EP2473290A1 - Composites de revêtement flexibles composés principalement d'une composition minérale - Google Patents
Composites de revêtement flexibles composés principalement d'une composition minéraleInfo
- Publication number
- EP2473290A1 EP2473290A1 EP10734069A EP10734069A EP2473290A1 EP 2473290 A1 EP2473290 A1 EP 2473290A1 EP 10734069 A EP10734069 A EP 10734069A EP 10734069 A EP10734069 A EP 10734069A EP 2473290 A1 EP2473290 A1 EP 2473290A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- coating
- substrate
- drying
- dispersion
- coatings
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 12
- 239000011707 mineral Substances 0.000 title claims abstract description 12
- 238000000576 coating method Methods 0.000 title claims description 105
- 239000011248 coating agent Substances 0.000 title claims description 87
- 239000000203 mixture Substances 0.000 title claims description 57
- 239000002131 composite material Substances 0.000 title description 22
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000004566 building material Substances 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims description 58
- 239000006185 dispersion Substances 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 229920000642 polymer Polymers 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 20
- 239000004815 dispersion polymer Substances 0.000 claims description 13
- 150000004756 silanes Chemical class 0.000 claims description 11
- 150000002484 inorganic compounds Chemical class 0.000 claims description 10
- 229910010272 inorganic material Inorganic materials 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- -1 3-glycidyloxypropyl Chemical group 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229920000620 organic polymer Polymers 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 238000005452 bending Methods 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920000193 polymethacrylate Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- 229910052716 thallium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 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 claims 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 26
- 239000010410 layer Substances 0.000 description 19
- 238000002360 preparation method Methods 0.000 description 18
- 238000009792 diffusion process Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 12
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 238000002454 metastable transfer emission spectrometry Methods 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 230000005855 radiation Effects 0.000 description 7
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 7
- 229910002012 Aerosil® Inorganic materials 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 230000035882 stress Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000012948 isocyanate Substances 0.000 description 5
- 150000002513 isocyanates Chemical class 0.000 description 5
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- OEBRKCOSUFCWJD-UHFFFAOYSA-N dichlorvos Chemical compound COP(=O)(OC)OC=C(Cl)Cl OEBRKCOSUFCWJD-UHFFFAOYSA-N 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000007761 roller coating Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229920001342 Bakelite® Polymers 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 239000011260 aqueous acid Substances 0.000 description 2
- 239000004637 bakelite Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- 125000001033 ether group Chemical group 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000003709 fluoroalkyl group Chemical group 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000417 fungicide Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 229910001960 metal nitrate Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920001601 polyetherimide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000003847 radiation curing Methods 0.000 description 2
- 239000005871 repellent Substances 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 150000003377 silicon compounds Chemical class 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- ANFXTILBDGTSEG-UHFFFAOYSA-N 1-methyl-4,5-dihydroimidazole Chemical compound CN1CCN=C1 ANFXTILBDGTSEG-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- 244000056139 Brassica cretica Species 0.000 description 1
- 235000003351 Brassica cretica Nutrition 0.000 description 1
- 235000003343 Brassica rupestris Nutrition 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 240000007154 Coffea arabica Species 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 229910004541 SiN Inorganic materials 0.000 description 1
- 229910020263 SiP Inorganic materials 0.000 description 1
- 240000003768 Solanum lycopersicum Species 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical class O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- QKSKPIVNLNLAAV-UHFFFAOYSA-N bis(2-chloroethyl) sulfide Chemical compound ClCCSCCCl QKSKPIVNLNLAAV-UHFFFAOYSA-N 0.000 description 1
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- YGUFXEJWPRRAEK-UHFFFAOYSA-N dodecyl(triethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OCC)(OCC)OCC YGUFXEJWPRRAEK-UHFFFAOYSA-N 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical compound O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000019674 grape juice Nutrition 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 125000001183 hydrocarbyl group Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 235000008960 ketchup Nutrition 0.000 description 1
- HNEGQIOMVPPMNR-NSCUHMNNSA-N mesaconic acid Chemical compound OC(=O)C(/C)=C/C(O)=O HNEGQIOMVPPMNR-NSCUHMNNSA-N 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 235000010460 mustard Nutrition 0.000 description 1
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 1
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 238000007645 offset printing Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007649 pad printing Methods 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
- OYGYKEULCAINCL-UHFFFAOYSA-N triethoxy(hexadecyl)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC OYGYKEULCAINCL-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/58—No clear coat specified
- B05D7/584—No clear coat specified at least some layers being let to dry, at least partially, before applying the next layer
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/08—Processes in which the treating agent is applied in powder or granular form
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06N3/047—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with fluoropolymers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/18—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials
- D06N3/183—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with two layers of different macromolecular materials the layers are one next to the other
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N7/00—Flexible sheet materials not otherwise provided for, e.g. textile threads, filaments, yarns or tow, glued on macromolecular material
- D06N7/0094—Fibrous material being coated on one surface with at least one layer of an inorganic material and at least one layer of a macromolecular material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2701/00—Coatings being able to withstand changes in the shape of the substrate or to withstand welding
- B05D2701/30—Coatings being able to withstand changes in the shape of the substrate or to withstand welding withstanding bending
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/147—Stainproof, stain repellent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/06—Building materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
Definitions
- the present invention relates to a process for the production of a flexible predominantly mineral coating composite for the production or coating of building materials and the necessary manufacturing process.
