CN1321187A - 洗衣和清洁组合物 - Google Patents
洗衣和清洁组合物 Download PDFInfo
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- CN1321187A CN1321187A CN99808494A CN99808494A CN1321187A CN 1321187 A CN1321187 A CN 1321187A CN 99808494 A CN99808494 A CN 99808494A CN 99808494 A CN99808494 A CN 99808494A CN 1321187 A CN1321187 A CN 1321187A
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- composition
- methyl
- amino
- acid
- perfume
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- 239000000203 mixture Substances 0.000 title claims abstract description 212
- 238000004140 cleaning Methods 0.000 title claims abstract description 35
- 239000002304 perfume Substances 0.000 claims abstract description 110
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 23
- -1 polyoxyethylene Polymers 0.000 claims description 85
- 239000003599 detergent Substances 0.000 claims description 67
- 239000004744 fabric Substances 0.000 claims description 57
- 239000003205 fragrance Substances 0.000 claims description 51
- 239000004927 clay Substances 0.000 claims description 45
- 150000001412 amines Chemical class 0.000 claims description 42
- 239000007795 chemical reaction product Substances 0.000 claims description 42
- 150000001875 compounds Chemical class 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 38
- 229920001002 functional polymer Polymers 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 150000002576 ketones Chemical class 0.000 claims description 24
- 150000001299 aldehydes Chemical class 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 22
- 229920001308 poly(aminoacid) Polymers 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 13
- VAMXMNNIEUEQDV-UHFFFAOYSA-N methyl anthranilate Chemical compound COC(=O)C1=CC=CC=C1N VAMXMNNIEUEQDV-UHFFFAOYSA-N 0.000 claims description 13
- 229920001577 copolymer Polymers 0.000 claims description 12
- 229920000656 polylysine Polymers 0.000 claims description 12
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- AKGGYBADQZYZPD-UHFFFAOYSA-N benzylacetone Chemical compound CC(=O)CCC1=CC=CC=C1 AKGGYBADQZYZPD-UHFFFAOYSA-N 0.000 claims description 10
- KVWWIYGFBYDJQC-UHFFFAOYSA-N methyl dihydrojasmonate Chemical compound CCCCCC1C(CC(=O)OC)CCC1=O KVWWIYGFBYDJQC-UHFFFAOYSA-N 0.000 claims description 10
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- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 8
- ULDHMXUKGWMISQ-UHFFFAOYSA-N carvone Chemical compound CC(=C)C1CC=C(C)C(=O)C1 ULDHMXUKGWMISQ-UHFFFAOYSA-N 0.000 claims description 8
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 claims description 8
- SATCULPHIDQDRE-UHFFFAOYSA-N piperonal Chemical compound O=CC1=CC=C2OCOC2=C1 SATCULPHIDQDRE-UHFFFAOYSA-N 0.000 claims description 8
- PSQYTAPXSHCGMF-BQYQJAHWSA-N β-ionone Chemical compound CC(=O)\C=C\C1=C(C)CCCC1(C)C PSQYTAPXSHCGMF-BQYQJAHWSA-N 0.000 claims description 8
- XEJGJTYRUWUFFD-FNORWQNLSA-N (e)-1-(2,6,6-trimethyl-1-cyclohex-3-enyl)but-2-en-1-one Chemical compound C\C=C\C(=O)C1C(C)C=CCC1(C)C XEJGJTYRUWUFFD-FNORWQNLSA-N 0.000 claims description 7
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- 229940102398 methyl anthranilate Drugs 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 5
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- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 5
- ZFNVDHOSLNRHNN-UHFFFAOYSA-N xi-3-(4-Isopropylphenyl)-2-methylpropanal Chemical compound O=CC(C)CC1=CC=C(C(C)C)C=C1 ZFNVDHOSLNRHNN-UHFFFAOYSA-N 0.000 claims description 5
- SFEOKXHPFMOVRM-UHFFFAOYSA-N (+)-(S)-gamma-ionone Natural products CC(=O)C=CC1C(=C)CCCC1(C)C SFEOKXHPFMOVRM-UHFFFAOYSA-N 0.000 claims description 4
- MBDOYVRWFFCFHM-SNAWJCMRSA-N (2E)-hexenal Chemical compound CCC\C=C\C=O MBDOYVRWFFCFHM-SNAWJCMRSA-N 0.000 claims description 4
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- 125000002947 alkylene group Chemical group 0.000 claims description 4
- UZFLPKAIBPNNCA-UHFFFAOYSA-N alpha-ionone Natural products CC(=O)C=CC1C(C)=CCCC1(C)C UZFLPKAIBPNNCA-UHFFFAOYSA-N 0.000 claims description 4
- KSMVZQYAVGTKIV-UHFFFAOYSA-N decanal Chemical compound CCCCCCCCCC=O KSMVZQYAVGTKIV-UHFFFAOYSA-N 0.000 claims description 4
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 claims description 4
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- PHXATPHONSXBIL-UHFFFAOYSA-N xi-gamma-Undecalactone Chemical compound CCCCCCCC1CCC(=O)O1 PHXATPHONSXBIL-UHFFFAOYSA-N 0.000 claims description 4
- JRJBVWJSTHECJK-LUAWRHEFSA-N (z)-3-methyl-4-(2,6,6-trimethylcyclohex-2-en-1-yl)but-3-en-2-one Chemical compound CC(=O)C(\C)=C/C1C(C)=CCCC1(C)C JRJBVWJSTHECJK-LUAWRHEFSA-N 0.000 claims description 3
- MZZRKEIUNOYYDF-UHFFFAOYSA-N 2,4-dimethylcyclohex-3-ene-1-carbaldehyde Chemical compound CC1C=C(C)CCC1C=O MZZRKEIUNOYYDF-UHFFFAOYSA-N 0.000 claims description 3
- NFAVNWJJYQAGNB-UHFFFAOYSA-N 2-methylundecanal Chemical compound CCCCCCCCCC(C)C=O NFAVNWJJYQAGNB-UHFFFAOYSA-N 0.000 claims description 3
- PANBRUWVURLWGY-UHFFFAOYSA-N 2-undecenal Chemical group CCCCCCCCC=CC=O PANBRUWVURLWGY-UHFFFAOYSA-N 0.000 claims description 3
- ZAXCZCOUDLENMH-UHFFFAOYSA-N 3,3,3-tetramine Chemical compound NCCCNCCCNCCCN ZAXCZCOUDLENMH-UHFFFAOYSA-N 0.000 claims description 3
- XUSNPFGLKGCWGN-UHFFFAOYSA-N 3-[4-(3-aminopropyl)piperazin-1-yl]propan-1-amine Chemical compound NCCCN1CCN(CCCN)CC1 XUSNPFGLKGCWGN-UHFFFAOYSA-N 0.000 claims description 3
- 238000005299 abrasion Methods 0.000 claims description 3
- GUUHFMWKWLOQMM-NTCAYCPXSA-N alpha-hexylcinnamaldehyde Chemical compound CCCCCC\C(C=O)=C/C1=CC=CC=C1 GUUHFMWKWLOQMM-NTCAYCPXSA-N 0.000 claims description 3
- GUUHFMWKWLOQMM-UHFFFAOYSA-N alpha-n-hexylcinnamic aldehyde Natural products CCCCCCC(C=O)=CC1=CC=CC=C1 GUUHFMWKWLOQMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- AXEYWFGSQDLHDX-UHFFFAOYSA-N hexane-1,3,6-triamine Chemical compound NCCCC(N)CCN AXEYWFGSQDLHDX-UHFFFAOYSA-N 0.000 claims description 3
- HZYHMHHBBBSGHB-UHFFFAOYSA-N (2E,6E)-2,6-Nonadienal Natural products CCC=CCCC=CC=O HZYHMHHBBBSGHB-UHFFFAOYSA-N 0.000 claims description 2
- HZYHMHHBBBSGHB-DYWGDJMRSA-N (2e,6e)-nona-2,6-dienal Chemical compound CC\C=C\CC\C=C\C=O HZYHMHHBBBSGHB-DYWGDJMRSA-N 0.000 claims description 2
- 239000001674 (E)-1-(2,6,6-trimethyl-1-cyclohexenyl)but-2-en-1-one Substances 0.000 claims description 2
- BGTBFNDXYDYBEY-UHFFFAOYSA-N 1-(2,6,6-trimethylcyclohexen-1-yl)but-2-en-1-one Chemical compound CC=CC(=O)C1=C(C)CCCC1(C)C BGTBFNDXYDYBEY-UHFFFAOYSA-N 0.000 claims description 2
- PARHMNZPOUVEIQ-UHFFFAOYSA-N 1-(4-hydroxyphenyl)butan-2-one Chemical compound CCC(=O)CC1=CC=C(O)C=C1 PARHMNZPOUVEIQ-UHFFFAOYSA-N 0.000 claims description 2
- CTLDWNVYXLHMAS-UHFFFAOYSA-N 2,4,4,7-tetramethyloct-6-en-3-one Chemical compound CC(C)C(=O)C(C)(C)CC=C(C)C CTLDWNVYXLHMAS-UHFFFAOYSA-N 0.000 claims description 2
- HMKKIXGYKWDQSV-UHFFFAOYSA-N 2-benzylideneheptanal Chemical compound CCCCCC(C=O)=CC1=CC=CC=C1 HMKKIXGYKWDQSV-UHFFFAOYSA-N 0.000 claims description 2
- BGTBFNDXYDYBEY-FNORWQNLSA-N 4-(2,6,6-Trimethylcyclohex-1-enyl)but-2-en-4-one Chemical compound C\C=C\C(=O)C1=C(C)CCCC1(C)C BGTBFNDXYDYBEY-FNORWQNLSA-N 0.000 claims description 2
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 claims description 2
- 239000006001 Methyl nonyl ketone Substances 0.000 claims description 2
- KMPQYAYAQWNLME-UHFFFAOYSA-N Undecanal Natural products CCCCCCCCCCC=O KMPQYAYAQWNLME-UHFFFAOYSA-N 0.000 claims description 2
- POIARNZEYGURDG-UHFFFAOYSA-N beta-damascenone Natural products CC=CC(=O)C1=C(C)C=CCC1(C)C POIARNZEYGURDG-UHFFFAOYSA-N 0.000 claims description 2
- PHXATPHONSXBIL-JTQLQIEISA-N gamma-Undecalactone Natural products CCCCCCC[C@H]1CCC(=O)O1 PHXATPHONSXBIL-JTQLQIEISA-N 0.000 claims description 2
- 229940020436 gamma-undecalactone Drugs 0.000 claims description 2
- YJSUCBQWLKRPDL-UHFFFAOYSA-N isocyclocitral Chemical compound CC1CC(C)=CC(C)C1C=O YJSUCBQWLKRPDL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
- MBDOYVRWFFCFHM-UHFFFAOYSA-N trans-2-hexenal Natural products CCCC=CC=O MBDOYVRWFFCFHM-UHFFFAOYSA-N 0.000 claims description 2
- KYWIYKKSMDLRDC-UHFFFAOYSA-N undecan-2-one Chemical compound CCCCCCCCCC(C)=O KYWIYKKSMDLRDC-UHFFFAOYSA-N 0.000 claims description 2
- WGPCZPLRVAWXPW-UHFFFAOYSA-N xi-Dihydro-5-octyl-2(3H)-furanone Chemical compound CCCCCCCCC1CCC(=O)O1 WGPCZPLRVAWXPW-UHFFFAOYSA-N 0.000 claims description 2
- UZFLPKAIBPNNCA-BQYQJAHWSA-N alpha-ionone Chemical compound CC(=O)\C=C\C1C(C)=CCCC1(C)C UZFLPKAIBPNNCA-BQYQJAHWSA-N 0.000 claims 1
- 150000003141 primary amines Chemical group 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 55
- 239000007844 bleaching agent Substances 0.000 description 45
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- 239000002253 acid Chemical group 0.000 description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 32
- 239000003795 chemical substances by application Substances 0.000 description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 31
- 239000011734 sodium Substances 0.000 description 29
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Classifications
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- 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
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- 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
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- 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
- C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
-
- 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
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- 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
