CN113667554B - Liquid detergent compositions containing amphiphilic graft polymers - Google Patents
Liquid detergent compositions containing amphiphilic graft polymers Download PDFInfo
- Publication number
- CN113667554B CN113667554B CN202111110540.1A CN202111110540A CN113667554B CN 113667554 B CN113667554 B CN 113667554B CN 202111110540 A CN202111110540 A CN 202111110540A CN 113667554 B CN113667554 B CN 113667554B
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- Prior art keywords
- liquid detergent
- surfactant
- detergent composition
- viscosity
- polymer
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- 239000000203 mixture Substances 0.000 title claims abstract description 153
- 239000003599 detergent Substances 0.000 title claims abstract description 113
- 239000007788 liquid Substances 0.000 title claims abstract description 81
- 229920000578 graft copolymer Polymers 0.000 title claims abstract description 39
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 25
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 17
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims description 32
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000002736 nonionic surfactant Substances 0.000 claims description 22
- 239000003945 anionic surfactant Substances 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 18
- 102000004190 Enzymes Human genes 0.000 claims description 15
- 108090000790 Enzymes Proteins 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 239000002738 chelating agent Substances 0.000 claims description 10
- 239000003755 preservative agent Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 230000002335 preservative effect Effects 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002888 zwitterionic surfactant Substances 0.000 claims description 7
- 229920001002 functional polymer Polymers 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005282 brightening Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 239000002304 perfume Substances 0.000 claims description 2
- 150000005846 sugar alcohols Polymers 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 23
- 229920000642 polymer Polymers 0.000 description 48
- -1 alkylbenzene sulfonate Chemical class 0.000 description 36
- 239000002689 soil Substances 0.000 description 36
- 229920000728 polyester Polymers 0.000 description 35
- 239000004744 fabric Substances 0.000 description 34
- 235000014113 dietary fatty acids Nutrition 0.000 description 32
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- 229930195729 fatty acid Natural products 0.000 description 32
- 239000000047 product Substances 0.000 description 28
- 230000008859 change Effects 0.000 description 24
- 238000005406 washing Methods 0.000 description 22
- 125000000217 alkyl group Chemical group 0.000 description 19
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 18
- 239000000693 micelle Substances 0.000 description 16
- 125000004432 carbon atom Chemical group C* 0.000 description 15
- 150000004665 fatty acids Chemical class 0.000 description 15
- 229940088598 enzyme Drugs 0.000 description 14
- 238000007046 ethoxylation reaction Methods 0.000 description 13
- 238000005338 heat storage Methods 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
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- 238000003756 stirring Methods 0.000 description 10
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- 238000000034 method Methods 0.000 description 9
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- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 7
- 239000002280 amphoteric surfactant Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000004519 grease Substances 0.000 description 7
- 229920000570 polyether Polymers 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
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- 230000007062 hydrolysis Effects 0.000 description 6
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- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
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- 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
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 238000005202 decontamination Methods 0.000 description 4
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- 229910021641 deionized water Inorganic materials 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 4
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- 239000011572 manganese Substances 0.000 description 4
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- 150000003839 salts Chemical class 0.000 description 4
- UYZVDMGEEIRMSK-UHFFFAOYSA-N 3-propylheptan-1-ol Chemical compound CCCCC(CCC)CCO UYZVDMGEEIRMSK-UHFFFAOYSA-N 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 3
- 108091005804 Peptidases Proteins 0.000 description 3
- 239000004365 Protease Substances 0.000 description 3
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 3
- 150000003926 acrylamides Chemical class 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 150000007942 carboxylates Chemical class 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 229940079919 digestives enzyme preparation Drugs 0.000 description 3
- 125000004185 ester group Chemical group 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000008233 hard water Substances 0.000 description 3
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- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 3
- 239000011118 polyvinyl acetate Substances 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 3
- 238000010257 thawing Methods 0.000 description 3
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 2
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
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- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
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- 229920001290 polyvinyl ester Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
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- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
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- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
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- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 108010038851 tannase Proteins 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229940087291 tridecyl alcohol Drugs 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- OHOTVSOGTVKXEL-UHFFFAOYSA-K trisodium;2-[bis(carboxylatomethyl)amino]propanoate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C(C)N(CC([O-])=O)CC([O-])=O OHOTVSOGTVKXEL-UHFFFAOYSA-K 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- 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
- C11D10/00—Compositions of detergents, not provided for by one single preceding group
- C11D10/04—Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
Abstract
The invention discloses a liquid detergent composition containing an amphiphilic graft polymer, and relates to the technical field of detergents. The liquid detergent composition comprises 0.1-5% of amphiphilic graft polymer and 1-10% of fatty alcohol polyoxyethylene ether by weight percent. The liquid detergent compositions of the present invention have good secondary detergency and are storage stable in alkaline environments.