- the substrates that are coated can have very different properties.
- hard substrates ie non-flexible substrates
- flexible building materials e.g. Surface coverings for walls, floors and ceilings.
- material composites such as flexible tiles, textiles, wallpaper or floor coverings such as linoleum should be mentioned here.
- All substrates have in common that they must have a surface that withstands a more or less heavy use during use.
- One requirement is that they be resistant to material influences, such as e.g. aggressive chemicals or environmental factors, such as UV radiation and water must be.
- material influences such as e.g. aggressive chemicals or environmental factors, such as UV radiation and water must be.
- a permeable composite material is known.
- a coating is applied to a material-permeable carrier, which is subsequently cured.
- the coating contains at least one inorganic component, wherein an inorganic component comprises at least one compound of a metal, semimetal or misch metal with at least one element of the third to seventh main group of the periodic table.
- the coating composition can be obtained by hydrolysis of a precursor. In this case, a sol can form, which is subsequently applied to the material-permeable substrate.
- the fabric-permeable composite materials disclosed in WO 99/15262 are characterized by the fact that they constitute a robust material composite, which protect the substrate or the substrate to which they are applied, and even at low radii of curvature of the composite no impairment of the applied coating occurs , Disadvantages of these composites are their high and intended material permeability, the high absorbency for liquids and related the low stain and abrasion resistance, which does not ensure sufficient protection of substrates and / or substrates for the applications sought. The attempt to improve the tightness of such composite materials, and overcome these disadvantages, but so far led to brittle material or a material with significantly reduced flexibility.
- the document DE 10 2004 006612 A1 teaches to protect a carrier material with a ceramic coating against scratching stress and to make the material washable.
- an intermediate layer containing particles of Al 2 O 3, ZrO 2, ⁇ 2 and / or SiO 2 surrounded by a silicate network can be applied.
- a major disadvantage of such material composites is the easy soiling and the high brittleness, the latter by the fact that the desirable scratch resistance is produced by the use of the adhesion promoters described therein.
- a disadvantage of this procedure is the relatively high material costs, which preclude a commercial distribution of this material. They result from the thicker layers and possibly from the use of fluorosilanes. In the absence of the use of fluorosilanes, these materials show no stain resistance. Another disadvantage is that the resulting materials are subject to aging, which manifests itself in the increase in brittleness over time. This is disadvantageous for processing older material.
- the technical task on which the present invention is based is the provision of cost-effective, coated substrates which have a coating which protects the substrate or the substrate from environmental influences and a stress during use, the substrate also being flexible can and the coating is not adversely affected by a deformation of such a composite material even after aging.
- Another object of the present invention is to provide a method for making such improved composite materials.
- the composition contains at least one inorganic compound
- the coating being a mixture
- R is an alkyl or alicyclic radical having 1 to 18 carbon atoms and all Rs may be the same or different,
- the advantage of the coating obtained according to step 2) of the method according to the invention consists in the increase of mechanical resistance and provides a resistant body, which realizes a basic protection of the substrate and possibly the substrate, equivalent to a spatial barrier.
- substrates susceptible to cracking or cracking are mechanically stabilized by this method step according to the invention.