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- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3719—Polyamides or polyimides
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- 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
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- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3723—Polyamines or polyalkyleneimines
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- 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
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Abstract
本发明涉及含有洗涤剂组分和含有至少一个伯和/或仲胺基团的氨基官能团聚合物和香料组分的反应产物的洗衣和清洁组合物,通过本发明,获得了与使用香料本身相比在较长时间内释放香料组分。
Description
发明领域
本发明涉及含有氨基官能团聚合物和香料组分,尤其是醛或酮香料之间的反应产物的洗衣和清洁组合物,所述聚合物含有至少一个伯和/或仲胺基团。
发明背景
洗衣和清洁产品在现有技术中是已知的,然而,消费者对洗衣和清洁产品的接受不仅由这些产品所达到的性能决定,而且由与其相关的美学决定,因此,香料组分是该商业产品的成功配制的重要方面。
对于洗涤的织物消费者还需要保持长时间的愉快香料。事实上,香料添加剂使得洗衣组合物对于消费者来说更加美观愉快,并且在某些情况下香料物质给予所处理的织物愉快的香味。然而,由含水洗衣槽中夹带到织物上的香料的数量通常是最低限度的,在织物上不能长久持续,此外香料通常是非常昂贵的,它们在洗衣和清洁组合物中的未充分利用和未有效提供给织物导致对消费者和洗衣和清洁生产商非常高的成本。因此,工业上持续迫切需要在洗衣和清洁产品中更充分和有效提供香味,尤其需要在向织物长时间地提供香味方面的改善。
一种解决方法是使用香料提供的载体机理,例如采用包胶囊,这在现有技术中教导,在US5188753中描述。
另一解决方法是配制化合物,与使用香料本身相比,它提供较长时间的香料延迟释放,该化合物可在WO95/04809、WO95/08976和未审申请EP95303762.9中找到。
然而,虽然现有技术中取得了进步,但人们仍需要能提供香料组分的延迟释放的化合物。
这种需要对于特征为新鲜标志,即醛和酮香料组分的香料组分是更加急切的。事实上,在它们提供新鲜香味同时,这些香料同样是非常挥发的,在所处理的表面,如织物上具有低的牢固程度。
因此,本发明的目的是提供含有香料组分的洗衣和清洁组合物,所述香料组分提供新鲜香味,并对于所处理的表面是牢固的。
申请人现在发现含有至少一个伯和/或仲胺基团的氨基官能团聚合物与活泼醛或酮的特殊反应产物,例如亚胺化合物,同样提供了活性组分,例如香料的延迟释放。
亚胺化合物在现有技术中是已知的,称为Schiff碱,它是醛香料与邻氨基苯甲酸酯的缩合,典型描述在US4853369中找到。通过该化合物,使得醛香料对于织物是牢固的,然而,该Schiff碱所带来的问题是邻氨基苯甲酸甲酯化合物也显示强香气,结果产生香味混合物,从而降低甚至抑制醛和/酮香料感觉。
为获得具有可比较的醛或酮新鲜标志而同时具有令人满意的织物牢固度的香料组合物,围绕组份配制香料。例如使用用于该气味标志的栽体或包胶囊材料,例如环糊精、沸石或淀粉。
另一解决方法是使用如JP09040687中描述的葡糖胺。然而该化合物被发现在洗衣/清洁过程中具有非常低的稳定性,结果,用这些葡糖胺化合物在所处理的织物和/或硬表面上具有不充分的香料残余。
另一解决方法在Chemical release control,Kamogawa等,J.Poly.Sci.Polym.Chem.Ed.20卷,3121(1982)中描述,它描述了与醛香料缩合的氨基苯乙烯化合物,因此香料的释放通过该化合物的共聚或酸化引发,然而,未提及它在洗衣和清洁产品中的应用。
申请人现在发现在含有至少一个伯和/或仲胺基团的氨基官能团聚合物和香料之间的反应产物也满足了该需要。
本发明化合物的另一优点是它们容易制备,使得它们的应用最可取。
发明概述
本发明涉及含有洗涤剂组分和含有至少一个伯和/或仲胺基团的氨基官能团聚合物和选自酮、醛和它们的混合物的香料组分之间的反应产物的洗衣和清洁组合物,其特征在于所述氨基官能团聚合物具有比在一缩二丙二醇中的1%邻氨基苯甲酸甲酯溶液低的香气强度系数,和反应产物具有超过5的干表面香气系数。
本发明的另一方面是提供一种通过本发明的化合物或组合物向表面提供残余香味的方法。发明的详细描述1-氨基官能团聚合物和香料组分之间的反应产物
本发明的一个基本组分是含有至少一个伯和/仲胺基团的氨基官能团聚合物和香料组分之间的反应产物,下文所谓的“胺反应产物”。A-氨基官能团聚合物
氨基官能团聚合物的特征在于具有比在一缩二丙二醇中的1%邻氨基苯甲酸甲酯溶液低的香气强度系数。香气强度系数方法
香气强度系数是指纯化学物质在香料中使用的无香味溶剂,一缩二丙二醇中稀释至1%。该百分数是更具代表性使用含量,将气味条或所谓的“吸墨纸”浸入,提供给专家小组成员进行评价。专家小组成员是在香味等级方面培训至少6个月的顾问,他们评出的分级相对进行的基准的准确性和重复性经过核查。对于每个氨基官能团聚合物,向专家小组提供两个吸墨纸:参考物(邻氨基苯甲酸甲酯,对于专家小组成员是未知的)和样品。专家小组成员把气味条分成0-5香气强度等级,0是未检测到香气,5表示存在非常强的香气。结果:
如下表示适用于本发明的并根据上述方法的氨基官能团聚合物的香气强度系数。在每种情况下,数值是5位专家小组成员的算术平均值,结果是以95%的置信水平在统计学上明显不同的:邻氨基苯甲酸甲酯1%(参考物) 3.41,4-二(3-氨基丙基)哌嗪1%(BNPP) 1.0
本发明的含有至少一个伯胺基团的氨基官能团聚合物的一般结构如下:
(NH2)n-[B]其中n是至少1的数值,B是聚合物骨架。B可选择性地含有支链基团C,因而氨基官能团聚合物是如下结构式的物质:
(NH2)n-[B]-[C]x,其中x≥0
含有仲胺基团的氨基官能团聚合物具有如上的类似结构,只是聚合物含有一个或多个-NH-基团而不是-NH2。此外,聚合物结构还可同时带有一个或多个-NH2和-NH-基团。
本发明的氨基官能团聚合物含有通过称为R*的基团的氢取代、或其它合适插入或取代而连接于主链的至少一个自由、未改性的伯和/或仲氨基基团,同样合适的是含有在侧链上存在的未改性伯和/或仲氨基的氨基官能团聚合物。
本发明的氨基官能团聚合物优选含有若干,更优选超过10个氨基,本发明的氨基官能团聚合物优选以150-2.10E6,更优选400-50000,最优选600-40000的分子量(MW)存在。
氨基官能团聚合物可以是线性均-、共-聚物和选择性地支链化、接枝和/或交联的。
用于本发明的合适聚合物骨架B含有如下聚合物单元:其中×=2-105
箭头表示在位置2,3或4中取代
本发明的氨基官能团聚合物还可含有在主链或侧链上的取代基R*,通常R*替换氢原子,该R*基团可直接或以连接基团L连接于主链或侧链,合适的连接基团L是上述的插入基团I。
R*基团是C1-C22烷基、烯基、烷基苯链和/或它们相应的取代衍生物,该相应取代的衍生物包括脂环族、芳香、杂环芳香或杂环体系,插入主链中或通过取代主链中的H原子加入;在主链中的如上定义的插入基团I和/或定义如下的端基E。
此外,聚合物骨架B和R*包括端基E,典型的端基E可以是H、NH2基团、芳香、脂环族、杂芳基或杂环基团,包括单-、二-、寡糖、多糖:
此外,R*基团还可以是通过一个或多个H原子取代改性,所述取代可以是如上所述的端基E或插入基团I,而插入基团被H、E或R*基团终止。
合适的用于本发明的优选氨基官能团聚合物优选聚乙烯基胺、它们的衍生物、它们的共聚物、亚烷基聚胺、聚氨基酸和它们的共聚物、交联聚氨基酸、氨基取代的聚乙烯基醇、聚氧乙烯二胺或二氨基烷基、氨基烷基哌嗪和衍生物、N,N’-二(3-氨基丙基)-1,3-丙二胺、直链或支链(TPTA)和它们的混合物。
聚氨基酸是一种合适和优选种类的氨基官能团聚合物,聚氨基酸是氨基酸或化学改性的氨基酸构成的化合物。它们可含有丙氨酸、丝氨酸、天门冬氨酸、精氨酸、缬氨酸、苏氨酸、谷氨酸、亮氨酸、半胱氨酸、组氨酸、赖氨酸、异亮氨酸、酪氨酸、天门冬酰胺、蛋氨酸、脯氨酸、色氨酸、苯基丙氨酸、谷氨酸盐、甘氨酸或它们的混合物。在化学改性的氨基酸中,氨基酸的胺或酸性官能团与化学试剂反应,通常这样进行是为了在随后的反应中保护氨基酸的这些化学胺和酸官能团或给氨基酸提供特定性质,例如改善的稳定性。该化学改性的实例是苄氧羰基、氨基丁酸、丁酯、焦谷氨酸。氨基酸的一般改性和小氨基酸片段的实例可在Bachem,1996,Peptides andBiochemicals Catalog中找到。
优选的聚氨基酸是聚赖氨酸、聚精氨酸、聚谷氨酸盐、聚天门冬酰胺、聚组氨酸、聚色氨酸或它们的混合物。最优选聚赖氨酸或其中超过50%的氨基酸是赖氨酸的聚氨基酸,因为在赖氨酸的侧链中伯胺官能团是所有氨基酸中最活泼的胺。
优选的氨基酸具有500-10000000,更优选5000-750000的分子量。
聚氨基酸可以是交联的,交联可例如通过缩合氨基酸,如赖氨酸的侧链中的氨基与氨基酸上的羧基官能团或蛋白质交联剂,如PEG衍生物得到,交联的聚氨基酸还需要保留自由伯和/或仲胺基团以便与活性组分反应。
优选的交联聚氨基酸具有20000-10000000,更优选200000-2000000的分子量。
聚氨基酸或氨基酸可与其它试剂,如酸、酰胺、酰氯共聚,更具体地与氨基己酸、己二酸、乙基己酸、己内酰胺或它们的混合物共聚,在这些共聚物中使用的摩尔比为1∶1(试剂/氨基酸(赖氨酸))-1∶20,更优选1∶1-1∶10。
聚氨基酸,如聚赖氨酸可部分乙氧基化。
含有赖氨酸、精氨酸、谷氨酸盐、天门冬酰胺的聚氨基酸的实例和来源在Bachem,1996,Peptides and Biochemicals Catalog中找到。
在与活性组分反应之前,聚氨基酸可以盐的形式得到,例如聚赖氨酸可作为聚赖氨酸氢溴酸盐得到,聚赖氨酸氢溴酸盐在商业上可由Sigma,Applichem,Bachem and Fluka得到。
用于本发明的含有至少一种伯和/或仲胺基团的合适氨基官能团聚合物的实例是:-聚乙烯胺,MW约300-2.10E6;-乙氧基化聚乙烯胺,MW约600,1200或3000,乙氧基化程度0.5;-聚乙烯基胺乙烯基醇-摩尔比2∶1、聚乙烯基胺乙烯基甲酰胺-摩尔比1∶2和聚乙烯基胺乙烯基甲酰胺摩尔比2∶1;-三亚乙四胺、二亚乙三胺、四亚乙五胺;-二氨基丙基哌嗪;-聚氨基酸(L-赖氨酸/月桂酸,摩尔比10/1)、聚氨基酸(L-赖氨酸/氨基己酸/己二酸,摩尔比5/5/1)、聚氨基酸(L-赖氨酸/氨基己酸/乙基己酸,摩尔比5/3/1)、聚氨基酸(聚赖氨酸共聚己内酰胺)、聚赖氨酸氢溴酸盐、交联聚赖氨酸。-氨基取代的聚乙烯基醇,MW400-300,000;-聚氧乙烯二[胺],由例如Sigma得到;-聚氧乙烯二[6-氨基己基],由例如Sigma得到;-N,N’-二(3-氨基丙基)-1,3-丙二胺直链或支链(TPTA);和-1,4-二(3-氨基丙基)哌嗪(BNPP)。
含有至少一个伯和/或仲胺基团的优选氨基官能团聚合物是:-聚乙烯胺,MW600、1200、3K、20K、25K或50K;-氨基取代的聚乙烯基醇,MW400-300,000;-聚氧乙烯二[胺],由例如Sigma得到;-聚氧乙烯二[6-氨基己基],由例如Sigma得到;-N,N’-二(3-氨基丙基)-1,3-丙二胺直链或支链(TPTA);和-1,4-二(3-氨基丙基)哌嗪(BNPP)-聚赖氨酸氢溴酸盐;-交联聚赖氨酸。
此外,含有至少一个伯和/或仲胺氨基的该氨基官能团聚合物和胺反应产物提供织物外观效果,尤其是颜色护理和保护织物磨损。事实上,织物,例如衣服、被褥、家用织物,如餐布的外观是消费者关心的方面之一,事实上,随着织物典型的消费者使用,例如织物穿用、洗涤、漂洗和/或转鼓干燥,观察到织物外观的损失,至少部分是由于彩色逼真度和彩色清晰度的损失,该颜色损失问题在多次洗涤周期后是尤其严重的。我们发现本发明的组合物提供改善的织物外观和保护织物磨损,和对于洗涤的织物,尤其是在多次洗涤周期后改善的彩色护理。
因此,本发明的组合物可同时提供织物护理和长持久的香料效果。B-香料
对于上述化合物,香料酮或活性醛优选是指含有至少一个碳原子,优选至少5个碳原子的任何链。
传统用于香料的合适酮和/或醛的典型公开内容可在“perfumeand Flavor Chemicals”,卷I和II,S.Arctander,AlluredPublishing,1994,ISBN 0-931710-35-5中找到。
香料酮组分包括具有香味性质的组分。
对于上述化合物,香料酮对于其香味特征优选选自buccoxime、异茉莉酮、甲基β-萘基酮、麝香二氢茚酮、tonalid/麝香plus、α-二氢大马酮、β-二氢大马酮、δ-二氢大马酮、异二氢大马酮、大马酮、Damarose、甲基二氢茉莉酸酯、薄荷酮、香芹酮、樟脑、茴香酮、α-紫罗兰酮、β-紫罗兰酮、γ-甲基所谓的紫罗兰酮、Fleuramone、二氢茉莉酮、顺茉莉酮、异-E-Super、甲基-雪松基酮或甲基雪松酮、苯乙酮、甲基苯乙酮、对甲氧基苯乙酮、甲基-β-萘基酮、苄基丙酮、二苯酮、对羟基苯基丁酮、芹菜酮或Livescone、6-异丙基十氢-2-萘酮、二甲基-辛烯酮、Freskomenthe、4-(1-乙氧基乙烯基)-3,3,5,5-四甲基-环己酮、甲基庚酮、2-(2-(4-甲基-3-环己烯-1-基)丙基)环戊酮、1-(p-薄荷烯-6(2)-基)-1-丙酮、4-(4-羟基-3-甲氧基苯基)-2-丁酮、2-乙酰基-3,3-二甲基降冰片酮、6,7-二氢-1,1,2,3,3-五甲基-4(5H)-二氢茚酮、4-Damascol、Dulcinyl或金合欢酮、Gelsone、Hexalon、异环烯酮E、甲基环柠檬酮、甲基-薰衣草酮、Orivon、对叔丁基环己酮、Verdone、Delphone、麝香酮、Neobutenone、Plicatone、Veloutone、2,4,4,7-四甲基辛-6-烯-3-酮、Tetrameran、十一烷酸内酯和γ-十一烷酸内酯。
对于上述化合物,就其气味特征来说,优选的酮选自α-二氢大马酮、δ-二氢大马酮、异二氢大马酮、香芹酮、γ-甲基紫罗兰酮、异-E-Super、2,4,4,7-四甲基辛-6-烯-3-酮、苄基丙酮、β-二氢大马酮、大马酮、甲基二氢茉莉酸酯、甲基雪松酮和它们的混合物。
香料醛组分包括具有香味性质的组分。
对于上述化合物,就其气味特征来说,优选的香料醛根据其香料特征选自adoxal、茴香醛、cymal、乙基香兰素、florhydral、天芥菜醛、天芥菜精、羟基香茅醛、koavone、月桂基醛、lyral、甲基壬基乙醛、P.T.bucinal、苯基乙醛、十一碳烯醛、香兰素、2,6,10-三甲基-9-十一碳烯醛、3-十二碳烯-1-醛、α-正戊基肉桂醛、4-甲氧基苯甲醛、苯甲醛、3-(4-叔丁基苯基)-丙醛、2-甲基-3-(对甲氧基苯基)丙醛、2-甲基-4-(2,6,6-三甲基-2(1)-环己烯-1-基)丁醛、3-苯基-2-丙烯醛、顺-/反-3,7-二甲基-2,6-辛二烯1-醛、3,7-二甲基-6-辛烯-1-醛、[(3,7-二甲基-6-辛烯基)氧基]乙醛、4-异丙基苯甲醛、1,2,3,4,5,6,7,8-八氢-8,8二甲基-2-萘甲醛、2,4-二甲基-3-环己烯-1-基甲醛、2-甲基-3-(异丙基苯基)丙醛、1-癸醛、癸醛、2,6-二甲基-5-庚醛、4-(三环[5.2.1.0(2,6)]-次癸基-8)-丁醛、八氢-4,7-桥亚甲基-1H-茚醛、3-乙氧基-4-羟基苯甲醛、对乙基-α,α-二甲基氢化肉桂醛、α-甲基-3,4-(亚甲二氧基)-氢化肉桂醛、3,4-亚甲二氧基苯甲醛、α-正己基肉桂醛、m-对异丙基甲苯-7-甲醛、α-甲基苯基乙醛、7-羟基-3,7-二甲基辛醛、十一碳烯醛、2,4,6-三甲基-3-环己烯-1-醛、4-(3)(4-甲基-3-戊烯基)-3-环己烯醛、1-十二烷醛、2,4-二甲基环己烯-3-甲醛、4-(4-羟基-4-甲基戊基)-3-环己烯-1-甲醛、7-甲氧基-3,7-二甲基辛-1-醛、2-甲基十一醛、2-甲基十二烷醛、1-壬醛、1-辛醛、2,6,10-三甲基-5,9-十一碳二烯醛、2-甲基-3-(4-叔丁基)丙醛、二氢肉桂醛、1-甲基-4-(4-甲基-3-戊烯基)-3-环己烯-1-甲醛、5或6甲氧基六氢-4,7-桥亚甲基二氢化茚-1或2-甲醛、3,7-二甲基辛-1-醛、1-十一醛、10-十一碳烯-1-醛、4-羟基-3-甲氧基苯甲醛、1-甲基-3-(4-甲基戊基)-3-环己烯甲醛、7-羟基-3,7-二甲基苯基辛醛、反-4-癸烯醛、2,6-壬二烯醛、对甲苯基乙醛、4-甲基苯基乙醛、2-甲基-4-(2,6,6-三甲基-1-环己烯-1-基)-2-丁烯醛、邻-甲氧基肉桂醛、3,5,6-三甲基-3-环己烯醛、3,7-二甲基-2-亚甲基-6-辛烯醛、苯氧基乙醛、5,9-二甲基-4,8-癸二烯醛、芍药醛(6,10-二甲基-3-氧代-5,9-十一碳二烯-1-醛)、六氢-4,7-桥亚甲基二氢化茚-1-甲醛、2-甲基辛醛、α-甲基-4-(1-甲基乙基)苯乙醛、6,6-二甲基-2-降蒎烯-2-丙醛、对甲基苯氧基乙醛、2-甲基-3-苯基-2-丙烯-1-醛、3,5,5-三甲基己醛、六氢-8,8-二甲基-2-萘甲醛、3-丙基-双环[2.2.1]-庚-5-烯-2-甲醛、9-癸烯醛、3-甲基-5-苯基-1-戊醛、甲基壬基乙醛、己醛、反-2-己烯醛、1-p-薄荷烯-q-甲醛和它们的混合物。
就其气味特征,最优选的醛选自1-癸醛、苯甲醛、florhydral、2,4-二甲基-3-环己烯-1-甲醛、顺-/反-3,7-二甲基-2,6-辛二烯-1-醛、天芥菜精、2,4,6-三甲基-3-环己烯-1-甲醛、2,6-壬二烯醛、α-正戊基肉桂醛、α-正己基肉桂醛、P.T.Buci nal、lyral、cymal、甲基壬基乙醛、己醛、反-2-己烯醛和它们的混合物。
在上述所述的香料组分中,某些是本领域技术人员已知的商业名称,并且还包括异构体,该异构体也适用于本发明中。
在另一实施方案中,尤其适用于本发明的是特征为低气味检测阈值的香料化合物,优选香料酮或醛。在控制的气相色谱法(GC)条件下,例如下文描述的条件下,该气味检测阈值(ODT)应低于1ppm,优选低于10ppb。该参数涉及通常用于香料领域的数值,它是某些气味物质存在时发生明显检测的最低浓度。请查阅例如“Compilation ofOdor and Taste Threshold Value Data(ASTM DS 48A)”,由F.A.Fazzalari编辑,Interna tional Business Machines,HopwellJunction,NY和Calkin等,Perfumery,Practice and Principles,John Willey & Sons,Inc.,243页后(1994)。对于本发明,气味检测阈值根据如下方法测定:
气相色谱法的特征在于测定通过注射器注射的物质的准确体积、精确的分流比和用已知浓度和链长分布的烃标准的烃响应。空气流速是准确测量的,假定人吸入持续0.02分钟,计算取样体积。由于在检测器中在任何点的精确浓度是已知的,每吸入的体积的质量是已知的,因此物质的浓度是已知的。为检测香料物质的ODT,以倒退计算的浓度向吸气口提供溶液,专门小组成员吸入GC流出气流,当注意到气味时确定持续时间。所有成员的平均值确定值得注意的阈值。分析的所需量注射入柱中以获得在检测器中的某些浓度,例如10ppb,用于检测气味检测阈值的典型气相色谱法参数如下。GC:5890系列II,FID检测器7673自动取样器柱:J & W Scientific DB-1长度30米ID0.25mm膜厚度1微米方法:分流注射:17/1分流比自动取样器:每次注射1.13微升柱流速:1.10ml/分空气流速:345ml/分入口温度:245℃检测器温度:285℃温度信息最初温度:50℃速率:5℃/分最终温度:280℃最终时间:6分钟预先假定:每吸气0.02分钟GC空气加入样品稀释中。
该优选香料组分的实例选自:2-甲基-2-(对-异丙基苯基)-丙醛、1-(2,6,6-三甲基-2-环己-1-基)-2-丁烯-1-酮和/或对甲氧基苯乙酮。更优选的是具有用如上方法测定的ODT≤10ppb的如下化合物:十一碳烯醛、γ十一烷酸内酯、天芥菜精、γ十二烷酸内酯、对-茴香醛、对羟基-苯基-丁酮、cymal、苄基丙酮、α紫罗兰酮、p.t.bucinal、大马酮、β紫罗兰酮和甲基壬基酮。
香料的一般含量按胺反应产物重量计为10-90%,优选30-85%,更优选45-80%。
优选的胺反应混合物是由聚氨基酸,如聚赖氨酸、BNPP或TPTA与一种或多种如下的α二氢大马酮、δ二氢大马酮、香芹酮、二氢茉莉酮酸甲酯、Florhydral、铃兰醛、天芥菜精、γ-甲基-紫香酮、和2,4-二甲基-3-环己烯-1-甲醛和它们的混合物反应得到的产物。
胺反应产物最优选是BNPP或TPTA与α和δ二氢大马酮反应得到的产物。方法
组分的制备方法在如下合成实施例中给出,通常酮和醛的氮类似物称为甲亚氨、Schiff碱或更优选称为亚胺。这些亚胺可容易地通过脱水由伯胺和羰基化合物的缩合制备。
通过该简单的方法,制备化合物含有所述化合物的混合物,获得该活性组分的延迟释放。
如上可以看出,香料组分通常以与胺官能团等摩尔数量存在以确保反应进行,并得到胺反应产物。当然,并不排除较高的数量,当胺化合物含有超过一个胺官能团时甚致是更优选的。释放机理
通过本发明,获得香料组分,即酮或醛的延迟释放,尽管不限制于理论,但释放被认为通过如下机理发生:
对于亚胺化合物,香料组分在亚胺键断裂时释放,导致香料组分和伯胺化合物的释放,这可以通过水解、光化学裂解、氧化裂解或酶裂解进行。
