EP3414301A1 - Brandschutzgel - Google Patents
BrandschutzgelInfo
- Publication number
- EP3414301A1 EP3414301A1 EP17705010.1A EP17705010A EP3414301A1 EP 3414301 A1 EP3414301 A1 EP 3414301A1 EP 17705010 A EP17705010 A EP 17705010A EP 3414301 A1 EP3414301 A1 EP 3414301A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fire protection
- protection gel
- carboxylic acids
- unsaturated carboxylic
- gel according
- 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- Withdrawn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
- 230000004224 protection Effects 0.000 title claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 19
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 150000001735 carboxylic acids Chemical class 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 12
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 150000003254 radicals Chemical class 0.000 claims description 9
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 8
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 8
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- -1 alkali metal salt Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- UZFMOKQJFYMBGY-UHFFFAOYSA-N 4-hydroxy-TEMPO Chemical group CC1(C)CC(O)CC(C)(C)N1[O] UZFMOKQJFYMBGY-UHFFFAOYSA-N 0.000 claims description 5
- 239000004971 Cross linker Substances 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- 125000001931 aliphatic group Chemical group 0.000 claims description 5
- 125000004386 diacrylate group Chemical group 0.000 claims description 5
- 230000003287 optical effect Effects 0.000 claims description 5
- NYUTUWAFOUJLKI-UHFFFAOYSA-N 3-prop-2-enoyloxypropane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCOC(=O)C=C NYUTUWAFOUJLKI-UHFFFAOYSA-N 0.000 claims description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims description 4
- 229960003237 betaine Drugs 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- 230000006750 UV protection Effects 0.000 claims description 3
- 239000002318 adhesion promoter Substances 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 2
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- KFNGWPXYNSJXOP-UHFFFAOYSA-N 3-(2-methylprop-2-enoyloxy)propane-1-sulfonic acid Chemical compound CC(=C)C(=O)OCCCS(O)(=O)=O KFNGWPXYNSJXOP-UHFFFAOYSA-N 0.000 claims description 2
- BYLRZCIZXYKLQL-UHFFFAOYSA-N 3-[3-(3-sulfopropoxycarbonyl)but-3-enoyloxy]propane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCOC(=O)CC(=C)C(=O)OCCCS(O)(=O)=O BYLRZCIZXYKLQL-UHFFFAOYSA-N 0.000 claims description 2
- BCAIDFOKQCVACE-UHFFFAOYSA-N 3-[dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azaniumyl]propane-1-sulfonate Chemical compound CC(=C)C(=O)OCC[N+](C)(C)CCCS([O-])(=O)=O BCAIDFOKQCVACE-UHFFFAOYSA-N 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 125000005336 allyloxy group Chemical group 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 235000011148 calcium chloride Nutrition 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000011814 protection agent Substances 0.000 claims description 2
- 159000000000 sodium salts Chemical class 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 7
- 235000011147 magnesium chloride Nutrition 0.000 claims 1
- 239000003223 protective agent Substances 0.000 claims 1
- 239000000499 gel Substances 0.000 abstract description 39
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 239000003999 initiator Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000017 hydrogel Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 150000003841 chloride salts Chemical class 0.000 description 3
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 2
- 230000003505 mutagenic effect Effects 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 231100001260 reprotoxic Toxicity 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- HJIAMFHSAAEUKR-UHFFFAOYSA-N (2-hydroxyphenyl)-phenylmethanone Chemical class OC1=CC=CC=C1C(=O)C1=CC=CC=C1 HJIAMFHSAAEUKR-UHFFFAOYSA-N 0.000 description 1
- ISDMPOQQGNAVDG-UHFFFAOYSA-N 1-phenylbenzotriazol-4-ol Chemical compound OC1=CC=CC=2N(N=NC=21)C1=CC=CC=C1 ISDMPOQQGNAVDG-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- VMRIVYANZGSGRV-UHFFFAOYSA-N 4-phenyl-2h-triazin-5-one Chemical class OC1=CN=NN=C1C1=CC=CC=C1 VMRIVYANZGSGRV-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- IYABWNGZIDDRAK-UHFFFAOYSA-N allene Chemical group C=C=C IYABWNGZIDDRAK-UHFFFAOYSA-N 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical class [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 description 1
- PMPJQLCPEQFEJW-HPKCLRQXSA-L disodium;2-[(e)-2-[4-[4-[(e)-2-(2-sulfonatophenyl)ethenyl]phenyl]phenyl]ethenyl]benzenesulfonate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=CC=CC=C1\C=C\C1=CC=C(C=2C=CC(\C=C\C=3C(=CC=CC=3)S([O-])(=O)=O)=CC=2)C=C1 PMPJQLCPEQFEJW-HPKCLRQXSA-L 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 229960002337 magnesium chloride Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000219 mutagenic Toxicity 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003873 salicylate 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
- FWFUWXVFYKCSQA-UHFFFAOYSA-M sodium;2-methyl-2-(prop-2-enoylamino)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(C)(C)NC(=O)C=C FWFUWXVFYKCSQA-UHFFFAOYSA-M 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical group OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
Definitions
- the present invention relates to a fire protection gel, its preparation and its use in fire-resistant glass.
