EP0541541A1 - Joint sealants with early water resistance - Google Patents
Joint sealants with early water resistanceInfo
- Publication number
- EP0541541A1 EP0541541A1 EP90914905A EP90914905A EP0541541A1 EP 0541541 A1 EP0541541 A1 EP 0541541A1 EP 90914905 A EP90914905 A EP 90914905A EP 90914905 A EP90914905 A EP 90914905A EP 0541541 A1 EP0541541 A1 EP 0541541A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- compounds according
- joint
- joint sealing
- sealing compounds
- 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- Withdrawn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
- 239000000565 sealant Substances 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000006185 dispersion Substances 0.000 claims abstract description 49
- 239000000945 filler Substances 0.000 claims abstract description 20
- -1 hydroxyethylmethyl Chemical group 0.000 claims abstract description 20
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000003755 preservative agent Substances 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 13
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims abstract description 10
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims abstract description 10
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 7
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002562 thickening agent Substances 0.000 claims abstract description 7
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920003086 cellulose ether Polymers 0.000 claims description 45
- 150000001875 compounds Chemical class 0.000 claims description 34
- 238000007789 sealing Methods 0.000 claims description 24
- 229920001577 copolymer Polymers 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 16
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 15
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 11
- 239000005977 Ethylene Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000470 constituent Substances 0.000 claims description 9
- 239000004815 dispersion polymer Substances 0.000 claims description 9
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004606 Fillers/Extenders Substances 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 6
- 239000000080 wetting agent Substances 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 4
- YACLQRRMGMJLJV-UHFFFAOYSA-N chloroprene Chemical compound ClC(=C)C=C YACLQRRMGMJLJV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001021 polysulfide Polymers 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- RZBXSLICNMYVAJ-UHFFFAOYSA-N ethenyl acetate;2-methylprop-2-enoic acid Chemical compound CC(=O)OC=C.CC(=C)C(O)=O RZBXSLICNMYVAJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 abstract description 40
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 abstract description 3
- 230000003111 delayed effect Effects 0.000 abstract description 3
- 230000003712 anti-aging effect Effects 0.000 abstract description 2
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 239000001913 cellulose Substances 0.000 abstract description 2
- 235000010980 cellulose Nutrition 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 2
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000003085 diluting agent Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 239000000725 suspension Substances 0.000 abstract 1
- 238000004078 waterproofing Methods 0.000 abstract 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 39
- 239000000203 mixture Substances 0.000 description 37
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 30
- 238000009499 grossing Methods 0.000 description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 8
- 239000012188 paraffin wax Substances 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 8
- 230000002335 preservative effect Effects 0.000 description 8
- 239000004033 plastic Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 239000013065 commercial product Substances 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000008199 coating composition Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 229920001083 polybutene Polymers 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 2
- 229920004482 WACKER® Polymers 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- JBSLOWBPDRZSMB-FPLPWBNLSA-N dibutyl (z)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C/C(=O)OCCCC JBSLOWBPDRZSMB-FPLPWBNLSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- DMYOHQBLOZMDLP-UHFFFAOYSA-N 1-[2-(2-hydroxy-3-piperidin-1-ylpropoxy)phenyl]-3-phenylpropan-1-one Chemical compound C1CCCCN1CC(O)COC1=CC=CC=C1C(=O)CCC1=CC=CC=C1 DMYOHQBLOZMDLP-UHFFFAOYSA-N 0.000 description 1
- CFKMVGJGLGKFKI-UHFFFAOYSA-N 4-chloro-m-cresol Chemical compound CC1=CC(O)=CC=C1Cl CFKMVGJGLGKFKI-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 101100117236 Drosophila melanogaster speck gene Proteins 0.000 description 1
- 229920013646 Hycar Polymers 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920001079 Thiokol (polymer) Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000013466 adhesive and sealant Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229940015043 glyoxal Drugs 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920006173 natural rubber latex Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001485 poly(butyl acrylate) polymer Polymers 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/34—Filling pastes
-
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K3/1006—Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by the chemical nature of one of its constituents
- C09K3/1015—Polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/284—Alkyl ethers with hydroxylated hydrocarbon radicals
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2003/1034—Materials or components characterised by specific properties
- C09K2003/1081—Water-proofed materials
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- C—CHEMISTRY; METALLURGY
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/02—Inorganic compounds
- C09K2200/0217—Salts
- C09K2200/023—Sulfur-containing compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/02—Inorganic compounds
- C09K2200/0239—Oxides, hydroxides, carbonates
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- C—CHEMISTRY; METALLURGY
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/02—Inorganic compounds
- C09K2200/0243—Silica-rich compounds, e.g. silicates, cement, glass
- C09K2200/0247—Silica
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/04—Non-macromolecular organic compounds
- C09K2200/0405—Hydrocarbons
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/04—Non-macromolecular organic compounds
- C09K2200/0411—Halogen-containing compounds
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0607—Rubber or rubber derivatives
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0617—Polyalkenes
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0617—Polyalkenes
- C09K2200/062—Polyethylene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0622—Polyvinylalcohols, polyvinylacetates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0615—Macromolecular organic compounds, e.g. prepolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09K2200/0625—Polyacrylic esters or derivatives thereof
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- C—CHEMISTRY; METALLURGY
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- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0645—Macromolecular organic compounds, e.g. prepolymers obtained otherwise than by reactions involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/0645—Macromolecular organic compounds, e.g. prepolymers obtained otherwise than by reactions involving carbon-to-carbon unsaturated bonds
- C09K2200/065—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/068—Containing also other elements than carbon, oxygen or nitrogen in the polymer main chain
- C09K2200/0682—Containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/06—Macromolecular organic compounds, e.g. prepolymers
- C09K2200/068—Containing also other elements than carbon, oxygen or nitrogen in the polymer main chain
- C09K2200/0685—Containing silicon
Definitions
- the invention relates to joint sealants which are resistant to early rain
- Non-ionic cellulose ethers (II) from the group formed by hydroxyethyl, hydroxyethylimethyl, hydroxypropylmethyl and hydroxypropyl cellulose
- customary additives such as fillers, pigments, plasticizers, extenders, thickeners, defoamers, dispersing aids, pH regulators, preservatives and preservatives and
- Joint sealants are known to the person skilled in the art and have proven themselves in practice. The use of joint sealant is problematic in areas where there is a possibility or risk that the joint sealant is exposed to water pollution, for example by spray water or roe, before it hardens. For example, many of the jointing compounds that have also been used outdoors are partially or completely washed out by a heavy downpour that started shortly after they were applied.
- DE 3814078-A1 discloses the use of non-ionic cellulose ethers in joint sealants or coating compositions based on acrylate dispersions.
- Non-ionic cellulose ethers are also known as constituents of coating compositions and paints, e.g. those based on aqueous dispersions of organopolysiloxanes as described in DE 1284007 or those based on vinyl acetate / maleic acid dibutyl ester dispersions as described in DE 21 08365.
- cellulose ethers are also suitable for joint sealants based on the same polymer dispersion and lead to the desired effects.
- the specialist magazine Resin Review .35,2 describes a roof coating ace that contains a polyacrylate dispersion as a binder and, in addition to fillers and other auxiliary substances, also hydroxyethyl cellulose as a thickener. contains.
- This coating ace is advertised as particularly wash-resistant. However, this property is attributed to the specific setting behavior of the polyacrylate emulsions specially developed and used for such coating compositions. It was therefore not obvious to a person skilled in the art to use hydroxyethyl cellulose in joint sealants to improve the early rain strength.
- coating compounds do not meet the requirements placed on joint sealing compounds. These are in particular requirements such as those required by DIN 52456 “Determining the Processability of Sealants” and DIN .52454 “Stability”. In particular when it comes to durability, joint sealing compounds must have the property that they do not run off, or only slightly, from a U-profile filled with this compound, which is placed upright after filling. Coating compounds are generally less viscous because. on the one hand they should be applicable by spraying or rolling and on the other hand they should show a certain course for leveling the mass. Although joint sealants and coating compounds can in principle be produced from the same constituents, it should also be possible to produce a reasonably usable coating ace by diluting a joint sealant, but conclusions cannot necessarily be drawn in the reverse manner.
- nonionic cellulose ether derivatives such as hydroxyethyl cellulose (HEC), hydroxyethyl methyl cellulose (HEMC) and hydroxy - Propyl-methylcellulose (HPMC) can be used in plastic plasters and emulsion paints, among other things, to improve water retention, open time, wet grip and thickening and setting behavior.
- HEC hydroxyethyl cellulose
- HEMC hydroxyethyl methyl cellulose
- HPMC hydroxy - Propyl-methylcellulose
- paints such as emulsion paints and plastic mortars represent another area of technology that is not comparable to joint sealants.
- plastic plasters can possibly be used to decay joints, but generally have no pronounced sealing properties and, in contrast to the joint sealing compounds, can be portioned and processed with a trowel when they are applied.
- the object of the invention is to provide joint sealants based on polymer dispersions which, in addition to good smoothing behavior, have an early rain resistance of the uncured compositions without other desired properties such as modulus of elasticity, elongation at break and resilience, and resistance to migration and coagulum and Speck freedom can be adversely affected. It was also an object of the invention to provide a method which makes it possible to produce such compositions.
- the object was achieved by early rain-resistant joint sealants containing aqueous polymer dispersions (I) non-ionic cellulose ethers (II) from the group formed by hydroxyethyl, hydroxyethylimethyl, hydroxypropylmethyl and hydroxypropyl cellulose, and if appropriate conventional additives such as fillers, pigments, plasticizers, extenders Thickeners, defoamers, dispersing aids, pH regulators, preservatives and anti-aging agents as well as at least one organic liquid component from the group of conventional additives and can be prepared by intimately mixing (I) with the other constituents, characterized in that that (II) in the delayed and / or non-retarded form, suspended in the liquid organic component, is added and mixed in.
- aqueous polymer dispersions I
- non-ionic cellulose ethers II
- conventional additives such as fillers, pigments, plasticizers, extenders Thickeners, defoamers, dispersing aids
- joint sealant The individual components of the joint sealant are known to the person skilled in the art as such, for example from DE 38 14078-Al. Further suitable polymer dispersions for the production of joint sealants are commercially available and / or are known to the person skilled in the art from the patent and specialist literature, for example from E. Flick, Construction and structural adhesives and sealants, Noyes Publications, Park Ridge 1988 or E. Flick, Adhesives and sealant compound formulations, Noyes Publications, Park Ridge 1978. Particularly advantageous joint sealing compounds contain dispersions of polyacrylates and / or acrylate copolymers capable of film formation.
- joint sealants which are selected from dispersions of polymers or copolymers capable of film formation from those of ethylene / vinyl acetate, butadiene / styrene, vinyl acetate / maleic acid ester, silicone, urethane, vinyl acetate methacrylic acid / chloroprene and Isoprene polymers or copolymers formed group.
- dispersions of polymers or copolymers capable of film formation from those of ethylene / vinyl acetate, butadiene / styrene, vinyl acetate / maleic acid ester, silicone, urethane, vinyl acetate methacrylic acid / chloroprene and Isoprene polymers or copolymers formed group.
- Different polymer dispersions can be combined.
- polysulfide dispersions prove to be particularly suitable in connection with polymers capable of film formation. For the sake of simplicity, the following text speaks only of polymer dispersions.
- the cellulose ethers suitable according to the invention are slurried in the liquid organic component.
- Such components are, for example, plasticizers, extenders and / or wetting agents.
- Retarded and / or non-retarded cellulose ethers can optionally be used.
- the aqueous dispersions contained in the joint sealants of the invention preferably have solids contents of 40 to 75, in particular 45 to 65% by weight.
- Their pH value can be at least 6, in particular 7 to 9, and is adjusted to these values if necessary.
- the cellulose ethers contained in the jointing compounds according to the invention preferably have Brookfield viscosities of at least 5,000 mPas as a 2% strength aqueous solution at 20 ° C. Those with a value of at least 25,000 mPas, for example medium-viscosity hydroxyethyl celluloses, are preferred. So-called highly viscous cellulose ether types which have a corresponding value of at least 70,000 mPas are particularly suitable, e.g. highly viscous hydroxyethyl cellulose. Commercial high viscosity hydroxyethyl cellulose e.g. as a 2% solution at 20 ° C a viscosity of 100,000 mPas.
- the ratio of the amounts of cellulose ether to "free” water is obviously important, which is decisive for whether this solubility limit. is exceeded or not.
- Free water is understood here to mean the water content of the sealing compound which is available to the cellulose ethers " to dissolve in.
- the total water content of the joint sealing compound cannot be used for a corresponding calculation. Rather, it must be taken into account that the others Constituents also require a certain amount of water or bind more or less tightly, so-called water values are known for most fillers, which is, for example, 11 g water per 100 g heavy spar for spar spar.
- silica for example, for the HDK type V 15 from Wacker-Chemie, values between 350 and 400 g of water per 100 g of silica can be determined. These values offer the person skilled in the art an indication of what amounts of "bound” water he has to subtract from the total water content of the sealant in order to free the amount "Water. It is therefore preferred that this amount of” free "water in relation z u the amount of the cellulose ether type used in each case gives a ratio which is above the respective solubility limit.