对β-氨基酮化合物,用湿空气和/或水处理成功地释放香料组分和胺化合物,然而,并不排除其它释放方法,如水解、光化学裂解、氧化裂解或酶裂解。
还可考虑释放亚胺以及β-氨基酮化合物的其它方法,例如所处理的织物的熨烫的蒸汽过程、转鼓干燥和/或穿用。洗衣和清洁组合物
本发明包括洗衣和清洁组合物,它们通常用于洗涤织物和清洁硬表面,例如餐具、地板、浴室、厕所和其它需要香料酮和/或醛延迟释放的表面。因此,洗衣和清洁组合物理解为包括提供织物洗涤效果的洗涤剂组合物,还包括组合物,例如提供硬表面清洁效果的硬表面清洁剂。
优选能导致本发明的化合物与织物接触的那些洗衣组合物。
加入该洗衣和清洁组合物的胺反应产物优选提供超过5,优选至少10的干表面香气系数。
干表面香气系数是指胺反应产物提供超过5的Δ,其中Δ是用胺反应产物处理的干表面香气系数与仅用香料原料处理的干表面香气系数的差值。干表面香气系数的测量方法:
对于上述干表面香气系数,适用于本发明的胺反应产物需要满足如下两项试验的至少一项,优选的适用于本发明的胺反应产物满足两项试验。1)-用于硬表面产品制备:
将胺反应产物加入未加香料的产品中。
未加香料的产品如下,其中缩写如以下实施例中所定义:
组合物 | 重量% |
LAS | 16 |
NaSKS-6 | 6 |
PB1 | 8 |
TAED | 2.4 |
碳酸盐 | 1 |
碳酸钠 | 1 |
HEDP | 0.4 |
SRP1 | 0.2 |
光漂白剂 | 0.013 |
柠檬酸 | 1.0 |
蛋白酶 | 0.3 |
脂酶 | 0.1 |
纤维素酶 | 0.1 |
淀粉酶 | 0.3 |
沸石 | 3.0 |
TFAA | 3.0 |
QAS1 | 2.5 |
硅氧烷消泡剂 | 1.0 |
微量组分平衡至100% |
选择胺反应产物的含量以得到干织物上至少20的香气等级,在仔细混合后,在液体的情况下通过摇晃容器,在粉末的情况下用刮刀,使产品放置24小时。洗涤方法:
将得到的产品以适合其种类的剂量和在分配器中加入洗衣机中,质量相当于相应市场产品的建议剂量:通常对于洗涤剂粉末或液体为70-150g,用现有的计量装置,如granulette或ariellette。负荷由4条浴巾(170g)组成,使用Miele W830洗衣机,40℃的短周期,水输入:15度硬度,温度10-18℃,1200rpm的完全旋转。
相同的方法用于相应的游离香料组分,它用作参考,对于参考和样品,剂量、织物负荷和洗涤周期是相同的。干燥过程:
在洗涤周期结束后2小时内,旋转过的但仍湿润的织物用下述等级评价其香味,随后一半织物悬挂在线上干燥24小时,离开任何可能的污染,除非另有说明,该干燥在室内进行。室内条件是温度18-25℃,空气湿度50-80%。其余一半放在转鼓干燥机中,进行完全的“非常干”周期,例如在Miele,Novotronic T430设置在程序白色-额外干燥(完全周期),转鼓干燥的织物也在第二天评价。织物随后在无香味的房内贮存在开口的铝袋中,在7天后再次评价。香味评价:
香味通常由专家小组成员闻织物评价,0-100的等级用于所述织物香味分类,分类等级如下:
100=极强的香料香味
75=非常强的香料香味
50=强香味
40=中等香料香味
30=轻微的香料香味
20=弱香料香味
10=非常弱的香料香味
0=无香味
在1天和/或7天后在胺反应产物和香料原料之间超过5级的差值是统计学上明显的,在1天和/或7天后10或以上等级的差值表示阶跃变化。换句话说,当在1天或7天或同时1天和7天后观察到胺反应产物与香料原料之间超过5,优选至少10的等级差值时,它可得到结论,即胺反应产物适用于本发明,其条件是胺化合物满足香气强度系数。2)-用于硬表面产品制备:
加入香料原料或其混合物,以0.255%仔细混合在未加香料的硬表面清洁剂中。
未加香料的产品如下,其中缩写如以下实施例中所定义。
用于硬表面试验的组合物 | 重量% |
C12-14EO21 | 2 |
C12-14EO5 | 2.5 |
C9-11EO5 | 2.5 |
LAS | 0.8 |
Na2CO3 | 0.2 |
柠檬酸 | 0.8 |
Caustic acid | 0.5 |
脂肪酸 | 0.5 |
SCS | 1.5 |
水和微量组分平衡至100% |
在混合和静置24小时后,检查产品的均匀性,在由于香料组分差的溶解性而相分离的情况下,加入适量的对异丙基甲苯磺酸钠或其它增溶剂直至得到均匀溶液。清洁方法:
将5g该溶液均匀施用在瓷砖(875cm2,例如由Vileroy-Boch获得)上面,1分钟后,该瓷砖用1升自来水清洗,随后将瓷砖垂直放置3分钟使清洁水滴下。
最后将瓷砖放置在带有可除去的盖的清洁和充气的透明塑料盒(38×40×32cm)中,其具有滑动罩(10×10cm)使得专家评价者闻到盒子的内部气味。
盒子中的香味在刚放入瓷砖(新鲜读数)和1,2和6小时后评价。香味评价:
分类等级如下:
50=非常强的香味
40=强香味
30=中等香味
20=轻微香味
10=弱香味
0=无香味
每项试验包括blanc(未加香料的硬表面清洁剂),和在试验香料前体,所谓的胺反应产物情况下,还包括相应的游离香料组分以适当地测量栽体的效果。
与用于织物的干表面香气系数方法相同,在1天和/或7天后在胺反应产物和香料原料之间超过5级的差值是统计学上明显的,在1天和/或7天后10或以上等级的差值表示阶跃变化。换句话说,当在1天或7天或同时1天和7天后观察到胺反应产物与香料原料之间超过5,优选至少10的等级差值时,可得到结论,即胺反应产物适用于本发明,其条件是胺化合物满足香气强度系数。
本文定义的胺反应产物通常以按组合物重量计0.0001%-10%,优选0.001%-5%,更优选0.01%-2%包含在组合物中,该化合物的混合物也可使用。
胺反应产物在洗衣和清洁组合物中的加入过程,如果需要,可通过常规加入方法,例如喷洒、用淀粉包胶囊(例如如GB1464616中所述)、干加入或在环糊精中包胶囊方便地进行。优选胺反应产物在加入洗衣和清洁组合物之前预先形成,换句话说,香料组分和本发明的氨基官能团聚合物首先在一起反应以得到本发明定义的胺反应产物和仅在一旦形成后加入洗衣和清洁组合物中。通过在加入全配制组合物之前预先形成,能够较好地控制所制备的化合物。因此,与存在于全配制组合物中的香料成分的相互反应被避免,同样可避免可能发生的副反应。此外,通过该加入方法,能够有效地控制化合物的收率和纯度。
最优选的是,当洗衣和清洁组合物含有香料时,胺反应产物与香料分开加入组合物,由此,胺反应产物和随后的香料释放是更加受控制的。
洗衣和清洁组合物通常含有洗涤剂组分和下文所述的作为选择性组分的其它选择性组分。洗涤剂组分
以按重量计1%-55%的含量用于本发明的表面活性剂的非限制性例子包括常规的C11-C18烷基苯磺酸盐(“LAS”)和伯、支链和无规C10-C20烷基磺酸盐(“AS”)、式为CH3(CH2)x(CHOSO3 -M+)CH3和CH3(CH2)y(CHOSO3 -M+)CH2CH3的C10-C18仲(2,3)烷基硫酸盐,其中x和(y+1)是至少为7,优选至少为9的整数,且M为水溶性的阳离子,尤其是钠、不饱和硫酸盐,如油基硫酸盐、C10-C18烷基烷氧基硫酸盐(“AExS”;特别是x多至7EO乙氧基硫酸盐),C10-C18烷基烷氧基羧酸盐(特别是EO 1-5乙氧基羧酸盐),C10-18甘油醚、C10-C18烷基聚糖苷及其相应的硫酸化聚糖苷,和C12-C18α-磺化脂肪酸酯。如果需要,在总组合物中也可以包括常规的非离子和两性表面活性剂,如包括所谓窄峰烷基乙氧基化物的C12-C18烷基乙氧基化物(“AE”)和C6-C12烷基酚烷氧基化物(特别是乙氧基化物和混合的乙氧基/丙氧基化物)、C12-C18甜菜碱和磺基甜菜碱、C10-C18氧化胺、阳离子表面活性剂等。还可以使用C10-C18N-烷基多羟基脂肪酸酰胺,典型的例子包括C12-C18N-甲基葡糖酰胺,参见WO9206154。其它的糖衍生表面活性剂包括N-烷氧基多羟基脂肪酰胺,如C10-C18N-(3-甲氧基丙基)葡糖酰胺。N-丙基至N-己基C12-C18葡糖酰胺可用于低泡沫的场合。也可使用常规的C10-C20皂。如果需要高泡沫,可使用支链C10-C16皂。阴离子和非离子表面活性剂的混合物是特别有用的。其它常规使用的表面活性剂在标准文章中列出。
除上述组分之外,全配制的洗衣和清洁组合物优选含有一种或多种如下组分。助洗剂
洗涤剂助洗剂可选择性地包含在组合物中,以帮助控制矿物硬度。可使用无机和有机助洗剂。通常助洗剂被用于织物洗涤组合物中以帮助去除颗粒污垢。
助洗剂的含量可根据组合物的最终用途及其所需物理形式作很大变化。如果存在,组合物一般含有至少1%,优选1%-80%的助洗剂。液体配方一般含有按重量计5%-50%,更一般地5%-30%的洗涤剂助洗剂。颗粒配方一般含有按重量计1%-80%,更一般地为5%-约50%的洗涤剂助洗剂。然而,这并不意味着排除助洗剂的较低或较高含量。
无机或含磷洗涤剂助洗剂包括,但不限于,碱金属、铵和烷醇铵的多磷酸盐(具体有三聚磷酸盐、焦磷酸盐和玻璃态聚合偏磷酸盐)、膦酸盐、肌醇六磷酸、硅酸盐、碳酸盐(包括碳酸氢盐和倍半碳酸盐)、硫酸盐和硅铝酸盐。然而,在某些地区需要非磷助洗剂。重要的是,本发明的组合物即使在所谓“弱”助洗剂(与磷酸盐相比)如柠檬酸盐的存在下,或在沸石或层状硅酸盐助洗剂可能遇到的所谓“助洗不足”状态下,也能令人惊奇地发挥作用。
硅酸盐助洗剂的例子为碱金属硅酸盐,特别是那些SiO2∶Na2O比率为1.0∶1-3.2∶1的硅酸盐和层状硅酸盐,如在US4664839中描述的层状硅酸钠。NaSKS-6是由Hoechst供应的结晶层状硅酸盐的商标(通常缩写为“SKS-6”)。不象沸石助洗剂,NaSKS-6硅酸盐助洗剂不含铝。NaSKS-6具有层状硅酸盐的δ-Na2SiO5形态,它可以通过例如DE-A-3417649和DE-A-3742043中描述的方法制备。SKS-6是一种用于本发明的更优选的层状硅酸盐,但也可使用其它这类层状硅酸盐,如具有通式NaMSixO2x+1·yH2O的硅酸盐,其中M为钠或氢,x为1.9-4之间的数,优选为2,且y为0-20之间的数,优选为0。来自Hoechst的其它各种层状硅酸盐包括分别为α、β和γ形式的NaSKS-5、NaSKS-7和NaSKS-11。如上所述,δ-Na2SiO5(SKS-6形式)是最优选用于本发明的。其它硅酸盐也是有用的,例如硅酸镁,它可在颗粒状配方中用作松脆剂,用作氧漂白剂的稳定剂,以及用作泡沫控制体系中的组份。
碳酸盐助洗剂的例子是在DE2321001中描述的碱土和碱金属碳酸盐。
硅铝酸盐助洗剂在本发明中是有用的。硅铝酸盐助洗剂在最近销售的重垢颗粒洗涤剂组合物中是非常重要的,且在液体洗涤剂配方中也是个重要的助洗剂成份。硅铝酸盐助洗剂包括具有下述经验式的那些物质:
Mz/n[(AlO2)z(SiO2)y]xH2O其中z和y是至少为6的整数,z与y的摩尔比在1.0-0,且x为0-264的整数,和M是具有化合价n的IA和IIA族元素,例如钠、钾、镁、钙。
有用的硅铝酸盐离子交换物质是可买到的。这些硅铝酸盐在结构上可以是结晶的或无定型的,且可以是天然产生的硅铝酸盐或合成的。US3985669描述了一种用于生产硅铝酸盐离子交换物质的方法。用于本发明的优选的合成结晶硅铝酸盐离子交换物质可在ZeoliteA、Zeolite P(B)、Zeolite MAP和Zeolite X的牌号下得到。在特别优选的实施方案中,结晶硅铝酸盐离子交换物质具有结构式:
Na12[(AlO2)12(SiO2)12]xH2O,其中x为20-30,特别是27。该物质已知为Zeolite A.脱水沸石(x=0-10)可用于本发明。硅铝酸盐的颗粒尺寸优选为直径0.1-10微米。
适用于本发明的有机洗涤剂助洗剂包括,但不限制于,各种多羧酸盐化合物,用于本发明的“多羧酸盐”是指具有许多羧酸盐基团,优选为至少3个羧酸盐基团的化合物。多羧酸盐助洗剂一般以酸性形式加入组合物中,但也可以中和盐的形式加入。当以盐的形式使用时,碱金属,如钠、钾和锂的盐,或烷醇铵盐是优选的。
多羧酸盐包括各种有用物质的种类,一个重要种类的多羧酸盐助洗剂包括醚多羧酸盐助洗剂,包括氧联二琥珀酸盐,US3128287和US3635830中所述。还参见US4663071中的“TMS/TDS”助洗剂;合适的醚多羧酸盐还包括环状化合物,尤其是脂环族化合物,如在US3923679、3835163、4158635、4120874和4102903中所描述的那些化合物。
其它合适的洗涤剂助洗剂包括醚羟基多羧酸,马来酸酐与乙烯或乙烯基甲醚的共聚物,1,3,5-三羟基苯-2,4,6-三磺酸;和羧甲基氧联琥珀酸;多乙酸如乙二胺四乙酸和次氮基三乙酸的各种碱金属、铵和取代铵盐;以及多羧酸,例如苯六甲酸、均苯四酸、琥珀酸、氧联二琥珀酸、多马来酸、苯1,3,5-三羧酸、羧甲基氧联琥珀酸,及其水溶盐。
由于柠檬酸盐助洗剂,如柠檬酸及其水溶盐(特别是钠盐)由可再生资源得到和可生物降解性,对于重垢液体洗涤剂配方来说,它们是特别重要的多羧酸盐助洗剂。柠檬酸盐也可用于颗粒组合物中,特别是与沸石和/或层状硅酸盐助洗剂混合使用。氧联二琥珀酸盐在这种组合物和混合物中也是特别有用的。
在US4566984中所披露的3,3-二羧基-4-氧杂-1,6-己二酸酯和相关化合物也适合于本发明洗涤组合物。有用的琥珀酸助洗剂包括C5-C20烷基和链烯基琥珀酸及其盐。特别优选的这种化合物是十二碳烯基琥珀酸。琥珀酸助洗剂的具体例子包括:月桂基琥珀酸、十四烷基琥珀酸、十六烷基琥珀酸、2-十二碳烯基琥珀酸(优选)、2-十五碳烯基琥珀酸等。月桂基琥珀酸是其中优选的,它在EP0200263中描述。
其它合适的多羧酸盐在US4144226和US3308067中描述。还参见US3723322。
脂肪酸,如C12-C18单羧酸,例如油酸和/或其盐也可单独地,或与前述助洗剂,特别是柠檬酸盐和/或琥珀酸盐助洗剂混合加入组合物中以产生附加的助洗剂活性。脂肪酸的这种用途可导致泡沫减少,这是配制者应该考虑到的。
在可使用磷基助洗剂的场合中,且特别是在用于手工洗衣的块配方中,可以使用各种碱金属磷酸盐,如已知的三聚磷酸钠、焦磷酸钠和正磷酸钠。也可使用膦酸盐助洗剂,如乙烷-1-羟基-1,1-二膦酸盐和其它已知的膦酸盐(参见,例如US3159581、3213030、3422021、3400148和3422137)。漂白化合物-漂白剂和漂白活性剂
本发明的洗涤剂组合物可选择性地含有漂白剂或含有漂白剂和一种或多种漂白活性剂的漂白组合物。如果存在,尤其是用于织物洗涤时,漂白剂的含量一般为洗涤剂组合物的1%-30%,更常用为5%-20%。如果存在的话,漂白活性剂的数量一般为含有漂白剂和漂白活性剂的漂白组合物的0.1%-60%,更一般地为0.5%-40%。
用于本发明的漂白剂可以是在织物洗涤或其它已知或将要已知的洗涤应用中对洗涤剂组合物有用的任何漂白剂。这些包括氧漂白剂以及其它漂白剂,例如次氯酸盐漂白剂。本发明可以使用过硼酸盐漂白剂,如过硼酸钠(如单-或四-水过硼酸钠)。当使用次氯酸盐时,更优选的次氯酸盐漂白组分是碱金属次氯酸盐。尽管碱金属次氯酸盐是优选的,但其它次氯酸盐也可用于本发明中,其选自次氯酸钙和镁。优选的用于本发明的碱金属次氯酸盐是次氯酸钠。
可不受限制地使用的另一种类的漂白剂包括过羧酸漂白剂及其盐。这种漂白剂的合适例子包括六水单过氧化邻苯二甲酸镁、偏氯过苯甲酸的镁盐、4-壬氨基-4-氧基过氧化丁酸和二过氧化十二烷二酸。US4483781、US740446、EP0133354和US4412934披露了这种漂白剂。更优选的漂白剂还包括6-壬氨基-6-氧基过氧化己酸,这在US4634551中描述。
也可使用过氧漂白剂。合适的过氧漂白化合物包括过氧水合碳酸钠和相应的“过碳酸盐”漂白剂、过氧水合焦磷酸钠、过氧水合脲和过氧化钠。也可使用过硫酸盐漂白剂(如工业上由DuPont生产的OXONE)。
优选的过碳酸盐漂白剂包括平均颗粒直径在500微米-1000微米范围内的干燥颗粒,其中不多于按重量计10%的所述颗粒小于200微米,且不多于按重量计10%的所述颗粒大于1250微米。可选择性地用硅酸盐、硼酸盐或水溶性表面活性剂涂覆过碳酸盐。过碳酸盐可从各种商业途径,如FMC、Solvay和Tokai Denka获得。
也可以使用漂白剂混合物。
过氧漂白剂、过硼酸盐、过碳酸盐等优选与漂白活性剂混合,其中活性剂可导致在水溶液(即在洗涤过程中)中就地生成与漂白活性剂相应的过氧酸。US4915854和US4412934披露了活性剂的各种非限制性例子。壬酰基氧苯磺酸酯(NOBS)、3,5,5-三甲基己酰基氧苯磺酸酯(ISONOBS)和四乙酰乙二胺(TAED)活性剂是典型的,也可使用其混合物。用于本发明的其它典型漂白剂和活性剂参见US4634551。
酰氨基衍生的漂白活性剂更优选是具有如下结构式的那些物质:R1N(R5)C(O)R2C(O)L或R1C(O)N(R5)R2C(O)L其中R1为含有6-12个碳原子的烷基,R2为含有1-6个碳原子的亚烷基,R5为H或含有1-10个碳原子的烷基、芳基或烷芳基,且L为任何合适的离去基团。离去基团是由过水解阴离子对漂白活性剂进行亲核进攻后从漂白活性剂中置换出的任何基团,优选的离去基团为苯磺酸根。
具有上式的漂白活性剂的优选例子包括(6-辛酰氨基-己酰基)氧联苯磺酸酯、(6-壬酰氨基己酰基)氧联苯磺酸酯、(6-癸酰氨基-己酰基)氧联苯磺酸酯及其混合物,这在US4634551中描述,列为本文参考文献。
另外一种优选的漂白活性剂包括酰基内酰胺活性剂,特别是具有如下结构式的酰基己内酰胺和酰基戊内酰胺:其中R6为H或含有1-12个碳原子的烷基、芳基、烷氧基芳基或烷芳基。更优选的内酰胺活性剂包括苯甲酰基己内酰胺、辛酰基己内酰胺、3,5,5-三甲基己酰基己内酰胺、壬酰基己内酰胺、癸酰基己内酰胺、十一烷酰基己内酰胺、苯甲酰基戊内酰胺、辛酰基戊内酰胺、癸酰基戊内酰胺、十一烷酰基戊内酰胺、壬酰基戊内酰胺、3,5,5-三甲基己酰基戊内酰胺及其混合物。另外参见1985年10月8日颁布的Sanderson的US4545784(列为本文参考文献),它披露了吸附到过硼酸钠中的包括苯甲酰基己内酰胺在内的酰基己内酰胺。
除了氧漂白剂之外的漂白剂在本领域中也是已知的,且可用于本发明。一种具有特殊价值的非氧漂白剂包括光活化漂白剂如磺化的锌和/或铝酞菁。参见US4033718。如果使用的话,洗涤剂组合物一般含有按重量计0.025%-1.25%的这种漂白剂,特别是磺化的锌酞菁。
如果需要,漂白化合物可用锰化合物进行催化。这种化合物在本领域中是已知的,并且包括,例如,披露于US5246621、US5244594、US5194416、US5114606,和EP549271A1、549272A1、544440A2和544490A1中的锰基催化剂。这种催化剂的优选实例包括MnIV 2(u-O)3(1,4,7-三甲基-1,4,7-三氮杂环壬烷)2(PF6)2、MnIII 2(u-O)1(u-OAc)2(1,4,7-三甲基-1,4,7-三氮环杂壬烷)2(ClO4)2、MnIV 4(u-O)6(1,4,7-三氮杂环壬烷)4(ClO4)4、MnIIIMnIV 4(u-O)1(u-OAc)2(1,4,7-三甲基-1,4,7-三氮杂环壬烷)2(ClO4)3、MnIV(1,4,7-三甲基-1,4,7-三氮杂环壬烷)2-(OCH3)3(PF6)及其混合物。其它的金属基漂白催化剂包括US4430243和US5114611中所披露的那些。以下US4728455、5284944、5246612、5256779、5280117、5274147、5153161和5227084也报道了使用镁和各种络合配位体以提高漂白性能。
实际上,且不为了限制,可对本发明的组合物和方法进行调整以提供洗涤水溶液中含有至少一千万分之一份的活性漂白催化剂物质,且优选在洗涤液中含有0.1ppm-700ppm,更优选为1ppm-500ppm的催化剂物质。增白剂
本发明的组合物还可选择性地含有按重量计0.005%至5%的某些类型的亲水荧光增白剂,它也提供了染料转移抑制作用。如果使用,本发明的组合物优选含有按重量计0.001%-1%的该荧光增白剂。
在本发明中使用的亲水荧光增白剂具有如下结构式:其中R1选自苯胺基、N-2-双羟基乙基和NH-2-羟基乙基;R2选自N-2-双-羟基乙基、N-2-羟基乙基-N-甲基氨基、吗啉代、氯和氨基;M是成盐阳离子,例如钠或钾。
当在上述式中,R1是苯胺基,R2是N-2-双-羟基乙基和M是阳离子,例如钠时,增白剂是4,4’-双[(4-苯胺基-6-(N-2-双-羟基乙基)-s-三嗪-2-基)氨基]-2,2’-茋二磺酸和二钠盐。具体的增白剂物质在商业上由Ciba-Geigy公司以商品名Tinopal-UNPA-GX销售。Tinopal-UNPA-GX是用于本发明在漂洗时加入的组合物中的优选亲水荧光增白剂。
当在上述式中,R1是苯胺基,R2是N-2-羟基乙基-N-2-甲基氨基和M是阳离子,例如钠时,增白剂是4,4’-双[(4-苯胺基-6-(N-2-羟基乙基-N-甲基氨基)-s-三嗪-2-基)氨基]-2,2’-茋二磺酸二钠盐。具体的增白剂物质在商业上由Ciba-Geigy公司以商品名Tinopal 5BM-GX销售。
当在上述式中,R1是苯胺基,R2是吗啉代和M是阳离子,例如钠时,增白剂是4,4’-双[(4-苯胺基-6-吗啉代-s-三嗪-2-基)氨基]2,2’-茋二磺酸二钠盐。具体增白剂在商业上由Ciba-Geigy以商品名TinopalAMS-GX销售。去污剂
在本发明中,可加入选择性的去污剂,去污剂在组合物中加入的典型含量为0%-10%,优选为0.2%-5%,该去污剂优选是聚合物。
去污剂合乎需要地用于本发明的织物柔软组合物中,本领域中技术人员已知的任何聚合去污剂可选择性地用于本发明的组合物中。聚合去污剂的特征在于同时含有用于使疏水纤维,例如聚酯和尼龙表面亲水化的亲水片段和沉积在疏水纤维上,在整个洗涤和漂洗周期完成后保持粘附于纤维上,因而用作亲水片段的固定剂的疏水片段。这能够确保用去污剂处理的污渍在以后的洗涤过程中更易除去。
如果使用,去污剂通常占本发明洗涤剂组合物的约0.01%-约10.0%,常见的为约0.1%-约5%,优选约0.2%-约3.0%。