- the benefit of the coating obtained after step 3) or after step 4) of the method according to the invention lies in a solidification of the coating of step 2) and the preparation of the surface to form the desired surface properties in the implementation of step 5).
- the advantage of the coating obtained after step 5) of the method according to the invention is the formation of the surface properties of the composite material according to the invention.
- the process of the present invention is not limited to any specific substrates.
- the substrates can be both open-pored and closed-pore.
- the substrate in step 1) may be a flexible and / or rigid substrate.
- the substrate of step 1) is a knitted fabric, a woven fabric, a braid, a film and / or a sheet.
- the substrate is substantially thermally stable under the drying conditions of steps 2), 3) or 4) and 5).
- the inorganic compound of step 2) is selected from TiO 2 , Al 2 O 3 , SiO 2 , ZrO 2 , Y 2 O 3 , BC, SiC, Fe 2 O 3 , SiN, SiP, aluminosilicate, Aluminum phosphates, zeolites, partially exchanged zeolites or mixtures thereof.
- Preferred zeolites are, for example, Wessalith® types or ZSM types or amorphous microporous mixed oxides.
- the inorganic compound of step 2) has a particle size of 1 nm to 10,000 nm. It can be advantageous if the composite material according to the invention has at least two particle size fractions of the at least one inorganic compound.
- the particle size ratio may be from 1: 1 to 1: 10,000, preferably from 1: 1 to 1: 100.
- the quantitative ratio of the particle size fractions in the composition of step 2) may preferably be from 0.01: 1 to 1: 0.01.
- the composition of step 2) is preferably a suspension, which is preferably an aqueous suspension.
- the suspension may preferably comprise a liquid selected from water, alcohol, acid or a mixture thereof.
- the inorganic compound of step 2) can be obtained by hydrolyzing a precursor of the inorganic compound containing the metal and / or semimetal.
- the hydrolyzing can be done for example by water and / or alcohol.
- an initiator may be present, which is preferably an acid or base, which is preferably an aqueous acid or base.
- the precursor of the inorganic compound is preferably selected from metal nitrate, metal halide, metal carbonate, metal alcoholate, semi-metal halide, half metal alcoholate or mixture thereof.
- Preferred precursors are e.g. Titanium alcoholates, e.g. Titanium isopropylate, silicon alcoholates, e.g. Tetraethoxysilane, zirconium alcoholates.
- Preferred metal nitrates are e.g. Zirconium.
- in the composition with respect to the hydrolyzable precursor based on the hydrolysable group of the precursor, at least half the molar ratio of water, water vapor or ice, are included.
- the composition of step 2) is a sol.
- it is possible to add commercially available sols such as, for example, titanium nitrate sol, zirconium nitrate sol or silica sol.
- silanes of the formula (Z 2 ) Si (OR) 3, where Z 2 is R, OR, Gly (Gly 3-glycidyloxypropyl), AP (aminopropyl) and / or AEAP (N-2-aminoethyl 3-aminopropyl) and R is an alkyl radical of 1 to 18 carbon atoms and all R may be the same or different and oxide particles selected from the oxides of Ti, Si, Zr, Al, Y, Sn, Zn, Ce or mixtures thereof may be added , The oxide particles may have a particle size of 10 nm to ⁇ ⁇ .
- the drying of the composition in step 2) is carried out by heating to a temperature between 50 ° C and 1, 000 ° C. In a preferred embodiment is dried for 10 seconds to 5 hours at a temperature of 50 ° C to 500 ° C and most preferably dried at a temperature of 120 ° C to 250 ° C for 20 seconds to 30 minutes.
- the drying in step 2) can be carried out by means of heated air, hot air or electrically generated heat.
- radiation curing may follow, for example, by infrared or microwave irradiation.
- a further coating can be carried out according to steps 3) or 4).
- the function of this coating is essentially the formation of a robust material composite.
- steps 3) and 4) can be carried out in any order. This procedure advantageously increases the resistance of the building material, since after the repetition of 3) and / or 4) a plurality of intimately and yet not rigidly interconnected thin layers are obtained.
- the coating of step 3) comprises a polymer dispersion, a mixture of different polymer dispersions or a formulation of at least one polymer dispersion.