- fillers can be contained in the joint sealants of the invention in an amount of 0 to 60, in particular 2 to 60% by weight, based on the total mass of the joint sealants.
- Such compositions if they contain little or no fillers, are highly transparent.
- Low filler contents can be present, in particular, in those compositions in which the fillers have an additional thickening effect, such as silica. Only fillers used do not have this zu ⁇ sharmlichen effect, the content thereof is usually between 35 and 60 "wt .-%. We speak here of highly filled compositions.
- the jointing compounds contain chlorinated hydrocarbons, in particular chlorinated paraffins, as plasticizers, and nonionic surfactants as wetting agents.
- chlorinated paraffins with a. Chain length of about 10 to 18 carbon atoms and a chlorine content of about 40 to 70% by weight.
- the joint sealants contain
- Additives such as thickeners, defoamers and
- Pigments at least sufficient amounts of organic liquid component and up to 1.5% by weight of cellulose ether for slurrying the cellulose ethers
- the cellulose ether content should not be much less than 0.1% by weight. Good results are shown in particular in the case of joint sealants in which, taking into account the general parameters such as cellulose ether type and free water content, the cellulose ether content is in a range from about 0.1 to 0.5% by weight, based on the total amount.
- the cellulose ethers are slurried in the organic liquid component before the addition in the production of the joint sealing compound according to the invention.
- This ratio of cellulose ether to liquid is preferably in a range from 1: 2 to 1: 4, in particular approximately 1: 3.
- One of the usual additives for joint sealants, such as plasticizers, extenders and / or wetting agents, is preferably used as the liquid organic component .
- a neutral to basic setting of the joint sealing compounds can have a favorable effect on their stability, in particular on their shear stability.
- the polymer dispersion is usually initially taken in the preparation of the joint sealing compounds according to the invention.
- the usual additives with the exception of the pH regulators are then added and mixed in.
- the mixture is then mixed with the cellulose ethers slurried in the organic liquid component and, after the fillers have been subsequently mixed in, the pH regulators are added.
- stirring can be carried out under vacuum.
- joint sealants are preferably used as intended. They are particularly suitable for use in areas in which they are exposed to splash water, rain or other early water pollution.
- the irrigation equipment consisted of a housing made of transparent plastic with the dimensions: height 70 cm, width 60 cm and depth 60 cm. It comprised a housing 1, a shower head 2, a sample bowl 3, a pump 4, a floor drain 5 and a shut-off valve 6 for the drain.
- the sample pan consisted of a vessel measuring 7 x 7 cm and had a depth of 2.5 cm.
- the shower head was a conventional hand shower as used for body care and was set so that the sample was irrigated evenly. The distance between sample 3 and shower head 2 was 30 cm.
- the apparatus was operated with demineralized water, the pump generating an excess pressure of approximately 0.4 bar.
- the water flow rate was 300 l / h.
- the spraying with water was carried out 5 minutes, in each case 1 minute after filling and smoothing the surface of the masses to be tested.
- the washout (in% by weight) was determined by differential weighing before and after sprinkling.
- the processability was measured according to DIN 52456. A 4 m bore, a pressure of 2 bar and a test volume of 200 ml were used.
- Copolymer of vinyl acetate and ethylene (approximately 60% solids), with a pH of approximately 4.5 and a viscosity of approximately 1600 mPa.s at 20 ° C. (trade name: Vinnapas EP 17, from Wacker), 250 g chlorinated paraffin (C12-C14, 49% chlorine), 2800 g barium sulfate (trade name: Schwerspat EW0), 100 g titanium dioxide (trade name: KR0N0S RN 56) 25 g sodium carbonate (technical, pure commercial product), 25 g ethylene oxide adduct (approx. 9, 5 E0) of nonylphenol, 5 g of commercially available halogenated preservative, 37 g of hydroxyethyl cellulose with a viscosity of about
- the procedure was such that the polymer dispersion was initially introduced.
- the ethylene oxide adduct (emulsifier), the preservative, the titanium dioxide (pigment) and part of the chlorinated paraffin were then added.
- the hydroxyethyl cellulose was slurried and also added, and the whole was mixed well.
- the barium sulfate (filler) was added and stirred until smooth.
- This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- composition according to Example 1 was prepared, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of styrene and butadiene (approximately 64% solids) with a pH of 10.5 and a viscosity of about 800 mPa.s at 20 ° C (trade name: Polysar 2105, Hycar) were used.
- This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of vinyl acetate and Maleic acid di-n-butyl ester, solids content approx. 53%, pH value 4 to 5, viscosity (Brookfield, 20 ° C., 20 rpm) 1000 to 3000 mPa.s, trade name Mowilith DM 2HB, Hoechst, were used.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available silicon emulsion (elastically drying from the emulsion, approximately 45% solids), a pH of approx. 5 and a density of about 1.0 at 20 ° C, trade name: Wacker silicone building protection agents.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion described there of a copolymer of vinyl acetate and ethylene 1750 g of an aqueous, commercially available Dispersion of a polysulfide polymer, approximately 55% solids, pH 9-10, trade name: ZW 2028, from Thiokol.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion of a polyurethane polymer, approximately 40% solids, pH 7.0 to 7.5, viscosity 10,000 to 18,000 mPa.s, trade name: VP-LA 3110, from Henkel.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a polyvinyl acetate, approximately 50% solids, pH about 6 to 7, viscosity about 10,000 to 18,000 mPa.s (Brookfield), trade name Mowilith DLR, Hoechst, were used.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of chloroprene and methacrylic acid, approximately 46.5 to 48.5% Solid, pH about 9, trade name Neoprene Latex 115, were used.
- the mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- a composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a natural rubber latex, approximately 70% Solid, pH about 9 to 10, trade name Revertex Standard, were used.
- This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
- Examples 1 to 9 were replaced by replacing the hydroxyethyl cellulose used there with a commercially available methyl hydroxypropyl cellulose (MHPC) with a viscosity of about 20,000 mPa.s of a 2% solution at 20 ° C. according to Brookfield and a hydroxypropyl group content of 3. 2% by weight measured again.
- MHPC methyl hydroxypropyl cellulose
- the spray rates according to DIN 52456 are comparable.
- the smoothing behavior can be assessed as good.
- Examples 1 to 9 were measured again after replacing the hydroxyethyl cellulose used there with a commercially available hydroxypropyl cellulose (HPC) with a viscosity of approximately 5000 mPa.s of a 2% solution at 20 ° C. according to Brookfield and a hydroxypropyl group content of 70% .
- the spray rates according to DIN 52456 are comparable. The smoothing behavior can be assessed as good.
- Examples 1 to 9 were measured again after replacing the hydroxyethyl cellulose (HEC) with a commercially available aqueous polyacrylic acid dispersion (approximately 25% solids, trade name: Rohagit SD 15).
- the injection rates according to DIN 52456 were comparable.
- the smoothing behavior is poor; the washout behavior is less favorable.
- Examples 1 to 9 were produced without hydroxyethyl cellulose (HEC) (trade name: Natrosol 250 HR).
- HEC hydroxyethyl cellulose
- the smoothing behavior is . deficient; the washout behavior is less favorable.
- the procedure was such that the polymer dispersion was initially introduced.
- the ethylene oxide adduct (emulsifier), the preservative, the titanium dioxide (pigment) and part of the chlorinated paraffin were then added.
- the hydroxyethyl cellulose was slurried and also added, and the whole was mixed thoroughly.
- the sodium carbonate was then mixed in as a 10% strength aqueous solution.
- the barium sulfate (filler) was added and stirred until smooth. This mixture was filled in 310 ml plastic cartridges and was stable for at least one year at temperatures up to 35 ° C.
- Example 12 In a planetary mixer, the constituents listed in Example 12 were mixed intensively for about 45 minutes using the same procedure, but instead of the hydroxyethyl cellulose:
- Example 12 In a planetary mixer, the constituents listed in Example 12 were mixed intensively for about 45 minutes using the same procedure, but using instead of the hydroxyethyl cellulose
- This mixture was filled in 310 ml plastic cartridges and was stable for at least one year at temperatures up to 35 ° C.
- Wacker-Ghemie 36 g aqueous ammonia solution (25%) 52 g chlorinated paraffin (C10-C1, 49% chlorine) 18 g hydroxyethyl cellulose with a viscosity of approximately 4000 mPas of a 1% aqueous solution and a hydroxyethyl group content of 55% by weight, trade name: Natrosol 250 HHR.
- the procedure was such that the dispersion was initially introduced.
- the ethylene oxide adduct (emulsifier), the preservative and the defoamer were then added.
- the hydroxyethyl cellulose was slurried in the chlorinated paraffin and likewise added, and the whole was thoroughly mixed. This was followed by the mixing in of the 25% aqueous ammonia solution. Finally, the disperse silica (filler) was added and stirred until smooth.
- the procedure was as follows, that the dispersion was introduced, then part of the polybutene, the ethylene oxide adduct, the preservative, the plasticizer and the water and the solvent were intimately mixed with one another.
- the other part of the polybutene was 3: 1 with the hydroxyethyl cellulose slurried and also added and mixed in and stirred for 5 minutes.
- the chalk and the titanium dioxide were then worked in and stirred for 10 minutes. After the ammonia had been added, stirring was continued for a further 15 minutes under vacuum at 40 mbar.
- a composition according to Example 1 was produced, a non-retarded, highly viscous hydroxyethyl cellulose, otherwise of the same specification, being used instead of the Natrosol 250 HHR type described there (trade name Natrosol 250 HH).
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
Des matériaux d'étanchéité résistant à l'eau avant leur durcissement contiennent des dispersions aqueuses de polymères (I); de l'éther non ionique de cellulose (II) du groupe formé par des celluloses d'hydroxyéthyle, d'hydroxyéthylméthyle, d'hydroxypropylméthyle et d'hydroxypropyle; le cas échéant des additifs tels que charges, pigments, plastifiants, diluants, épaississants, anti-moussants, dispersants, régulateurs du pH, conservateurs et anti-vieillisseurs, ainsi qu'au moins un composant organique liquide du groupe des additifs usuels. Ces matériaux peuvent être produits en mélangeant intimement (I) avec les autres composants. Afin de pouvoir ajouter des quantités du composant (II) au-dessus du seuil de solubilité, ces matériaux d'étanchéité se caractérisent par le fait que le composant (II) est ajouté en suspension sous forme retardée et/ou non retardée au composant organique liquide, puis mélangé.Waterproofing materials resistant to water before curing contain aqueous dispersions of polymers (I); nonionic cellulose (II) ether from the group formed by hydroxyethyl, hydroxyethylmethyl, hydroxypropylmethyl and hydroxypropyl celluloses; where appropriate additives such as fillers, pigments, plasticizers, diluents, thickeners, anti-foaming agents, dispersants, pH regulators, preservatives and anti-aging agents, as well as at least one liquid organic component from the group of usual additives. These materials can be produced by thoroughly mixing (I) with the other components. In order to be able to add quantities of component (II) above the solubility threshold, these sealants are characterized by the fact that component (II) is added in suspension in delayed and / or non-delayed form to the organic component. liquid, then mixed.
Description
Frühregenfeste Fugendichtungsmassen Early rainproof joint sealants
Die Erfindung betrifft frühregenfeste Fugendichtungsmassen enthal¬ tendThe invention relates to joint sealants which are resistant to early rain
- wäßrige Polymerdispersionen (I)- aqueous polymer dispersions (I)
- nicht-ionische Celluloseether (II) aus der von Hydroxyethyl-, Hydroxyethyimethyl-, Hydroxypropylmethyl- und Hydroxypropyl¬ cellulose gebildeten Gruppe- Non-ionic cellulose ethers (II) from the group formed by hydroxyethyl, hydroxyethylimethyl, hydroxypropylmethyl and hydroxypropyl cellulose
- gegebenenfalls übliche Zusätze wie Füllstoffe, Pigmente, Weichmacher, Extender, Verdickungsmittel, Entschäumer, Dis- pergierhilfsmittel , pH-Regulatoren, Konservierungs- und Alte¬ rungsschutzmittel sowie- If necessary, customary additives such as fillers, pigments, plasticizers, extenders, thickeners, defoamers, dispersing aids, pH regulators, preservatives and preservatives and
- mindestens eine organische flüssige Komponente aus der Gruppe üblicher Zusätze und herstellbar durch inniges Vermengen von (I) mit den übrigen Bestandteilen sowie ein Verfahren zur Herstellung derartiger Fugendichtungsmassen und deren Verwendung.