如下的本文参考文献描述了适用于本发明的去污聚合物。1976年5月25日颁布的Hays的US3959230;1975年7月8日颁布的Basadur的US3893929;1976年12月28日颁布的Nicol等的US4000093;1987年10月日27颁布的Gosselink的US4702857;11月6日颁布的Scheibel等的US4968451;1987年10月日27颁布的Gosselink的US4702857;1987年12月8日颁布的Gosselink等的US4711730;1988年1月26日颁布的Gosselink的US4721580;1989年10月31日颁布的Maldonado等的US4877896;1990年9月11日颁布的Gosselink等的US4956447;1995年5月16日颁布的Gosselink等的US5415807;1987年4月22日公开的Kud等的EP0219048。
其它合适的去污剂在如下本文参考文献中描述:Violland等的US4201824;Lagasse等的US4240918;Tung等的US4525524;Ruppert等的US4579681;US4240918;US4787989;US4525524;Rhone-PoulencChemie的EP279134A,1988;BASF的EP457205A(1991);和UnileverN.V.,1974,DE2335044。
商业上可获得的去污剂包括由Shin-etsu Kagaku Kogyo K.K.生产的METOLOSE SM100,METOLOSE SM200,SOKALAN类物质,例如SOKALAN HP-22,由BASF(德国)得到,ZELCON 5126(Dupont)和MILEASET(ICI)。浮垢分散剂
在本发明中,预混合物可与除去污剂之外的选择性浮垢分散剂混合,并加热至或高于组分的熔点。
本发明优选的浮垢分散剂通过高度乙氧基化疏水物质形成。疏水物质可以是脂肪醇、脂肪酸、脂肪胺、脂肪酸酰胺、氧化胺、季铵化合物或用于形成去污聚合物的疏水基团。优选的浮垢分散剂是高度乙氧基化的,例如每分子平均超过17,优选超过25,更优选超过40摩尔环氧乙烷,聚氧乙烯部分占总分子量的76%至97%,优选81%至94%。
浮垢分散剂的含量是在使用时浮垢足以保持在对消费者可接受的,优选不引人注意的,但不足以不利地影响柔软作用的含量。对于某些用途,要求不存在浮垢。根据在通常的洗衣过程的洗涤周期中使用的阴离子或非离子洗涤剂等的量、在加入本发明组合物之前漂洗步骤的效率和水的硬度,将改变在织物(衣服)中夹住的阴离子或非离子洗涤剂表面活性剂和洗涤剂助剂(尤其是磷酸盐和沸石)的量。通常,应使用最少量的浮垢分散剂以避免不利地影响柔软性能。基于柔软活性剂的含量,浮垢分散剂需要至少2%,优选至少4%(为最大地避免浮垢,至少6%,优选至少10%)。然而,在10%(相对于柔软剂物质)或更多的含量时,有损失产品柔软效果的风险,尤其是在织物含有高比例的在洗涤操作过程中吸附的非离子表面活性剂时。
优选的浮垢分散剂是Brij 700、Varonic U-250、GenapolT-500、Genapol T-800、Plurafac A-79和Neodol 25-50。杀菌剂
以按试剂重量计1至1000ppm用于本发明组合物中的杀菌剂的实例包括戊二醛、甲醛、由在Philadelphia,Pennsylvania的InolexChemicals以商品名称Bronopol销售的2-溴-2-硝基-丙-1,3-二醇,和由Rohm and Haas Company以商品名称Kathon销售的5-氯-2-甲基-4-异噻唑啉-3-酮和2-甲基-4-异噻唑啉-3-酮的混合物。香料
本发明可含有任何洗涤剂相容的香料。合适的香料在US5500138中公开,所述专利列为本文参考文献。
用于本文的香料包括香料物质或物质的混合物,包括天然(即通过提取开花植物、香草、叶、根、树皮、木材、花或植物得到)、人工(即不同天然油或油组分的混合物)和合成的(即合成得到的)带有气味的物质。该物质通过伴随着辅助物质,例如固定剂、补充剂、稳定剂和溶剂。这些辅助物质也包括在用于本文的“香料”的含义中。通常香料是许多种有机化合物的复杂混合物。
在本发明的香料中用作香料组分的实例包括,但并不限制于,己基肉桂醛、戊基肉桂醛、戊基水杨酸酯、己基水杨酸酯、萜品醇、3,7-二甲基-顺-2,6-辛二烯-1-醇、2,6-二甲基-2-辛醇、2,6-二甲基-7-辛烯-2-醇、3,7-二甲基-3-辛醇、3,7-二甲基-反-2,6-辛二烯-1-醇、3,7-二甲基-6-辛烯-1-醇、3,7-二甲基-1-辛醇、2-甲基-3-(对叔丁基苯基)-丙醛、4-(4-羟基-4-甲基戊基)-3-环己烯-1-甲醛、三环壬烯基丙酸酯、三环壬烯基乙酸酯、茴香醛、2-甲基-2-(对异丙基苯基)丙醛、乙基-3-甲基-3-苯基缩水甘油酸酯、4-(对羟基苯基)-丁-2-酮、1-(2,6,6-三甲基-2-环己烯-1-基)-2-丁烯-1-酮、对甲氧基苯乙酮、对甲氧基-α-苯基丙烯、甲基-2-正己基-3-氧代-环戊烷甲酸酯、γ十一烷酸内酯。
香料物质的其它实例包括,但不限制于,甜橙油、柠檬油、葡萄柚油、香柠檬油、丁香油、γ十二酸内酯、甲基-2-(2-戊基-3-氧代-环戊基)乙酸酯、β-萘酚甲基醚、甲基-β-萘基酮、香豆素、壬醛、苯甲醛、4-叔丁基环己基乙酸酯、α,α-二甲基苯乙基乙酸酯、甲基苯基甲醇基乙酸酯、4-(4-羟基-4-甲基戊基)-3-环己烯-1-基甲醛和甲基邻氨基苯甲酸酯的Schiff碱、十三烷二酸的环乙二醇二酯、3,7-二甲基-2,6-辛二烯-1-腈、γ-甲基紫罗兰酮、α-紫罗兰酮、β-紫罗兰酮、橙叶油、甲基雪松酮、7-乙酰基-1,2,3,4,5,6,7,8-八氢-1,1,6,7-四甲基-萘、甲基紫罗兰酮、甲基-1,6,10-三甲基-2,5,9-环十二碳三烯-1-基酮、7-乙酰基-1,1,3,4,4,6-六甲基四氢萘、4-乙酰基-6-叔丁基-1,1-二甲基二氢化茚、二苯酮、6-乙酰基-1,1,2,3,3,5-六甲基二氢化茚、5-乙酰基-3-异丙基-1,1,2,6-四甲基二氢化茚、1-十二烷醛、7-羟基-3,7-二甲基辛醛、10-十一碳烯-1-醛、异己烯基环己基甲醛、甲酰基三环壬烷、环十五酐、16-羟基-9-十六烯酸内酯、1,3,4,6,7,8-六氢-4,6,6,7,8,8-六甲基环戊-γ-2-苯并吡喃、ambroxane、十二氢-3a,6,6,9a-四甲基萘并-[2,1b]呋喃、雪松醇、5-(2,2,3-三甲基环戊-3-烯基)-3-甲基戊-2-醇、2-乙基-4-(2,2,3-三甲基-3-环戊烯-1-基)-2-丁烯-1-醇、石竹烯醇、雪松基乙酸酯、对叔丁基环己基乙酸酯、绿叶刺蕊草、乳香树脂、岩莰脂、爪哇香茅油、苦配巴香膏、加拿大香脂和缩合产物:羟基香茅酮和邻氨基苯甲酸甲酯、羟基香茅醛和吲哚、苯基乙醛和吲哚、4-(4-羟基-4-甲基戊基)-3-环己烯-1-甲醛和邻氨基苯甲酸甲酯。
香料组分的更多实施例是香叶醇、香叶基乙酸酯、里哪醇、里哪基乙酸酯、四氢里哪醇、香茅醇、香茅基乙酸酯、二氢月桂烯醇、二氢月桂烯基乙酸酯、四氢月桂烯醇、萜品基乙酸酯、诺卜醇、诺卜基乙酸酯、2-苯基乙醇、2-苯基乙基乙酸酯、苄醇、苄基乙酸酯、苄基水杨酸酯、苄基苯甲酸酯、肉桂基乙酸酯、二甲基苄甲醇、三氯甲基苯基甲醇基甲基苯基甲醇基乙酸酯、异壬基乙酸酯、岩半基乙酸酯、爪哇香茅醇、2-甲基-3-(对叔丁基萘基)-丙醛、2-甲基-3-(对异丙基萘基)-丙醛、3-(对叔丁基萘基)-丙醛、4-(4-甲基-3-苯乙基)-3-环己烯甲醛、4-乙酰氧基-3-戊基四氢吡喃、甲基二氢茉莉酸酯、2-正庚基环戊酮、3-甲基-2-戊基-环戊酮、正-壬醛、正十二醛、9-壬烯醇-1、苯氧基乙基异丁酸酯、苯基乙醛二甲基乙缩醛、苯基乙醛、二乙基乙缩醛、香叶腈、香茅腈、雪松基乙缩醛、3-异莰基环己醇、雪松基甲基醚、异长叶酮、茴香腈、茴香酸、胡椒醛、丁子香酸、香兰素、二苯基氧化物、羟基香茅酮紫罗兰酮、甲基紫罗兰酮、异甲基紫罗兰酮、甲基芷香酮、顺-3-己烯醇和它们的酯、二氢化茚麝香香料、四氢萘麝香香料、等色麝香香料、大环酮、大内酯麝香香料、亚乙基巴西基酸酯。
用于本发明的组合物的香料是基本上没有卤化物质和硝基麝香。
用于上述香料组分的合适溶剂、稀释剂或栽体包括乙醇、异丙醇、二甘醇单乙基醚、二丙二醇、邻苯二甲酸二乙酯、柠檬酸三乙酯等。该加入香料中的溶剂、稀释剂或载体的数量优选保持至提供均匀香料溶液所需的最小量。
香料可以按最终组合物重量计0%-10%,优选0.1%-5%,更优选0.2%-3%的含量存在,本发明的织物柔软剂组合物提供改善的织物香料沉积。螯合剂
本发明组合物和方法也可选择性地使用一种或多种铜和/或镍螯合剂。这种水溶性螯合剂可选自氨基羧酸盐,氨基膦酸盐,多官能团取代的芳香族螯合剂及其混合物,下文将对它们进行定义。通过该螯合剂明显改善或保持了织物的白度和亮度,改善在组合物中物质的稳定性。尽管不想受理论的局限,但我们认为这些物质的效果部分因为它们通过水溶性螯合物的形成从洗涤液中去除铁和锰离子。
可用作选择性螯合剂的氨基羧酸盐包括乙二胺四乙酸盐,N-羟乙基乙二胺三乙酸盐,次氮基三乙酸盐,乙二胺四丙酸盐,三亚乙基四胺六乙酸盐,二亚乙基三胺五乙酸盐和乙醇二甘氨酸,它们的碱金属、铵和取代铵盐,及其混合物。
当允许在洗涤剂组合物中使用至少低含量的总磷时,氨基膦酸盐也适合在本发明组合物中用作螯合剂,它包括乙二胺四(亚甲基膦酸盐),如DEQUEST。这些氨基膦酸盐优选不合多于6个碳原子的烷基或烯基。
多官能团取代的芳香族螯合剂也适合用于本发明组合物。参见1974年5月21日颁布的Connor等的US3812044。优选的酸态的这类化合物为二羟基二磺基苯,如1,2-二羟基-3,5-二磺基苯。
用于本发明的可生物降解的优选螯合剂是乙二胺二琥珀酸盐(“EDDS”),特别是如1987年11月3日颁布的Hartman和Perkins的US4704233中描述的[S,S]异构体。
本发明的组合物还可以含有水溶性甲基甘氨酸二乙酸(MGDA)盐(或酸式)作为螯合剂或与例如水不溶性助洗剂,例如沸石、层状硅酸盐等一起使用的辅助助洗剂。
优选螯合剂包括DETMP、DETPA、NTA、EDDS和它们的混合物。
如果使用,这些螯合剂一般为按本发明织物护理组合物重量的约0.1%-约15%。更加优选的是,如果使用,这些螯合剂为该组合物重量的约0.1%-约3.0%。结晶生长抑制剂组分
本发明的组合物还可含有结晶生长抑制剂组分,优选有机二膦酸组分,优选以按组合物重量计0.01%-5%,更优选0.1%-2%的含量加入。
有机二膦酸是指这样的有机二膦酸,它不含有氮作为其化学结构的部分。因此该定义排除了有机氨基膦酸盐,然而它可包括在本发明的组合物中作为重金属离子螯合剂。
有机二膦酸优选是C1-C4二膦酸,更优选C2二膦酸,例如亚乙基二膦酸,或最优选乙烷1-羟基-1,1-二膦酸(HEDP),可部分或全部离子化形式存在,尤其作为盐或配合物。
其它有用的结晶生长抑制剂是有机单膦酸。
有机单膦酸或其一种盐或配合物也适用作本文的CGI。
有机单膦酸是指这样的有机单膦酸,它不含有氮作为其化学结构的部分。因此该定义排除了有机氨基膦酸盐,然而它可包括在本发明的组合物中作为重金属离子螯合剂。
有机单膦酸组分可以酸形式或它与合适抗衡离子的一种盐或配合物的形式存在。优选任何盐/配合物是水溶性,碱金属和碱土金属盐/配合物是尤其优选的。
优选的有机单膦酸是2-膦酰基丁烷-1,2,4-三羧酸,商业上由Bayer以商品名Bayhibit得到。酶
本发明的组合物和方法可选择性地采用一种或多种酶,例如脂酶、蛋白酶、纤维素酶、淀粉酶和过氧化酶。用于本发明的优选酶是纤维素酶,事实上,这类酶还向所处理织物提供了颜色护理效果。用于本发明的纤维素酶包括细菌和真菌纤维素酶,它们优选具有5-9.5之间的pH最佳值。US4435307披露了由Humicola insolens或腐质霉菌株DSM1800或属于气单胞菌属的产生纤维素酶212-位的真菌得到的合适的真菌纤维素酶,以及从海生软体物Dolabella AuriculaSolander的肝胰腺提取的纤维素酶。GB-A-2075028、GB-A-2095275和DE-OS-2247832也披露了合适的纤维素酶。CAREZYME和CELLUZYME(Novo)是特别有用的。其它合适的纤维素酶在Novo的WO91/17243、WO96/34092、WO96/34945和EP-A-0739982中公开。在实际商业制剂中,典型的含量为每克洗涤剂组合物至多5mg(wt),更常见为0.01mg-3mg活性酶。换句话说,本发明的组合物将通常含有按重量计0.001%-5%,优选0.01%-1%商业酶制剂。在其中酶制剂的活性可以另一种方式定义的特殊情况下,例如对于纤维素酶,优选相应的活性单位(例如CEVU或纤维素酶等价粘度单位)。例如本发明的组合物可以相当于约0.5-1000CEVU/克组合物活性的含量含有纤维素酶。用于配制本发明的组合物的纤维素酶制剂通常在液体形式时具有1000-10000CEVU/克的活性,在固体形式时约1000CEVU/克。粘土
本发明的组合物可优选含有粘土,优选以按组合物重量计0.05%-40%,更优选0.5%-30%,最优选2%-20%的含量存在。为清楚起见,用于本文的术语粘土无机化合物排除硅铝酸钠沸石助洗剂化合物,然而它可作为选择性组分包括在本发明的组合物中。
一种优选的粘土可以是膨润土粘土,更优选是绿土粘土,例如由US3862058、3948790、3954632和4062647和EP-A-299575和EP-A-313146(均为P & G公司)中所述。
本文的术语绿土同时包括其中硅酸盐晶格中存在氧化铝的粘土和其中硅酸盐晶格中存在氧化镁的粘土。典型的绿土粘土化合物包括通式Al2(Si2O5)2(OH)2·nH2O的化合物和通式Mg3(Si2O5)2(OH)2·nH2O的化合物,绿土粘土趋向于采用可膨胀的三层结构。
合适绿土粘土的具体实例包括选自蒙脱石、水辉石、volchonskoite、囊脱石、滑石粉和sauconite,尤其是在结晶晶格结构中具有碱金属或碱土金属离子的粘土,钠或钙蒙脱石是尤其优选的。
合适的绿土粘土,尤其是蒙脱石由不同供应商销售,包括EnglishChina Clays、Laviosa、Georgia Kaolin和Colin StewartMinerals。
用于本文的粘土优选具有10nm-800nm,更优选20nm-500nm,最优选50nm-200nm的颗粒尺寸。
粘土无机化合物的微粒可作为含有其它洗涤剂化合物的附聚微粒的组分包括在内。当存在作为该组分时,术语粘土无机化合物的“最大微粒尺寸”是指粘土无机组分的最大尺寸,而不是作为整体的附聚微粒的尺寸。
在绿土粘土的结晶晶格结构中通常可发生小的阳离子,例如质子、钠离子、钾离子、镁离子和钙离子和某些有机分子,包括具有正电荷的官能团的取代。可选择一种能够优先吸附一种阳离子类型的粘土,该能力可通过测量相对离子交换能力评价。适用于本文的绿土通常具有至少50meq/100g的阳离子交换能力,US3954632描述了测量阳离子交换能力的方法。
粘土无机化合物的结晶晶格结构在优选实施中可含有在其中取代的阳离子织物柔软剂。该取代的粘土称为‘疏水活化的’粘土。阳离子织物柔软剂通常以阳离子织物柔软剂∶粘土为1∶200-1∶10、优选1∶100-1∶20的重量比存在。合适的阳离子织物柔软剂包括水溶性叔胺或二长链酰胺物质,如GB-A-1514276和EP-B-0011340中描述。
优选的商业可得到的‘疏水活化的’粘土是含有按重量计约40%的二甲基动物脂基季铵盐的膨润土,由English China ClaysInternational以商品名Claytone EM出售。
在本发明的更优选的实施方案中,粘土在与湿润剂和疏水化合物,优选石蜡或油,例如石蜡油形成的紧密混合物或微粒中存在。优选的湿润剂是有机化合物,包括丙二醇、乙二醇、乙二醇的二聚物或三聚物,最优选甘油,微粒优选是附聚物。此外,微粒可以是蜡或油和选择性的湿润剂在粘土上形成胶囊或此外,粘土是蜡或油和湿润剂的胶囊,优选的是微粒包含有机盐或氧化硅或硅酸盐。
然而,在本发明的另一实施方案中,粘土优选与一种或多种表面活性剂和选择性地助洗剂和选择性地水混合,在该情况下混合物优选随后干燥。优选该混合物进一步在喷雾干燥方法中加工以得到含有粘土的喷雾干燥的微粒。
在含有粘土的微粒或颗粒中优选还包含絮凝剂。
它还可以优选紧密混合物包含螯合剂。絮凝剂
本发明的组合物可含有粘土絮凝剂,优选以按组合物重量计0.005%-10%,更优选0.05%-5%,最优选0.1%-2%的含量存在。
粘土絮凝剂起作用使得在洗涤溶液中粘土化合物的微粒结合在一起,因此有助于它们沉积在洗涤的织物表面。该功能要求因此不同于粘土分散化合物,它通常加入洗衣洗涤剂组合物中以有助于除去由织物除去泥土污垢和使它们在洗涤溶液中分散。
作为粘土絮凝剂优选的是平均分子量100,000-10,000,000,优选150,000-5,000,000,更优选200,000-2,000,000的有机聚合物。
合适有机聚合物包括含有单体单元的均聚物或共聚物,所述单体选自烯化氧,尤其是环氧乙烷、丙烯酰胺、丙烯酸、乙烯基醇、乙烯基吡咯烷酮和乙烯亚胺。尤其是环氧乙烷,及丙烯酰胺和丙烯酸的均聚物是优选的。
EP-A-299575和EP-A-313146(P & G公司)描述了用于本文的优选有机聚合物粘土絮凝剂。
粘土与絮凝剂的重量比优选是1000∶1-1∶1,更优选500∶1-1∶1,最优选300∶1-1∶1,或更加优选80∶1-10∶1,或在某些应用中甚至60∶1-20∶1。
无机粘土絮凝剂也适用于本文,其典型实例包括石灰和明矾。
絮凝剂优选存在于洗涤剂基础颗粒中,例如洗涤剂附聚物、挤出物或喷雾干燥微粒,它们通常含有一种或多种表面活性剂和助洗剂。泡腾剂
泡腾物质也可选择性地用于本发明的组合物中。
本文定义的泡腾是指由液体挥发气泡,这是由于水溶性酸源和碱金属碳酸盐之间化学反应形成二氧化碳气体的结果。即
酸和碳酸盐源和其它泡腾体系的其它实例可在(PharmaceuticalDosage Forms:Tablets Volume 1 287-291页)中找到。碳酸盐
适用于本文的碱金属和/或碱土金属碳酸盐包括钾、锂、钠等的碳酸盐和碳酸氢盐,其中碳酸钠和钾是优选的。适用于本文的碳酸氢盐包括碳酸氢盐的任何碱金属盐,如锂、钠、钾等,其中碳酸氢钠和钾是优选的。然而,碳酸盐和碳酸氢盐或它们的混合物的选择取决于在其中溶解颗粒的含水介质的所需pH。例如当在含水介质中需要相对高的pH(例如超过pH9.5),可优选单独使用碳酸盐或使用碳酸盐和碳酸氢盐的混合物,其中碳酸盐的含量高于碳酸氢盐的含量。本发明的组合物的无机碱金属和/或碱土金属碳酸盐优选包含碳酸盐和/或碳酸氢盐的钾盐或更优选钠盐,碳酸盐优选包含碳酸钠,选择性地还有碳酸氢钠。
无机碳酸盐优选以按组合物重量计至少20%的含量存在,优选它们以按重量计至少23%或甚至25%或甚至30%,优选至多约按重量计60%或更优选至多55%或甚至按重量计50%的含量存在。
它们可完全或部分地作为单独的粉末或颗粒组分或作为与其它洗涤剂组分,例如其它盐或表面活性剂的共颗粒加入,在本发明的固体洗涤剂组合物中,它们还可完全或部分地存在于洗涤剂颗粒中,例如附聚物或喷雾干燥颗粒。
在本发明的一个实施方案中,存在泡腾剂源,优选包含有机酸,例如羧酸或氨基酸和碳酸盐,因此,优选的是部分或全部碳酸盐与有机酸预混合,因而存在于单独的颗粒组分中。
优选的泡腾剂源选自柠檬酸和碳酸盐并选择性地与粘合剂的压制微粒;和碳酸盐、碳酸氢盐和苹果酸或马来酸以重量比4∶2∶4的微粒,优选采用柠檬酸和碳酸盐的干添加形式。
碳酸盐可具有任何颗粒尺寸,在一实施方案中,尤其当碳酸盐存在于颗粒中和不作为单独加入的化合物时,碳酸盐优选具有5-375微米的体积平均颗粒尺寸,从而按体积计优选至少60%,优选至少70%或甚至至少80%或甚至至少90%具有1-425微米的颗粒尺寸。更优选二氧化碳源具有10-250微米的体积平均颗粒尺寸,从而按体积计优选至少60%,或甚至至少70%或甚至至少80%或甚至至少90%具有1-375微米的颗粒尺寸;或更优选10-200微米的颗粒尺寸,从而按体积计优选至少60%,优选至少70%或甚至至少80%或甚至至少90%具有1-250微米的颗粒尺寸。
尤其当碳酸盐作为单独的组分加入,比如‘干燥加入’或与其它洗涤剂组分混合时,碳酸盐可具有任何颗粒尺寸,包括上述的特定颗粒尺寸,但优选至少200微米,或甚至250微米或甚至300微米的体积平均颗粒尺寸。
优选所需颗粒尺寸的二氧化碳源是通过研磨较大颗粒尺寸的物质,随后选择性地用任何合适的方法选择所需颗粒尺寸的物质得到。
虽然过碳酸盐可作为漂白剂存在于本发明的组合物中,它们不包括在本文定义的碳酸盐中。
其它优选的选择性组分包括酶稳定剂、聚合物去污剂、在洗涤过程中有效抑制染料由一织物转移到另一织物上的物质(即染料转移抑制剂)、聚合物分散剂、抑泡剂、荧光增白剂或其它增白或增亮剂、抗静电剂、其它活性组分、载体、增溶剂、加工助剂、染料或颜料、用于溶液配方的溶剂和用于块组合物的固体填料。组合物的形式
本发明的组合物可采用各种物理形式,包括液体、凝胶、含水或非水形式的泡沫、颗粒和片形式。
液体洗涤剂组合物可含有水和其它溶剂作为载体,低分子量伯或仲醇,例如甲醇、乙醇、丙醇和异丙醇是合适的,单羟基醇优选用于增溶表面活性剂,但也可使用多醇,例如含有2-6个碳原子和2-6个羟基的物质(例如1,3-丙二醇、乙二醇、甘油和1,2-丙二醇)。组合物可含有5%-90%,通常10%-50%的这种载体。
颗粒洗涤剂可例如通过喷雾干燥(最终产物密度520g/l)或附聚(最终产物密度超过600g/l)基础颗粒制备,其余的干组分随后可以颗粒或粉末形式与基础颗粒混合,例如在旋转混合转筒中混合,而液体组分(例如非离子表面活性剂和香料)可喷洒。
本发明的洗涤剂组合物优选配制成在用于含水洗涤操作时洗涤水将具有6.5-11,优选7.5-10.5的pH,洗衣产品通常为pH9-11。用于控制pH在所需范围的技术包括使用缓冲剂、碱、酸等,是本领域技术人员已知的。
当在液体形式时,组合物还可用分散装置,例如喷雾分散器或气溶胶分散器分散。喷雾分散器
本发明还涉及加入喷雾分散器以产生制造产品的组合物,它可有助于用含有胺反应产物和其它组分(例如环糊精、多糖、聚合物、表面活性剂、香料、柔软剂)的所述组合物以有效、但在表面干燥时仍不被识别的含量处理织物和/或表面。喷雾分散器包括手工驱动和非手工动力(操作)的喷雾装置和含有处理组合物的容器。该喷雾分散器的典型公开内容在WO96/04940,19页21行-22页27行中找到。制造的产品优选是与使用的规程有关以确保消费者施用足够的组合物的组分以提供所需的效果。由喷雾器分散的典型组合物含有按使用组合物重量计约0.01%-约5%,优选约0.05%-约2%,更优选约0.1%-约1%的胺反应产物含量。使用方法