- the polymer dispersions may consist of polymeric substances of polyacrylates, polymethacrylates, polyurethanes, polyolefins, polycarbonates, polyesters, polyamides, polyimides, polyetherimides, silicone resins and combinations or copolymers / cocondensates, if appropriate with the use of further vinyl monomers thereof, which optionally contain additional functions for crosslinking , such as Epoxide, isocyanate, blocked isocyanates and / or radiation-curable double bonds.
- the average molecular weight of the polymers is preferably greater than 10,000 g / mol, more preferably greater than 20,000 g / mol.
- the polymer dispersions may be aqueous or contain organic solvents.
- the wet application rate of polymer dispersion is 10 to 200 g / m 2 at solids use concentrations of 0.1 to 150 g / L, preferably 3 to 100 g / L in the liquor. It is particularly preferred, in step 3), to use aqueous polymer dispersions. These dispersions may be self-emulsifying or stabilized with emulsifiers.
- polymer dispersions are used which have a high washing permanence.
- the polymer dispersions may in known manner be adjuvants such as e.g. Emulsifiers, defoamers, fixing resins, fungicides, antistatic agents or catalysts can be added for efficient use.
- the order of the polymer dispersions can be done by doctoring, spraying, rollercoating, dipping, padding, flooding, foam application or by brushing in a conventional manner.
- the drying of the composition in step 3) is carried out by heating to a temperature between 80 ° C and 250 ° C.
- a temperature between 80 ° C and 250 ° C.
- the drying during step 3) can be effected by means of heated air, hot air, IR radiation, microwave radiation or electrically generated heat.
- R and / or Z 1 in the general formula (Z 1 ) Si (OR) 3 in addition to the other meanings of Z 1 is methyl, ethyl or a straight-chain, branched or alicyclic alkyl radical with 3 , 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17 and / or 18 carbon atoms.
- the coating of step 4) comprises 3-glycidyloxypropyltriethoxysilane and / or 3-glycidyloxypropyltrimethoxysilane as silane, and 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-2-aminoethyl-3-aminopropyltrimethoxysilane, and / or N-2 Aminoethyl-3-aminopropyltriethoxysilane as second silane.
- the coating of step 4) contains as further silane a silane of the formula R z Si (OR) 4-z , where z is 1 or 2 and all Rs may be the same or different and contain from 1 to 18 carbon atoms. At 3 to 18 carbon atoms, the carbon chain may be branched or linear.
- the coating of step 4) contains a mixture of at least 2 polymers.
- step 4 Further preferred in the coating of step 4) are butyltriethoxysilane, isobutyltriethoxysilane, octyltriethoxysilane, dodecyltriethoxysilane and / or hexadecyltriethoxysilane. It has been found, in particular, that when using alkylsilanes in step 4 a synergistic effect on the unfolding of the stain-repellent properties on the final coating in the described composite material is achieved.
- the initiator contained in the coating of step 4) is an acid or base, which is preferably an aqueous acid or base.
- the surface of the oxide particles contained in the coating of step 4) is hydrophobic.
- On the surface of the oxide particles of the coating of step 4) are preferably bound to silicon atoms organic radicals Xi + 2 n C n present, where n is 1 to 20 and X is hydrogen and / or fluorine.
- the organic radicals may be the same or different.
- n is 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 and / or 20.
- the Silicon atoms bonded groups methyl, ethyl, propyl, butyl and / or pentyl groups. In a particularly preferred embodiment, trimethylsilyl groups are bonded to the surface of the oxide particles.
- the organic radicals can preferably be cleaved off and more preferably hydrolyzed.
- the oxide particles of the coating of step 4) may be selected from the oxides of Ti, Si, Zr, Al, Y, Sn, Zn, Ce or mixtures thereof.
- the oxide particles of the coating of this step are partially hydrolyzed under its reaction conditions on the surface of the oxide particles.
- reactive centers are preferably formed which react with the organic silicon compounds of the coating of step 4).
- These organic silicon compounds can be covalently bound to the oxide particles during drying, for example by -O bonds. As a result, the oxide particles are covalently crosslinked with the hardening coating.
- the oxide particles may have an average particle size of from 10 nm to 10 ⁇ m, preferably from 20 to 1000 nm, more preferably from 30 to 500 nm. If the coating is to be transparent and / or colorless, it is preferred to use only oxide particles which have an average particle size of from 10 to 250 nm.
- the mean particle size refers to the particle size of the primary particles or, if the oxides are present as agglomerates, on the size of the agglomerates. The particle size is determined by light-scattering methods, for example by a device of the HORIBA LB 550® type (from Retsch Technology).