- a disadvantage of the known acrylic acid derivative-based gels is the toxicity of the monomers which are classified as mutagenic, carcinogenic and / or reprotoxic. It was therefore the object to provide a fire protection gel which is just as effective but less toxic.
- dialdehyde-crosslinked polyvinyl alcohols in DE 38 38 806 C2 and organically modified alkali water glass DE 10 2006 035 262 A1.
- dialdehydes are also toxicologically problematic and organically modified
- Alkali water glass requires special UV protection.
- WO 00/65143 A1 and WO 2007/007115 A2 disclose hydrogels for medical applications which describe sulfonated carboxylic acid derivatives as monomers of hydrogels.
- a fire protection gel based on a polymer containing sulfonated derivatives of unsaturated aliphatic
- Carboxylic acids as monomers solves the task. These monomers and the polymers thereof are readily water soluble and the monomers become
- the invention therefore relates to fire protection gels comprising a polymer of one or more sulfonated derivatives of unsaturated aliphatic
- the invention further relates to a method for producing a fire protection gel, comprising the steps
- the monomers are esters or amides of aliphatic, unsaturated carboxylic acids substituted with an alkylsulfonic acid group.
- the carboxylic acid is in particular acrylic acid, methacrylic acid or itaconic acid.
- R 1 is H, methyl, ethyl, iso-propyl, n-propyl or 2-hydroxy-propyl, most preferably H and methyl.
- R 2 are methylene, ethylene or -CH 2 -CH 2 -CH 2 -, -CH (CH 3 ) -CH 2 -,
- the sulphonic acid group is present, except for betaines, as salt or ester, preferably as salt.
- Preferred salts are the alkali metal salts, especially the sodium salts and the potassium salts.
- the esters are short chain esters, i. Methyl, ethyl, propyl or butyl ester, preferably methyl or ethyl ester, to ensure the water solubility of the polymers. In principle, longer-chain esters would also be useful if the polymers are water-soluble.
- Particularly preferred monomers are acrylic acid (3-sulfopropyl) esters,
- Potassium salt available under the name Ralumer SPA from Raschig GmbH, DE
- 2-acrylamido-2-methylpropanesulfonic acid, sodium salt are methacrylic acid (3-sulfopropyl) ester, potassium salt (available under the name Ralumer SPM from Raschig GmbH, DE) and N, N-dimethyl-N- (2-methacryloxyethyl) -N- (3-sulfopropyl ) ammonium betaine (available under the name Ralumer SPE from Raschig GmbH, DE) advantageous.
- sulfonated ethers or polyethers based on allyl alcohol for example sodium 3- (allyloxy) -2-hydroxypropanesulfonate (available under the name Ralumer SPAE from Raschig GmbH, DE) and Polyethylene glycol allyl (3-sulfopropyl) diether, potassium salt (available under the name Ralumer SPPE from Raschig GmbH, DE).
- Useful gels contain from 5 to 30% by weight, preferably from 7.5 to 20% by weight and in particular from 10 to 15% by weight of polymerized monomers, based on the total weight of the fire protection gel.
- crosslinking agents for example poly (ethylene glycol) diacrylate (PEGDA), to the reaction solution.
- PEGDA poly (ethylene glycol) diacrylate
- the amount of crosslinker is preferably in the range of 0.1 to 1 wt .-%.
- the fire protection gels according to the invention preferably contain, like the known fire protection gels, one or more salts. These are usually chlorides, especially sodium chloride and magnesium chloride. These can be introduced according to the invention up to a total salt concentration of about 20% by weight, calculated as anhydrous salts. The optimal concentration depends on the ratio of the amounts of salt to each other. Other chlorides such as potassium chloride, calcium chloride or zinc chloride can also be used.