Fugendichtungsmassen sind dem Fachmann bekannt und haben sich in der Praxis bewährt. Problematisch ist der Einsatz von Fugendichtungs¬ masse in Bereichen wo die Möglichkeit bzw. die Gefahr besteht, daß die Fugendichtungsmasse vor dem Aushärten einer Wasserbelastung z.B. durch Spritzwasser oder Rogen ausgesetzt ist. So werden viele der bislang auch im Außenbereich verwendeten Fugendichtungsmassen durch einen kurz nach ihrem Auftragen einsetzenden heftigen Regenguß ganz ode teilweise ausgewaschen. Aus der DE 3814078-A-l ist die Ver- ' wendung von nicht-ionischen Celluloseethern in Fugendicht- bzw. Be- schichtungsmassen auf Basis von Acrylatdispersionen bekannt. Durch den Einsatz von bestimmten Celluloseethern in diesen Massen soll das Auswaschverhalten durch die Einwirkung von Wasser wie Regenwasser sowie das Glättverhalten verbessert werden. Die dort eingesetzten Mengen der angegebenen Celluloseethertypen sind auf den Festkörper¬ gehalt der Acrylatdispersion bezogen. Es wird keine explizite Angabe über das Verhältnis von "freiem" Wasser zu den Celluloseethern ge¬ macht. Aus den Beispielen geht zwar hervor, daß die dort aufge¬ führten Bestandteile zur Herstellung einer Fugendichtungsmasse in einem Planetenmischer hergestellt wurden, jedoch findet man keine Angaben darüber, in welcher Form und Reihenfolge die einzelnen Be¬ standteile miteinander in Mischung gebracht werden.- At least one organic liquid component from the group of conventional additives and can be produced by intimately mixing (I) with the other constituents and a method for producing such jointing compounds and their use. Joint sealants are known to the person skilled in the art and have proven themselves in practice. The use of joint sealant is problematic in areas where there is a possibility or risk that the joint sealant is exposed to water pollution, for example by spray water or roe, before it hardens. For example, many of the jointing compounds that have also been used outdoors are partially or completely washed out by a heavy downpour that started shortly after they were applied. DE 3814078-A1 discloses the use of non-ionic cellulose ethers in joint sealants or coating compositions based on acrylate dispersions. The use of certain cellulose ethers in these compositions is said to improve the washout behavior through the action of water such as rainwater and the smoothing behavior. The amounts of the specified cellulose ether types used there are based on the solids content of the acrylate dispersion. No explicit statement is made about the ratio of "free" water to the cellulose ethers. The examples show that the components listed there for the production of a joint sealant were produced in a planetary mixer, but there is no information about the form and sequence in which the individual components are mixed with one another.
Es hat sich jedoch in der Praxis erwiesen, daß bei derartigen früh- regenfesten Fugendichtungsmassen die Zugabe der einzelnen Bestand¬ teile sowie deren Form bei der Herstellung der Fugendichtungsmassen nicht beliebig ist. So lassen sich beispielsweise die genannten Celluloseether zwar im Labormaßstab in geringen Mengen in einige Polymerdispersionen einstreuen und lösen, jedoch nicht im Produk¬ tionsmaßstab und nicht in solchen Mengen, die bezogen auf das "freie" Wasser zu groß sind um eine vollständige Lösung zu erzielen. Bei einem solchen Versuch erhält man unweigerlich Klumpenbildung bzw. Brechen der Dispersion. Wenn es auch manchmal möglich ist, die Celluloseetherklumpen wieder zu homogenisieren, so ist es nicht
machbar, einmal koagulierte Dispersionsteilchen wieder zu disper- gieren. Auch bietet die DE 38 14078-A-l dem Fachmann keinen Hinweis darauf, daß derartige- frühregenfeste Fugendichtungsmassen mit ande¬ ren wäßrigen Polymerdispersionen als den dort angegebenen Acrylat- dispersionen herstellbar sind.However, it has been found in practice that the addition of the individual constituents and their shape is not arbitrary in the case of such early rainproof joint sealing compounds. For example, the aforementioned cellulose ethers can be sprinkled and dissolved in small amounts in some polymer dispersions on a laboratory scale, but not on a production scale and not in amounts that are too large in relation to the "free" water to achieve a complete solution. Such an attempt inevitably leads to lump formation or breakage of the dispersion. Even if it is sometimes possible to homogenize the cellulose ether lumps again, it is not feasible to disperse dispersion particles once coagulated. Also, DE 38 14078-Al does not provide the person skilled in the art with evidence that joint sealants which are resistant to early rain can be produced with aqueous polymer dispersions other than the acrylate dispersions specified there.
Nicht-ionische Celluloseether sind auch als Bestandteile von Be¬ schichtungsmassen und Anstrichmitteln bekannt z.B. solchen auf Basis von wäßrigen Dispersionen von Organo-Polysiloxanen wie in der DE 1284007 beschrieben oder solchen auf Basis von Vinylacetat/- Maleinsäuredibutylesterdispersionen wie in der DE 21 08365 be¬ schrieben. Dem kann der Fachmann jedoch keinen Hinweis entnehmen, daß derartige Celluloseether auch für Fugendichtungsmassen auf gleicher Polymerdispersionsbasis geeignet sind und zu den ge¬ wünschten Effekten führen.Non-ionic cellulose ethers are also known as constituents of coating compositions and paints, e.g. those based on aqueous dispersions of organopolysiloxanes as described in DE 1284007 or those based on vinyl acetate / maleic acid dibutyl ester dispersions as described in DE 21 08365. However, the person skilled in the art cannot derive any indication that such cellulose ethers are also suitable for joint sealants based on the same polymer dispersion and lead to the desired effects.
In der Fachzeitschrift Resin Review .35,2 ist eine Dachbeschichtungs- asse beschrieben, die als Bindemittel eine Polyacrylatdispersion und neben Füllstoffen und weiteren Hilfsstoffen auch Hydroxyethyl- cellulose als Verdickungsmittel . enthält. Diese Beschichtungs asse wird als besonders auswaschresistent ausgelobt. Diese Eigenschaft wird jedoch auf das spezifische Abbindeverhalten der speziell für derartige Beschichtungsmassen entwickelten und eingesetzten Poly- acrylatemulsionen zurückgeführt. Somit hat es für den Fachmann nicht nahegelegen, Hydroxyethylcellulose zur Verbesserung der Frühregen¬ festigkeit in Fugendichtungsmassen einzusetzen.The specialist magazine Resin Review .35,2 describes a roof coating ace that contains a polyacrylate dispersion as a binder and, in addition to fillers and other auxiliary substances, also hydroxyethyl cellulose as a thickener. contains. This coating ace is advertised as particularly wash-resistant. However, this property is attributed to the specific setting behavior of the polyacrylate emulsions specially developed and used for such coating compositions. It was therefore not obvious to a person skilled in the art to use hydroxyethyl cellulose in joint sealants to improve the early rain strength.
Darüber hinaus erfüllen Beschichtungsmassen nicht die Ansprüche, die an Fugendichtungsmassen gestellt werden. Dies sind insbesondere An¬ forderungen wie sie durch die DIN 52456 "Bestimmung der Verarbεit- barkeit von Dichtstoffen" sowie die DIN .52454 "Standvermögen" ge¬ fordert werden.
Insbesondere beim Standvermögen müssen Fugendichtungsmassen gegen¬ über den Beschichtungsmassen die Eigenschaft aufweisen, aus einem mit dieser Masse gefüllten U-Profil, welches nach dem Füllen in die Senkrechte gestellt wird, nicht oder nur geringfügig abzulaufen. Beschichtungsmassen sind in aller Regel niedrig-viskoser, da . sie einerseits durch Spritzen oder Rollen auftragbar sein sollen und andererseits einen gewissen Verlauf zur Nivellierung der Masse zei¬ gen sollen. Zwar kann man Fugendichtungsmassen als auch Beschich¬ tungsmassen im Prinzip aus den gleichen Bestandteilen herstellen, auch sollte es möglich sein, durch Verdünnen einer Fugendichtungs¬ masse eine halbwegs brauchbare Beschichtungs asse herzustellen, aber es lassen sich nicht zwingend in umgekehrter Weise Rückschlüsse ziehen.In addition, coating compounds do not meet the requirements placed on joint sealing compounds. These are in particular requirements such as those required by DIN 52456 "Determining the Processability of Sealants" and DIN .52454 "Stability". In particular when it comes to durability, joint sealing compounds must have the property that they do not run off, or only slightly, from a U-profile filled with this compound, which is placed upright after filling. Coating compounds are generally less viscous because. on the one hand they should be applicable by spraying or rolling and on the other hand they should show a certain course for leveling the mass. Although joint sealants and coating compounds can in principle be produced from the same constituents, it should also be possible to produce a reasonably usable coating ace by diluting a joint sealant, but conclusions cannot necessarily be drawn in the reverse manner.
Aus Ullmann, Enzyklopädie der technischen Chemie, 4. Auflage, Band 9, Verlag Chemie, Weinheim/Bergstraße 1974, Seite 208 - 209, ist bekannt, daß nichtionische Celluloseetherderivate wie Hydroxyethyl- cellulose (HEC), Hydroxyethyl-methylcellulose (HEMC) und Hydroxy- propyl-methylcellulose (HPMC) in Kunststoffputzen und Dispersions¬ farben u.a. zur Verbesserung des Wasserrückhaltevermögens, der Of¬ fenzeit, der Naßhaftung sowie des Andick- und Abbindeverhaltens ein¬ gesetzt werden. Dem kann jedoch der Fachmann keinen Hinweis darauf entnehmen, daß derartige Celluloseether in Fugendichtungsmassen zu einer Verbesserung der Streichfähigkeit, des Glättverhaltens und der Spritzwasserbeständigkeit der noch nicht erhärteten Oberflächen dieser Massen führen. Desweiteren repräsentieren Anstrichstoffe wie Dispersionsfarben sowie Kunststoffmörtel einen anderen Bereich der Technik, der nicht mit Fugendichtungsmassen vergleichbar ist. So lassen sich zwar Kunststoffputze möglicherweise zum Verfällen von Fugen einsetzen, weisen jedoch im allgemeinen keine ausgesprochenen Dichtungseigenschaften aus und lassen sich im Gegensatz zu den Fu¬ gendichtungsmassen bei ihrer Applikation mit der Kelle portionieren und verarbeiten.
Aufgabe der Erfindung ist es, Fugendichtungsmassen auf Basis von Polymerdispersionen zur Verfügung zu stellen, die neben einem guten Glättverhalten eine Frühregenfestigkeit der nicht ausgehärteten Massen aufweisen, ohne daß andere erwünschte Eigenschaften wie Ela¬ stizitätsmodul, Bruchdehnung und Rückstellvermögen sowie Migrati¬ onsbeständigkeit und Koagulat- und Stippenfreiheit davon beein¬ trächtigt werden. Es war darüber hinaus Aufgabe der Erfindung, ein Verfahren bereitzustellen, das es möglich macht, derartige Massen zu produzieren.From Ullmann, Encyclopedia of Industrial Chemistry, 4th edition, Volume 9, Verlag Chemie, Weinheim / Bergstrasse 1974, pages 208-209, it is known that nonionic cellulose ether derivatives such as hydroxyethyl cellulose (HEC), hydroxyethyl methyl cellulose (HEMC) and hydroxy - Propyl-methylcellulose (HPMC) can be used in plastic plasters and emulsion paints, among other things, to improve water retention, open time, wet grip and thickening and setting behavior. However, the person skilled in the art cannot derive any indication that such cellulose ethers in joint sealing compounds lead to an improvement in the spreadability, the smoothing behavior and the splash water resistance of the as yet unhardened surfaces of these compounds. Furthermore, paints such as emulsion paints and plastic mortars represent another area of technology that is not comparable to joint sealants. Thus, plastic plasters can possibly be used to decay joints, but generally have no pronounced sealing properties and, in contrast to the joint sealing compounds, can be portioned and processed with a trowel when they are applied. The object of the invention is to provide joint sealants based on polymer dispersions which, in addition to good smoothing behavior, have an early rain resistance of the uncured compositions without other desired properties such as modulus of elasticity, elongation at break and resilience, and resistance to migration and coagulum and Speck freedom can be adversely affected. It was also an object of the invention to provide a method which makes it possible to produce such compositions.
Die Aufgabe wurde gelöst durch frühregenfeste Fugendichtungsmassen enthaltend wäßrige Polymerdispersionen (I) nicht-ionische Celluloseether (II) aus der von Hydroxyethyl-, Hydroxyethyimethyl-, Hydroxypropylmethyl- und Hydroxypropyl¬ cellulose gebildeten Gruppe gegebenenfalls übliche Zusätze wie Füllstoffe, Pigmente, Weich¬ macher, Extender, Verdickungsmittel , Entschäumer, Dispergier- hilfs ittel, pH-Regulatoren, Konservierungs- und Alterungs¬ schutzmittel sowie mindestens eine organische flüssige Komponente aus der Gruppe üblicher Zusätze und herstellbar durch inniges Vermengen von (I) mit den übrigen Be¬ standteilen, dadurch gekennzeichnet, daß (II) in retardierter und/- oder nicht retardierter Form in der flüssigen organischen Komponente aufgeschlämmt zugegeben und untergemischt wird.The object was achieved by early rain-resistant joint sealants containing aqueous polymer dispersions (I) non-ionic cellulose ethers (II) from the group formed by hydroxyethyl, hydroxyethylimethyl, hydroxypropylmethyl and hydroxypropyl cellulose, and if appropriate conventional additives such as fillers, pigments, plasticizers, extenders Thickeners, defoamers, dispersing aids, pH regulators, preservatives and anti-aging agents as well as at least one organic liquid component from the group of conventional additives and can be prepared by intimately mixing (I) with the other constituents, characterized in that that (II) in the delayed and / or non-retarded form, suspended in the liquid organic component, is added and mixed in.