- the polymer preferably has an average weight average molecular weight of at least 3000 g / mol.
- the average weight average molecular weight is at least 5000 g / mol, more preferably at least 6000 g / mol, and most preferably at least 10,000 g / mol.
- the polymer of the coating of step 4) has an average degree of polymerization of at least 50. In a further preferred embodiment, the average degree of polymerization is at least 80, more preferably at least 95 and most preferably at least 150.
- the polymer of the coating of step 4) selected from polyamide, polyester, epoxy resins, melamine-formaldehyde condensate, urethane-polyol resin or mixtures thereof.
- the amount of coating applied is preferably such that, after drying, a layer of the dried coating with a layer thickness of 0.05 to 30 ⁇ is present.
- a coating of step 4) with a layer thickness of 0.1 ⁇ to 20 ⁇ and most preferably from 0.2 ⁇ to 10 ⁇ available.
- the application of the coating 4) can be done by doctoring, spraying, rollercoating, dipping, flooding, or by brushing in a conventional manner.
- the drying of the coating in step 4) may be carried out by any method known to those skilled in the art.
- the drying can be carried out in an oven. More preferably, the drying with a hot air oven, convection oven, microwave oven or by infrared radiation.
- the coating 4) is dried by heating at a temperature between 50 ° C and 300 ° C for 1 second to 30 minutes, and most preferably at 1 10 to 200 ° C in a period of 5 seconds to 10 minutes dried. If technically sensible and necessary, radiation curing by means of UV or electron radiation can be connected.
- step 4) is dried for 1 second to 10 minutes at a temperature of 100 ° C to 800 ° C.
- the coating of step 5) comprises a polymer dispersion, a mixture of different polymer dispersions or a formulation of at least one polymer dispersion.
- the polymer dispersions may consist of polymeric substances of polyacrylates, polymethacrylates, polyurethanes, polyolefins, polycarbonates, polyesters, polyamides, polyimides, polyetherimides, silicone resins and combinations or copolymers / cocondensates, if appropriate with the use of further vinyl monomers thereof, which optionally contain additional functions for crosslinking , such as Epoxide, isocyanate, blocked isocyanates and / or radiation-curable double bonds.
- the average molecular weight of the polymers is preferably greater than 10,000 g / mol, more preferably greater than 20,000 g / mol.
- the dispersions may be aqueous or contain organic solvents.
- the wet application rate of polymer dispersion is 10 to 200 g / m 2, at solids use concentrations of 0.1 to 120 g / L, preferably from 3 to 70 g / L in the liquor.
- aqueous polymer dispersions in step 5). These dispersions may be self-emulsifying or stabilized with emulsifiers.
- polymer dispersions are used which have a high washing permanence.
- the polymer dispersions can be prepared in known manner as auxiliary agents, e.g. Emulsifiers, defoamers, fixing resins, fungicides, antistatic agents or catalysts can be added for efficient use.
- the order of the polymer dispersions can be done by doctoring, spraying, rollercoating, dipping, padding, flooding, foam application or by brushing in a conventional manner.
- step 5) it may be advantageous, after step 3) or 4), to carry out step 5) repeatedly, particularly preferably to carry it out repeatedly, so that no other step of the method according to the invention is carried out between two successive executions of step 5). Furthermore, it may be advantageous to use fluorocarbons in at least one implementation of step 5), particularly preferably in the last-time implementation of this step. If step 5) is performed only once, it is most preferred to use fluorocarbons in this procedure.
- Polymers with fluorinated side chains can be used with particular preference, very particularly preferably those which are additionally combined with non-fluorinated hydrocarbon side chains.
- step 5 is carried out repeatedly and fluorocarbons are used in more than one operation, it may also be advantageous to use fluorocarbons having the same fluoroalkyl groups, the same ether chains, and / or the same side chains of the fluorinated chains in each run.
- the polymer dispersions may contain crosslinkers (e.g., blocked isocyanates).
- the polymer dispersions may preferably be cationically modified and contain booster and extender.
- the Crosslinker can also act as a booster.
- the order of organically bound fluorine is from 0.01 to 12 g / m 2, preferably from 0.1 to 6 g / m 2.
