WO2017071984A1 - Granulate, verfahren zu ihrer herstellung und ihre verwendung - Google Patents
Granulate, verfahren zu ihrer herstellung und ihre verwendung Download PDFInfo
- Publication number
- WO2017071984A1 WO2017071984A1 PCT/EP2016/074920 EP2016074920W WO2017071984A1 WO 2017071984 A1 WO2017071984 A1 WO 2017071984A1 EP 2016074920 W EP2016074920 W EP 2016074920W WO 2017071984 A1 WO2017071984 A1 WO 2017071984A1
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- Prior art keywords
- range
- alkyl
- general formula
- coom
- weight
- Prior art date
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- 239000008187 granular material Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 4
- 238000000034 method Methods 0.000 title claims description 30
- -1 alkali metal citrate Chemical class 0.000 claims abstract description 48
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 19
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 18
- 238000009472 formulation Methods 0.000 claims abstract description 13
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims abstract description 6
- 150000008041 alkali metal carbonates Chemical class 0.000 claims abstract description 6
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims abstract description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 238000002844 melting Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 13
- 238000004851 dishwashing Methods 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 239000003599 detergent Substances 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 8
- 239000002738 chelating agent Substances 0.000 claims description 5
- 239000002671 adjuvant Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005029 sieve analysis Methods 0.000 claims description 4
- 150000004760 silicates Chemical class 0.000 claims description 4
- 238000011156 evaluation Methods 0.000 claims description 3
- 235000010603 pastilles Nutrition 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 229920000388 Polyphosphate Polymers 0.000 claims 1
- 235000021317 phosphate Nutrition 0.000 claims 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 1
- 239000001205 polyphosphate Substances 0.000 claims 1
- 235000011176 polyphosphates Nutrition 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 abstract 1
- 239000013522 chelant Substances 0.000 abstract 1
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical group O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 239000011734 sodium Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 150000002170 ethers Chemical class 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 4
- 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 description 4
- 229920001400 block copolymer Polymers 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 4
- 239000007937 lozenge Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000003826 tablet Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 2
- 125000003542 3-methylbutan-2-yl group Chemical group [H]C([H])([H])C([H])(*)C([H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000001033 granulometry Methods 0.000 description 2
- 239000008240 homogeneous mixture Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 2
- 229920006030 multiblock copolymer Polymers 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 2
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229920005604 random copolymer Polymers 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- KKVZONPEMODBBG-UHFFFAOYSA-N (1-hydroxydodecane-1,1-diyl)bis(phosphonic acid) Chemical compound CCCCCCCCCCCC(O)(P(O)(O)=O)P(O)(O)=O KKVZONPEMODBBG-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- PMYUVOOOQDGQNW-UHFFFAOYSA-N hexasodium;trioxido(trioxidosilyloxy)silane Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] PMYUVOOOQDGQNW-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/08—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with fatty acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
- C11D1/721—End blocked ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/825—Mixtures of compounds all of which are non-ionic
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
- C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
- C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3707—Polyethers, e.g. polyalkyleneoxides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
Definitions
- the present invention relates to a process for preparing a formulation which is solid up to a temperature of at least 60 ° C, characterized in that
- R 1 is selected from C 4 -C 20 -alkyl
- R 2 is selected from C 8 -C 20 -alkyl
- AO are in each case identical or different and selected from C 2 -C 4 -alkylene
- x is in the range of 5 to 100
- R 3 is -CH (COOM 1 ) -N (CH 2 COOM 1 ) 2 (II) in which the variables are defined as follows:
- R 3 is selected from C 1 -C 4 -alkyl, phenyl, benzyl, CH 2 OH and CH 2 CH 2 COOM 1 ,
- M 1 is an alkali metal or a combination of at least two alkali metals, mixed in a mill and ground.
- the present invention relates to granules and their use.
- hydroxy mixed ethers are waxy-looking substances with a melting point below 60 ° C, below 50 ° C or even below 35 ° C. They are able to form supercooled melts, which show only a slight tendency to crystallize even after a long time. Some hydroxymix ethers are hygroscopic and, moreover, especially with small particle size, tend to stick. Although it is possible to improve the storage stability by adding a so-called anti-caking agent. However, these are in many cases incompatible with other ingredients of dishwasher formulations.