Die einzelnen Bestandteile der Fugendichtungsmasse sind dem Fachmann als solche bekannt z.B. aus der DE 38 14078-A-l. Weitere geeignete Polymerdispersionen für die Herstellung von Fugendichtungsmassen sind im Handel erhältlich und/oder sind dem Fachmann aus der Patent- und Fachliteratur bekannt z.B. aus E. Flick, Construction and struc- tural adhesives and sealants, Noyes Publications, Park Ridge 1988
oder E. Flick, Adhesives and sealant compound formulations, Noyes Publications, Park Ridge 1978. Besonders vorteilhafte Fugendich¬ tungsmassen enthalten Dispersionen von zur Filmbildung befähigten Pol acrylaten und/oder Acrylatcopolymeren. Vorteilhaft sind auch erfindungsgemäße Fugendichtungsmassen, die auf Dispersionen von zur Filmbildung befähigten Polymeren bzw. Copolymeren ausgewählt aus der von Ethylen/Vinylacetat-,- Butadien/Styrol-, Vinylacetat/Maleinsäure- ester-, Silikon-, Urethan-, Vinylacetatmethacrylsäure/Chloropren- und Isopren-Polymeren bzw. -Copolymeren gebildeten Gruppe beruhen. Es können unterschiedliche Polymer-Dispersionen kombiniert werden. Auch Polysulfiddispersionen . erweisen sich in Verbindung mit zur Filmbildung befähigten Polymeren als besonders geeignet. Der Ein¬ fachheit halber wird im folgenden Text nur von Polymer-Dispersionen gesprochen.The individual components of the joint sealant are known to the person skilled in the art as such, for example from DE 38 14078-Al. Further suitable polymer dispersions for the production of joint sealants are commercially available and / or are known to the person skilled in the art from the patent and specialist literature, for example from E. Flick, Construction and structural adhesives and sealants, Noyes Publications, Park Ridge 1988 or E. Flick, Adhesives and sealant compound formulations, Noyes Publications, Park Ridge 1978. Particularly advantageous joint sealing compounds contain dispersions of polyacrylates and / or acrylate copolymers capable of film formation. Also advantageous are joint sealants according to the invention which are selected from dispersions of polymers or copolymers capable of film formation from those of ethylene / vinyl acetate, butadiene / styrene, vinyl acetate / maleic acid ester, silicone, urethane, vinyl acetate methacrylic acid / chloroprene and Isoprene polymers or copolymers formed group. Different polymer dispersions can be combined. Also polysulfide dispersions. prove to be particularly suitable in connection with polymers capable of film formation. For the sake of simplicity, the following text speaks only of polymer dispersions.
Die meisten Bestandteile sind handelsüblich. So sind sowohl retar¬ dierte als auch nicht retardierte Celluloseether im Handel erhält¬ lich. Unter retardierte Celluloseethern versteht man solche, die in Wasser eingebracht gegenüber den unretardierten Substanzen verzögert anquellen. Dies wird z.B. durch eine Vernetzung mit Glyoxal an der Oberfläche der Celluloseetherteilchen erreicht, wie beispielsweise in der DE 24 15 556 beschrieben ist. Während es bisher üblich war, die genannten Celluloseether bereits in wäßriger Lösung oder in solchen Mengen einzubringen, die sich in dem in dem Massen bereits enthaltenen "freien" Wasser glatt lösen lassen, kennzeichnen sich die erfindungsgemäßen Fugendichtungsmassen durch ein neues Herstel¬ lungsverfahren bezüglich des Einbringens der Celluloseether.Most of the ingredients are commercially available. Both retarded and non-retarded cellulose ethers are commercially available. Retarded cellulose ethers are understood to mean those that swell in water after a delay compared to the unretarded substances. This will e.g. achieved by crosslinking with glyoxal on the surface of the cellulose ether particles, as described, for example, in DE 24 15 556. While it was previously customary to introduce the cellulose ethers mentioned already in aqueous solution or in amounts which can be readily dissolved in the "free" water already contained in the composition, the joint sealing compounds according to the invention are characterized by a new production process with regard to the introduction the cellulose ether.
Die erfindungsgemäß geeigneten Celluloseether werden in der flüs¬ sigen organischen Komponente aufgeschlämmt. Derartige Komponenten sind beispielsweise Weichmacher, Extender und/oder Netzmittel. Dabei
können wahlweise retardierte und/oder nicht retardierte Cellulose¬ ether eingesetzt werden.The cellulose ethers suitable according to the invention are slurried in the liquid organic component. Such components are, for example, plasticizers, extenders and / or wetting agents. there Retarded and / or non-retarded cellulose ethers can optionally be used.
Die in den Fugendichtungsmassen der Erfindung enthaltenen wäßrigen Dispersionen weisen bevorzugt Feststoffgehalte von 40 bis 75, ins¬ besondere 45 bis 65 Gew.-%, auf. Ihr pH-Wert kann mindestens 6, insbesondere 7 bis 9 betragen und wird, falls erforderlich, auf diese Werte eingestellt.The aqueous dispersions contained in the joint sealants of the invention preferably have solids contents of 40 to 75, in particular 45 to 65% by weight. Their pH value can be at least 6, in particular 7 to 9, and is adjusted to these values if necessary.
Die in den erfindungsgemäßen Fugendichtungsmassen enthaltenen Cellu¬ loseether haben bevorzugt als 2%-ige wäßrige Lösung bei 20°C Visko¬ sitäten nach Brookfield von mindestens 5.000 mPas. Bevorzugt werden solche mit einem Wert von mindestens 25.000 mPas also beispielsweise mittelviskose Hydroxyethylcellulosen. Besonders geeignet sind soge¬ nannte hochviskose Celluloseethertypen, die einen entsprechenden Wert von mindestens 70.000 mPas aufweisen z.B. hochviskose Hydroxy- ethylcellulose. Handelsübliche hochviskose Hydroxyethylcellulose erzielt z.B. als 2%-ige Lösung bei 20°C schon eine Viskosität von 100.000 mPas.The cellulose ethers contained in the jointing compounds according to the invention preferably have Brookfield viscosities of at least 5,000 mPas as a 2% strength aqueous solution at 20 ° C. Those with a value of at least 25,000 mPas, for example medium-viscosity hydroxyethyl celluloses, are preferred. So-called highly viscous cellulose ether types which have a corresponding value of at least 70,000 mPas are particularly suitable, e.g. highly viscous hydroxyethyl cellulose. Commercial high viscosity hydroxyethyl cellulose e.g. as a 2% solution at 20 ° C a viscosity of 100,000 mPas.
Gemäß den Herstellerangaben sind bei Hydroxyethylcellulose z.B. bei Natrosol 250 HHR bei einer Viskosität oberhalb von 200.000 mPas vollständige Lösungen nicht mehr zu erzielen. Bei den weniger hy¬ drophilen, erfindungsgemäß verwendbaren Celluloseether liegt diese Grenze noch niedriger, z.B. bei Hydroxypropylcellulose bei etwa 150.000 mPas oder bei Hydroxypropylmethylcellulose bei etwa 100.000 mPas. Mit höherer Konzentration bilden sich zunehmend gelartige Massen aus. Dies scheint jedoch eine besondere Rolle bei der Früh¬ regenfestigkeit der erfindungsgemäßen Fugendichtungsmassen zu spie¬ len. Auch wenn die genauen Zusammenhänge nicht geklärt sind, so läßt sich doch vermuten, daß beim Übersteigen dieser Löslichkeitsgrenze ein zunehmender Aufbau einer gelartigen Struktur mit dazu beiträgt,
- 8 -According to the manufacturer's instructions, complete solutions can no longer be achieved with hydroxyethyl cellulose, for example with Natrosol 250 HHR at a viscosity above 200,000 mPas. With the less hydrophilic cellulose ethers which can be used according to the invention, this limit is even lower, for example with hydroxypropyl cellulose around 150,000 mPas or with hydroxypropyl methyl cellulose around 100,000 mPas. With a higher concentration, gel-like masses increasingly form. However, this seems to play a special role in the early rain resistance of the joint sealants according to the invention. Even if the exact relationships are not clear, it can nevertheless be assumed that if this solubility limit is exceeded, an increasing build-up of a gel-like structure contributes to - 8th -
daß die Massen auch im nicht ausgehärteten Zustand durch Wasserbe¬ lastung wie Regen nicht oder nur wenig ausgewaschen werden.that the masses are not or only slightly washed out by water pollution such as rain even in the uncured state.
In diesem Zusammenhang kommt es offenbar auf das Verhältnis der Men¬ gen von Celluloseether zu "freiem" Wasser an, das ausschlaggebend dafür ist, ob diese Löslichkeitsgrenze. überschritten wird oder nicht. Unter "freiem" Wasser wird hier der Wassergehalt der Dich¬ tungsmasse verstanden, der den Celluloseethern zur Verfügung" steht um sich darin zu lösen. Somit kann nicht der Gesamtwassergehalt der Fugendichtungsmasse für eine entsprechende Berechnung herangezogen werden. Vielmehr ist zu berücksichtigen, daß die anderen Bestand¬ teile ebenfalls eine gewisse Menge Wasser beanspruchen, bzw. mehr oder weniger fest binden. So sind für die meisten Füllstoffe soge¬ nannte Wasserwerte bekannt. Dieser beträgt beispielsweise bei Schwerspat 11 g Wasser pro 100 g Schwerspat. Für Kieselsäure z.B. für die Type HDK V 15 der Wacker-Chemie lassen sich Werte zwischen 350 bis 400 g Wasser pro 100 g Kieselsäure ermitteln. Derartige Werte bieten dem Fachmann einen Anhaltspunkt dafür, welche Mengen "gebundenen" Wassers er von dem Gesamtwassergehalt άer Dichtmasse abziehen muß, um die Menge "freien" Wassers zu erhalten. Es ist es daher bevorzugt, daß diese Menge "freien" Wassers in Relation zu der Menge des jeweils eingesetzten Celluloseethertyps ein Verhältnis ergibt, das über der jeweiligen Löslichkeitsgrenze liegt.In this context, the ratio of the amounts of cellulose ether to "free" water is obviously important, which is decisive for whether this solubility limit. is exceeded or not. "Free" water is understood here to mean the water content of the sealing compound which is available to the cellulose ethers " to dissolve in. Thus, the total water content of the joint sealing compound cannot be used for a corresponding calculation. Rather, it must be taken into account that the others Constituents also require a certain amount of water or bind more or less tightly, so-called water values are known for most fillers, which is, for example, 11 g water per 100 g heavy spar for spar spar. For silica, for example, for the HDK type V 15 from Wacker-Chemie, values between 350 and 400 g of water per 100 g of silica can be determined.These values offer the person skilled in the art an indication of what amounts of "bound" water he has to subtract from the total water content of the sealant in order to free the amount "Water. It is therefore preferred that this amount of" free "water in relation z u the amount of the cellulose ether type used in each case gives a ratio which is above the respective solubility limit.
Etwas komplizierter wird die Sachlage, wenn der Fachmann einen Was¬ serbedarf berücksichtigen muß, der sich ergibt, wenn die disper- gierten Polymeren zur Salzbildung befähigte Gruppen enthalten. Er¬ gibt sich ein derartiger zusätzlicher Wasserbedarf, muß der Fachmann gegebenenfalls entsprechende Herstellerangaben hinzuziehen, auf Grund von Erfahrungswerten diesen Bedarf abschätzen oder durch ein¬ fache Handversuche näherungsweise bestimmen. Soll eine Fugendich¬ tungsmasse hergestellt werden, bei der die genannte Löslichkeits¬ grenze überschritten wird, so kann die Zugabe der Celluloseether
nicht wie üblich - also als Lösung - erfolgen. Mit dem erfindungsge¬ mäßen Verfahren wird ein Weg aufgezeigt, derartige Fugendichtungs¬ massen herzustellen.The situation becomes somewhat more complicated if the person skilled in the art has to take into account a water requirement which arises when the dispersed polymers contain groups capable of salt formation. If there is such an additional water requirement, the person skilled in the art may have to consult the appropriate manufacturer's information, estimate this need on the basis of empirical values or approximately determine it by simple manual tests. If a joint sealing compound is to be produced in which the solubility limit mentioned is exceeded, the cellulose ethers can be added not as usual - that is, as a solution. The method according to the invention shows a way of producing such joint sealing compounds.