- the drying of the composition in step 5) is carried out by heating to a temperature between 80 ° C and 250 ° C. In a preferred embodiment, it is dried for 10 seconds to 6 hours at a temperature of 110 ° C. to 210 ° C., and most preferably dried at a temperature of 130 ° C. to 190 ° C. for 20 seconds to 60 minutes.
- the drying of step 5) can be effected by means of heated air, hot air, IR radiation, microwave radiation or electrically generated heat.
- At least one further coating can be applied before the application of the coating in step 3) or 4) and 5) at least one further coating can be applied.
- This further coating can be, for example, a print.
- Such printing can be applied by any printing method known to those skilled in the art, in particular the offset printing method, flexographic printing method, pad printing or inkjet printing method. If the coated substrate in its finished embodiment is to be applied to a substrate, in a further embodiment, after application of the coating in step 2), 3) or 4) and 5), a further coating can be applied as a backside coating. This barrier layer then forms the back and if further coatings follow, they are applied only on the opposite side.
- This further coating is not limited and may be any coating known to those skilled in the art. This coating can also be a print.
- Coated substrates of the present invention surprisingly show very high flexibility if the substrate is flexible.
- the substrate can be bent without the applied coatings being destroyed or torn.
- a wide variety of protective layers can be applied as a coating, in particular protective layers against aggressive chemicals or dirt-repellent coatings.
- the water vapor diffusion resistance also called water vapor equivalent air layer thickness SD, expresses the extent to which a building material hampers the diffusion of water vapor in the sense of its thermally driven propagation.
- Water vapor diffusion resistances of various materials are related to the water vapor diffusion resistance of air by means of the water vapor diffusion resistance number.
- the water vapor diffusion resistance number (symbol ⁇ ) of a building material is a dimensionless material characteristic value. This indicates the factor by which the material in question is closer to water vapor than an equally thick, stationary air layer. The larger this material characteristic is, the denser a building material is against water vapor. For air is defined
- the determination of the water vapor-equivalent air layer thickness SD, unit meter, is given in the standard DIN 53122-1.
- the water vapor diffusion resistance is calculated as follows:
- the thickness is the thickness of the static air layer in m, which has the same water vapor diffusion resistance.
- a 20 cm thick brick wall has a diffusion resistance of
- polystyrene is quite permeable to vapor - comparable to wood, for example.
- the value of SD is between about 0.25 m and 10 m.
- vapor barrier films which are more porous in moist air than in dry air.
- the method according to the invention achieves mineral building materials whose water vapor-equivalent air layer thickness SD is far superior to that of the coatings from the cited prior art DE 10 2004 006612 A1 or WO 2007/051680.
- a low value of SD is important for the formation of a good indoor climate, which is temporarily exposed to high humidity.
- Another object of the present invention is therefore also the flexible mineral building material, which is obtained by the process according to the invention.
- the present invention is therefore also a flexible mineral building material having a stain resistance of at most 10, an elongation at break of at least 13%, an elongation after 7d storage at 60 ° C of at least 10%, a minimum bending radius of at most 3 mm, and a water vapor equivalent air layer thickness SD of at most 0.2 m.
- a laid PET nonwoven (basis weight: 45 gsm, thickness 0.39 mm) was impregnated with this dispersion and dried in the oven for 10 seconds at 220 ° C and cured. The dispersion was applied so much that the dry weight of the coated nonwoven was 220 g / m 2.
- Aerosil® R812S was dispersed in 67.7 g of GLYMO, followed by the addition of 26.0 g of bisphenol A and 3.4 g of 1% HCl with stirring. After stirring at 6 ° C. for 24 h, 2.3 g of methylimidazoline and 10.2 g of Bakelite EPR 760 were added and the mixture was stirred for a further 20 h.
- Stain resistance is achieved by adding 1 - 3 ml of coffee, tea, tomato ketchup, mustard, 1% NaOH, 10% citronic acid solution, shower gel "Hair & Body” by Stoko Skincare, grape juice, vegetable oil for one hour and rinsing with water without further
- the assessment is carried out by awarding points, in each case for each test equipment:
- Stain resistance is the sum of the points awarded for each test equipment.
- the abrasion resistance is determined in accordance with DIN EN 12956 and DIN EN 259-1 for highly abrasion-resistant surfaces. It is concretized by looking at it from three optical angles: top view with a magnifying glass (8x), at an acute angle to the surface, and across the illuminated surface against a black background.