本发明的组合物适用于家庭处理的任何步骤,即它是预处理组合物、洗衣添加剂、适用于洗衣和清洁过程的组合物。显然,可进行复合施用,如用本发明预处理组合物处理织物,随后用适于洗衣过程的组合物处理。
本发明还提供一种用于提供活性酮或醛的延迟释放的方法,其包括使需要处理的表面与本发明的化合物或组合物接触的步骤,和随后使所处理的表面与物质,优选含水介质,如水分接触或易于由胺反应产物释放香料的任何其它方法。
“表面”是指化合物可沉积在上面的任何表面,该物质的典型实例是织物、硬表面,例如餐具、地板、浴室、厕所、厨房和其它需要香料酮和/或醛的延迟释放的其它表面,例如担架,如动物担架。优选表面选自织物、瓷砖、陶瓷制品,更优选织物。
“延迟释放”是指与使用活性组分(例如香料)本身相比在较长的时间内释放活性组分(例如香料)。
用于如下洗衣和清洁组合物实施例的缩写
在洗衣和清洁组合物中,缩写组分说明具有如下含义:
在洗涤剂组合物中,缩写组分说明具有如下含义LAS :直链C11-13烷基苯磺酸钠TAS :动物脂烷基硫酸钠CXYAS :C1x-C1y烷基硫酸钠C46SAS :C14-C16仲(2,3)烷基硫酸钠CXYEZS :与z摩尔环氧乙烷缩合的C1x-C1y烷基硫酸钠CXYEZ :与平均z摩尔环氧乙烷缩合的主要C1x-C1y直链伯醇QAS :R2·N+(CH3)2(C2H4OH),R2=C12-C14QAS1 :R2·N+(CH3)2(C2H4OH),R2=C8-C11APA :C8-C10酰氨基丙基二甲基胺皂 :由动物脂和椰子油脂肪酸的80/20混合物得到的直链
烷基羧酸钠STS :甲苯磺酸钠CFAA :C12-C14(椰子)烷基N-甲基葡糖酰胺TFAA :C16-C18烷基N-甲基葡糖酰胺TPKFA :C12-C14拔顶全馏分脂肪酸STPP :无水三聚磷酸钠TSPP :焦磷酸四钠沸石A :式Na12(AlO2SiO2)12·27H2O的水合硅铝酸钠,主要颗粒
尺寸为0.1-10微米(基于无水基准表示的重量)NaSKS-6 :式δ-Na2Si2O5的结晶层状硅酸盐柠檬酸 :无水柠檬酸硼酸盐 :硼酸钠碳酸盐 :无水碳酸钠,颗粒尺寸200-900微米碳酸氢盐 :无水碳酸氢钠,颗粒尺寸分布为400-1200微米硅酸盐 :无定形硅酸钠(SiO2∶Na2O比率=2.0∶1)硫酸盐 :无水硫酸钠硫酸镁 :无水硫酸镁柠檬酸盐 :柠檬酸三钠二水合物,活性86.4%,颗粒尺寸分布
425-850微米MA/AA :1∶4马来酸/丙烯酸共聚物,平均分子量约70000MA/AA(1) :4∶6马来酸/丙烯酸共聚物,平均分子量约10000AA :平均分子量为4500的聚丙烯酸钠聚合物CMC :羧甲基纤维素钠纤维素醚 :甲基纤维素醚,聚合程度650,由Shin Etsu
Chemicals获得蛋白酶 :蛋白分解酶,含有按重量计3.3%活性酶,由Novo
Industries A/S以商品名Savinase销售蛋白酶1 :蛋白分解酶,含有按重量计4%活性酶,如WO95/10591
中所述,由Genencor Int.Inc.销售Alcalase :蛋白分解酶,含有按重量计5.3%活性酶,由Novo
Industries A/S销售纤维素酶 :纤维素分解酶,含有按重量计0.23%活性酶,由Novo
Industries A/S以商品名Carezyme销售淀粉酶 :淀粉分解酶,含有按重量计1.6%活性酶,由Novo
Industries A/S以商品名Termamyl 120T销售脂酶 :脂解酶,含有按重量计2.0%活性酶,由Novo
Industries A/S以商品名Lipolase销售脂酶(1) :脂解酶,含有按重量计2.0%活性酶,由Novo
Industries A/S以商品名Lipolase Ultra销售Endolase :内葡聚糖酶,含有按重量计1.5%活性酶,由Novo
Industries A/S销售PB4 :通式为NaBO2·3H2O·H2O2的过硼酸钠四水合物PB1 :通式为NaBO2·H2O2的无水过硼酸钠漂白剂过碳酸盐 :通式2Na2CO3·3H2O2的过碳酸钠NOBS :壬酰氧基苯磺酸盐,钠盐形式NAC-OBS :(6-壬酰氨基己酰基)氧苯磺酸盐TAED :四乙酰基乙二胺DTPA :二亚乙三胺五乙酸DTPMP :二亚乙三胺五(亚甲基膦酸),由孟山都以商品名
Dequest 2060销售EDDS :乙二胺-N,N’-二琥珀酸,(S,S)异构体,钠盐形式光活化漂 :在糊精溶解的聚合物中包胶囊的磺化锌酞菁白剂(1)光活化漂 :在糊精溶解的聚合物中包胶囊的磺化铝酞菁白剂(2)增白剂1 :4,4’-二(2-磺基茋)联苯二钠增白剂2 :4,4’-二(4-苯胺基-6-吗啉-1,3,5-三嗪-2-基)氨基)
茋-2:2’-二磺酸二钠HEDP :1,1-羟基乙烷二膦酸PEGx :聚乙二醇,分子量x(通常4000)PEO :聚环氧乙烷,平均分子量50000TEPAE :四亚乙五胺乙氧基化物PVI :聚乙烯咪唑,平均分子量为20000PVP :聚乙烯吡咯烷酮,平均分子量为60000PVNO :聚乙烯基吡啶-N-氧化物聚合物,平均分子量为50000PVPVI :乙烯基吡咯烷酮的乙烯基咪唑共聚物,平均分子量为
20000QEA :双((C2H5O)(C2H4O)n)(CH3)-N+-C6H12-N+-(CH3) 双
((C2H5O)-(C2H4O))n,其中n=20-30SRP1 :阴离子封端的聚酯SRP2 :二乙氧基化聚(1,2亚丙基邻苯二甲酸酯)短链嵌段聚
合物PEI :聚乙烯亚胺,平均分子量1800,每个N7个亚乙氧基
残基的平均乙氧基化程度聚硅氧烷 :用硅氧烷-氧化烯共聚物为分散剂的聚二甲基硅氧烷消泡剂 泡沫控制剂,所述泡沫控制剂与所述分散剂的比率为
10∶1-100∶1遮光剂 :水基单体苯乙烯乳胶混合物,由BASF以商品名
Lytron621销售蜡 :石蜡PA30 :平均分子量为约4500-8000的聚丙烯酸480N :7∶3丙烯酸酯/甲基丙烯酸酯无规共聚物,平均分子量
约3500Polygel/c :高分子交联聚丙烯酸酯arbopol偏硅酸盐 :偏硅酸钠(SiO2∶Na2O比率=1.0)非离子表 :C13-C15混合乙氧基化/丙氧基化脂肪醇,平均乙氧基化面活性剂 :程度3.8,平均丙氧基化程度4.5Neodol :C14-C15直链伯醇乙氧基化物,由Shell Chemical CO销45-13 售MnTACN :1,4,7-三甲基-1,4,7-三氮杂环壬烷合锰PAAC :五胺乙酸钴(III)盐石蜡 :由Wintershall以商标Winog70出售的石蜡油NaBz :苯甲酸钠BzP :苯甲酰基过氧化物SCS :枯烯磺酸钠BTA :苯并三唑pH :在20℃用在蒸馏水中的1%溶液测定ARP1 :1,4-二(3-氨基丙基)哌嗪与α-二氢大马酮的胺反应
产物,由合成实施例I制备ARP2 :N,N’二(氨基丙基)1,3-丙二胺与δ-二氢大马酮的胺反
应产物,由合成实施例II制备ARP3 :聚乙烯基胺MW1200与α-二氢大马酮的胺反应产物,由
合成实施例III制备粘土I :膨润土粘土粘土II :绿土粘土絮凝剂I :平均分子量200000-400000的聚环氧乙烷絮凝剂II :平均分子量400000-1000000的聚环氧乙烷絮凝剂III :平均分子量200000-400000的丙烯酰胺和/或丙烯酸
的聚合物DOBS :癸酰基氧联苯磺酸盐,钠盐形式SRP3 :多糖去污聚合物SRP4 :非离子封端的聚酯
如下是本发明中定义的化合物的合成实施例:I-1,4-二(3-氨基丙基)哌嗪与α-二氢大马酮的合成
为用香料取代两个伯胺基团,对于1当量氨基官能团聚合物使用2当量香料。向冰冷却的在6ml乙醇中的1mmolα-二氢大马酮和分子筛(4,20g)的搅拌溶液中用添加漏斗加入0.5eq 1,4-二(3-氨基丙基)哌嗪,将反应混合物在氮气和避光下搅拌。在游离香料原料的NMR谱吸收峰消失后(3-16小时),过滤混合物,真空蒸馏除去溶剂,β-氨基酮的形成收率约90%。
当α-二氢大马酮被Tripal、vertocitral、bourgeonal或香茅醛代替时得到类似的结果,在这种情况下形成Schiff碱。II-N,N’(3-氨基丙基)-1,3-丙二胺与δ-二氢大马酮的合成
向冰冷却的在30ml乙醇中的1mmolδ-二氢大马酮和分子筛(4,5g)的搅拌溶液中用添加漏斗加入0.5eqN,N’-二(3-氨基丙基)-1,3-丙二胺,将反应混合物在氮气和避光下搅拌。1天后,分别用过滤和真空蒸馏除去分子筛和溶剂,以85-90%的收率得到β-氨基酮。
当δ-二氢大马酮被Tripal、vertocitral、bourgeonal或香茅醛代替时得到类似的结果,在这种情况下形成Schiff碱。III-MW1200的聚乙烯基胺与α-二氢大马酮的合成
混合如下组分:0.6g硫酸钠与0.3g聚乙烯基胺MW1200的10%水溶液与0.3gα-二氢大马酮,在室温下在黑暗中,18天后反应完成。
当α-二氢大马酮被Tripal、vertocitral、bourgeonal或香茅醛代替时得到类似的结果,在这种情况下形成Schiff碱。
在如下配方实施例中,所有含量用按组合物重量计的%表示,除非另有说明。在全配制的组合物中加入下文所谓的“ARP”胺反应产物通过如GB-1464616中所述干添加(d)、喷洒(s)、在淀粉(es)或环糊精(ec)中包胶囊进行或在如上述所定义的组合物中。在配方实施例中在ARP的括号内的术语是指加入方法,如果未提供,实际上进行原样加入。无论加式与否,所给出的ARP的含量是指ARP本身而不是加工的ARP的含量。实施例1
根据本发明制备如下高密度颗粒洗衣洗涤剂组合物:
实施例2
A | B | C | D | E | F | G | |
LAS | 8.0 | 8.0 | 8.0 | 2.0 | 6.0 | 6.0 | 5.0 |
TAS | - | 0.5 | - | 0.5 | 1.0 | 0.1 | 1.5 |
C46(S)AS | 2.0 | 2.5 | - | - | - | - | - |
C25AS | - | - | - | 7.0 | 4.5 | 5.5 | 2.5 |
C68AS | 2.0 | 5.0 | 7.0 | - | - | - | 0.2 |
C25E5 | - | - | 3.4 | 10.0 | 4.6 | 4.6 | 2.6 |
C25E7 | 3.4 | 3.4 | 1.0 | - | - | - | - |
C25E3S | - | - | - | 2.0 | 5.0 | 4.5 | 0.5 |
QAS | - | 0.8 | - | - | - | - | - |
QAS(l) | - | - | - | 0.8 | 0.5 | 1.0 | 1.5 |
沸石A | 18.1 | 18.0 | 14.1 | 18.1 | 20.0 | 18.1 | 16.2 |
柠檬酸 | - | - | - | 2.5 | - | 2.5 | 1.5 |
碳酸盐 | 13.0 | 13.0 | 27.0 | 10.0 | 10.0 | 13.0 | 20.6 |
SKS-6 | - | - | - | 10.0 | - | 10.0 | 4.3 |
硅酸盐 | 1.4 | 1.4 | 3.0 | 0.3 | 0.5 | 0.3 | - |
柠檬酸盐 | - | 1.0 | - | 3.0 | - | - | 1.4 |
硫酸盐 | 26.1 | 26.1 | 26.1 | 6.0 | - | - | - |
硫酸镁 | 0.3 | - | - | 0.2 | - | 0.2 | 0.03 |
A | B | C | D | E | F | G | |
MA/AA | 0.3 | 0.3 | 0.3 | 4.0 | 1.0 | 1.0 | 0.6 |
CMC | 0.2 | 0.2 | 0.2 | 0.2 | 0.4 | 0.4 | 0.3 |
PB4 | 9.0 | 9.0 | 5.0 | - | - | - | - |
过碳酸盐 | - | - | - | - | 18.0 | 18.0 | 9.0 |
TAED | 1.5 | 0.4 | 1.5 | - | 3.9 | 4.2 | 3.2 |
NAC-OBS | - | 2.0 | 1.0 | - | - | - | - |
DTPMP | 0.25 | 0.25 | 0.25 | 0.25 | - | - | - |
SRP2 | - | - | - | 0.2 | - | 0.2 | - |
EDDS | - | 0.25 | 0.4 | - | 0.5 | 0.5 | 0.1 |
TFAA | - | - | - | - | - | - | 1.1 |
CFAA | - | 1.0 | - | 2.0 | - | - | - |
HEDP | 0.3 | 0.3 | 0.3 | 0.3 | 0.4 | 0.4 | 0.3 |
QEA | - | - | - | 0.2 | - | 0.5 | - |
蛋白酶1 | - | - | 0.26 | 1.0 | - | - | 0.3 |
蛋白酶 | 0.26 | 0.26 | - | - | 1.5 | 1.0 | - |
纤维素酶 | 0.3 | - | - | 0.3 | 0.3 | 0.3 | 0.3 |
淀粉酶 | 0.1 | 0.1 | 0.1 | 0.4 | 0.5 | 0.5 | 0.1 |
脂酶(1) | 0.3 | - | - | 0.5 | 0.5 | 0.5 | 0.1 |
光活化漂白剂(ppm) | 15ppm | 15ppm | 15ppm | - | 20ppm | 20 ppm | 20ppm |
PVNO/PVPVI | - | - | - | 0.1 | - | - | - |
增白剂1 | 0.09 | 0.09 | 0.09 | - | 0.09 | 0.09 | 0.01 |
增白剂2 | - | - | - | - | - | - | 0.09 |
香料喷洒 | 0.3 | 0.3 | 0.3 | 0.4 | 0.4 | 0.4 | 0.4 |
A | B | C | D | E | F | G | |
ARP 1 | 0.08(d) | 0.1(es) | - | - | 0.1(d) | 0.05(ec) | - |
ARP 2 | - | - | 0.08(s) | 0.1(ec) | 0.1(s) | - | - |
ARP 3(es) | - | - | - | - | - | - | 0.4 |
硅氧烷消泡剂 | 0.5 | 0.5 | 0.5 | - | 0.3 | 0.3 | 0.3 |
粘土II | 0.5 | 0.5 | 0.5 | - | 0.3 | 0.3 | 12.0 |
絮凝剂I | 0.5 | 0.5 | 0.5 | - | 0.3 | 0.3 | 0.3 |
甘油 | 0.5 | 0.5 | 0.5 | - | 0.3 | 0.3 | 0.6 |
石蜡 | 0.5 | 0.5 | 0.5 | - | 0.3 | 0.3 | 0.4 |
其它/微量成分至100% | |||||||
密度(g/l) | 850 | 850 | 850 | 850 | 850 | 850 | 850 |
根据本发明制备如下尤其用于欧洲洗衣机条件的颗粒洗衣洗涤剂组合物A-F:
实施例3
A | B | C | D | E | F | |
LAS | 5.5 | 7.5 | 5.0 | 5.0 | 6.0 | 7.0 |
TAS | 1.25 | 1.86 | - | 0.8 | 0.4 | 0.3 |
C24AS/C25AS | - | 2.24 | 5.0 | 5.0 | 5.0 | 2.2 |
C25E3S | - | 0.76 | 1.0 | 1.5 | 3.0 | 1.0 |
C45E7 | 3.25 | - | - | - | - | 3.0 |
TFAA | - | - | 2.0 | - | - | - |
C25E5 | - | 5.5 | - | - | - | - |
QAS | 0.8 | - | - | - | - | - |
QAS II | - | 0.7 | 1.0 | 0.5 | 1.0 | 0.7 |
STPP | 19.7 | - | - | - | - | - |
沸石A | - | 19.5 | 25.0 | 19.5 | 20.0 | 17.0 |
A | B | C | D | E | F | |
NaSKS-6/柠檬酸(79∶21) | - | 10.6 | - | 10.6 | - | - |
NaSKS-6 | - | - | 9.0 | - | 10.0 | 10.0 |
碳酸盐 | 6.1 | 21.4 | 9.0 | 10.0 | 10.0 | 18.0 |
碳酸氢盐 | - | 2.0 | 7.0 | 5.0 | - | 2.0 |
硅酸盐 | 6.8 | - | - | 0.3 | 0.5 | - |
柠檬酸盐 | - | - | 4.0 | 4.0 | - | - |
硫酸盐 | 39.8 | - | - | 5.0 | - | 12.0 |
硫酸镁 | - | - | 0.1 | 0.2 | 0.2 | - |
MA/AA | 0.5 | 1.6 | 3.0 | 4.0 | 1.0 | 1.0 |
CMC | 0.2 | 0.4 | 1.0 | 1.0 | 0.4 | 0.4 |
PB4 | 5.0 | 12.7 | - | - | - | - |
过碳酸盐 | - | - | - | - | 18.0 | 15.0 |
TAED | 0.5 | 3.1 | - | - | 5.0 | - |
NAC-OBS | 1.0 | 3.5 | - | - | - | 2.5 |
DTPMP | 0.25 | 0.2 | 0.3 | 0.4 | - | 0.2 |
HEDP | - | 0.3 | - | 0.3 | 0.3 | 0.3 |
QEA | - | - | 1.0 | 1.0 | 1.0 | - |
蛋白酶I | - | - | - | 0.5 | 1.2 | - |
蛋白酶 | 0.26 | 0.85 | 0.9 | 1.0 | - | 0.7 |
脂酶(1) | 0.15 | 0.15 | 0.3 | 0.3 | 0.3 | 0.2 |
纤维素酶 | 0.28 | 0.28 | 0.2 | 0.2 | 0.3 | 0.3 |
淀粉酶 | 0.1 | 0.1 | 0.4 | 0.4 | 0.6 | 0.2 |
PVNO/PVPVI | - | - | 0.2 | 0.2 | - | - |
PVP | 0.9 | 1.3 | - | - | - | 0.9 |
SRP1 | - | - | 0.2 | 0.2 | 0.2 | - |
光活化漂白剂(1) ppm | 15 | 27 | - | - | 20 | 20 |
光活化漂白剂(2) ppm | 15 | - | - | - | - | - |
增白剂1 | 0.08 | 0.19 | - | - | 0.09 | 0.15 |
增白剂2 | - | 0.04 | - | - | - | - |
香料 | 0.3 | 0.3 | 0.4 | 0.3 | 0.4 | 0.3 |
ARP1 | 0.1(d) | 1.0(d) | - | - | - | 0.1(es) |
A | B | C | D | E | F | |
ARP2 | - | - | 0.04(s) | 0.08(ec) | 0.1(d) | 0.1(es) |
硅氧烷消泡剂 | 0.5 | 2.4 | 0.3 | 0.5 | 0.3 | 2.0 |
微量组分至100% | ||||||
密度(g/l) | 750 | 750 | 750 | 750 | 750 | 750 |
制备如下根据本发明的尤其用于欧洲洗衣机条件的洗涤剂配方:
实施例4
A | B | C | D | |
吹制粉末 | ||||
LAS | 6.0 | 5.0 | 11.0 | 6.0 |
TAS | 2.0 | - | - | 2.0 |
沸石A | 24.0 | - | - | 20.0 |
STPP | - | 27.0 | 24.0 | - |
硫酸盐 | 4.0 | 6.0 | 13.0 | - |
MA/AA | 1.0 | 4.0 | 6.0 | 2.0 |
硅酸盐 | 1.0 | 7.0 | 3.0 | 3.0 |
CMC | 1.0 | 1.0 | 0.5 | 0.6 |
增白剂1 | 0.2 | 0.2 | 0.2 | 0.2 |
硅氧烷消泡剂 | 1.0 | 1.0 | 1.0 | 0.3 |
DTPMP | 0.4 | 0.4 | 0.2 | 0.4 |
喷洒液 | ||||
增白剂 | 0.02 | - | - | 0.02 |
C45E7 | - | - | - | 5.0 |
C45E2 | 2.5 | 2.5 | 2.0 | - |
C45E3 | 2.6 | 2.5 | 2.0 | - |
香料 | 0.5 | 0.3 | 0.5 | 0.2 |
硅氧烷消泡剂 | 0.3 | 0.3 | 0.3 | - |
干添加剂 | ||||
QEA | - | - | - | 1.0 |
EDDS | 0.3 | - | - | - |
硫酸盐 | 2.0 | 3.0 | 5.0 | 10.0 |
A | B | C | D | |
碳酸盐 | 6.0 | 13.0 | 15.0 | 14.0 |
柠檬酸 | 2.5 | - | - | 2.0 |
QASII | 0.5 | - | - | 0.5 |
SKS-6 | 10.0 | - | - | - |
过碳酸盐 | 18.5 | - | - | - |
PB4 | - | 18.0 | 10.0 | 21.5 |
TAED | 2.0 | 2.0 | - | 2.0 |
NAC-OBS | 3.0 | 2.0 | 4.0 | - |