- Solid formulations for example powder granules containing hydroxy mixed ethers, may tend to stick or cake in some cases. With powders or granules serving as intermediates, such sticking or caking will make further processing difficult. In the case of powders or granules which serve as end products, that is to be delivered to the consumer, such sticking or baking leads to negative feedback.
- the process according to the invention is a process for the preparation of a formulation which is solid up to a temperature of at least 60 ° C.
- DSC differential scanning calorimetry
- the melting point for example by differential scanning calorimetry (DSC), advantageously with a heating rate of 10K / min ⁇ 1 K / min; Initial weight 6-7 mg; Purge gas 3 l IS / h, AI crucible, open).
- the method according to the invention comprises several steps.
- the method according to the invention is based on at least one nonionic surfactant of the general formula (I) which, in connection with the present invention, can also be called component (a),
- R is -CH (OH) -CH 2 - (AO) x R 2 (I) in which the variables are defined as follows:
- R 1 is selected from C 4 -C 20 -alkyl, preferably n-C 4 -C 20 -alkyl.
- Examples are n-butyl, sec-butyl, isobutyl, n-pentyl, isopentyl, sec-pentyl, neo-pentyl, 1,2-dimethylpropyl, iso-amyl, n-hexyl, iso-hexyl, sec-hexyl, n-heptyl, n-octyl, 2-ethylhexyl, n-nonyl, n-decyl, n-dodecyl, iso-dodecyl, n-tetradecyl, iso-tetradecyl, stearyl, palmityl, and n-eicosyl.
- Preferred examples are n-butyl, n-pentyl, iso-pentyl, n-hexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, n-dodecyl, n-tetradecyl, stearyl, palmityl, and n- eicosyl.
- Particularly preferred examples are n-octyl and n-decyl.
- R 2 is selected from C 8 -C 20 -alkyl, preferably n-C 2 -C 20 -alkyl, examples being n-octyl,
- Preferred examples are n-octyl, n-nonyl, n-decyl, n-undecyl, iso-Cn H23, n-dodecyl, is-dodecyl, n-tetradecyl, stearyl, palmityl and n-eicosyl.
- Particularly preferred examples are iso-Cn H 2 3-
- AO are each the same or different and selected from C 2 -C 4 -alkylene, for example
- AO is in each case identical and CH 2 -CH 2 -O, in short also "EO" x is in the range from 5 to 100, preferably 5 to 60, more preferably 10 to 50 and particularly preferably 20 to 40.
- (AO) x is selected from (CH 2 CH 2 O) xi, where x1 is in the range of 1 to 50.
- (AO) x is selected from
- (AO) x is selected from - (CH 2 CH 2 O) x 4 wherein x 4 is in the range of 10 to 50, AO is EO, and R 1 and R 2 are each selected from Ce-Cu-alkyl become.
- x, x1, x2, x3, x4 are each to be understood as average values, the number average being preferred. Therefore, x or x1 or x2 or x3 or x4, if present, may be a non-integer although individual molecules each have an integer number of AO units.
- R 1 is n-Cs-C-io-alkyl
- R 2 is Cs-C 12 -alkyl, straight-chain or iso-Cs-C 12 -alkyl
- x is in the range of 20 to 25.
- component (a) has a melting point in the range of 30 to 60 ° C, preferably 35 to 55 ° C.
- the melting point of component (a) can be measured as mentioned above.
- Component (a) is mixed with (B) at least one second substance, in the context of the present invention also called component (b), and which is selected from polyethylene glycol and nonionic surfactants, which are different from surfactants of the formula (I).
- polyethylene glycol are polyaddition products of ethylene oxide having an average molecular weight M w in the range of 1 .000 to 50,000 g / mol, preferably 2,000 to 20,000 g / mol.
- nonionic surfactants other than component (a) are alcohol alkoxylates, di- and multiblock copolymers of ethylene oxide and propylene oxide, and reaction products of sorbitan with ethylene oxide or propylene oxide, and also alkyl glycosides.
