EA; unit: m 2 / g) and the like.
- the evaluation value according to the FM standard is a value obtained by submitting a test piece to the mutual insurance organization by the person requesting the evaluation value, and the mutual insurance organization evaluates this test piece, so the evaluation value is obtained until the evaluation result is obtained. It was time-consuming and inefficient.
- the fire spread index (FP I) according to the above FM standard is the evaluation value regarding the calorific value such as the maximum calorific value (PHRR), average calorific value (AHRR), and total calorific value (THR) measured by the above cone calorimeter. Has a strong correlation.
- the smoke index (SDI) according to the FM standard mentioned above has a strong correlation with the indicators related to the extinction volume such as the maximum extinction volume (PSEA) and the average extinction volume (ASEA) measured by the cone calorimeter. Have.
- the corrosion index (CD I) according to the FM standard mentioned above has a strong correlation with an index related to mass loss such as the mass loss rate (AMLR) measured by the cone calorimeter described above.
- the FM standard requires a fire spread index (FP I) of 6 or less and a smoke index (SD I) of 0.4 or less.
- the maximum heat value (PH RR) is 130 KwZm 2 or less
- the average heat value (AHRR) is 82 Kw / m 2 or less
- the total heat value (THR) l OOMJZm 2 or less Mass loss rate (AMLR) 13 g / sec -m 2 or less
- average extinction volume (ASEA) 1000 m 2 Zg or less especially average heat generation the amount (AHRR), since the average light attenuation volume (ASEA) is dominant with respect to flame retardancy, average calorific value (AHRR) 65kWZm 2 or less, and an average light attenuation volume (ASEA) 80 Om 2 / g or less and It is preferred to do so.
- the thermal properties of the molded article of the present invention are preferably such that the vicat softening temperature measured according to the JIS K 7206 B method load of 49.03 N is 70 ° C. or higher.
- Vinyl chloride resin with a polymerization degree of 800 Taiyo PVC's product name "TH-800”
- Smoke control agent 1 zinc hydroxystannate (Alcan Chemical's product name "FIamt ard H")
- Smoke control agent 2 Ammonium molybdate (Nippon Inorganic Chemical Co., Ltd. product name "Moryan AHM”)
- Metal hydroxide Magnesium hydroxide (Kyowa Chemical Co., Ltd. product name "Magsalat F”)
- Zeolite Na-type A zeolite (Tosoichi Co., Ltd. product name "GSL-1000”)
- Processing aid Methyl methacrylate-based copolymer (trade name by Rohm & Haas)
- Calcium silicate added as a dynamic viscosity improver (trade name "Solexx” manufactured by Tokuyama Soda Co., Ltd.)
- Tin powder stabilizer (trade name "MA300” manufactured by Nitto Kasei Co., Ltd.)
- Liquid tin-based stabilizer (Trade name "N-200” by Tokasei Co., Ltd.)
- Peroxide Hydroperoxide (trade name “Parkmill P” manufactured by NOF Corporation)
- Crosslinking agent Triazinethiol (trade name “Disnet DB” manufactured by Sankyo Kasei Co., Ltd.)
- Heat stabilizer Hydrotalcite (Kyowa Chemical Co., Ltd.)
- the product name is "Almizer 1".
- Smoke suppressant 0 4 4 4 4 4 0 15 4 4 Metal hydroxide 0 0 0 0.5 0 0 0 0.5 15 0.5 Processing aid 1.5 1.5 1.5 0 1.5 1.5 1.5 1.5 15 Tin powder stabilizer 3 3 3 6 0 0 3 3 3 Liquid tin-based stabilizer 0 0 0 0 3 4 0 0 0 Calcium silicate 0 0 0.5 0 0 0 0 0.5 0 0 [Evaluation of extrusion processing characteristics]
- Tables 3 and 4 show the results evaluated by the following evaluation methods.
- ASEA (m 2 / g) 814 762 758 730 762 771 822 623 657 726 Bicat softening temperature (° G) 77 77 77 77 75 68 67 79 78 77 Dynamic thermal stability (min) 24 12 10 21 13 24 36 9 21 13 Appearance O um ⁇ X ⁇ um OXX um [Evaluation of force render press molding characteristics]
- Tables 5 and 6 show the results evaluated by the following evaluation methods.
- ASEA (m 2 / g) 832 776 763 721 763 762 829 663 641 715 Vicat softening temperature (° C) 78 77 77 77 76 68 68 78 78 77 Thermal stability of press (min) 30 10 10 20 10 25 35 10 15 10
- Tables 5 and 6 show the results evaluated by the following evaluation methods.
- Extrusion press thermal stability The compositions of Examples 1 to 9 and Comparative Examples 1 to 10 were extruded into a 4 mm-thick plate by a twin-screw extruder, and were extruded by a hot plate at 200.