- Evaluation 0 points for no change, 10 points for visible change according to standard, 1 point for visibility of protruding fibers, 2 points for many protruding fibers and 3 points for change in gloss at an acute angle. The sum of the evaluation criteria is formed. The elongation at break is measured using a device from Zwick, type Z2.5 / PN1 S.
- PET nonwoven PET FFKH 7210 was applied with this dispersion in a thickness of 50 ⁇ and dried in an oven at 130 ° C for 30 min.
- PET nonwoven PET FFKH 7210 was soaked with this dispersion and incorporated in the
- the previously coated substrate was coated with this mixture and dried at 150 ° C in the oven.
- a PET nonwoven (basis weight: 45 gsm, thickness 0.39 mm) was impregnated with this dispersion and oven dried at 230 ° C and cured.
- the previously coated PET nonwoven was coated with this mixture and dried at 150 ° C in the oven.
- a PET nonwoven (basis weight: 45 gsm, thickness 0.39 mm) was impregnated with this dispersion and oven dried at 230 ° C and cured.
- a PET nonwoven (basis weight: 45 gsm, thickness 0.39 mm) was impregnated with this dispersion and oven dried at 220 ° C.
- Dynasylan GLYEO In 18.8 g of Dynasylan GLYEO, 1.6 g of water and 0.03 g of 65% HNO 3 were introduced and stirred until clear. 7.8 g of Aerosil R812S and 44.4 g of ethanol were added to this solution. To this suspension was added 16 g of Dynasylan AMEO and 2.3 g of Dynasylan IBTEO and stirred for a further 24 h at room temperature.
- the previously coated substrate was coated with this mixture and dried at 150 ° C in the oven.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Finishing Walls (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
La présente invention concerne un procédé de fabrication d'un matériau de construction minéral flexible, ainsi que le matériau de construction obtenu selon ce procédé.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102009029152A DE102009029152A1 (de) | 2009-09-03 | 2009-09-03 | Flexible Beschichtungsverbünde mit überwiegend mineralischer Zusammensetzung |
PCT/EP2010/059609 WO2011026668A1 (fr) | 2009-09-03 | 2010-07-06 | Composites de revêtement flexibles composés principalement d'une composition minérale |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2473290A1 true EP2473290A1 (fr) | 2012-07-11 |
Family
ID=42802252
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10734069A Withdrawn EP2473290A1 (fr) | 2009-09-03 | 2010-07-06 | Composites de revêtement flexibles composés principalement d'une composition minérale |
Country Status (8)
Country | Link |
---|---|
US (1) | US9180487B2 (fr) |
EP (1) | EP2473290A1 (fr) |
JP (1) | JP2013503989A (fr) |
BR (1) | BR112012004902A2 (fr) |
DE (1) | DE102009029152A1 (fr) |
RU (1) | RU2547737C9 (fr) |
UA (1) | UA106995C2 (fr) |
WO (1) | WO2011026668A1 (fr) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9234310B2 (en) * | 2011-10-11 | 2016-01-12 | The Sweet Living Group, LLC | Fabric having ultraviolet radiation protection, enhanced resistance to degradation, and enhanced resistance to fire |
US8690964B2 (en) * | 2011-10-11 | 2014-04-08 | The Sweet Living Group, LLC | Fabric having ultraviolet radiation protection |
JP2016002681A (ja) * | 2014-06-16 | 2016-01-12 | ニチハ株式会社 | 建材とその製作方法 |
EP3218541A4 (fr) * | 2014-11-12 | 2018-07-11 | The University Of Houston System | Revêtements résistants à la salissure, résistants aux taches et procédés d'application sur des matériaux textiles ou d'autres matériaux flexibles |
JP6803836B2 (ja) | 2014-11-12 | 2020-12-23 | ユニバーシティー オブ ヒューストン システム | 耐候性、真菌耐性および耐染色性のコーティング、ならびに木材、レンガまたは他の多孔質材料に適用する方法 |