Weiterhin können in den Fugendichtungsmassen der Erfindung Füll¬ stoffe in einer Menge von 0 bis 60, insbesondere 2 bis 60 Gew.-%, bezogen auf die Gesamtmasse der Fugendichtungsmassen, enthalten sein. Derartige Massen, weisen, wenn sie keine oder nur sehr wenig Füllstoffe enthalten, eine hohe Transparenz auf. Niedrige Füll¬ stoffgehalte können insbesondere bei solchen Massen vorliegen bei denen die Füllstoffe einen zusätzlichen verdickenden Effekt bewirken wie Kieselsäure. Werden nur Füllstoffe eingesetzt, die diesen zu¬ sätzlichen Effekt nicht aufweisen, liegt deren Gehalt meist zwischen 35 und 60"Gew.-%. Man spricht hier von hochgefüllten Massen.Furthermore, fillers can be contained in the joint sealants of the invention in an amount of 0 to 60, in particular 2 to 60% by weight, based on the total mass of the joint sealants. Such compositions, if they contain little or no fillers, are highly transparent. Low filler contents can be present, in particular, in those compositions in which the fillers have an additional thickening effect, such as silica. Only fillers used do not have this zu¬ sätzlichen effect, the content thereof is usually between 35 and 60 "wt .-%. We speak here of highly filled compositions.
Gemäß einer weiteren vorteilhaften Ausführungsform der Erfindung enthalten die Fugendichtungsmassen als Weichmacher chlorierte Kohlenwasserstoffe, insbesondere chlorierte Paraffine, und als Netz¬ mittel nichtionische Tenside. Bevorzugt sind handelsübliche chlo¬ rierte Paraffine mit einer. Kettenlänge von etwa 10 bis 18 Kohlen¬ stoffatomen und einem Chlorgehalt von etwa 40 bis 70 Gew.-%.According to a further advantageous embodiment of the invention, the jointing compounds contain chlorinated hydrocarbons, in particular chlorinated paraffins, as plasticizers, and nonionic surfactants as wetting agents. Commercially available chlorinated paraffins with a. Chain length of about 10 to 18 carbon atoms and a chlorine content of about 40 to 70% by weight.
In einer bevorzugten Ausführungsform enthalten die Fugendichtungs¬ massenIn a preferred embodiment, the joint sealants contain
25 - 90 Gew.-% Polymerdispersion, bei hochgefüllten25 - 90 wt .-% polymer dispersion, with highly filled
Fugendichtungsmassen insbesondereJoint sealants in particular
25 - 40 Gew.-% Polymerdispersion,25-40% by weight polymer dispersion,
0 - 60 Gew.-% insbesondere 2 bis 60 Gew.-% Füllstoffe0 - 60 wt .-% in particular 2 to 60 wt .-% fillers
0 - 1 Gew.-% insbesondere 0,3 bis 0,5 Gew.-% Netzmittel0 - 1 wt .-% in particular 0.3 to 0.5 wt .-% wetting agent
0 - 20 Gew.-% insbesondere 5 bis 15 Weichmacher und bis zu0-20% by weight, in particular 5 to 15 plasticizers and up to
10 Gew.-% insbesondere 4 bis 6 Gew.-% weitere übliche
Zusätze wie Verdickungsmittel, Entschäumer und10% by weight, in particular 4 to 6% by weight, of other customary ones Additives such as thickeners, defoamers and
Pigmente mindestens zum Aufschlämmen der Celluloseether ausreichende Men¬ gen an organischer flüssiger Komponente und bis zu 1,5 Gew.-% CelluloseetherPigments at least sufficient amounts of organic liquid component and up to 1.5% by weight of cellulose ether for slurrying the cellulose ethers
- Gew.-%-Angaben jeweils bezogen auf die Gesamtmenge.-% by weight - information in each case based on the total amount.
Dabei sollte der Celluloseethergehalt nicht viel weniger als 0,1 Gew.-% betragen. Gute Ergebnisse zeigen sich insbesondere bei Fu¬ gendichtungsmassen, bei denen unter Berücksichtigung der Rahmenpa¬ rameter wie Celluloseethertyp und Gehalt an freiem Wasser der Celluloseethergehalt in einem Bereich von etwa 0,1 bis 0,5 Gew.-% bezogen auf die Gesamtmenge liegt.The cellulose ether content should not be much less than 0.1% by weight. Good results are shown in particular in the case of joint sealants in which, taking into account the general parameters such as cellulose ether type and free water content, the cellulose ether content is in a range from about 0.1 to 0.5% by weight, based on the total amount.
Wie bereits erwähnt, werden die Celluloseether vor der Zugabe bei der Herstellung der erfindungsgemäßen Fugendichtungsmasse in der organischen flüssigen Komponente aufgeschlämmt. Dieses Verhältnis von Celluloseether zu Flüssigkeit liegt bevorzugt in einem Bereich von 1 : 2 bis 1 : 4, insbesondere bei etwa 1 : 3. Vorzugsweise wird als flüssiger organischer Bestandteil einer der übliche Zusätze für Fugendichtungsmassen eingesetzt wie z.B. Weichmacher, Extender und/- oder Netzmittel. Desweitereπ wird bevorzugt, bei der Herstellung die Zugabe der pH-Regulatoren, insbesondere der Basen, erst nach Zugabe der Celluloseether vorzunehmen. Dies ist insbesondere bei retar¬ dierten Celluloseethern von Vorteil, da im basischen Bereich die Retardierung schneller aufgehoben wird. Andererseits kann eine neu¬ trale bis basische Einstellung der Fugendichtungsmassen sich günstig auf deren Stabilität, insbesondere auf deren Scherstabilität, aus¬ wirken.
Üblicherweise wird bei der Herstellung der erfindungsgemäßen Fugen¬ dichtungsmassen die Polymerdispersion vorgelegt. Es werden dann in einer bevorzugten Form des Verfahrens die üblichen Zusätze mit Aus¬ nahme der pH-Regulatoren zugefügt und untergemischt. Anschließend erfolgt die Vermischung mit den in,der organischen flüssigen Kompo¬ nente aufgeschlämmten Celluloseethern und nach anschließendem Un¬ termischen der Füllstoffe die Zu ischung der pH-Regulatoren.As already mentioned, the cellulose ethers are slurried in the organic liquid component before the addition in the production of the joint sealing compound according to the invention. This ratio of cellulose ether to liquid is preferably in a range from 1: 2 to 1: 4, in particular approximately 1: 3. One of the usual additives for joint sealants, such as plasticizers, extenders and / or wetting agents, is preferably used as the liquid organic component . Furthermore, it is preferred to add the pH regulators, in particular the bases, during the preparation only after the addition of the cellulose ethers. This is particularly advantageous in the case of retarded cellulose ethers, since the retardation is eliminated more quickly in the basic area. On the other hand, a neutral to basic setting of the joint sealing compounds can have a favorable effect on their stability, in particular on their shear stability. The polymer dispersion is usually initially taken in the preparation of the joint sealing compounds according to the invention. In a preferred form of the process, the usual additives with the exception of the pH regulators are then added and mixed in. The mixture is then mixed with the cellulose ethers slurried in the organic liquid component and, after the fillers have been subsequently mixed in, the pH regulators are added.
Es kann sich auch als vorteilhaft erweisen, wenn die Zugabe des Füllstoffs erst nach der Zugabe des pH-Regulators erfolgt.It can also prove to be advantageous if the filler is only added after the pH regulator has been added.
Zur Vermeidung des Einrühren.s von Luft und der Bildung von Luftbla¬ sen im Produkt kann das Rühren unter Vakuum vorgenommen werden.To avoid the stirring in of air and the formation of air bubbles in the product, stirring can be carried out under vacuum.
Die Verwendung der Fugendichtungsmassen erfolgt vorzugsweise be¬ stimmungsgemäß. Sie sind insbesondere für die Verwendung in Berei¬ chen geeignet, in denen sie Spritzwasser, Regen oder sonstiger Frühwasserbelastung ausgesetzt sind.The joint sealants are preferably used as intended. They are particularly suitable for use in areas in which they are exposed to splash water, rain or other early water pollution.
Die Erfindung wird im folgenden anhand bevorzugter Ausführungsbei¬ spiele näher erläutert.
The invention is explained in more detail below on the basis of preferred exemplary embodiments.
B e i s p i e l eB e i s p i e l e
Die in den Beispielen beschriebenen Massen sowie weitere, zu Ver¬ gleichszwecken hergestellte Massen wurden einem Auswaschungstest unterworfen, wobei eine .Beregnungsapparatur gemäß der DE 38 14078-A-l Fig. 1 verwendet wurde; die gleiche Apparatur ist in Fig. 2 in Seitenansicht- gezeigt.The masses described in the examples, as well as other masses produced for comparison purposes, were subjected to a washout test, using an irrigation apparatus according to DE 38 14078-A-1 FIG. 1; the same apparatus is shown in side view in FIG.
Die Beregnungsapparatur bestand aus einem Gehäuse aus durchsichtigem Kunststoff mit den Abmessungen: Höhe 70 cm, Breite 60 cm und Tiefe 60 cm. Sie umfaßte ein Gehäuse 1, einen Brausenkopf 2, eine Proben¬ schale 3, eine Pumpe 4, einen Bodenablauf 5 und einen Absperrhahn 6 für den Ablauf. Die Probenschale bestand aus einem Gefäß der Abmes¬ sung 7 x 7 cm und wies eine Tiefe von 2,5 cm auf. Bei dem Brausen¬ kopf handelte es sich um eine übliche Handbrause, wie sie zur Kör¬ perpflege verwendet wird und die so eingestellt war, daß eine gleichmäßige Beregnung der Probe erfolgte. Der Abstand zwischen Probe 3 und Brausenkopf 2 betrug 30 cm.The irrigation equipment consisted of a housing made of transparent plastic with the dimensions: height 70 cm, width 60 cm and depth 60 cm. It comprised a housing 1, a shower head 2, a sample bowl 3, a pump 4, a floor drain 5 and a shut-off valve 6 for the drain. The sample pan consisted of a vessel measuring 7 x 7 cm and had a depth of 2.5 cm. The shower head was a conventional hand shower as used for body care and was set so that the sample was irrigated evenly. The distance between sample 3 and shower head 2 was 30 cm.
Die Apparatur wurde mit demineralisiertem Wasser betrieben, wobei durch die Pumpe ein Überdruck von etwa 0,4 bar erzeugt wurde. Der Wasserdurchsatz betrug 300 1/h. Das Besprühen mit Wasser wurde 5 Minuten, jeweils 1 min nach dem Einfüllen und Glattstreichen der Oberfläche der zu prüfenden Massen, vorgenommen. Die Auswaschung (in Gew.-%) wurde durch Differenzwägung vor und nach dem Beregnen be¬ stimmt.The apparatus was operated with demineralized water, the pump generating an excess pressure of approximately 0.4 bar. The water flow rate was 300 l / h. The spraying with water was carried out 5 minutes, in each case 1 minute after filling and smoothing the surface of the masses to be tested. The washout (in% by weight) was determined by differential weighing before and after sprinkling.
Die Verarbeitbarkeit wurde nach DIN 52456 gemessen. Dabei wurde eine Bohrung von 4 m , ein Druck von 2 bar und ein Prüfvolumen von 200 ml eingesetzt.The processability was measured according to DIN 52456. A 4 m bore, a pressure of 2 bar and a test volume of 200 ml were used.
Die in den Beispielen beschriebenen Massen wurden weiterhin einem Test hinsichtlich ihres Glätteverhaltens unterzogen. Dieser Test
wurde von 7 unabhängig arbeitenden Personen so durchgeführt, daß nach Auftragen eines 30 cm langen Massenstrangs auf eine glatte, ebene, dunkle Unterlage die Masse mit Spatel und Fingern geglättet wurde. Das Glätteverhalten wurde nach einer Notenskala von 1 (= sehr gut) bis 6 (= ungenügend) beurteilt.The compositions described in the examples were also subjected to a test for their smoothness behavior. This test was carried out by 7 independently working people so that after applying a 30 cm long strand of mass to a smooth, flat, dark surface, the mass was smoothed with a spatula and fingers. The smoothness behavior was assessed on a scale from 1 (= very good) to 6 (= insufficient).
Beispiel 1example 1
In einem Planetenmischer wurden die folgenden Bestandteile während etwa 45 Minuten intensiv gemischt:The following components were mixed intensively in a planetary mixer for about 45 minutes:
1750 g wäßrige, handelsübliche Dispersion auf Basis eines .1750 g of aqueous, commercially available dispersion based on a.
Copolymerisats aus Vinylacetat und Ethylen (ungefähr 60 % Feststoff), mit einem pH-Wert von ca. 4,5 und einer Viskosi¬ tät von etwa 1600 mPa.s bei 20°C (Handelsname: Vinnapas EP 17, Fa. Wacker), 250 g Chlorparaffin (C12-C14, 49 % Chlor), 2800 g Bariumsulfat (Handelsname: Schwerspat EW0), 100 g Titandioxid (Handelsname: KR0N0S RN 56) 25 g Natriumcarbonat (technisch, reine Handelsware), 25 g Ethylenoxidaddukt (ungefähr 9,5 E0) an Nonylphenol, 5 g handelsübliches halogeniertes Konservierungsmittel, 37 g Hydroxyethylcellulose mit einer Viskosität von etwaCopolymer of vinyl acetate and ethylene (approximately 60% solids), with a pH of approximately 4.5 and a viscosity of approximately 1600 mPa.s at 20 ° C. (trade name: Vinnapas EP 17, from Wacker), 250 g chlorinated paraffin (C12-C14, 49% chlorine), 2800 g barium sulfate (trade name: Schwerspat EW0), 100 g titanium dioxide (trade name: KR0N0S RN 56) 25 g sodium carbonate (technical, pure commercial product), 25 g ethylene oxide adduct (approx. 9, 5 E0) of nonylphenol, 5 g of commercially available halogenated preservative, 37 g of hydroxyethyl cellulose with a viscosity of about
100.000 mPa.s einer 2 %-igen, wäßrigen Lösung bei 20°C und einem Hydroxyethylgruppengehalt von 55 Gew.-% (Handelsname: Natrosol 250 HHR).100,000 mPa.s of a 2% strength aqueous solution at 20 ° C. and a hydroxyethyl group content of 55% by weight (trade name: Natrosol 250 HHR).