- alkoxylated alcohols and alkoxylated fatty alcohols are, for example, compounds of the general formula (III)
- R 4 is selected from linear C 1 -C 4 -alkyl, preferably ethyl and more preferably methyl,
- R 5 selected from Cs-C22-alkyl, for example n-CsHiz, n-CioF i, n-Ci2H25, n-Ci4H29, n-Ci6H33
- R 6 is selected from C 1 -C 10 -alkyl, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, isopentyl, sec. -Pentyl, neo-pentyl, 1, 2-dimethylpropyl, iso-amyl, n-
- Hexyl, iso -hexyl, sec-hexyl, n-heptyl, n-octyl, 2-ethylhexyl, n-nonyl, n-decyl or iso-decyl, m and n are in the range of zero to 300, the sum of n and m is at least one.
- m is in the range of 1 to 100 and n is in the range of 0 to 30.
- Compounds of the general formula (I) may be block copolymers or random copolymers, preference being given to block copolymers.
- Other preferred examples of alkoxylated alcohols and alkoxylated fatty alcohols are, for example, compounds of the general formula (IV) where the variables are defined as follows:
- R 4 is identical or different and selected from linear C 1 -C 4 -alkyl, preferably in each case identical and ethyl and particularly preferably methyl,
- R 7 is selected from C 6 -C 20 -alkyl, in particular n-CeHi 7, n-CioH 2 i, n-Ci 2 H 2 5, n-Ci4H 2 9, n-Ci6H 3 3,
- a is a number in the range of 1 to 6
- b is a number in the range of 4 to 20
- d is a number in the range of 4 to 25.
- these may be block copolymers or random copolymers, preference being given to block copolymers.
- suitable nonionic surfactants are selected from di- and multiblock copolymers, composed of ethylene oxide and propylene oxide.
- suitable nonionic surfactants are selected from ethoxylated or propoxylated sorbitan esters and isosorbitol esters.
- Further suitable nonionic surfactants are selected from di-fatty acid esters of polyethylene glycol, for example polyethyleneglycol esterified twice with stearic acid and having an average molecular weight M w in the range from 1500 to 2500 g / mol.
- alkyl polyglycosides are compounds of the general formula (VI)
- R 8 is hydrogen or C 1 -C 4 -alkyl, preferred are ethyl, n-propyl and isopropyl and also hydrogen,
- R 9 is - (CH 2 ) 2 -R 8
- G 1 is selected from monosaccharides having 4 to 6 carbon atoms, in particular glucose and xylose, w is in the range of 1, 1 to 4, w being an average, in particular the number average.
- w is in the range of 1.1 to 2, and more preferably in the range of 1.2 to 1.8. It is preferred to determine w by high temperature gas chromatography (HTGC).
- HTGC high temperature gas chromatography
- component (b) has a melting point in the range of 35 to 70 ° C, preferably 50 to 65 ° C.
- the melting point of component (b) can also be measured by dynamic DSC.
- the melting point of component (a) is below that of component (b).
- component (a) and (b) are first mixed in the molten state.
- the temperature for mixing is chosen so that the lower-melting component - ie component (b) or preferably component (a) - is in the molten state.
- the higher melting component may be in the solid or molten state.
- Component (a) and component (b) are preferably mixed in the proportions intended for the formulation in question.
- component (a) is melted during mixing.
- Component (a) and component (b) are preferably mixed at a temperature which is at least 5 ° C. above the melting point of component (a), more preferably at least 10 ° C.
- component (a) and component (b) are mixed at a temperature at least 5 ° C above the temperature at which the higher melting component melts.
- mixing process one can proceed by introducing components (a) and (b) in solid form in a mixing vessel and heating with mixing, for example shaking or preferably with stirring, until the lower-melting component has melted. Thereafter, the mixing is continued until you perceive with unaided eye a homogeneous mixture, so neither separate particles nor streaks can recognize.
- suitable mixing vessels are stirred vessels such as stirred reactors and stirred tanks.
- the mixture obtained in the first step of the process according to the invention is prepared.
- this is understood to mean that the mixture from the first step is processed so that it is converted into solid particles having the desired dimensions.
- Preferred examples are pastilles, flakes, grindings, and combinations of at least two of the foregoing. If it is desired to ground the mixture obtainable in the first step of the process according to the invention, they are allowed to solidify first.
- Pastillation can be carried out, for example, by pouring a mixture obtained in the first step of the process according to the invention into a mold with corresponding wells and allowing the mixture to cool in the appropriate mold. Then remove the cooled mixture - just the lozenges - from the mold and poured again mixture into the mold.
- cooling belts are selected for pastillation.