蛋白酶 | 1.0 | 1.0 | 1.0 | 1.0 |
脂酶 | - | 0.4 | - | 0.2 |
脂酶(1) | 0.4 | - | 0.4 | - |
淀粉酶 | 0.2 | 0.2 | 0.2 | 0.4 |
增白剂1 | 0.05 | - | - | 0.05 |
ARP3 | 0.03 | 0.1(es) | 1.0 | 0.10.05(ec) |
其他/微量成分至100% |
根据本发明制备如下颗粒洗涤剂配方:
实施例5
A | B | C | D | E | F | |
吹制粉末 | ||||||
LAS | 23.0 | 8.0 | 7.0 | 9.0 | 7.0 | 7.0 |
TAS | - | - | - | - | 1.0 | - |
C45AS | 6.0 | 6.0 | 5.0 | 8.0 | - | - |
C45AES | - | 1.0 | 1.0 | 1.0 | - | - |
C45E35 | - | - | - | - | 2.0 | 4.0 |
沸石A | 10.0 | 18.0 | 14.0 | 12.0 | 10.0 | 10.0 |
MA/AA | - | 0.5 | - | - | - | 2.0 |
MA/AA(1) | 7.0 | - | - | - | - | - |
AA | - | 3.0 | 3.0 | 2.0 | 3.0 | 3.0 |
硫酸盐 | 5.0 | 6.3 | 14.3 | 11.0 | 15.0 | 19.3 |
硅酸盐 | 10.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
A | B | C | D | E | F | |
碳酸盐 | 15.0 | 20.0 | 10.0 | 20.7 | 8.0 | 6.0 |
PEG 4000 | 0.4 | 1.5 | 1.5 | 1.0 | 1.0 | 1.0 |
DTPA | - | 0.9 | 0.5 | - | - | 0.5 |
增白剂2 | 0.3 | 0.2 | 0.3 | - | 0.1 | 0.3 |
喷洒液 | ||||||
C45E7 | - | 2.0 | - | - | 2.0 | 2.0 |
C25E9 | 3.0 | - | - | - | - | - |
C23E9 | - | - | 1.5 | 2.0 | - | 2.0 |
香料 | 0.3 | 0.3 | 0.3 | 2.0 | 0.3 | 0.3 |
ARP2 | 0.1(s) | 0.05(s) | - | - | - | - |
附聚物 | ||||||
C45AS | - | 5.0 | 5.0 | 2.0 | - | 5.0 |
LAS | - | 2.0 | 2.0 | - | - | 2.0 |
沸石A | - | 7.5 | 7.5 | 8.0 | - | 7.5 |
碳酸盐 | - | 4.0 | 4.0 | 5.0 | - | 4.0 |
PEG 4000 | - | 0.5 | 0.5 | - | - | 0.5 |
微量组分(水等) | - | 2.0 | 2.0 | 2.0 | - | 2.0 |
干添加剂 | ||||||
QAS(I) | - | - | - | - | 1.0 | - |
柠檬酸 | - | - | - | - | 2.0 | - |
PB4 | - | - | - | - | 12.0 | 1.0 |
PB1 | 4.0 | 1.0 | 3.0 | 2.0 | - | - |
过碳酸盐 | - | - | - | - | 2.0 | 10.0 |
碳酸盐 | - | 5.3 | 1.8 | - | 4.0 | 4.0 |
NOBS | 4.0 | - | 6.0 | - | - | 0.6 |
甲基纤维素 | 0.2 | - | - | - | - | - |
SKS-6 | 8.0 | - | - | - | - | - |
STS | - | - | 2.0 | - | 1.0 | - |
枯烯磺酸 | - | 1.0 | - | - | - | 2.0 |
脂酶 | 0.2 | - | 0.2 | - | 0.2 | 0.4 |
纤维素酶 | 0.2 | 0.2 | 0.2 | 0.3 | 0.2 | 0.2 |
淀粉酶 | 0.2 | - | 0.1 | - | 0.2 | - |
蛋白酶 | 0.5 | 0.5 | 0.5 | 0.3 | 0.5 | 0.5 |
A | B | C | D | E | F | |
PVPVI | - | - | - | - | 0.5 | 0.1 |
PVP | - | - | - | - | 0.5 | - |
PVNO | - | - | 0.5 | 0.3 | - | - |
QEA | - | - | - | - | 1.0 | - |
SRP1 | 0.2 | 0.5 | 0.3 | - | 0.2 | - |
ARP2 | 0.1 | 0.2 | 0.04(d) | 0.02 | 0.01(es) | 0.02(es) |
硅氧烷消泡剂 | 0.2 | 0.4 | 0.2 | 0.4 | 0.1 | - |
硫酸镁 | - | - | 0.2 | - | 0.2 | - |
微量组分至100% |
G | H | I | J | |
吹制粉末 | ||||
粘土I或II | 7.0 | 10.0 | 6.0 | 2.0 |
LAS | 16.0 | 5.0 | 11.0 | 6.0 |
TAS | - | 5.0 | - | 2.0 |
沸石A | - | 20.0 | - | 10.0 |
STPP | 24.0 | - | 14.0 | - |
硫酸盐 | - | 2.0 | - | - |
MA/AA | - | 2.0 | 1.0 | 1.0 |
硅酸盐 | 4.0 | 7.0 | 3.0 | - |
CMC | 1.0 | - | 0.5 | 0.6 |
增白剂1 | 0.2 | 0.2 | 0.2 | 0.2 |
碳酸盐 | 10.0 | 10.0 | 20.0 | - |
DTPMP | 0.4 | 0.4 | 0.2 | - |
喷洒液 | ||||
增白剂1 | 0.02 | - | - | 0.02 |
C45E7或E9 | - | - | 2.0 | 1.0 |
C45E3或E4 | - | - | 2.0 | 4.0 |
香料 | 0.5 | - | 0.5 | 0.2 |
硅氧烷消泡剂 | 0.3 | - | - | - |
干添加剂 | ||||
絮凝剂I或II | 0.3 | 1.0 | 1.0 | 0.5 |
QEA | - | - | - | 1.0 |
HEDP/EDDS | 0.3 | - | - | - |
硫酸盐 | 2.0 | - | - | - |
碳酸盐 | 20.0 | 13.0 | 15.0 | 24.0 |
柠檬酸 | 2.5 | - | - | 2.0 |
QAS | - | - | 0.5 | 0.5 |
NaSKS-6 | 3.5 | - | - | 5.0 |
过碳酸盐 | - | - | - | 9.0 |
PB4 | - | - | 5.0 | |
NOBS | - | - | - | 1.3 |
TAED | - | - | 2.0 | 1.5 |
蛋白酶 | 1.0 | 1.0 | 1.0 | 1.0 |
脂酶 | - | 0.4 | - | 0.2 |
淀粉酶 | 0.2 | 0.2 | 0.2 | 0.4 |
增白剂2 | 0.05 | - | - | 0.05 |
香料 | 1.0 | 0.2 | 0.5 | 0.3 |
斑点 | 1.2 | 0.5 | 2.0 | - |
ARP1 | 0.08 | 1.5(d) | 0.2 | 0.05 |
ARP2 | 3.0(d) | 0.6 | 0.2 | 0.1 |
微量组分至100% |
根据本发明制备如下尤其用于洗涤带色织物的不含漂白剂的洗涤剂配方:
实施例6
A | B | C | |
吹制粉末 | |||
沸石A | 15.0 | 15.0 | - |
硫酸盐 | 0.0 | 5.0 | - |
LAS | 3.0 | 3.0 | - |
DTPMP | 0.4 | 0.5 | - |
CMC | 0.4 | 0.4 | - |
MA/AA | 4.0 | 4.0 | - |
附聚物 | |||
C45AS | - | - | 11.0 |
A | B | C | |
LAS | 6.0 | 5.0 | - |
TAS | 3.0 | 2.0 | - |
硅酸盐 | 4.0 | 4.0 | - |
沸石A | 10.0 | 15.0 | 13.0 |
CMC | - | - | 0.5 |
MA/AA | - | - | 2.0 |
碳酸盐 | 9.0 | 7.0 | 7.0 |
喷洒液 | |||
香料 | 0.3 | 0.3 | 0.5 |
C45E7 | 4.0 | 4.0 | 4.0 |
C25E3 | 2.0 | 2.0 | 2.0 |
ARP2 | 0.08(s) | - | - |
干添加剂 | |||
MA/AA | - | - | 3.0 |
NaSKS-6 | - | - | 12.0 |
柠檬酸盐 | 10.0 | - | 8.0 |
碳酸氢盐 | 7.0 | 3.0 | 5.0 |
碳酸盐 | 8.0 | 5.0 | 7.0 |
PVPVI/PVNO | 0.5 | 0.5 | 0.5 |
Alcalase | 0.5 | 0.3 | 0.9 |
脂酶 | 0.4 | 0.4 | 0.4 |
淀粉酶 | 0.6 | 0.6 | 0.6 |
纤维素酶 | 0.6 | 0.6 | 0.6 |
ARP1 | 0.05 | 0.08 | 0.1(es) |
硅氧烷消泡剂 | 5.0 | 5.0 | 5.0 |
干添加剂 | |||
硫酸盐 | 0.0 | 9.0 | 0.0 |
其他/微量成分至100% | 100.0 | 100.0 | 100.0 |
密度(g/l) | 700 | 700 | 700 |
根据本发明制备如下颗粒洗涤剂配方:
实施例7
A | B | C | D | |
基础颗粒 | ||||
沸石A | 30.0 | 22.0 | 24.0 | 10.0 |
硫酸盐 | 10.0 | 5.0 | 10.0 | 7.0 |
MA/AA | 3.0 | - | - | - |
AA | - | 1.6 | 2.0 | - |
MA/AA(1) | - | 12.0 | - | 6.0 |
LAS | 14.0 | 10.0 | 9.0 | 20.0 |
C45AS | 8.0 | 7.0 | 9.0 | 7.0 |
C45AES | - | 1.0 | 1.0 | - |
硅酸盐 | - | 1.0 | 0.5 | 10.0 |
皂 | - | 2.0 | - | - |
增白剂1 | 0.2 | 0.2 | 0.2 | 0.2 |
碳酸盐 | 6.0 | 9.0 | 10.0 | 10.0 |
PEG4000 | - | 1.0 | 1.5 | - |
DTPA | - | 0.4 | - | - |
喷洒液 | ||||
C25E9 | - | - | - | 5.0 |
C45E7 | 1.0 | 1.0 | - | - |
C23E9 | - | 1.0 | 2.5 | - |
香料 | 0.2 | 0.3 | 0.3 | - |
ARP2 | 0.04(s) | - | - | - |
干添加剂 | ||||
碳酸盐 | 5.0 | 10.0 | 18.0 | 8.0 |
PVPVI/PVNO | 0.5 | - | 0.3 | - |
蛋白酶 | 1.0 | 1.0 | 1.0 | 0.5 |
脂酶 | 0.4 | - | - | 0.4 |
淀粉酶 | 0.1 | - | - | 0.1 |
纤维素酶 | 0.1 | 0.2 | 0.2 | 0.1 |
NOBS | - | 4.0 | - | 4.5 |
PB1 | 1.0 | 5.0 | 1.5 | 6.0 |
硫酸盐 | 4.0 | 5.0 | - | 5.0 |
SRPl | - | 0.4 | - | - |
A | B | C | D | |
ARP1 | 0.05 | 0.08 | 0.1(es) | - |
ARP2 | 0.05 | - | - | 0.02(es) |
抑泡剂 | - | 0.5 | 0.5 | - |
其他/微量成分至100% |
根据本发明制备如下颗粒洗涤剂组合物:
实施例8
A | B | C | |
吹制粉末 | |||
沸石A | 20.0 | - | 15.0 |
STPP | - | 20.0 | - |
硫酸盐 | - | - | 5.0 |
碳酸盐 | - | - | 5.0 |
TAS | - | - | 1.0 |
LAS | 6.0 | 6.0 | 6.0 |
C68AS | 2.0 | 2.0 | - |
硅酸盐 | 3.0 | 8.0 | - |
MA/AA | 4.0 | 2.0 | 2.0 |
CMC | 0.6 | 0.6 | 0.2 |
增白剂1 | 0.2 | 0.2 | 0.1 |
DTPMP | 0.4 | 0.4 | 0.1 |
STS | - | - | 1.0 |
喷洒液 | |||
C45E7 | 5.0 | 5.0 | 4.0 |
硅氧烷消泡剂 | 0.3 | 0.3 | 0.1 |
香料 | 0.2 | 0.2 | 0.3 |
ARP1 | 0.1(s) | 0.05(s) | 0.08(s) |
干添加剂 | |||
QEA | - | - | 1.0 |
碳酸盐 | 14.0 | 9.0 | 10.0 |
PB1 | 1.5 | 2.0 | - |
PB4 | 18.5 | 13.0 | 13.0 |
A | B | C | |
TAED | 2.0 | 2.0 | 2.0 |
QAS(I) | - | - | 1.0 |
光活化漂白剂 | 15ppm | 15ppm | 15ppm |
SKS-6 | - | - | 3.0 |
蛋白酶 | 1.0 | 1.0 | 0.2 |
脂酶 | 0.2 | 0.2 | 0.2 |
淀粉酶 | 0.4 | 0.4 | 0.2 |
纤维素酶 | 0.1 | 0.1 | 0.2 |
硫酸盐 | 10.0 | 20.0 | 5.0 |
微量组分至100% | |||
密度(g/l) | 700 | 700 | 700 |
根据本发明制备如下洗涤剂组合物:
实施例9
A | B | C | |
吹制粉末 | |||
沸石A | 15.0 | 15.0 | 15.0 |
硫酸盐 | 0.0 | 5.0 | 0.0 |
LAS | 3.0 | 3.0 | 3.0 |
QAS | - | 1.5 | 1.5 |
DTPMP | 0.4 | 0.2 | 0.4 |
EDDS | - | 0.4 | 0.2 |
CMC | 0.4 | 0.4 | 0.4 |
MA/AA | 4.0 | 2.0 | 2.0 |
附聚物 | |||
LAS | 5.0 | 5.0 | 5.0 |
TAS | 2.0 | 2.0 | 1.0 |
硅酸盐 | 3.0 | 3.0 | 4.0 |
沸石A | 8.0 | 8.0 | 8.0 |
碳酸盐 | 8.0 | 8.0 | 4.0 |
喷洒液 |
A | B | C | |
香料 | 0.3 | 0.3 | 0.3 |
C45E7 | 2.0 | 2.0 | 2.0 |
C25E3 | 2.0 | - | - |
ARP2 | 0.02(s) | - | - |
干添加剂 | |||
柠檬酸盐 | 5.0 | - | 2.0 |
碳酸氢盐 | - | 3.0 | - |
碳酸盐 | 8.0 | 15.0 | 10.0 |
TAED | 6.0 | 2.0 | 5.0 |
PP1 | 14.0 | 7.0 | 10.0 |
PEO | - | - | 0.2 |
ARP1 | 0.1 | 0.2 | 0.08(ec) |
膨润土 | - | - | 10.0 |
蛋白酶 | 1.0 | 1.0 | 1.0 |
脂酶 | 0.4 | 0.4 | 0.4 |
淀粉酶 | 0.6 | 0.6 | 0.6 |
纤维素酶 | 0.6 | 0.6 | 0.6 |
硅氧烷消泡剂 | 5.0 | 5.0 | 5.0 |
干添加剂 | |||
硫酸钠 | 0.0 | 3.0 | 0.0 |
其他/微量成分至100% | 100.0 | 100.0 | 100.0 |
密度(g/l) | 850 | 850 | 850 |
D | E | F | G | H | |
吹制粉末 | |||||
STPP/沸石A | 9.0 | 15.0 | 15.0 | 9.0 | 9.0 |
絮凝剂II或III | 0.5 | 0.2 | 0.9 | 1.5 | - |
LAS | 7.5 | 23.0 | 3.0 | 7.5 | 7.5 |
QAS | 2.5 | 1.5 | - | - | - |
DTPMP | 0.4 | 0.2 | 0.4 | 0.4 | 0.4 |
HEDP或EDDS | - | 0.4 | 0.2 | - | - |
CMC | 0.1 | 0.4 | 0.4 | 0.1 | 0.1 |
碳酸钠 | 5.0 | 20.0 | 20.0 | 10.0 | - |
增白剂 | 0.05 | - | - | 0.05 | 0.05 |
粘土I或II | - | 10.0 | - | - | - |
STS | 0.5 | - | - | 0.5 | 0.5 |
MA/AA | 1.5 | 2.0 | 2.0 | 1.5 | 1.5 |
附聚物 | |||||
抑泡剂(硅氧烷) | 1.0 | 1.0 | - | 2.0 | 0.5 |
附聚物 | |||||
粘土 | 9.0 | - | - | 4.0 | 10.0 |
石蜡 | 0.5 | - | - | 0.5 | 1.5 |
甘油 | 0.5 | - | - | 0.5 | 0.5 |
附聚物 | |||||
LAS | - | 5.0 | 5.0 | - | - |
TAS | - | 2.0 | 1.0 | - | - |
硅酸盐 | - | 3.0 | 4.0 | - | - |
沸石A | - | 8.0 | 8.0 | - | - |
碳酸盐 | - | 8.0 | 4.0 | - | - |
喷洒液 | |||||
香料 | 0.3 | - | - | 0.3 | 0.3 |
C45E7或E9 | 2.0 | - | - | 2.0 | 2.0 |
C25E3或E4 | 2.0 | - | - | 2.0 | 2.0 |
干添加剂 | |||||
柠檬酸或盐 | 2.5 | - | 2.0 | 2.5 | 2.5 |
粘土I或II | - | 5.0 | 5.0 | - | - |
絮凝剂I或II | - | - | - | - | 0.2 |
碳酸氢盐 | - | 3.0 | - | - | - |
碳酸盐 | 15.0 | - | - | 25.0 | 31.0 |
TAED | 1.0 | 2.0 | 5.0 | 1.0 | - |
过硼酸或过碳酸钠 | 6.0 | 7.0 | 10.0 | 6.0 | - |
SRP1,2,3或4 | 0.2 | 0.1 | 0.2 | 0.5 | 0.3 |
CMC或非离子纤维素醚 | 1.0 | 1.5 | 0.5 | - | - |
蛋白酶 | 0.3 | 1.0 | 1.0 | 0.3 | 0.3 |
脂酶 | - | 0.4 | 0.4 | - | - |
淀粉酶 | 0.2 | 0.6 | 0.6 | 0.2 | 0.2 |
纤维素酶 | 0.2 | 0.6 | 0.6 | 0.2 | 0.2 |
硅氧烷消泡剂 | - | 5.0 | 5.0 | - | - |
香料(淀粉) | 0.2 | 0.3 | 1.0 | 0.2 | 0.2 |
斑点 | 0.5 | 0.5 | 0.1 | - | 1.0 |
NaSKS-6(硅酸盐2R) | 3.5 | - | - | - | 3.5 |
光漂白剂 | 0.1 | - | - | 0.1 | 0.1 |
皂 | 0.5 | 2.5 | - | 0.5 | 0.5 |
硫酸钠 | - | 3.0 | - | - | - |
ARP1 | 0.1 | 1.0(d) | 0.05 | 3.0(es) | 0.09 |
其他/微量成分至100% | 100.0 | 100.0 | 100.0 | 100.0 | 100.0 |
密度(g/l) | 850 | 850 | 850 | 850 | 850 |
根据本发明制备如下洗涤剂配方:
实施例10
A | B | C | D | |
LAS | 18.0 | 14.0 | 24.0 | 20.0 |
QAS | 0.7 | 1.0 | - | 0.7 |
TFAA | - | 1.0 | - | - |
C23E56.5 | - | - | 1.0 | - |
C45E7 | - | 1.0 | - | - |
C45E3S | 1.0 | 2.5 | 1.0 | - |
STPP | 32.0 | 18.0 | 30.0 | 22.0 |
硅酸盐 | 9.0 | 5.0 | 9.0 | 8.0 |
碳酸盐 | 11.0 | 7.5 | 10.0 | 5.0 |
碳酸氢盐 | - | 7.5 | - | - |
A | B | C | D | |
PB1 | 3.0 | 1.0 | - | - |
PB4 | - | 1.0 | - | - |
NOBS | 2.0 | 1.0 | - | - |
DTPMP | - | 1.0 | - | - |
DTPA | 0.5 | - | 0.2 | 0.3 |
SRP1 | 0.3 | 0.2 | - | 0.1 |
MA/AA | 1.0 | 1.5 | 2.0 | 0.5 |
CMC | 0.8 | 0.4 | 0.4 | 0.2 |
PEI | - | - | 0.4 | - |
硫酸钠 | 20.0 | 10.0 | 20.0 | 30.0 |
硫酸镁 | 0.2 | - | 0.4 | 0.9 |