- ASEA (mVg) 771 752 744 666 715 781 744 758 741 Vicat softening temperature (° C) 77 77 77 77 77 77 77 76 77
- Extrusion press thermal stability (min) 20 15 15 20 15 20 15 15 20
- ASEA (m 2 / g) 825 758 761 739 781 769 815 633 681 751 Vicat softening temperature (° C) 77 77 77 77 75 68 66 78 78 77 Extrusion press thermal stability (min) 20 10 10 15 10 15 25 10 15 10 Appearance ⁇ ⁇ ⁇ XO ⁇ OXX
- Example 4 In each of the molded articles obtained by the extrusion molding method, the calendar press molding method, and the continuous extrusion press molding method, the composition of Example 4 showing almost the same thermal stability was used. mm compacts were produced by extrusion molding, force render press molding, and extrusion continuous press molding. In the case of the calendar press molding method, 5 or 10 sheets having a thickness of 1 mm were laminated in the same manner as described above.
- a 5 mm thick compact is placed horizontally, and the end surface of a 5 mm thick compact of the same composition is placed vertically on the surface of the compact.
- the thickness distribution of a molded product having a thickness of 1 Omm was evaluated by the thickness deviation R.
- vinyl chloride resin vinyl chloride homopolymer having a polymerization degree of 780
- test piece A AHRR (Kw / m 2 ) and ASEA (m 2 / g) were measured according to AST ME 1354 using a cone calorimeter manufactured by Atlas.
- Specimen A was immersed in 2 Om I pure water heated to 60 ° G. After holding for 8 hours, the change in hue before and after immersion was measured using a color difference measuring device, and the ⁇ of value was determined.
- test piece A was immersed in 20 ml of pure water heated to 60 ° G. In this state: After holding for 48 hours, the pH of the aqueous solution was measured with a pH meter.
- a sheet-like extruded product was obtained in the same manner as the above test piece, and this was cut into a size of 10 Omm x 10 Omm to obtain a test piece B. Heating was performed in an oven at 200 ° C, and the time during which no blackening occurred was visually determined and evaluated according to the following criteria.
- test piece B was applied to an X-ray fluorescence spectrometer to perform qualitative analysis of lead metal, and evaluated according to the following criteria.
- ASEA (m 2 / g) 536 601 721 704 654 Discoloration resistance After immersion in water at 60 ° C for 48 hours Aa 0.22 0.20 0.02-0.08-0.29
- ASEA (m 2 / g) 729 631 592 698 Discoloration resistance After immersion in water at 60 ° C for 48 hours Aa -0.01 -0.33 0.18 -0.11
- Polyvinyl chloride resin polymerization degree 780 100 100 100 100 100 100 100 100 100 100 100
- Comparative Example 15 Although the basic compound was not blended, a result excellent in discoloration resistance was obtained. This is because the lead stabilizer used in Comparative Example 15 was It is presumed that the basicity is stronger than that of the organotin-based stabilizer used in the present invention.
- the obtained solid was dried, calcined, and pulverized to obtain a smoke suppressant in which a molybdenum-based compound was coated with titanium oxide or a basic compound as a nucleating agent.
- the flame-retardant vinyl chloride resin compositions shown in Tables 11 and 12 were molded by extrusion molding, calendar press molding, and continuous extrusion press molding, and the present invention and comparative plate-shaped moldings having the following dimensions were used. A molded body was obtained, and the following properties were evaluated for the molded body. The results are shown in Tables 11 and 12.
- AHRR kW / m 2
- ASEA mVg
- a molded body having a thickness of 1 mm, a width of 2 Omm, and a length of 2 Omm was heated in an oven at 200 ° C, and the time during which no blackening occurred was visually determined and evaluated according to the following criteria.
- a molded body having a thickness of 5 mm, a width of 2 Omm, and a length of 2 Omm was applied to a fluorescent X-ray measuring apparatus to conduct qualitative analysis of lead metal, and evaluated based on the following criteria.
- a molded body having a thickness of 1 mm, a width of 2 Omm and a length of 2 Omm was immersed in 35% hydrochloric acid at 60 ° G for 48 hours, and the weight before and after immersion was measured to determine the rate of change.
- the state of aggregation and dispersion of the smoke preventive agent was visually determined, and evaluated according to the following criteria.