- the fire protection gel can also contain water-miscible alcohols, for example ethylene glycol, glycerol and / or isopropyl alcohol, which are known as typical antifreeze additives. A concentration of at most 10% by weight of alcohol is expedient. It is also the use of optical brighteners, UV protectants and / or dyes conceivable. As an optical brightener is about Tinopal CBS-X (BASF SE, DE) in question. UV protectants can be selected from known groups such as, for example, the salicylates, the hydroxybenzophenones, the
- Hydroxyphenylbenzotriazolen or hydroxyphenyltriazines are selected, provided that sufficient water solubility and no staining or turbidity of the gel occurs.
- the use of multiple UV protection agents is conceivable.
- the fire-retardant gel may have adhesion promoter, e.g. Silane coupling agent, contained in the usual amounts.
- adhesion promoter e.g. Silane coupling agent
- a preferred fire protection gel contains:
- a particularly preferred fire protection gel contains:
- the preparation according to the invention typically comprises, as a first step, the admixture of an aqueous solution containing from 20 to 60% by weight, preferably from 30 to 55% by weight and in particular about 50% by weight, of sulphonated derivatives of unsaturated carboxylic acids. If desired, the further components crosslinker and / or salt (s) are then added to the solution.
- the initiation of the polymerization is possible by typical free-radical initiators such as sodium persulfate.
- typical free-radical initiators such as sodium persulfate.
- the amount of radical generator is e.g. in case of
- a polymerization accelerator such as triethanolamine (TEA) can be used. Amounts of 0.01 to 0.5% by weight, especially 0.02 to 0.2% by weight, are useful. If no polymerization accelerator is used, temperatures of 50-70 ° C., preferably 55-65 ° C., are required. In the presence of a polymerization accelerator, the reaction can also be carried out at room temperature.
- TAA triethanolamine
- the polymerization is started by addition of the radical generator, if appropriate in admixture with the polymerization accelerator or after its addition, wherein the required temperature is to be observed.
- the polymerization usually takes a few minutes to a few hours, often from 15 to 60 minutes. To prevent premature polymerization during the preparation, transport or storage of the still containing no initiator
- Monomer solution is preferably added an inhibitor.
- a particularly preferred inhibitor is 4-hydroxy-2,2,6,6-tetramethyl-piperidine-1-oxyl, but also some aromatic compounds such as derivatives of phenol or hydroquinone have a stabilizing effect.
- several inhibitors can be used. The amounts are usually from 1 to 100 ppm, preferably 10 to 30 ppm per inhibitor. It should be noted that the
- the fire protection gel according to the invention comes as the known
- Fire protection gels usually as a filling between at least two
- the glass sheets may also be known per se, special, high-temperature resistant discs.
- the thickness of the panes and the fire protection gel layer corresponds to the usual dimensions of the respective fire resistance class. In case of fire, the gel cools the side of the pane facing away from the fire by evaporating water and also forms an insulating crust, at the latest when the pane facing the fire is no longer intact.
- Gelation must be sufficient here and can be adjusted by varying the amount of initiator and accelerator if necessary, taking into account the inhibitor used.
- the invention also relates to all combinations of preferred embodiments, as far as these are not mutually exclusive.
- the information "about” or “approx.” in conjunction with a numerical indication, means that at least 10% higher or lower values or 5% higher or lower values and in any case 1% higher or lower values are included.
- AMPS 2-acrylamido-2-methylpropanesulphonic acid
- demineralized water demineralized water
- 12.84 g of sodium hydroxide were added gradually and the pH was adjusted to 9.7 with another 2.41 g of 1 M sodium hydroxide solution.
- the yellowish-colored solution was then decolorized with 1.75 g of activated carbon ("1 wt .-% based on the solution) and stirred vigorously for one hour. The subsequent filtration caused a mass loss of 8.63 g, but the solution had only a slight yellowish hue.
- composition of the solution according to the weighings and taking into account the filtration loss was: 11, 6 wt .-% SPA, 1, 56 wt .-% PEGDA and 36.1 wt .-% Na-AMPS.
- Hydroquinone monomethyl ether in the range of 10 to 15 ppm.
- composition of the solution according to the weights and taking into account the filtration loss and the samples taken were: 11, 6 wt .-% SPA, 1, 55 wt .-% PEGDA, 36.7 wt .-% Na-AMPS.