蛋白酶 | 0.8 | 1.0 | 0.5 | 0.5 |
淀粉酶 | 0.5 | 0.4 | - | 0.25 |
脂酶 | 0.2 | - | 0.1 | - |
纤维素酶 | 0.15 | - | - | 0.05 |
光活化漂白剂(ppm) | 30ppm | 20ppm | - | 10ppm |
ARP3 | 0.04(s) | 0.08(ec) | 0.1(s) | 0.04(es) |
香料喷洒 | 0.3 | 0.3 | 0.1 | 0.2 |
增白剂1/2 | 0.05 | 0.2 | 0.08 | 0.1 |
其他/微量成分至100% |
根据本发明制备如下液体洗涤剂配方(含量用重量份数表示):
实施例11
A | B | C | D | E | |
LAS | 11.5 | 8.8 | - | 3.9 | - |
C25E2.5S | - | 3.0 | 18.0 | - | 16.0 |
C45E2.25S | 11.5 | 3.0 | - | 15.7 | - |
C23E9 | - | 2.7 | 1.8 | 2.0 | 1.0 |
C23E7 | 3.2 | - | - | - | - |
CFAA | - | - | 5.2 | - | 3.1 |
TPKFA | 1.6 | - | 2.0 | 0.5 | 2.0 |
柠檬酸(50%) | 6.5 | 1.2 | 2.5 | 4.4 | 2.5 |
甲酸钙 | 0.1 | 0.06 | 0.1 | - | - |
甲酸钠 | 0.5 | 0.06 | 0.1 | 0.05 | 0.05 |
枯烯磺酸钠 | 4.0 | 1.0 | 3.0 | 1.18 | - |
硼酸盐 | 0.6 | - | 3.0 | 2.0 | 2.9 |
NaOH | 5.8 | 2.0 | 3.5 | 3.7 | 2.7 |
乙醇 | 1.75 | 1.0 | 3.6 | 4.2 | 2.9 |
1,2丙二醇 | 3.3 | 2.0 | 8.0 | 7.9 | 5.3 |
单乙醇胺 | 3.0 | 1.5 | 1.3 | 2.5 | 0.8 |
TEPAE | 1.6 | - | 1.3 | 1.2 | 1.2 |
蛋白酶 | 1.0 | 0.3 | 1.0 | 0.5 | 0.7 |
脂酶 | - | - | 0.1 | - | - |
纤维素酶 | - | - | 0.1 | 0.2 | 0.05 |
淀粉酶 | - | - | - | 0.1 | - |
SRP1 | 0.2 | - | 0.1 | - | - |
DTPA | - | - | 0.3 | - | - |
PVNO | - | - | 0.3 | - | 0.2 |
ARP1 | 0.3 | - | - | 0.1 | - |
ARP2 | - | 0.04 | - | - | 0.1 |
ARP3 | - | - | 0.3 | - | - |
增白剂1 | 0.2 | 0.07 | 0.1 | - | - |
硅氧烷消泡剂 | 0.04 | 0.02 | 0.1 | 0.1 | 0.1 |
水/微量组分 |
根据本发明制备如下液体洗涤剂配方(含量用重量份数表示):
实施例12
A | B | C | D | E | F | G | H | |
LAS | 10.0 | 13.0 | 9.0 | - | 25.0 | - | - | - |
C25AS | 4.0 | 1.0 | 2.0 | 10.0 | - | 13.0 | 18.0 | 15.0 |
C25E3S | 1.0 | - | - | 3.0 | - | 2.0 | 2.0 | 4.0 |
C25E7 | 6.0 | 8.0 | 13.0 | 2.5 | - | - | 4.0 | 4.0 |
TFAA | - | - | - | 4.5 | - | 6.0 | 8.0 | 8.0 |
APA | - | 1.4 | - | - | 3.0 | 1.0 | 2.0 | - |
TPKFA | 2.0 | - | 13.0 | 7.0 | - | 15.0 | 11.0 | 11.0 |
柠檬酸 | 2.0 | 3.0 | 1.0 | 1.5 | 1.0 | 1.0 | 1.0 | 1.0 |
十二碳烯基/十四碳烯基琥珀酸 | 12.0 | 10.0 | - | - | 15.0 | - | - | - |
菜子脂肪酸 | 4.0 | 2.0 | 1.0 | - | 1.0 | - | 3.5 | - |
乙醇 | 4.0 | 4.0 | 7.0 | 2.0 | 7.0 | 2.0 | 3.0 | 2.0 |
1,2丙二醇 | 4.0 | 4.0 | 2.0 | 7.0 | 6.0 | 8.0 | 10.0 | 13.0 |
单乙醇胺 | - | - | - | 5.0 | - | - | 9.0 | 9.0 |
三乙醇胺 | - | - | 8.0 | - | - | - | - | - |
TEPAE | 0.5 | - | 0.5 | 0.2 | - | - | 0.4 | 0.3 |
DTPMP | 1.0 | 1.0 | 0.5 | 1.0 | 2.0 | 1.2 | 1.0 | - |
蛋白酶 | 0.5 | 0.5 | 0.4 | 0.25 | - | 0.5 | 0.3 | 0.6 |
Alcalase | - | - | - | - | 1.5 | - | - | - |
脂酶 | - | 0.10 | - | 0.01 | - | - | 0.15 | 0.15 |
淀粉酶 | 0.25 | 0.25 | 0.6 | 0.5 | 0.25 | 0.9 | 0.6 | 0.6 |
纤维素酶 | - | - | - | 0.05 | - | - | 0.15 | 0.15 |
Endolase | - | - | - | 0.10 | - | - | 0.07 | - |
SRP2 | 0.3 | - | 0.3 | 0.1 | - | - | 0.2 | 0.1 |
硼酸 | 0.1 | 0.2 | 1.0 | 2.0 | 1.0 | 1.5 | 2.5 | 2.5 |
氯化钙 | - | 0.02 | - | 0.01 | - | - | - | - |
膨润土 | - | - | - | - | 4.0 | 4.0 | - | - |
增白剂1 | - | 0.4 | - | - | 0.1 | 0.2 | 0.3 | - |
A | B | C | D | E | F | G | H | |
抑泡剂 | 0.1 | 0.3 | - | 0.1 | 0.4 | - | - | - |
遮光剂 | 0.5 | 0.4 | - | 0.3 | 0.8 | 0.7 | - | - |
ARP1 | 0.3 | - | 0.1 | - | 0.05 | - | 0.1 | 0.08 |
ARP2 | - | 0.04 | - | 0.02 | - | 0.1 | 0.08 | 0.1 |
水/微量组分 | ||||||||
NaOH pH | 8.0 | 8.0 | 7.6 | 7.7 | 8.0 | 7.5 | 8.0 | 8.2 |
根据本发明制备如下液体洗涤剂配方(含量用重量份数表示):
实施例13
A | B | |
LAS | 27.6 | 18.9 |
C45AS | 13.8 | 5.9 |
C13E8 | 3.0 | 3.1 |
油酸 | 3.4 | 2.5 |
柠檬酸 | 5.4 | 5.4 |
NaOH | 0.4 | 3.6 |
甲酸钙 | 0.2 | 0.1 |
甲酸钠 | - | 0.5 |
乙醇 | 7.0 | - |
单乙醇胺 | 16.5 | 8.0 |
1,2丙二醇 | 5.9 | 5.5 |
二甲苯磺酸 | - | 2.4 |
TEPAE | 1.5 | 0.8 |
蛋白酶 | 1.5 | 0.6 |
PEG | - | 0.7 |
增白剂2 | 0.4 | 0.1 |
香料喷洒 | 0.5 | 0.3 |
ARP1 | 0.3 | - |
ARP3 | - | 0.04 |
水/微量组分 |
根据本发明制备如下片、块、挤出物或颗粒形式的组合物:
实施例14
A | B | C | D | E | F | G | |
C11-C13烷基苯磺酸钠 | 12.0 | 16.0 | 23.0 | 19.0 | 18.0 | 20.0 | 16.0 |
C14-C15醇硫酸钠 | 4.5 | - | - | - | 4.0 | ||
C14-C15醇乙氧基化(3)硫酸盐 | - | - | 2.0 | - | 1.0 | 1.0 | 1.0 |
C14-C15醇乙氧基化钠 | 2.0 | 2.0 | - | 1.3 | - | - | 5.0 |
C9-C14烷基二甲基羟基乙基季铵盐 | - | - | 1.0 | 0.5 | 2.0 | ||
牛油脂肪酸 | - | - | - | - | 1.0 | ||
三聚磷酸钠/沸石 | 23.0 | 25.0 | 14.0 | 22.0 | 20.0 | 10.0 | 20.0 |
碳酸钠 | 25.0 | 22.0 | 35.0 | 20.0 | 28.0 | 41.0 | 30.0 |
聚丙烯酸钠(45%) | 0.5 | 0.5 | 0.5 | 0.5 | - | - | - |
聚丙烯酸/马来酸钠聚合物 | - | - | 1.0 | 1.0 | 1.0 | 2.0 | 0.5 |
硅酸钠 (1∶6NaO/SiO2)(46%) | 3.0 | 6.0 | 9.0 | 8.0 | 9.0 | 6.0 | 8.0 |
硫酸钠 | - | - | - | - | - | 2.0 | 3.0 |
过硼酸/过碳酸钠 | 5.0 | 5.0 | 10.0 | - | 3.0 | 1.0 | - |
聚(乙二醇),MW~4000(50%) | 1.5 | 1.5 | 1.0 | 1.0 | - | - | 0.5 |
羧基甲基纤维素钠 | 1.0 | 1.0 | 1.0 | - | 0.5 | 0.5 | 0.5 |
NOBS/DOBS | - | 1.0 | - | - | 1.0 | 0.7 | - |
TAED | 1.5 | 1.0 | 2.5 | - | 3.0 | 0.7 | - |
SRP1 | 1.5 | 1.5 | 1.0 | 1.0 | - | 1.0 | - |
粘土I或II | 5.0 | 6.0 | 12.0 | 7.0 | 10.0 | 4.0 | 3.0 |
絮凝剂I或III | 0.2 | 0.2 | 3.0 | 2.0 | 0.1 | 1.0 | 0.5 |
润湿剂 | 0.5 | 1.0 | 0.5 | 1.0 | 0.5 | 0.5 | - |
石蜡 | 0.5 | 0.5 | 1.0 | - | - | 0.5 | 0.5 |
水分 | 7.5 | 7.5 | 6.0 | 7.0 | 5.0 | 3.0 | 5.0 |
硫酸镁 | - | - | - | - | - | 0.5 | 1.5 |
螯合剂 | - | - | - | - | 0.8 | 0.6 | 1.0 |
酶,包括淀粉酶,纤维素酶,蛋白酶和脂酶 | - | - | - | - | 2.0 | 1.5 | 2.0 |
ARP2 | 0.3 | 3.0(d) | - | - | - | - | - |
ARP1 | 0.08 | 0.1 | 3.0(d) | 1.5(es) | 0.05 | 1.0(d) | 0.05 |
斑点 | 2.5 | 4.1 | 4.2 | 4.4 | 5.6 | 5.0 | 5.2 |
微量组分,如香料,PVP,PVPVI/PVNO增白剂,光漂白剂 | 2.0 | 1.0 | 1.0 | 1.0 | 2.5 | 1.5 | 1.0 |
H | I | J | K | |
C11-C13烷基苯磺酸钠 | 23.0 | 13.0 | 20.0 | 18.0 |
C14-C15醇硫酸钠 | - | 4.0 | - | - |
粘土I或II | 5.0 | 10.0 | 14.0 | 6.0 |
絮凝剂I或II | 0.2 | 0.3 | 0.1 | 0.9 |
石蜡 | 0.5 | 0.5 | 1.0 | - |
润湿剂(甘油/硅酸) | 0.5 | 2.0 | 1.5 | - |
C14-C15醇乙氧基化硫酸盐 | - | - | - | 2.0 |
C14-C15醇乙氧基化钠 | 2.5 | 3.5 | - | - |
C9-C14烷基二甲基羟基乙基季铵盐 | - | - | - | 0.5 |
牛油脂肪酸 | 0.5 | - | - | - |
牛油醇乙氧基化物(50) | - | - | 1.3 | |
三聚磷酸钠 | - | 41.0 | - | 20.0 |
沸石A,水合物(0.1-10微米) | 26.3 | - | 21.3 | - |
碳酸钠 | 24.0 | 22.0 | 35.0 | 27.0 |
聚丙烯酸钠(45%) | 2.4 | - | 2.7 | - |
聚丙烯酸/马来酸钠聚合物 | - | - | 1.0 | 2.5 |
硅酸钠 (1.6或2或2.2NaO/SiO2)(46%) | 4.0 | 7.0 | 2.0 | 6.0 |
硫酸钠 | - | 6.0 | 2.0 | - |
过硼酸钠/过碳酸钠 | 8.0 | 4.0 | - | 12.0 |
聚(乙二醇),MW~4000(50%) | 1.7 | 0.4 | 1.0 | - |
羧基甲基纤维素钠 | 1.0 | - | - | 0.3 |
柠檬酸 | - | - | 3.0 | - |
NOBS/DOBS | 1.2 | - | - | 1.0 |
TAED | 0.6 | 1.5 | - | 3.0 |
香料 | 0.5 | 1.0 | 0.3 | 0.4 |
SRP1 | - | 1.5 | 1.0 | 1.0 |
水分 | 7.5 | 3.1 | 6.1 | 7.3 |
硫酸镁 | - | - | - | 1.0 |
螯合剂 | - | - | - | 0.5 |
斑点 | 1.0 | 0.5 | 0.2 | 2.7 |
酶,包括淀粉酶,纤维素酶,蛋白酶和脂酶 | - | 1.0 | - | 1.5 |
ARP1 | 0.1 | 3.0(d) | 1.0(es) | 0.3 |
微量组分,如增白剂,光漂白剂 | 1.0 | 1.0 | 1.0 | 1.0 |
根据本发明制备如下洗衣块洗涤剂组合物(含量用重量份数表示):
实施例15
A | B | C | D | E | F | G | H | |
LAS | - | - | 19.0 | 15.0 | 21.0 | 6.75 | 8.8 | - |
C28AS | 30.0 | 13.5 | - | - | - | 15.75 | 11.2 | 22.5 |
月桂酸钠 | 2.5 | 9.0 | - | - | - | - | - | - |
沸石A | 2.0 | 1.25 | - | - | - | 1.25 | 1.25 | 1.25 |
碳酸盐 | 20.0 | 3.0 | 13.0 | 8.0 | 10.0 | 15.0 | 15.0 | 10.0 |
碳酸钙 | 27.5 | 39.0 | 35.0 | - | - | 40.0 | - | 40.0 |
A | B | C | D | E | F | G | H | |
硫酸盐 | 5.0 | 5.0 | 3.0 | 5.0 | 3.0 | - | - | 5.0 |
TSPP | 5.0 | - | - | - | - | 5.0 | 2.5 | - |
STPP | 5.0 | 15.0 | 10.0 | - | - | 7.0 | 8.0 | 10.0 |
膨润土 | - | 10.0 | - | - | 5.0 | - | - | - |
DTPMP | - | 0.7 | 0.6 | - | 0.6 | 0.7 | 0.7 | 0.7 |
CMC | - | 1.0 | 1.0 | 1.0 | 1.0 | - | - | 1.0 |
滑面 | - | - | 10.0 | 15.0 | 10.0 | - | - | - |
硅酸盐 | - | - | 4.0 | 5.0 | 3.0 | - | - | - |
PVNO | 0.02 | 0.03 | - | 0.01 | - | 0.02 | - | - |
MA/AA | 0.4 | 1.0 | - | - | 0.2 | 0.4 | 0.5 | 0.4 |
SRP1 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
蛋白酶 | - | 0.12 | - | 0.08 | 0.08 | - | - | 0.1 |
脂酶 | - | 0.1 | - | 0.1 | - | - | - | - |
淀粉酶 | - | - | 0.8 | - | - | - | 0.1 | - |
纤维素酶 | - | 0.15 | - | - | 0.15 | 0.1 | - | - |
PEO | - | 0.2 | - | 0.2 | 0.3 | - | - | 0.3 |
香料 | 1.0 | 0.5 | 0.3 | 0.2 | 0.4 | - | - | 0.4 |
硫酸镁 | - | - | 3.0 | 3.0 | 3.0 | - | - | - |
ARP1 | 0.3 | - | - | 0.04 | - | 0.5 | - | - |
ARP2 | - | 0.04 | - | - | 0.1 | - | 0.08 | - |
ARP3 | - | - | 0.3 | - | - | - | - | 0.3 |
增白剂 | 0.15 | 0.10 | 0.15 | - | - | - | - | 0.1 |
光活化漂白剂(ppm) | - | 15.0 | 15.0 | 15.0 | 15.0 | - | - | 15.0 |
根据本发明制备如下洗涤剂添加剂组合物:
A B CLAS - 5.0 5.0STPP 30.0 - 20.0沸石A - 35.0 20.0PB1 20.0 15.0 -
A B CTAED 10.0 8.0 -ARP1 0.3 - 0.1ARP2 - 0.04 0.02蛋白酶 - 0.3 0.3淀粉酶 - 0.06 0.06微量组分,水 至100%实施例16
根据本发明制备如下高密度(0.96kg/l)餐具洗涤剂组合物:
A B C D E F G HSTPP - - 54.3 51.4 51.4 - - 50.9柠檬酸盐 35.0 17.0 - - - 46.1 40.2 -碳酸盐 - 17.5 14.0 14.0 14.0 - 8.0 32.1碳酸氢盐 - - - - - 25.4 - -硅酸盐 32.0 14.8 14.8 10.0 10.0 1.0 25.0 3.1偏硅酸盐 - 2.5 - 9.0 9.0 - - -PB1 1.9 9.7 7.8 7.8 7.8 - - -PB4 8.6 - - - - - - -过碳酸盐 - - - - - 6.7 11.8 4.8非离子表面活性剂1.5 2.0 1.5 1.7 1.5 2.6 1.9 5.3TAED 5.2 2.4 - - - 2.2 - 1.4HEDP - 1.0 - - - - - -DTPMP - 0.6 - - - - - -MnTACN - - - - - - 0.008 -PAAC - - 0.008 0.01 0.007 - - -BzP - - - - 1.4 - - -石蜡 0.5 0.5 0.5 0.5 0.5 0.6 - -ARP3 0.1 0.3 0.2 0.05 - - - 0.8ARP1 - - - - 0.3 0.03 0.5 -蛋白酶 0.072 0.072 0.029 0.053 0.046 0.026 0.059 0.06淀粉酶 0.012 0.012 0.006 0.012 0.013 0.009 0.017 0.03脂酶 - 0.001 - 0.005 - - - -BTA 0.3 0.3 0.3 0.3 0.3 - 0.3 0.3
A B C D E F G HMA/AA - - - - - - 4.2 -480N 3.3 6.0 - - - - - 0.9香料 0.2 0.2 0.2 0.2 0.2 0.2 0.1 0.1硫酸盐 7.0 20.0 5.0 2.2 0.8 12.0 4.6 -pH 10.8 11.0 10.8 11.3 11.3 9.6 10.8 10.9微量组分和水 至100%实施例17
根据本发明制备如下堆积密度1.02kg/l的颗粒餐具洗涤剂组合物:
A B C D E F G HSTPP 30.0 30.0 33.0 34.2 29.6 31.1 26.6 17.6碳酸盐 30.5 30.5 31.0 30.0 23.0 39.4 4.2 45.0硅酸盐 7.4 7.4 7.5 7.2 13.3 3.4 43.7 12.4偏硅酸盐 - - 4.5 5.1 - - - -过碳酸盐 - - - - - 4.0 - -PB1 4.4 4.2 4.5 4.5 - - - -NADCC - - - - 2.0 - 1.6 1.0非离子表面活性剂1.2 1.0 0.7 0.8 1.9 0.7 0.6 0.3TAED 1.0 - - - - 0.8 - -PAAC - 0.004 0.004 0.004 - - - -BzP - - - 1.4 - - - -石蜡 0.25 0.25 0.25 0.25 - - - -ARP3 0.3 0.1(ec) 0.8 0.2(es) - - 0.1(ec) 0.2ARP1 - - - - 0.3 0.1(ec) 0.1(ec) 0.2蛋白酶 0.036 0.015 0.03 0.028 - 0.03 - -淀粉酶 0.003 0.003 0.01 0.006 - 0.01 - -脂酶 0.005 - 0.001 - - - - -BTA 0.15 0.15 0.15 0.15 - - - -香料 0.2 0.2 0.2 0.2 0.1 0.2 0.2 -硫酸盐 23.4 25.0 22.0 18.5 30.1 19.3 23.1 23.6pH 10.8 10.8 11.3 11.3 10.7 11.5 12.7 10.9微量组分和水 至100%实施例18