Dabei wurde so vorgegangen, daß zunächst die Polymerdispersion vor¬ gelegt wurde. Es wurden dann das Ethylenoxidaddukt (Emulgator), das Konservierungsmittel, das Titandioxid (Pigment) sowie ein Teil des Chlorparaffins hinzugegeben. In dem änderen Teil des Chlorparaffins wurde die Hydroxyethylcellulose aufgeschlämmt und ebenfalls zugege¬ ben und das Ganze gut durchmischt. Es folgte die Untermischung des
Natriumcarbonats als 10 %-ige wäßrige Lösung. Zum Schluß wurde das Bariumsulfat (Füllstoff) zugegeben und glattgerührt.The procedure was such that the polymer dispersion was initially introduced. The ethylene oxide adduct (emulsifier), the preservative, the titanium dioxide (pigment) and part of the chlorinated paraffin were then added. In the other part of the chlorinated paraffin, the hydroxyethyl cellulose was slurried and also added, and the whole was mixed well. The mixing of the Sodium carbonate as a 10% aqueous solution. Finally, the barium sulfate (filler) was added and stirred until smooth.
Diese Mischung wurde in 310 ml Kartuschen abgefüllt und war wenig¬ stens ein Jahr bei Temperaturen bis 35°C lagerstabil.This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN.52456: 2300 g/min Glättverhalten: gutProcessability according to DIN.52456: 2300 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 2Example 2
Es wurde eine "Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion auf Basis eines Copoly erisats aus Styrol und Butadien (ungefähr 64 % Feststoff) mit einem pH-Wert von ca. 10,5 und einer Viskosität von etwa 800 mPa.s bei 20°C (Handelsname: Polysar 2105, Fa. Hycar) eingesetzt wurden.A " composition according to Example 1 was prepared, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of styrene and butadiene (approximately 64% solids) with a pH of 10.5 and a viscosity of about 800 mPa.s at 20 ° C (trade name: Polysar 2105, Hycar) were used.
Diese Mischung wurde in 310 ml Kartuschen abgefüllt und war wenig¬ stens ein Jahr bei Temperaturen bis 35°C lagerstabil.This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1980 g/min Glättverhalten: gutProcessability according to DIN 52456: 1980 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 3Example 3
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion auf Basis eines Copolymerisats aus Vinylacetat und
Maleinsäure-di-n-butylester, Festkörpergehalt ca. 53 %, pH-Wer 4 bis 5, Viskosität (Brookfield, 20°C, 20 U/min) 1000 bis 3000 mPa.s, Handelsname Mowilith DM 2HB, Fa. Hoechst, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of vinyl acetate and Maleic acid di-n-butyl ester, solids content approx. 53%, pH value 4 to 5, viscosity (Brookfield, 20 ° C., 20 rpm) 1000 to 3000 mPa.s, trade name Mowilith DM 2HB, Hoechst, were used.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 2030 g/min Glättverhalten: gutProcessability according to DIN 52456: 2030 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 4Example 4
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Si¬ liconemulsion (aus der Emulsion elastisch auftrocknend, ungefähr 45 % Feststoff), einem pH-Wert von ca. 5 und einer Dichte von etwa 1,0 bei 20°C, Handelsname: Wacker Siliconbautenschutzmittel, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available silicon emulsion (elastically drying from the emulsion, approximately 45% solids), a pH of approx. 5 and a density of about 1.0 at 20 ° C, trade name: Wacker silicone building protection agents.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1790 g/min Glättverhalten: gutProcessability according to DIN 52456: 1790 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 5Example 5
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen
Dispersion eines Polysulfidpolymers, ungefähr 55 % Feststoff, pH-Wert 9 bis 10, Handelsname: ZW 2028, Fa. Thiokol, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion described there of a copolymer of vinyl acetate and ethylene 1750 g of an aqueous, commercially available Dispersion of a polysulfide polymer, approximately 55% solids, pH 9-10, trade name: ZW 2028, from Thiokol.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1790 g/min Glättverhalten: gutProcessability according to DIN 52456: 1790 g / min Smoothing behavior: good
Auswaschung: 2 % Verlust.Washout: 2% loss.
Beispiel 6Example 6
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion eines Polyurethanpolymers, ungefähr 40 % Feststoff, pH-Wert 7,0 bis 7,5, Viskosität 10.000 bis 18.000 mPa.s, Handelsname: VP-LA 3110, Fa. Henkel, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion of a polyurethane polymer, approximately 40% solids, pH 7.0 to 7.5, viscosity 10,000 to 18,000 mPa.s, trade name: VP-LA 3110, from Henkel.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1820 g/min Glättverhalten: gutProcessability according to DIN 52456: 1820 g / min Smoothing behavior: good
Auswaschung: 3 % Verlust.Washout: 3% loss.
Beispiel 7Example 7
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion auf Basis eines Polyvinylacetats, ungefähr 50 % Feststoff,
pH-Wert ca. 6 bis 7, Viskosität etwa 10.000 bis 18.000 mPa.s (Brook- field), Handelsname Mowilith DLR, Fa. Hoechst, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a polyvinyl acetate, approximately 50% solids, pH about 6 to 7, viscosity about 10,000 to 18,000 mPa.s (Brookfield), trade name Mowilith DLR, Hoechst, were used.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1670 g/min Glättverhalten: gutProcessability according to DIN 52456: 1670 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 8Example 8
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion auf Basis eines Copolymerisats aus Chloropren und Meth- acrylsäure, ungefähr 46,5 bis 48,5 % Feststoff, pH-Wert ca. 9, Han¬ delsname Neoprene Latex 115, eingesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a copolymer of chloroprene and methacrylic acid, approximately 46.5 to 48.5% Solid, pH about 9, trade name Neoprene Latex 115, were used.
Die Mischung wurde in 310 ml Kartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 2030 g/min Glättverhalten: gutProcessability according to DIN 52456: 2030 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Beispiel 9Example 9
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Dispersion eines Copolymeren von Vinylacetat und Ethylen 1750 g einer wäßrigen, handelsüblichen Di¬ spersion auf Basis eines Naturkautschuk-Latex, ungefähr 70 %
Feststoff, pH-Wert ca. 9 bis 10, Handelsname Revertex Standard, ein¬ gesetzt wurden.A composition was prepared according to Example 1, wherein instead of the dispersion of a copolymer of vinyl acetate and ethylene described there, 1750 g of an aqueous, commercially available dispersion based on a natural rubber latex, approximately 70% Solid, pH about 9 to 10, trade name Revertex Standard, were used.
Diese Mischung wurde in 310 ml Kartuschen abgefüllt und war wenig¬ stens ein Jahr bei Temperaturen bis 35°C lagerstabil.This mixture was filled into 310 ml cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 1740 g/min Glättverhalten: gutProcessability according to DIN 52456: 1740 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.
Washout: 1% loss.
Beispiel 10Example 10
Die Beispiele 1 bis 9 wurden nach Austausch der dort verwendeten Hydroxyethylcellulose durch eine handelsübliche Methylhydroxypropyl¬ cellulose (MHPC) mit einer Viskosität von etwa 20.000 mPa.s einer 2 %-igen Lösung bei 20°C nach Brookfield und einem Hydroxypropylgrup- pengehalt von 3,2 Gew.-% erneut gemessen. Die Ausspritzraten nach DIN 52456 sind vergleichbar. Das Glättverhalten ist mit gut zu be¬ urteilen.Examples 1 to 9 were replaced by replacing the hydroxyethyl cellulose used there with a commercially available methyl hydroxypropyl cellulose (MHPC) with a viscosity of about 20,000 mPa.s of a 2% solution at 20 ° C. according to Brookfield and a hydroxypropyl group content of 3. 2% by weight measured again. The spray rates according to DIN 52456 are comparable. The smoothing behavior can be assessed as good.
Ergebnis:Result:
Zusammensetzung gemäß Auswaschung in % VerlustComposition according to washout in% loss
Beispiel Nr., jedoch mit MHPCExample No., but with MHPC
l' 1,8l ' 1.8
2 1,02 1.0
3 1,03 1.0
4 1,44 1.4
5 2,65 2.6
6 3,06 3.0
7 1,47 1.4
8 1,08 1.0
9 1,3
9 1.3
Beispiel 11.Example 11.
Die Beispiele 1 bis 9 wurden nach Austausch der dort verwendeten Hydroxyethylcellulose durch eine handelsübliche Hydroxypropylcellu¬ lose (HPC) mit einer Viskosität von etwa 5000 mPa.s einer 2 %-igen Lösung bei 20°C nach Brookfield und einem Hydroxypropylgruppengehalt von 70 % erneut gemessen. Die Ausspritzraten nach DIN 52456 sind vergleichbar. Das Glättverhalten ist mit gut zu beurteilen.Examples 1 to 9 were measured again after replacing the hydroxyethyl cellulose used there with a commercially available hydroxypropyl cellulose (HPC) with a viscosity of approximately 5000 mPa.s of a 2% solution at 20 ° C. according to Brookfield and a hydroxypropyl group content of 70% . The spray rates according to DIN 52456 are comparable. The smoothing behavior can be assessed as good.
Ergebnis:Result:
Zusammensetzung gemäß Auswaschung in % VerlustComposition according to washout in% loss
Beispiel Nr. , jedoch mit HPCExample No., but with HPC
1 2,21 2.2
2 1,92 1.9
3 . 2,3 Third 2.3
4 1,34 1.3
5 2,05 2.0
6 2,56 2.5
7 1,07 1.0
8 2,08 2.0
9 1,0
9 1.0
Vergleichsversuch A.Comparative experiment A.
Die Beispiele 1 bis 9 wurden nach Austausch der Hydroxyethylcellu¬ lose (HEC) durch eine handelsübliche wäßrige Polyacrylsäuredisper- sion (ungefähr 25 % Feststoff, Handelsname: Rohagit SD 15) erneut gemessen. Die Ausspritzraten nach DIN 52456 waren vergleichbar. Das Glättverhalten ist mangelhaft; das Auswaschverhalten ist ungünsti¬ ger.Examples 1 to 9 were measured again after replacing the hydroxyethyl cellulose (HEC) with a commercially available aqueous polyacrylic acid dispersion (approximately 25% solids, trade name: Rohagit SD 15). The injection rates according to DIN 52456 were comparable. The smoothing behavior is poor; the washout behavior is less favorable.
Ergebnisse im Auswaschversuch:Results in the washout test:
Zusammensetzung gemäß Auswaschung (in % Verlust)Composition according to washout (in% loss)
Beispiel Nr. (ohne HEC, mit PolyacrylSäuredispersion)Example No. (without HEC, with polyacrylic acid dispersion)
1 41 4
2 102 10
3 113 11
4 284 28
5 305 30
6 1006 100
7 147 14
8 48 4
9 16
9 16
Vergleichsversuch B.Comparative experiment B.
Die Beispiele 1 bis 9 wurden ohne Hydroxyethylcellulose (HEC) (Han¬ delsname: Natrosol 250 HR) hergestellt. Das Glättverhalten ist.man¬ gelhaft; das Auswaschverhalteπ ist ungünstiger.Examples 1 to 9 were produced without hydroxyethyl cellulose (HEC) (trade name: Natrosol 250 HR). The smoothing behavior is . deficient; the washout behavior is less favorable.
Ergebnisse im Auswaschversuch:Results in the washout test:
Zusammensetzung gemäß Auswaschung (in % Verlust)Composition according to washout (in% loss)
Beispiel Nr. (ohne HEC)Example No. (without HEC)
1 141 14
2 202 20
3 100 -4 643 100 -4 64
5 985 98
6 1006 100
7 957 95
8 78 7
9 90
9 90
Beispiel 12Example 12
In einem Planetenmischer wurden die folgenden Bestandteile während insgesamt etwa 45 Minuten intensiv gemischt:The following components were mixed intensively in a planetary mixer for a total of about 45 minutes:
1750 g wäßrige, handelsübliche Polybutylacrylesterdispersion1750 g of aqueous, commercially available polybutyl acrylate dispersion
(ungefähr 62 % Feststoff), einem pH-Wert von 6,0 - 6,5, einer Glasübergangstemperatur Tg -50°C, einer Viskosität von etwa 250 mPas bei 23°C und einer mittleren Teilchengröße von 0,4 μ , 250 g Chlorparaffin (C12-C14, 49 % Chlor), 2800 g Bariumsulfat (Handelsprodukt: Schwerspat EW0), 100 g Titandioxid (Handelsprodukt KR0N0S RN 56), 25 g Natriumcarbonat (techn. reine Handelsware), 25 g Ethylenoxidaddukt (ungefähr 9,5 E0) an Nonylphenol, 5 g handelsübliches halogeniertes Konservierungsmittel, 37 g Hydroxyethylcellulose mit einer Viskosität von etwa 4000 mPas einer 1 %-igen, wäßrigen Lösung bei 20°C und einem Hydroxyethylgruppengehalt von 55 Gew.-%, Handelsname: Natrosol 250 HHR.(approximately 62% solids), a pH of 6.0-6.5, a glass transition temperature Tg -50 ° C, a viscosity of about 250 mPas at 23 ° C and an average particle size of 0.4 μ, 250 g Chlorinated paraffin (C12-C14, 49% chlorine), 2800 g barium sulfate (commercial product: Schwerspat EW0), 100 g titanium dioxide (commercial product KR0N0S RN 56), 25 g sodium carbonate (technically pure commercial product), 25 g ethylene oxide adduct (approximately 9.5 E0 ) of nonylphenol, 5 g of commercially available halogenated preservative, 37 g of hydroxyethyl cellulose with a viscosity of about 4000 mPas of a 1% strength aqueous solution at 20 ° C. and a hydroxyethyl group content of 55% by weight, trade name: Natrosol 250 HHR.