- Pastilles may for example have a diameter in the range of 4 to 10 mm.
- Scaling can be done, for example, by using a flaking roller. The size of the flakes may vary depending on the product characteristics and the machine settings. As a rule, irregularly shaped scales are obtained. As average dimensions, for example, lengths in the range of 1 mm to 2 cm, widths of 1 mm to 1, 5 cm and thicknesses in the range of 0.5 mm to 3 mm are suitable.
- Examples of particularly suitable equipment for grinding are impact mills and cutting mills. When mixing in a mill you grind simultaneously.
- silicic acid or silicate in the context of the present invention also silica (c) or silicate (c) or more generally called component (c), and
- component (d) at least one auxiliary, also referred to as auxiliary (d) or component (d), wherein component (d) is selected from alkali metal citrate, for example trisodium citrate, alkali metal carbonate such as potassium carbonate or sodium carbonate, or at least one chelating agent, selected from compounds of general formula (II) R 3 -CH (COOM) -N (CH 2 COOM) 2 (II) in which the variables are defined as follows:
- R 3 is selected from C 1 -C 4 -alkyl, for example methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, preferred are methyl, sec-butyl and isobutyl and very particularly preferably R 3 Methyl; furthermore phenyl, benzyl, CH 2 OH and CH 2 CH 2 COOM 1 , M 1 is an alkali metal or a combination of at least two alkali metals, for example lithium, sodium, potassium, preferred are potassium, sodium and combinations of potassium and sodium, for example in a molar ratio in the range of 1: 2 to 2: 1, and most preferably M 1 is sodium.
- Silica (c) can be selected from precipitated silicas and fumed silicas.
- silicates (c) are sodium disilicate and sodium metasilicate, zeolites and phyllosilicates, especially those of the formula a-Na 2 Si 2 0s, ⁇ -Na 2 Si 2 0s and 5-Na 2 Si 2 0s.
- the auxiliary (c) used is either two different silica gels or two different silicates. Different silica gels or different silicates can each differ in particle size, surface acidity or crystal structure.
- the auxiliary (c) used is a silica and a silicate.
- silica (c) has a mean particle diameter (volume average) in the range from 5 to 100 ⁇ m, preferably from 5 ⁇ m to at most 20 ⁇ m, determined by laser diffraction according to ISO 13320-1 (2009). In one embodiment of the present invention, silicate (c) has an average particle diameter (volume average) in the range of 5 ⁇ to at most 20 ⁇ , determined by laser diffraction according to ISO 13320-1 (2009).
- mills for the third step of the process according to the invention are selected from mills having a relatively low energy input. Preference is given to impact and cutting mills.
- the proportion of component (b) is at least as high as the proportion of nonionic surfactant of general formula (I).
- the proportions for the process according to the invention are selected as follows:
- (C) a total of 1 to 5 wt .-% silica or silicate, preferably 2 to 3 wt .-%, and
- component (d) overall in the range of from 40 to 70% by weight of component (d), preferably from 42 to 60% by weight.
- Granules obtainable by the process according to the invention are easy to process, for example to tablets ("tabs") for ADW and to clear rinse tablets for ADW granules obtainable by the process according to the invention are less hygroscopic and less prone to sticking or caking.
- Granules according to the invention have an average particle diameter in the range from 0.5 to 1.6 mm and contain (a) in the range from 15 to 25% by weight of nonionic surfactant of the general formula (I)
- R 1 is selected from C 4 -C 20 -alkyl
- R 2 is selected from C 8 -C 20 -alkyl
- AO are in each case identical or different and selected from C 2 -C 4 -alkylene
- x is in the range of 5 to 100
- R 3 is -CH (COOM) -N (CH 2 COOM) 2 (Ii) in which the variables are defined as follows: R 3 is selected from C 1 -C 4 -alkyl, phenyl, benzyl, CH 2 OH and CH 2 CH 2 COOM 1 ,
- M 1 is an alkali metal or a combination of at least two alkali metals, granules according to the invention being solid at a temperature of up to 60 ° C.
- Components (a), (b), (c) and (d) are described in more detail above.