- As a result of the raw materials used there was also a content of 13 ppm of the inhibitor hydroquinone monomethyl ether.
- Example 2 containing 11, 6 wt .-% SPA, 1, 55 wt .-% PEGDA, 36.7 wt .-% Na AMPS, examined and confirmed the effectiveness.
- Example 4 containing 11, 6 wt .-% SPA, 1, 55 wt .-% PEGDA, 36.7 wt .-% Na AMPS, examined and confirmed the effectiveness.
- Example 4 containing 11, 6 wt .-% SPA, 1, 55 wt .-% PEGDA, 36.7 wt .-% Na AMPS, examined and confirmed the effectiveness.
- Example 4 Example 4
- DI demineralised
- Polymerization inhibitor added to the solution.
- 2740 g of a 49.2% sodium hydroxide solution were metered in slowly via the dropping funnel, the temperature of the solution not exceeding 30 ° C.
- a pH of 9.6 was set.
- 2440 g of SPA were added with stirring.
- the solution thus obtained was stirred with 103 g of activated carbon for two hours at a temperature of 20 to 25 ° C.
- 20420 g of the solution were present. This still 319.6 PEGDA were added and adjusted with 14.0 g of a 25% sodium hydroxide solution to a pH of 7.5.
- composition of the solution according to the HPLC analysis was 37.8% Na-AMPS, 12.1% SPA and 1.42% PEGDA.
- the content of 4-hydroxy TEMPO corresponding to the initial weight was 25 ppm.
- hydrogels were prepared from a monomer solution prepared only in 2 L scale according to Example 4. To this was dissolved in 25.84 g of this solution, 30.00 g of magnesium chloride hexahydrate and 2.50 g of sodium chloride and diluted with 35.00 g of water. The solution was then degassed for one hour at room temperature and a pressure of about 50 mbar in a vacuum oven. The resulting loss of water of 380 mg was compensated by adding new demineralised water. The solution was then overlaid with argon and then the initiator solution of 0.035 g of sodium persulfate, 0.1 g of triethanolamine and 6.53 g of water was added.
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Abstract
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DE102016201857 | 2016-02-08 | ||
PCT/EP2017/000108 WO2017137148A1 (de) | 2016-02-08 | 2017-01-30 | Brandschutzgel |
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EP3414301A1 true EP3414301A1 (de) | 2018-12-19 |
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Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2346548A1 (fr) | 1976-03-30 | 1977-10-28 | Saint Gobain | Vitrage multiple anti-feu, comportant une couche intercalaire de gel |
DE3530968A1 (de) | 1985-08-30 | 1987-03-12 | Ver Glaswerke Gmbh | Feuerwiderstandsfaehige verglasung |
FR2624546B1 (fr) | 1987-12-15 | 1993-11-26 | Saint Gobain Vitrage | Vitrage antifeu et procede de fabrication |
GB9909349D0 (en) | 1999-04-23 | 1999-06-16 | First Water Ltd | Process |
US20040057986A1 (en) * | 2001-03-30 | 2004-03-25 | The Procter & Gamble Company | Polymerized hydrogel adhesives comprising low amounts of residual monomers |
DE10237395B4 (de) | 2002-01-24 | 2012-12-20 | C. G. I. International Limited | Verfahren zur Herstellung einer Brandschutzverglasung und Brandschutzverglasung |
GB0403510D0 (en) * | 2004-02-18 | 2004-03-24 | Mantra Internat Ltd | Bioadhesive compositions and their use in medical electrodes |
DE102005018842B4 (de) | 2005-04-22 | 2017-05-11 | Hero-Glas Veredelungs Gmbh | Polymerisierbare Zusammensetzung zum Herstellen eines Hydrogels, Hydrogel sowie Verwendung des Hydrogels |
WO2007007115A2 (en) | 2005-07-14 | 2007-01-18 | First Water Limited | Treatment of chronic ulcerous skin lesions |
DE102006035262A1 (de) | 2006-07-29 | 2008-01-31 | Schott Ag | UV-undurchlässige Brandschutzverglasung |
EP2234653B1 (de) * | 2008-01-17 | 2014-07-30 | First Water Limited | Hydrogel-copolymer-zusammensetzung und verwendungen davon, z. b. als wundverband |
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2017
- 2017-01-30 EP EP17705010.1A patent/EP3414301A1/de not_active Withdrawn
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