Dabei wurde so vorgegangen, daß zunächst die Polymerdispersion vor¬ gelegt wurde. Es wurden dann das Ethylenoxidaddukt (Emulgator), das Konservierungsmittel, das Titandioxid (Pigment) sowie ein Teil des Chlorparaffins hinzugegeben. In dem anderen Teil des Chlorparaff ns wurde die Hydroxyethylcellulose aufgeschlämmt und ebenfalls zugege¬ ben und das Ganze gut durchmischt. Es folgte die Üntermischung des Natriumcarbonats als 10 %-ige wäßrige Lösung. Zum Schluß wurde das Bariumsulfat (Füllstoff) zugegeben und glattgerührt.
Diese Mischung wurde in 310 ml Kunststoffkartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.The procedure was such that the polymer dispersion was initially introduced. The ethylene oxide adduct (emulsifier), the preservative, the titanium dioxide (pigment) and part of the chlorinated paraffin were then added. In the other part of the chlorinated paraffin, the hydroxyethyl cellulose was slurried and also added, and the whole was mixed thoroughly. The sodium carbonate was then mixed in as a 10% strength aqueous solution. Finally, the barium sulfate (filler) was added and stirred until smooth. This mixture was filled in 310 ml plastic cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 2260 g/min Glättverhalten: - gutProcessability according to DIN 52456: 2260 g / min Smoothing behavior: - good
Auswaschung: 1 % VerlustWashout: 1% loss
Bei einem Zusatz von insgesamt 50 g derselben Hydroxyethylcellulose wurden folgende Ergebnisse gefunden:The following results were found when a total of 50 g of the same hydroxyethyl cellulose was added:
Verarbeitbarkeit nach DIN 52456: 1300 g/min Glättverhalten: sehr gutProcessability according to DIN 52456: 1300 g / min Smoothing behavior: very good
Auswaschung: 0,3 % VerlustWashout: 0.3% loss
Beispiel 13Example 13
In einem Planetenmischer wurden die wie in Beispiel 12 aufgeführten Bestandteile während etwa 45 Minuten intensiv gemischt bei gleicher Vorgehensweise, wobei jedoch anstelle der Hydroxyethylcellulose:In a planetary mixer, the constituents listed in Example 12 were mixed intensively for about 45 minutes using the same procedure, but instead of the hydroxyethyl cellulose:
20 g einer Hydroxypropylcellulose mit einer Viskosität von etwa 5000 mPas einer 2 %-igen, wäßrigen Lösung bei 20°C und einem Hydroxypropylgruppengehalt von 70 %, Handelsname Klucel M20 g of a hydroxypropyl cellulose with a viscosity of about 5000 mPas of a 2% strength aqueous solution at 20 ° C. and a hydroxypropyl group content of 70%, trade name Klucel M
eingesetzt wurden.were used.
Diese Mischung wurde in 310 ml Kunststoffkartuschen abgefüllt und war wenigstens bei Temperaturen bis 35°C lagerstabil.
Verarbeitbarkeit nach DIN 52456: 2100 g /min Glättverhalten: gutThis mixture was filled into 310 ml plastic cartridges and was stable in storage at least up to 35 ° C. Processability according to DIN 52456: 2100 g / min Smoothing behavior: good
Auswaschung: 5 % VerlustWashout: 5% loss
Beispiel 14Example 14
In einem Planetenmischer wurden die wie in Beispiel 12 aufgeführten Bestandteile während etwa 45 Minuten intensiv gemischt bei gleicher Vorgehensweise, wobei jedoch anstelle der HydroxyethylcelluloseIn a planetary mixer, the constituents listed in Example 12 were mixed intensively for about 45 minutes using the same procedure, but using instead of the hydroxyethyl cellulose
37 g einer Methylhydroxypropylcellulose mit einer Viskosität von etwa 20000 mPas einer 2 %-igen, wäßrigen Lösung bei 20°C und einem Hydroxypropylgruppengehalt von 3,2 Gew.-%, Handels¬ name: Culminal MHPC 20000 PR37 g of a methylhydroxypropyl cellulose with a viscosity of about 20,000 mPas of a 2% strength aqueous solution at 20 ° C. and a hydroxypropyl group content of 3.2% by weight, trade name: culinary MHPC 20000 PR
eingesetzt wurden.were used.
Diese Mischung wurde in 310 ml Kunststoffkartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.This mixture was filled in 310 ml plastic cartridges and was stable for at least one year at temperatures up to 35 ° C.
Verarbeitbarkeit nach DIN 52456: 2870 g/min Glättverhalten: gutProcessability according to DIN 52456: 2870 g / min Smoothing behavior: good
Auswaschung: 3.5 % Verlust
Washout: 3.5% loss
Beispiel 15Example 15
In einem Planetenmischer wurden die folgenden Bestandteile während etwa 45 Minuten intensiv gemischt.The following components were mixed intensively in a planetary mixer for about 45 minutes.
4700 g wäßrige Dispersion eines Polyacrylsäurebutylesters mit geringen Mengen einpolymerisierten Acrylnitrils (60 % Fest¬ stoffgehalt), pH-Wert etwa 5 - 6, 52 g Ethylenoxidaddukt (ungefähr 9,5 E0) an Nonylphenol 25 g handelsübliches Silikon-KW-Entschäumergemisch 13 g handelsübliches phenolisches Konservierungsmittel4700 g of aqueous dispersion of a polyacrylic acid butyl ester with small amounts of copolymerized acrylonitrile (60% solids content), pH about 5-6, 52 g of ethylene oxide adduct (about 9.5 E0) of nonylphenol 25 g of commercially available silicone / KW defoamer mixture 13 g of commercially available phenolic preservative
(Parmetol, Schulke-Mayr, Hamburg) 102 g disperse Kieselsäure (Handelsprodukt HDK V 15,(Parmetol, Schulke-Mayr, Hamburg) 102 g disperse silica (commercial product HDK V 15,
Wacker-Ghemie) 36 g wäßrige Ammoniaklösung (25 %-ig) 52 g Chlorparaffin (C10-C1 , 49 % Chlor) 18 g einer Hydroxyethylcellulose mit einer Viskosität von etwa 4000 mPas einer 1 %-igen, wäßrigen Lösung und einem Hy- droxyethylgruppengehalt von 55 Gew.-%, Handelsname: Natrosol 250 HHR.Wacker-Ghemie) 36 g aqueous ammonia solution (25%) 52 g chlorinated paraffin (C10-C1, 49% chlorine) 18 g hydroxyethyl cellulose with a viscosity of approximately 4000 mPas of a 1% aqueous solution and a hydroxyethyl group content of 55% by weight, trade name: Natrosol 250 HHR.
Dabei wurde so vorgegangen, daß zunächst die Dispersion vorgelegt wurde. Es wurden dann das Ethylenoxidaddukt (Emulgator), das Kon¬ servierungsmittel und der Entschäumer hinzugegeben. Im Chlorparaffin wurde die Hydroxyethylcellulose aufgeschlämmt und ebenfalls zugege¬ ben und das ganze gut durchmischt. Es folgte die Untermischung der 25%-igen wäßrigen Ammoniaklösung. Zum Schluß wurde die disperse Kie¬ selsäure (Füllstoff) zugegeben und glattgerührt.The procedure was such that the dispersion was initially introduced. The ethylene oxide adduct (emulsifier), the preservative and the defoamer were then added. The hydroxyethyl cellulose was slurried in the chlorinated paraffin and likewise added, and the whole was thoroughly mixed. This was followed by the mixing in of the 25% aqueous ammonia solution. Finally, the disperse silica (filler) was added and stirred until smooth.
Diese Mischung wurde in 310 ml Kunststoffkartuschen abgefüllt und war wenigstens ein Jahr bei Temperaturen bis 35°C lagerstabil.
Verarbeitbarkeit nach DIN 52456: 3700 g/min Glättverhalten: gutThis mixture was filled in 310 ml plastic cartridges and was stable for at least one year at temperatures up to 35 ° C. Processability according to DIN 52456: 3700 g / min Smoothing behavior: good
Auswaschung: 4,5 % VerlustWashout: 4.5% loss
Beispiel 16Example 16
In einem Planetenmischer wurden die folgenden Bestandteile während insgesamt etwa 30 Minuten intensiv gemischt:The following components were mixed intensively in a planetary mixer for a total of about 30 minutes:
1200 g handelsübliche Dispersion eines Acrylsäureestercopolymerisats mit ungefähr 55 Gew.-% Feststoff und freien Carboxygruppen Handelsname: Prima! E 17851200 g commercially available dispersion of an acrylic acid ester copolymer with approximately 55% by weight solids and free carboxy groups Trade name: Great! E 1785
200 g Polybuten als Extender200 g polybutene as an extender
20 g Ethylenoxidaddukt als Netzmittel20 g ethylene oxide adduct as a wetting agent
4 g handelsübliches halogeniertes Konservierungsmittel (AKTIZID TL 526)4 g commercially available halogenated preservative (AKTIZID TL 526)
200 g Butylbenzylphthalat als Weichmacher200 g of butyl benzyl phthalate as a plasticizer
200 g Wasser200 g water
80 g aliphatisches aro atenarmes Lösungsmittel (SHELLS0L D 60)80 g aliphatic aro-low solvent (SHELLS0L D 60)
4 g Hydroxyethylcellulose. hochviskos (NATROSOL 250 HHR)4 g of hydroxyethyl cellulose. highly viscous (NATROSOL 250 HHR)
2040g ungecoatete Kreide2040g uncoated chalk
40 g Titandioxid und40 g titanium dioxide and
12 g 25%-ige wäßrige Ammoniaklösung12 g of 25% aqueous ammonia solution
Verarbeitbarkeit nach DIN 52456: 1000 g/min Glättverhalten: gutProcessability according to DIN 52456: 1000 g / min Smoothing behavior: good
Auswaschung: 4,3 % VerlustWashout: 4.3% loss
Dabei wurde wie folgt verfahren, daß die Dispersion vorgelegt wurde, dann ein Teil des Polybutens, das Ethylenoxidaddukt, das Konservie¬ rungsmittel, der Weichmacher und das Wasser sowie das Lösungsmittel innig miteinander vermischt wurden. Der andere Teil des Polybutens wurde im Verhältnis von 3 : 1 mit der Hydroxyethylcellulose
aufgeschlämmt und ebenfalls zugegeben und untergemischt und 5 Minu¬ ten gerührt. Anschließend wurde die Kreide und das Titandioxid ein¬ gearbeitet und 10 Minuten nachgerührt. Nach Zugabe des Ammoniaks wurde nochmals 15 Minuten unter Vakuum bei 40 mbar glattgerührt..The procedure was as follows, that the dispersion was introduced, then part of the polybutene, the ethylene oxide adduct, the preservative, the plasticizer and the water and the solvent were intimately mixed with one another. The other part of the polybutene was 3: 1 with the hydroxyethyl cellulose slurried and also added and mixed in and stirred for 5 minutes. The chalk and the titanium dioxide were then worked in and stirred for 10 minutes. After the ammonia had been added, stirring was continued for a further 15 minutes under vacuum at 40 mbar.
Beispiel 17Example 17
Es wurde eine Zusammensetzung gemäß Beispiel 1 hergestellt, wobei anstelle der dort beschriebenen Natrosol 250 HHR Type eine nicht- retardierte hochviskose Hydroxyethylcellulose ansonsten gleicher Spezifikation eingesetzt wurde (Handelsname Natrosol 250 HH)A composition according to Example 1 was produced, a non-retarded, highly viscous hydroxyethyl cellulose, otherwise of the same specification, being used instead of the Natrosol 250 HHR type described there (trade name Natrosol 250 HH).
Verarbeitbarkeit nach DIN 52456: 2300 g/min Glättverhalten: gutProcessability according to DIN 52456: 2300 g / min Smoothing behavior: good
Auswaschung: 1 % Verlust.Washout: 1% loss.