- granules according to the invention have a particle diameter distribution as follows: d m is in the range from 0.5 to 1.8 mm, d63.3 is in the range from 0.4 to 1.8 mm and n is in the range from 0.5 to 1.8 mm Range from 0.7 to 10, determined in each case with the aid of a sieve analysis according to DIN ISO 3310-1 (1992) and evaluation according to DIN 66145 (1976).
- Granules according to the invention can be made into dishwasher tablets and especially into rinse tablets, but also into rinse aid for an automatic dishwashing machine or as component for an x-in-1 ground dishwashing detergent, for example a 2-in-1 dishwashing detergent or a 3-in-1 detergent.
- the rinse aid is a rinse aid for an automatic dishwasher or a component for an x-in-1 dishwashing detergent, for example a 2-in-1 dishwashing or a 3-in-1 dishwashing detergent. 1 dishwashing detergent.
- granules according to the invention without further additives as a rinse aid in a dishwashing machine, in particular in x.in-1 dishwashers.
- at least one additive is added, selected from water and acids, for example citric acid.
- the components (a.1) and (b.1) were melted together in a beaker at 70 ° C and mixed with a propeller stirrer. Subsequently, the melt was poured onto aluminum foil (20 cm ⁇ 10 cm ⁇ 1 cm) and solidified at room temperature. Waxy plates were obtained.
- the lozenges thus produced were ground in a hammer mill (knife mill). For this purpose, the mill was operated with 2 knives and a peripheral speed of 14 m / s.
- Mahlsieb was a Rundlochsieb with a hole diameter of 3.2 mm and a free
- the particle diameter distribution of the exemplary granules was determined as follows by sieve analysis: sieving machine: AS 200 control, Fa. Retsch, test sieves to DIN ISO 3310-1, height 25 mm; 0 200 mm
- V-G.3 received no measurable granules
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Detergent Compositions (AREA)
Abstract
Description
Claims
Priority Applications (9)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2018521634A JP6885936B2 (ja) | 2015-10-26 | 2016-10-18 | 顆粒、その製造方法及び使用方法 |
BR112018008210-4A BR112018008210A2 (pt) | 2015-10-26 | 2016-10-18 | processo para produzir uma formulação, grânulo, e, uso de um grânulo. |
ES16785417T ES2765237T3 (es) | 2015-10-26 | 2016-10-18 | Granulados, procedimiento para su fabricación y su uso |
PL16785417T PL3368645T3 (pl) | 2015-10-26 | 2016-10-18 | Granulaty, sposób ich wytwarzania i ich zastosowanie |
US15/770,532 US10717952B2 (en) | 2015-10-26 | 2016-10-18 | Granulates, method for the production and use thereof |
CN201680062436.0A CN108350397B (zh) | 2015-10-26 | 2016-10-18 | 颗粒、其生产方法和用途 |
RU2018119305A RU2736331C2 (ru) | 2015-10-26 | 2016-10-18 | Грануляты, способ их получения и их применение |
KR1020187014363A KR20180074737A (ko) | 2015-10-26 | 2016-10-18 | 과립, 이의 제조 방법 및 용도 |
EP16785417.3A EP3368645B1 (de) | 2015-10-26 | 2016-10-18 | Granulate, verfahren zu ihrer herstellung und ihre verwendung |
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Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP15191376.1 | 2015-10-26 | ||
EP15191376 | 2015-10-26 |
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WO2017071984A1 true WO2017071984A1 (de) | 2017-05-04 |
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PCT/EP2016/074920 WO2017071984A1 (de) | 2015-10-26 | 2016-10-18 | Granulate, verfahren zu ihrer herstellung und ihre verwendung |
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US (1) | US10717952B2 (de) |
EP (1) | EP3368645B1 (de) |
JP (1) | JP6885936B2 (de) |
KR (1) | KR20180074737A (de) |
CN (1) | CN108350397B (de) |
BR (1) | BR112018008210A2 (de) |