- ASEA (mVg) 705 705 705 Resistance to hot water discoloration 48 hours at 60 ° C 3-0.03-0.03-0.03
- ASEA (mVg) 689 682 721 Discoloration resistance to hot water at 60 ° C for 48 hours Aa 0.26 0.16-0.09 Thermal stability ⁇ ⁇ ⁇ Presence or absence of environmentally hazardous substances (lead compounds) ⁇ ⁇ ⁇ ⁇ Chemical resistance at 60 ° C for 48 hours 35% hydrochloric acid 0.34 0.34 0.3 Appearance (dispersibility) ⁇ ⁇ ⁇
- Example 32 Vinyl chloride resin polymerization degree 780 100 100
- ASEA 856 697 643 Hot water discoloration resistance 60 ° G for 48 hours um a-0.02 -0.11 -0.68 Thermal stability ⁇ X ⁇
- Environmentally hazardous substance (lead content) ⁇ ⁇ ⁇ ⁇
- Chemical resistance 60 ° G for 48 hours 35%
- Hydrochloric acid 0.23 0.29 0.31
- Appearance (dispersibility) O ⁇ ⁇
- ASEA (mVg) 674 674 674 Hot water discoloration resistance 60 ° G for 48 hours a-0.72-0.91 -0.82 Thermal stability ⁇ ⁇ ⁇ Environmentally hazardous substances (lead content) O ⁇ ⁇ ⁇ Chemical resistance 60 ° G 48 hours 35% hydrochloric acid 0.34 0.48 0.41 Appearance (dispersibility) ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ Open
- the flame-retardant vinyl chloride resin composition of the present invention As is clear from Tables 11 and 12, according to the flame-retardant vinyl chloride resin composition of the present invention and the molded article thereof, since the components in the composition are well dispersed, the molded article is It shows an excellent appearance without poor dispersion, and also has excellent hot water discoloration resistance, flame retardancy, chemical resistance, and the like.
- the flame-retardant vinyl chloride resin composition of the present invention since not only the flame retardancy is excellent but also the moldability is excellent, molded articles of various forms can be easily obtained by various molding methods. In addition, the molded article has excellent flame retardancy, generates a small amount of smoke, has a high softening temperature, and has good appearance.
- molded articles made of the resin composition of the present invention can be used for transport equipment inside and outside of aircraft, ships, and vehicles; interior and exterior materials for buildings; daily necessities such as furniture and office tools; and housing materials for home appliances and electronic devices. Suitable as a component of a semiconductor device.
- molded articles produced by the continuous extrusion press molding method do not lose gloss during thermal processing, are excellent in solvent resistance> chemical resistance, and have high thickness accuracy. Can be used well.
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Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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US10/533,814 US20060014874A1 (en) | 2002-11-05 | 2003-11-04 | Flame-resistant vinyl chlorride based resin composition and formed product therefrom |
US12/153,464 US20080227895A1 (en) | 2002-11-05 | 2008-05-20 | Fire retardant vinyl chloride-based resin composition and molded article thereof |
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JP2002-320677 | 2002-11-05 | ||
JP2002320677 | 2002-11-05 | ||
JP2003309719 | 2003-09-02 | ||
JP2003-309719 | 2003-09-02 | ||
JP2003-343842 | 2003-10-01 | ||
JP2003343842A JP4869549B2 (ja) | 2003-10-01 | 2003-10-01 | 難燃性塩化ビニル系樹脂組成物および難燃性塩化ビニル系樹脂成形体 |
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US12/153,464 Division US20080227895A1 (en) | 2002-11-05 | 2008-05-20 | Fire retardant vinyl chloride-based resin composition and molded article thereof |
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WO2004041930A1 true WO2004041930A1 (ja) | 2004-05-21 |
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PCT/JP2003/014052 WO2004041930A1 (ja) | 2002-11-05 | 2003-11-04 | 難燃性塩化ビニル系樹脂組成物およびその成形体 |
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US (2) | US20060014874A1 (ja) |
KR (1) | KR101014640B1 (ja) |
TW (1) | TWI334428B (ja) |
WO (1) | WO2004041930A1 (ja) |
Cited By (4)
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WO2007035027A1 (en) * | 2005-09-23 | 2007-03-29 | Lg Chem, Ltd. | Adhesive sheet and manufacturing method thereof |
US8070990B2 (en) * | 2006-11-03 | 2011-12-06 | J.M. Huber Corporation | Smoke suppressants |
CN103242607A (zh) * | 2013-05-23 | 2013-08-14 | 苏州富通高新材料科技股份有限公司 | 一种可刨可钉的pvc仿木地板及其制备方法 |
CN108384403A (zh) * | 2018-02-12 | 2018-08-10 | 莆田学院 | 一种核壳结构纳米二氧化硅/锡酸锌阻燃环氧丙烯酸酯涂层的制备方法 |
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DE102008018872A1 (de) * | 2008-04-14 | 2009-10-15 | Ika Innovative Kunststoffaufbereitung Gmbh & Co. Kg | Stabilisatorsystem für halogenhaltige Polymere |
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CN108384403B (zh) * | 2018-02-12 | 2019-12-31 | 莆田学院 | 一种核壳结构纳米二氧化硅/锡酸锌阻燃环氧丙烯酸酯涂层的制备方法 |
Also Published As
Publication number | Publication date |
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US20080227895A1 (en) | 2008-09-18 |
KR20050057685A (ko) | 2005-06-16 |
TWI334428B (en) | 2010-12-11 |
TW200422341A (en) | 2004-11-01 |
KR101014640B1 (ko) | 2011-02-16 |
US20060014874A1 (en) | 2006-01-19 |
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