Vergleichsversuch CComparative experiment C
a) Beispiel 12 wurde unter Weglassung dera) Example 12 was omitted
Hydroxyethylcellulose wiederholt:Hydroxyethyl cellulose repeats:
23 % Auswaschung23% washout
b) Beispiel 12 wurde wiederholt, wobei anstelle derb) Example 12 was repeated, using instead of
Hydroxyethylcellulose Carboxylmethylcellulose (DS 0,8, Vis¬ kosität 400 mPas in 2 %-iger, wäßriger Lösung bei 20 °C ein¬ gesetzt wurden:Hydroxyethylcellulose Carboxylmethylcellulose (DS 0.8, viscosity 400 mPas in 2% aqueous solution at 20 ° C were used:
27 % Auswaschung27% washout
c) Beispiel 15 wurde unter Weglassung vonc) Example 15 was omitted from
Hydroxyethylcellulose wiederholt:Hydroxyethyl cellulose repeats:
20 % Auswaschung.
20% washout.
Claims
1. Frühregenfeste Fugendichtungsmassen enthaltend1. Containing early rainproof joint sealants
- wäßrige Polymerdispersionen (I)- aqueous polymer dispersions (I)
- nicht-ionische Celluloseether (II) aus der von Hydroxyethyl-, Hydroxyethyimethyl-, Hydroxypropylmethyl- und Hydroxypropyl¬ cellulose gebildeten Gruppe- Non-ionic cellulose ethers (II) from the group formed by hydroxyethyl, hydroxyethylimethyl, hydroxypropylmethyl and hydroxypropyl cellulose
- gegebenenfalls übliche Zusätze wie Füllstoffe, Pigmente, Weichmacher, Extender, Verdickungsmittel, Entschäumer, Dis- pergierhilfs ittel, pH-Regulatoren, Konservierungs- und Alte¬ rungsschutzmittel sowie- If necessary, conventional additives such as fillers, pigments, plasticizers, extenders, thickeners, defoamers, dispersing aids, pH regulators, preservatives and preservatives and
- mindestens eine organische flüssige Komponente aus der Gruppe üblicher Zusätze und herstellbar durch inniges Vermengen von (I) mit den übrigen Bestandteilen, dadurch gekennzeichnet, daß (II) in retardierter und/oder nicht retardierter Form in der flüssigen organischen Komponente aufgeschlämmt zugegeben und untergemischt wird.- At least one organic liquid component from the group of conventional additives and which can be prepared by intimately mixing (I) with the other constituents, characterized in that (II) is added in slurried and / or non-retarded form in the liquid organic component and mixed in .
2. Fugendichtungsmassen nach Anspruch 1, dadurch gekennzeichnet, daß sie Dispersionen von zur Filmbildung befähigten Polyacry- laten und/oder Acrylatcopolymeren enthalten.2. Joint sealing compounds according to claim 1, characterized in that they contain dispersions of polyacrylicates capable of film formation and / or acrylate copolymers.
3. Fugendichtungsmassen nach Anspruch 1, dadurch gekennzeichnet, daß sie Dispersionen von zur Filmbildung befähigten Polymeren bzw. Copolymeren ausgewählt aus der von Ethylen/Vinylacetat-, Butadien/Styrol-, Vinylacetat/Maleinsäureester-, Silikon-, Ure- than-, Vinylacetatmethacrylsäure/Chloropren- und Isopren-Poly¬ meren bzw. -Copolymeren gebildeten Gruppe enthält. 3. Joint sealing compounds according to claim 1, characterized in that they selected dispersions of film-forming polymers or copolymers selected from that of ethylene / vinyl acetate, butadiene / styrene, vinyl acetate / maleic acid ester, silicone, urethane, vinyl acetate methacrylic acid / Contains chloroprene and isoprene polymers or copolymers.
4. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß sie eine wäßrige Dispersion von Poly- sulfidpolymeren enthalten.4. Joint sealing compounds according to one of the preceding claims, characterized in that they contain an aqueous dispersion of polysulfide polymers.
5. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß die wäßrigen Polymer- bzw. Copolymer- dispersioneπ Feststoffgehalte von 40 bis 75 Gew.-%, insbesondere von von 45 bis 65 Gew.-% aufweisen.5. Joint sealing compounds according to one of the preceding claims, characterized in that the aqueous polymer or copolymer dispersions have solids contents of 40 to 75% by weight, in particular 45 to 65% by weight.
6. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß Celluloseether enthalten sind, die in 2%-iger wäßriger Lösung bei 20°C Viskositäten nach Brookfield von mindestens 5000, insbesondere mindestens 25.000, vorzugs¬ weise mindestens 70.000 mPas aufweisen.6. Joint sealing compounds according to one of the preceding claims, characterized in that cellulose ethers are contained which, in 2% strength aqueous solution at 20 ° C., have Brookfield viscosities of at least 5000, in particular at least 25,000, preferably at least 70,000 mPas.
7. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß das Verhältnis von Celluloseethern zu freiem Wasser so gewählt ist, daß eine vollständige Lösung der Celluloseether nicht mehr zu erzielen ist.7. Joint sealing compounds according to one of the preceding claims, characterized in that the ratio of cellulose ethers to free water is selected such that a complete solution of the cellulose ethers can no longer be achieved.
8. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß sie8. Joint sealing compounds according to one of the preceding claims, characterized in that they
25 - 90 Gew.-% Polymerdispersion, bei hochgefüllten Fugendichtungsmassen insbesondere25 - 90% by weight polymer dispersion, especially for highly filled joint sealants
25 - 40 -Gew.-% Polymerdispersion,25-40% by weight polymer dispersion,
0 - 60 Gew.-% insbesondere 2 bis 60 Gew.-% Füllstoffe0 - 60 wt .-% in particular 2 to 60 wt .-% fillers
0 - 1 Gew.-% insbesondere 0,3 bis 0,5 Gew.-% Netzmittel0 - 1 wt .-% in particular 0.3 to 0.5 wt .-% wetting agent
0 - 20 Gew.-% insbesondere 5 bis 15 Weichmacher und bis zu0-20% by weight, in particular 5 to 15 plasticizers and up to
10 Gew.-% insbesondere 4 bis 6 Gew.-% weitere übliche10% by weight, in particular 4 to 6% by weight, of other conventional
Zusätze wie Verdickungsmittel, Entschäumer und Pigmente mindestens zum Aufschlämmen der Celluloseether ausreichende Men¬ gen an organischer flüssiger Komponente und bis zu 1,5 Gew.-% CelluloseetherAdditives such as thickeners, defoamers and pigments sufficient quantities of organic liquid component and up to 1.5% by weight of cellulose ether at least to slurry the cellulose ethers
- Gew.-%-Angaben jeweils bezogen auf die Gesamtmenge - enthalten.-% by weight - information based on the total amount.
9. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß bei deren Herstellung die Cellulose¬ ether in aufgeschlämmter Form in einem Verhältnis von 1 : 2 bis 1 : 4, insbesondere etwa 1 : 3, zu der flüssigen Komponente der Aufschlämmung eingesetzt werden.9. Joint sealing compounds according to one of the preceding claims, characterized in that the cellulose ethers used in their slurry form in a ratio of 1: 2 to 1: 4, in particular about 1: 3, to the liquid component of the slurry in their manufacture become.
10. Fugendichtungsmassen nach einem der vorstehenden Ansprüche, da¬ durch gekennzeichnet, daß bei deren Herstellung die Zugabe der pH-Regulatoren, insbesondere Basen, nach Zugabe der Cellulose¬ ether erfolgt.10. Joint sealing compounds according to one of the preceding claims, characterized in that, during their manufacture, the pH regulators, in particular bases, are added after the addition of the cellulose ethers.
11. Verfahren zur Herstellung von Fugendichtungsmassen nach vorste¬ henden Ansprüchen, dadurch gekennzeichnet, daß die Polymerdi¬ spersion vorgelegt wird, die üblichen Zusätze mit Ausnahme der pH-Regulatoren untergemischt werden, dann die Vermischung mit den in der flüssigen organischen Komponente z.B. im Weichmacher aufgeschlämmten Celluloseether erfolgt und nach anschließendem Untermischen der Füllstoffe die Zumischung der pH-Regulatoren erfolgt.11. A process for the preparation of jointing compounds according to the preceding claims, characterized in that the polymer dispersion is presented, the usual additives with the exception of the pH regulators are mixed in, then the mixing with those in the liquid organic component, e.g. Slurried cellulose ether in the plasticizer and after the fillers have been mixed in, the pH regulators are added.
12. Verfahren zur Herstellung von Fugendichtungsmassen nach Anspruch 11, dadurch gekennzeichnet, daß die Zugabe des Füllstoffs nach der Zugabe des pH-Regulators erfolgt. 12. A method for producing joint sealants according to claim 11, characterized in that the addition of the filler takes place after the addition of the pH regulator.
13. Verwendung der Fugendichtungsmassen als solche insbesondere in Bereichen, in denen die Fugendichtungsmassen Spritzwasser oder Regen ausgesetzt sein können. 13. Use of the joint sealants as such, particularly in areas in which the joint sealants can be exposed to splashing water or rain.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3934870A DE3934870C2 (en) | 1989-10-19 | 1989-10-19 | Joint sealant or coating compositions based on aqueous polymer dispersions and use of nonionic cellulose ethers as additives to these compositions |
| DE3934870 | 1989-10-19 | ||
| DE19904024551 DE4024551A1 (en) | 1990-08-02 | 1990-08-02 | Joint sealants with early resistance to rain-water |
| DE4024551 | 1990-08-02 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0541541A1 true EP0541541A1 (en) | 1993-05-19 |
Family
ID=25886257
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP90119449A Pending EP0423612A1 (en) | 1989-10-19 | 1990-10-10 | Rapid rain-resistant grouting mass |
| EP90914905A Withdrawn EP0541541A1 (en) | 1989-10-19 | 1990-10-10 | Joint sealants with early water resistance |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP90119449A Pending EP0423612A1 (en) | 1989-10-19 | 1990-10-10 | Rapid rain-resistant grouting mass |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US5118731A (en) |
| EP (2) | EP0423612A1 (en) |
| JP (1) | JPH05501271A (en) |
| KR (1) | KR920702399A (en) |
| CN (1) | CN1051052A (en) |
| BR (1) | BR9007753A (en) |
| CA (1) | CA2070638C (en) |
| MX (1) | MX172030B (en) |
| WO (1) | WO1991005826A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4224044A1 (en) * | 1992-07-21 | 1994-01-27 | Bostik Gmbh | Early rainproof sealant based on aqueous acrylic dispersions and process for their production |
| KR20000072715A (en) * | 2000-09-21 | 2000-12-05 | 홍승익 | The manufacturing method of waterproofing mortar for EIFS construction work |
| PL1947070T3 (en) * | 2005-11-09 | 2019-05-31 | Yoshino Gypsum Co | A wall, a partition, a ceiling or a floor comprising gypsum boards for shielding radioactive rays |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1284007B (en) * | 1963-10-16 | 1968-11-28 | Wacker Chemie Gmbh | Paints containing aqueous dispersions of organopolysiloxanes and organic resins |
| GB1354436A (en) * | 1971-02-22 | 1974-06-05 | Hoechst Ag | Alkyd resin-modified dispersions |
| DE2415556C3 (en) * | 1974-03-30 | 1982-09-09 | Henkel KGaA, 4000 Düsseldorf | Process for the production of high molecular weight substances treated with glyoxal |
| DE3814078A1 (en) * | 1988-04-26 | 1989-11-09 | Henkel Kgaa | USE OF NONTIONAL CELLULOSE ETHERS IN JOINT DENSITY AND / OR COATING MATERIALS |
-
1990
- 1990-10-10 EP EP90119449A patent/EP0423612A1/en active Pending
- 1990-10-10 JP JP2513897A patent/JPH05501271A/en active Pending
- 1990-10-10 CA CA002070638A patent/CA2070638C/en not_active Expired - Lifetime
- 1990-10-10 BR BR909007753A patent/BR9007753A/en not_active Application Discontinuation
- 1990-10-10 EP EP90914905A patent/EP0541541A1/en not_active Withdrawn
- 1990-10-10 KR KR1019920700894A patent/KR920702399A/en not_active Application Discontinuation
- 1990-10-10 WO PCT/EP1990/001700 patent/WO1991005826A1/en not_active Application Discontinuation
- 1990-10-17 CN CN90108466A patent/CN1051052A/en active Pending
- 1990-10-17 MX MX022887A patent/MX172030B/en unknown
- 1990-10-19 US US07/600,454 patent/US5118731A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| See references of WO9105826A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1991005826A1 (en) | 1991-05-02 |
| CA2070638A1 (en) | 1991-04-20 |
| US5118731A (en) | 1992-06-02 |
| JPH05501271A (en) | 1993-03-11 |
| KR920702399A (en) | 1992-09-04 |
| CA2070638C (en) | 1994-09-13 |
| BR9007753A (en) | 1992-08-11 |
| MX172030B (en) | 1993-11-29 |
| CN1051052A (en) | 1991-05-01 |
| EP0423612A1 (en) | 1991-04-24 |
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