ES (1) | ES2765237T3 (de) |
PL (1) | PL3368645T3 (de) |
RU (1) | RU2736331C2 (de) |
WO (1) | WO2017071984A1 (de) |
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CN115916940A (zh) * | 2020-07-03 | 2023-04-04 | 宝洁公司 | 粒状衣物洗涤组合物 |
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WO2001048131A2 (de) * | 1999-12-24 | 2001-07-05 | Cognis Deutschland Gmbh & Co. Kg | Tensidgranulate mit verbesserter auflösegeschwindigkeit |
EP1306422A1 (de) * | 2001-10-23 | 2003-05-02 | Cognis Deutschland GmbH & Co. KG | Feste Wasch-, Spül- und Reinigungsmittel |
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WO1995005440A1 (en) * | 1993-08-13 | 1995-02-23 | The Procter & Gamble Company | Granular automatic dishwashing detergent with long-chain amine oxides |
WO1998011185A1 (en) * | 1996-09-11 | 1998-03-19 | The Procter & Gamble Company | Detergent composition |
JPH1135999A (ja) * | 1997-07-23 | 1999-02-09 | Lion Corp | 粒状ノニオン洗剤組成物の製造方法 |
ES2142783T1 (es) * | 1997-11-26 | 2000-05-01 | Procter & Gamble | Tableta de detergentes de varias capas que tiene porciones comprimidas y porciones no comprimidas. |
JP2000192098A (ja) * | 1998-12-25 | 2000-07-11 | Lion Corp | タブレット洗剤組成物 |
DE10019936A1 (de) * | 1999-12-04 | 2001-10-25 | Henkel Kgaa | Wasch- und Reinigungsmittel |
RU2169175C1 (ru) * | 1999-12-17 | 2001-06-20 | Общество с ограниченной ответственностью "Чистые технологии" | Моющее средство для очистки поверхности от органических загрязнений и способ его получения |
JP2003105375A (ja) * | 2001-09-28 | 2003-04-09 | Lion Corp | 粒状洗剤組成物 |
EP1956076A1 (de) * | 2007-02-02 | 2008-08-13 | Kemira Oyj | Kogranulat zur Verwendung in festen Waschmittelzusammensetzungen |
-
2016
- 2016-10-18 ES ES16785417T patent/ES2765237T3/es active Active
- 2016-10-18 JP JP2018521634A patent/JP6885936B2/ja active Active
- 2016-10-18 PL PL16785417T patent/PL3368645T3/pl unknown
- 2016-10-18 US US15/770,532 patent/US10717952B2/en active Active
- 2016-10-18 BR BR112018008210-4A patent/BR112018008210A2/pt active Search and Examination
- 2016-10-18 CN CN201680062436.0A patent/CN108350397B/zh not_active Expired - Fee Related
- 2016-10-18 WO PCT/EP2016/074920 patent/WO2017071984A1/de active Application Filing
- 2016-10-18 EP EP16785417.3A patent/EP3368645B1/de not_active Not-in-force
- 2016-10-18 RU RU2018119305A patent/RU2736331C2/ru active
- 2016-10-18 KR KR1020187014363A patent/KR20180074737A/ko unknown
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WO2001048131A2 (de) * | 1999-12-24 | 2001-07-05 | Cognis Deutschland Gmbh & Co. Kg | Tensidgranulate mit verbesserter auflösegeschwindigkeit |
EP1306422A1 (de) * | 2001-10-23 | 2003-05-02 | Cognis Deutschland GmbH & Co. KG | Feste Wasch-, Spül- und Reinigungsmittel |
DE102007019458A1 (de) * | 2007-04-25 | 2008-10-30 | Basf Se | Phosphatfreies Maschinengeschirrspülmittel mit ausgezeichneter Klarspülleistung |
DE102011084934A1 (de) * | 2011-10-21 | 2013-04-25 | Henkel Ag & Co. Kgaa | Klarspül- und Geschirrspülmittel |
Also Published As
Publication number | Publication date |
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JP6885936B2 (ja) | 2021-06-16 |
US10717952B2 (en) | 2020-07-21 |
CN108350397A (zh) | 2018-07-31 |
RU2736331C2 (ru) | 2020-11-13 |
RU2018119305A3 (de) | 2019-11-28 |
KR20180074737A (ko) | 2018-07-03 |
BR112018008210A2 (pt) | 2018-10-23 |
PL3368645T3 (pl) | 2020-04-30 |
EP3368645A1 (de) | 2018-09-05 |
ES2765237T3 (es) | 2020-06-08 |
RU2018119305A (ru) | 2019-11-28 |
JP2018533656A (ja) | 2018-11-15 |
CN108350397B (zh) | 2021-02-26 |
EP3368645B1 (de) | 2019-10-16 |
US20190055501A1 (en) | 2019-02-21 |
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