WO2016077550A1 (fr) * | 2014-11-12 | 2016-05-19 | University Of Houston System | Revêtements résistant à la salissure, résistant aux taches sans fluor et procédés d'application sur des matériaux |
Family Cites Families (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US612439A (en) | 1898-10-18 | Potato-digger | ||
CA1068178A (fr) | 1975-09-11 | 1979-12-18 | United Technologies Corporation | Couche thermofuge pour superalliage a base de nickel |
US4347277A (en) * | 1978-11-03 | 1982-08-31 | General Signal Corporation | Corrosion resistant coated articles which include an intermediate coating layer of a thermosetting polymer and non-siliceous filler |
US4284668A (en) * | 1979-08-27 | 1981-08-18 | Tough-Guard, Inc. | Paint sealant with Teflon T.F.E |
JPH03269184A (ja) * | 1990-03-15 | 1991-11-29 | Kao Corp | 耐汚染性壁紙 |
US5458960A (en) * | 1993-02-09 | 1995-10-17 | Roctex Oy Ab | Flexible base web for a construction covering |
DE19647369A1 (de) | 1996-11-15 | 1998-05-20 | Inst Neue Mat Gemein Gmbh | Verbundwerkstoffe |
DE19741498B4 (de) | 1997-09-20 | 2008-07-03 | Evonik Degussa Gmbh | Herstellung eines Keramik-Edelstahlgewebe-Verbundes |
DE102006008130A1 (de) * | 2006-02-20 | 2007-08-23 | Degussa Gmbh | Verfahren zur Beschichtung von Substraten und Trägersubstraten |
DE102004006612A1 (de) | 2004-02-10 | 2005-08-25 | Degussa Ag | Keramischer Wandverkleidungsverbund |
DE102004046568A1 (de) | 2004-09-24 | 2006-04-06 | Construction Research & Technology Gmbh | Fluormodifizierte Reaktivharzsysteme, Verfahren zu ihrer Herstellung und deren Verwendung |
DE102004046385A1 (de) | 2004-09-24 | 2006-04-06 | Construction Research & Technology Gmbh | Flüssige fluorhaltige Zusammensetzungen für die Oberflächenbehandlung mineralischer und nichtmineralischer Untergründe |
DE102005052940A1 (de) * | 2005-11-03 | 2007-05-10 | Degussa Gmbh | Verfahren zur Beschichtung von Substraten |
DE102006001640A1 (de) * | 2006-01-11 | 2007-07-12 | Degussa Gmbh | Keramische Wandverkleidungsverbände mit IR-Strahlung reflektierenden Eigenschaften |
DE102006001641A1 (de) * | 2006-01-11 | 2007-07-12 | Degussa Gmbh | Substrate mit bioziden und/oder antimikrobiellen Eigenschaften |
EP2085442A1 (fr) | 2008-02-01 | 2009-08-05 | Evonik Degussa GmbH | Compositions contenant du fluor et ayant des propriétés de surface améliorées |
DE102009029153A1 (de) | 2009-09-03 | 2011-03-17 | Evonik Degussa Gmbh | Waschpermanente Wandbeläge |
-
2009
- 2009-09-03 DE DE102009029152A patent/DE102009029152A1/de not_active Ceased
-
2010
- 2010-07-06 EP EP10734069A patent/EP2473290A1/fr not_active Withdrawn
- 2010-07-06 RU RU2012112613/05A patent/RU2547737C9/ru not_active IP Right Cessation
- 2010-07-06 US US13/393,979 patent/US9180487B2/en not_active Expired - Fee Related
- 2010-07-06 WO PCT/EP2010/059609 patent/WO2011026668A1/fr active Application Filing
- 2010-07-06 UA UAA201204068A patent/UA106995C2/uk unknown
- 2010-07-06 JP JP2012527254A patent/JP2013503989A/ja not_active Ceased
- 2010-07-06 BR BR112012004902A patent/BR112012004902A2/pt not_active IP Right Cessation
Non-Patent Citations (1)
Title |
---|
See references of WO2011026668A1 * |
Also Published As
Publication number | Publication date |
---|---|
RU2012112613A (ru) | 2013-10-10 |
RU2547737C2 (ru) | 2015-04-10 |
US9180487B2 (en) | 2015-11-10 |
WO2011026668A1 (fr) | 2011-03-10 |
BR112012004902A2 (pt) | 2016-04-12 |
DE102009029152A1 (de) | 2011-03-17 |
RU2547737C9 (ru) | 2015-12-20 |
UA106995C2 (uk) | 2014-11-10 |
US20120196134A1 (en) | 2012-08-02 |
JP2013503989A (ja) | 2013-02-04 |
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