根据本发明通过使用标准12头旋转压制机在13KN/cm2压力下压制颗粒餐具洗涤剂组合物制备如下片状洗涤剂组合物:
A B C D E FSTPP - 48.8 49.2 38.0 - 46.8柠檬酸盐 26.4 - - - 31.1 -碳酸盐 - 5.0 14.0 15.4 14.4 23.0硅酸盐 26.4 14.8 15.0 12.6 17.7 2.4ARP1 0.3 - - - 0.06 -ARP2 - 0.04 - - - 0.08ARP3 - - 0.3 0.1(ec) - -蛋白酶 0.058 0.072 0.041 0.033 0.052 0.013淀粉酶 0.01 0.03 0.012 0.007 0.016 0.002脂酶 0.005 - - - - -PB1 1.6 7.7 12.2 10.6 15.7 -PB4 6.9 - - - - 14.4非离子表面活性剂 1.5 2.0 1.5 1.65 0.8 6.3PAAC - - 0.02 0.009 - -MnTACN - - - - 0.007 -TAED 4.3 2.5 - - 1.3 1.8HEDP 0.7 - - 0.7 - 0.4DTPMP 0.65 - - - - -石蜡 0.4 0.5 0.5 0.55 - -BTA 0.2 0.3 0.3 0.3 - -PA30 3.2 - - - - -MA/AA - - - - 4.5 0.55香料 - - 0.05 0.05 0.2 0.2硫酸盐 24.0 13.0 2.3 - 10.7 3.4片重量 25g 25g 20g 30g 18g 20gpH 10.6 10.6 10.7 10.7 10.9 11.2微量组分和水 至100%实施例19
根据本发明制备如下密度1.40kg/l液体餐具洗涤剂组合物:
A B C DSTPP 17.5 17.5 17.2 16.0碳酸盐 2.0 - 2.4 -硅酸盐 5.3 6.1 14.6 15.7NaOCl 1.15 1.15 1.15 1.25Polygen/carbopol 1.1 1.0 1.1 1.25非离子表面活性剂 - - 0.1 -NaBz 0.75 0.75 - -ARP3 0.3 0.5 0.05 0.1NaOH - 1.9 - 3.5KOH 2.8 3.5 3.0 -pH 11.0 11.7 10.9 11.0硫酸盐,微量组分和水 至100%实施例20
根据本发明制备如下液体漂清助剂组合物:
A B C非离子表面活性剂 12.0 - 14.5非离子表面活性剂混合物 - 64.0 -柠檬酸 3.2 - 6.5HEDP 0.5 - -PEG - 5.0 -SCS 4.8 - 7.0乙醇 6.0 8.0 -ARP1 0.3 - 0.1ARP2 - 0.04 0.01液体pH 2.0 7.5 /微量组分和水 至100%实施例21
根据本发明制备如下液体餐具洗涤组合物:
A B C D EC17ES 28.5 27.4 19.2 34.1 34.1氧化胺 2.6 5.0 2.0 3.0 3.0C12葡糖酰胺 - - 6.0 - -甜菜碱 0.9 - - 2.0 2.0二甲苯磺酸盐 2.0 4.0 - 2.0 -Neodol C11E9 - - 5.0 - -多羟基脂肪酸酰胺 - - - 6.5 6.5二亚乙五乙酸钠 - - 0.03 - -(40%)TAED - - - 0.06 0.06蔗糖 - - - 1.5 1.5乙醇 4.0 5.5 5.5 9.1 9.1烷基二苯基氧化物二磺酸盐 - - - - 2.3甲酸钙 - - - 0.5 1.1柠檬酸铵 0.06 0.1 - - -NaCl - 1.0 - - -MgCl2 3.3 - 0.7 - -CaCl2 - - 0.4 - -Na2SO4 - - 0.06 - -MgSO4 0.08 - - - -Mg(OH)2 - - - 2.2 2.2NaOH - - - 1.1 1.1H2O2 200ppm 0.16 0.006 - -ARP3 0.3 - 0.1 - 0.1ARP1 - 0.3 - 0.1 0.1蛋白酶 0.017 0.005 .0035 0.003 0.002香料 0.18 0.09 0.09 0.2 0.2水和微量组分 至100%实施例22
根据本发明制备如下液体硬表面清洁组合物:
A B C D EARP2 0.04 - 0.08 - 0.01ARP3 - 0.3 - 0.125 0.1淀粉酶 0.01 0.002 0.005 - -蛋白酶 0.05 0.01 0.02 - -过氧化氢 - - - 6.0 6.8乙酰基三乙基柠檬酸盐 - - - 2.5 -DTPA - - - 0.2 -丁基羟基甲苯 - - - 0.05 -EDTA* 0.05 0.05 0.05 - -柠檬酸/盐 2.9 2.9 2.9 1.0 -LAS 0.5 0.5 0.5 - -C12AS 0.5 0.5 0.5 - -C10AS - - - - 1.7C12(E)S 0.5 0.5 0.5 - -C12,13 E6.5nonionic 7.0 7.0 7.0 - -Neodol 23-6.5 - - - 12.0 -Dobanol 23-3 - - - - 1.5Dobenol 91-10 - - - - 1.6C25AE1.8S - - - 6.0链烷磺酸钠 - - - 6.0香料 1.0 1.0 1.0 0.5 0.2丙二醇 - - - 1.5乙氧基化四亚乙五亚胺 - - - 1.0 -2,丁基辛醇 - - - - 0.5Hexyl carditol** 1.0 1.0 1.0 - -SCS 1.3 1.3 1.3 - -pH调节至 7-12 7-12 7-12 4 -微量组分和水 至100%*乙二胺二乙酸四钠**二甘醇单己基醚实施例23
根据本发明制备如下用于清洁硬表面和除去家庭霉斑的喷雾组合物:ARP2 0.04淀粉酶 0.01蛋白酶 0.01辛基硫酸钠 2.0十二烷基硫酸钠 4.0氢氧化钠 0.8硅酸盐 0.04Butyl carbitol* 4.0香料 0.35水/微量组分 至100%*二甘醇单丁基醚实施例24
根据本发明制备如下厕所用洗涤块组合物:
A B CC16-C18脂肪醇/50EO 80.0 - -LAS - - 80.0非离子表面活性剂 - 1.0 -油酰胺表面活性剂 - 26.0 -乙烯基甲基醚和马来酸酐的部分酯化 5.0 - -共聚物,粘度0.1-0.5聚乙二醇,MW8000 - 39.0 -水溶性K-聚丙烯酸酯,MW4000-8000 - 12.0 -丙烯酰胺(70%)和丙烯酸(30%)的水 - 19.0 -溶性钠共聚物,低MW三聚磷酸钠 10.0 - -碳酸盐 - - 8.0ARP2 0.04 - 0.01ARP3 - 0.25 0.1染料 2.5 1.0 1.0香料 3.0 - 7.0KOH/盐酸溶液 pH6-11实施例25
根据本发明制备如下抽水马桶清洁组合物:
A BC14-15直链醇7EO 2.0 10.0柠檬酸 10.0 5.0ARP2 0.04 -ARP3 - 0.1DTPMP - 1.0染料 2.0 1.0香料 3.0 3.0NaOH pH6-11水和微量组分 至100%
Claims (18)
1.一种含有洗涤剂组分和含有至少一种伯和/或仲胺基团的氨基官能团聚合物和选自酮、醛和它们的混合物的香料组分之间的反应产物的洗衣和/或清洁组合物,其特征在于所述氨基官能团聚合物具有比在一缩二丙二醇中的1%邻氨基苯甲酸甲酯溶液低的香气强度系数,和反应产物具有超过5的干表面香气系数。
2.权利要求1的组合物,其中所述氨基官能团聚合物含有超过一个氨基,优选超过10个氨基。
3.权利要求1-2的组合物,其中所述氨基官能团聚合物具有150-2.10E6,优选400-50000,更优选600-40000的分子量。
4.权利要求1-3的组合物,其中所述氨基官能团聚合物选自聚乙烯基胺、它们的衍生物、它们的共聚物、亚烷基聚胺、聚氨基酸和它们的共聚物、交联聚氨基酸、氨基取代的聚乙烯基醇、聚氧乙烯二胺或二氨基烷基、氨基烷基哌嗪和其衍生物、N,N’-二(3-氨基丙基)-1,3-丙二胺直链或支链和它们的混合物。
5.权利要求4的组合物,其中所述氨基官能团聚合物是选自聚乙烯胺,MW600-50K;氨基取代的聚乙烯基醇,MW400-300000;聚氧乙烯二[胺];聚氧乙烯二[6-氨基己基];N,N’二(3-氨基丙基)-1,3-丙二胺;1,4-二(3-氨基丙基)哌嗪;聚赖氨酸;交联聚赖氨酸和/或它们的混合物。
6.权利要求1-5任何之一的组合物,其中所述反应产物在加入洗衣和清洁组合物之前预先形成。
7.权利要求1-6任何之一的组合物,其中所述反应产物以按组合物重量计0.0001%-10%,优选0.001%-5%,更优选0.01%-2%的数量存在。
8.权利要求1-7任何之一的组合物,其中所述香料是香料醛,其选自1-癸醛、苯甲醛、florhydral、2,4-二甲基-3-环己烯-1-甲醛、顺-/反-3,7-二甲基-2,6-辛二烯-1-醛、天芥菜精、2,4,6-三甲基-3-环己烯-1-甲醛、2,6-壬二烯醛、α-正戊基肉桂醛、α-正己基肉桂醛、P.T.Bucinal、lyral、cymal、甲基壬基乙醛、己醛、反-2-己烯醛和它们的混合物。
9.权利要求1-7任何之一的组合物,其中所述香料是香料酮,其选自α-二氢大马酮、δ-二氢大马酮、异二氢大马酮、香芹酮、γ-甲基紫罗兰酮、异-E-Super、2,4,4,7-四甲基辛-6-烯-3-酮、苄基丙酮、β-二氢大马酮、大马酮、甲基二氢茉莉酸酯、甲基雪松酮和它们的混合物。
10.权利要求1-7任何之一的组合物,其中所述香料具有低于1ppm,更优选低于10ppb的气味检测阈值。
11.权利要求10的组合物,其中所述香料选自十一碳烯醛、γ十一烷酸内酯、天芥菜精、γ十二烷酸内酯、对-茴香醛、对羟基-苯基-丁酮、cymal、苄基丙酮、α紫罗兰酮、p.t.bucinal、大马酮、β紫罗兰酮和甲基壬基酮,和/或它们的混合物。
12.权利要求1-11任何之一的组合物,其中组合物还含有粘土。
13.一种向表面提供残余香味的方法,其包括使所述表面与权利要求1-12的任何之一的组合物接触的步骤,和随后使所处理的表面与一种物质接触从而使香料释放。
14.权利要求13的方法,其中所述物质是水。
15.权利要求1-12任何之一中定义的化合物在生产向所处理的表面提供残余香味的洗衣和清洁组合物中的应用。
16.权利要求15的应用,其中所述表面是织物。
17.权利要求15的应用,其中所述表面是瓷砖和/或陶瓷制品。
18.一种向织物表面,尤其在多次洗涤后提供改善的织物外观、改善的织物磨损保护和改善的色彩护理的方法,其包括使所述表面与伯和/或仲胺化合物与选自酮、醛和它们的混合物的香料组分的反应产物或权利要求1-11的任何之一中定义的组合物接触的步骤。
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EP98870155 | 1998-10-28 | ||
EP99870025A EP0971026A1 (en) | 1998-07-10 | 1999-02-11 | Laundry and cleaning compositions |
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US9920288B2 (en) | 2014-07-11 | 2018-03-20 | Diversey, Inc. | Tablet dishwashing detergent and methods for making and using the same |
US9139799B1 (en) | 2014-07-11 | 2015-09-22 | Diversey, Inc. | Scale-inhibition compositions and methods of making and using the same |
US9693675B2 (en) * | 2014-12-20 | 2017-07-04 | Medivators Inc. | Cleaning composition |
CA3192947A1 (en) | 2015-04-29 | 2016-11-03 | Shutterfly, Inc | Image product creation based on face images grouped using image product statistics |
JP6629003B2 (ja) * | 2015-08-06 | 2020-01-15 | 花王株式会社 | 食器用液体洗浄剤組成物 |
JP6591277B2 (ja) * | 2015-12-15 | 2019-10-16 | 花王株式会社 | 食器用液体洗浄剤組成物 |
JP6862035B2 (ja) * | 2017-01-20 | 2021-04-21 | 株式会社Adeka | 中性洗浄剤組成物 |
EP3947620A1 (en) * | 2019-03-26 | 2022-02-09 | Unilever Global Ip Limited | Composition |
JP7421920B2 (ja) | 2019-12-17 | 2024-01-25 | 花王株式会社 | 繊維製品用洗浄剤組成物 |
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DE1133847B (de) † | 1960-08-11 | 1962-07-26 | Haarmann & Reimer Gmbh | Verwendung der Kondensationsprodukte von Aldehyden und Ketonen mit Oxyaminen in der Parfuemerie |
CA1130058A (en) * | 1978-11-17 | 1982-08-24 | James B. Melville | Liquid formulations |
US4853369A (en) | 1987-12-18 | 1989-08-01 | International Flavors & Fragrances Inc. | Schiff base reaction product of ethyl vanillin and methyl anthranilate and organoleptic uses thereof |
US5008437A (en) † | 1987-12-18 | 1991-04-16 | International Flavors & Fragrances Inc. | Schiff base reaction product of ethyl vanillin and methyl anthranilate and organoleptic uses thereof |
GB8908199D0 (en) * | 1989-04-12 | 1989-05-24 | Unilever Plc | Malodors reduction |
US5188753A (en) | 1989-05-11 | 1993-02-23 | The Procter & Gamble Company | Detergent composition containing coated perfume particles |
GB8921995D0 (en) * | 1989-09-29 | 1989-11-15 | Unilever Plc | Perfumed laundry detergents |
US5649979A (en) | 1993-08-09 | 1997-07-22 | Firmenich S.A. | Process for perfuming textiles |
HUT74082A (en) | 1993-09-30 | 1996-10-28 | Procter & Gamble | Active substance delivery system |
USH1468H (en) * | 1994-04-28 | 1995-08-01 | Costa Jill B | Detergent compositions containing cellulase enzyme and selected perfumes for improved odor and stability |
JP3631298B2 (ja) | 1995-07-31 | 2005-03-23 | 長谷川香料株式会社 | 置換グルコサミン誘導体および持続性香料組成物 |
EP0831143A1 (en) * | 1996-09-19 | 1998-03-25 | The Procter & Gamble Company | Polymeric compound comprising one or more active alcohols |
EP0841391A1 (en) * | 1996-11-07 | 1998-05-13 | The Procter & Gamble Company | Perfume compositions |
-
1999
- 1999-02-11 EP EP99870025A patent/EP0971026A1/en not_active Withdrawn
- 1999-07-12 HU HU0200238A patent/HUP0200238A3/hu unknown
- 1999-07-12 TR TR2001/00002T patent/TR200100002T2/xx unknown
- 1999-07-12 ES ES99932388T patent/ES2273504T3/es not_active Expired - Lifetime
- 1999-07-12 DE DE69933230T patent/DE69933230T3/de not_active Expired - Lifetime
- 1999-07-12 CZ CZ200158A patent/CZ200158A3/cs unknown
- 1999-07-12 BR BR9912033-0A patent/BR9912033A/pt not_active IP Right Cessation
- 1999-07-12 AT AT99932388T patent/ATE339494T1/de not_active IP Right Cessation
- 1999-07-12 JP JP2000559205A patent/JP4493849B2/ja not_active Expired - Fee Related
- 1999-07-12 ID IDW20010074A patent/ID28314A/id unknown
- 1999-07-12 AU AU48702/99A patent/AU4870299A/en not_active Abandoned
- 1999-07-12 WO PCT/US1999/015678 patent/WO2000002982A2/en active IP Right Grant
- 1999-07-12 CN CN99808494A patent/CN1321187A/zh active Pending
- 1999-07-12 EP EP99932388A patent/EP1123376B2/en not_active Expired - Lifetime
- 1999-07-12 CA CA002336666A patent/CA2336666A1/en not_active Abandoned
- 1999-07-12 KR KR1020017000417A patent/KR20010053480A/ko not_active Application Discontinuation
- 1999-07-12 MA MA25671A patent/MA24922A1/fr unknown
Also Published As
Publication number | Publication date |
---|---|
BR9912033A (pt) | 2001-05-22 |
MA24922A1 (fr) | 2000-04-01 |
TR200100002T2 (tr) | 2002-09-23 |
HUP0200238A2 (hu) | 2002-07-29 |
EP1123376B1 (en) | 2006-09-13 |
AU4870299A (en) | 2000-02-01 |
DE69933230D1 (de) | 2006-10-26 |
EP1123376A2 (en) | 2001-08-16 |
ID28314A (id) | 2001-05-10 |
EP1123376B2 (en) | 2012-10-17 |
DE69933230T3 (de) | 2013-02-07 |
JP2002520495A (ja) | 2002-07-09 |
ATE339494T1 (de) | 2006-10-15 |
WO2000002982A2 (en) | 2000-01-20 |
EP0971026A1 (en) | 2000-01-12 |
CA2336666A1 (en) | 2000-01-20 |
ES2273504T3 (es) | 2007-05-01 |
CZ200158A3 (cs) | 2002-04-17 |
HUP0200238A3 (en) | 2004-01-28 |
WO2000002982A3 (en) | 2001-06-14 |
KR20010053480A (ko) | 2001-06-25 |
DE69933230T2 (de) | 2007-08-30 |
JP4493849B2 (ja) | 2010-06-30 |
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