Description
Technical Field
The invention relates to the technical field of detergents, in particular to a liquid detergent composition containing an amphiphilic graft polymer and a preparation method thereof.
Background
Oily soils adhere to fabric surfaces in the form of oil films/droplets, the ease of removal of which is related to the contact angle that the oily soil forms with the fabric surface. The smaller the contact angle formed between the oily soil and the fabric surface, the more tightly the oily soil and fabric adhere, and the more difficult the removal. It is generally believed that oily soils on polar fabric surfaces typically have contact angles greater than 90 ° and greasy soils on non-polar fabric (e.g. polyester) surfaces have contact angles less than 90 °.
To improve the oil stain resistance of polyester fabrics, the polyester fabric surface may be modified to increase the hydrophilicity of the fabric to reduce oil stain adhesion, such surface modification may be achieved by treating the fabric directly, for example as outlined in US3416952 a. Or more preferably by using a Soil Release Polymer (SRP) in the wash process. The block polymer of the polyester polyether has a functional group composition very similar to that of polyester fibers, and can generate binding force with the surfaces of the weak polar fabric fibers such as polyester, nylon and the like. The block type polymer of the polyester polyether at least comprises two parts of structures, on one hand, the chain segment structure formed by the ester repeating units can be combined with the surface of the fabric to anchor the copolymer on the surface of the matrix; on the other hand, the chain segment structure composed of ethylene oxide repeating units ensures the sufficient hydrophilic property of the polymer, and can be fully dispersed and effectively migrated in aqueous solution.
It is known to include anionic moieties in the polymer structure to improve the efficacy of these soil release polymers, particularly to improve their anti-redeposition properties. For example, DE 10 2007 013 217 and EP 1 966 273 disclose anionic polyesters which are useful as soil release agents in laundry detergents. Such anionic soil release polymers are particularly useful in powder detergents in view of compatibility with detergent compositions.
The use of nonionic soil release agents in liquid laundry detergents is well known in the art. GB 1,466,639, US 4,132,680, US 4,702,857, EP 0 199 403, US 4,711,730, US 4,713,194 and US 4,759,876 disclose aqueous detergent compositions containing soil release polymers, but secondary soil release of the detergent composition has not been studied, and polyester soil release polymers of polyester polyethers are susceptible to structural failure of the polymer due to hydrolysis of the polyester in alkaline environments due to poor alkali resistance of the ester groups, thereby losing the original soil release activity. Accordingly, the problem addressed by the present invention is to provide a liquid detergent composition which has good secondary detergency and which is storage stable in alkaline environments.
Disclosure of Invention
Since polyester polyether soil release polymers are susceptible to hydrolysis in alkaline environments, which results in liquid detergent composition stability, it is necessary to provide a liquid detergent composition that has good secondary soil release properties and is stable in the liquid detergent composition for long periods of time.
The liquid detergent composition containing the amphiphilic graft polymer comprises, by weight, 0.1% -5% of the amphiphilic graft polymer and 1% -10% of fatty alcohol polyoxyethylene ether.
The amphiphilic graft polymer is preferably a graft copolymer of a polyethylene glycol graft substrate and an ethyl acetate side chain, and has the structural characteristics shown in a formula (I):
in formula (I), n ranges from 30 to 70, and the weight average molecular weight Mw of the amphiphilic graft polymer ranges from 3000 to 100,000.
The fatty alcohol-polyoxyethylene ether has the structural characteristics shown in the formula (II):
in formula (II), n is 6 to 24; x is 1 to 30; y is 0 to 10.
The viscosity of the liquid detergent composition at 25 ℃ is 200 mPa.s-5000 mPa.s, the pH is 7.5-10, the heat storage viscosity change rate is less than 20%, and the secondary quick detergency of the combination in washing of polyester cloth is more than 35%.
Preferably, the amphiphilic graft polymer has an average of 1 grafting site or less per 50 alkylene oxide units.
Preferably, in formula (I), n ranges from 50 to 55, and the weight average molecular weight Mw of the amphiphilic graft polymer ranges from 25000 to 30000.
Preferably, the fatty alcohol in the fatty alcohol polyoxyethylene ether is an isomeric alcohol; in formula (II), n is 8 to 18; x is 6 to 12; y is 1 to 8.
Further, the liquid detergent composition of the present invention comprises the following ingredients in weight percent:
0.1-70% of a surfactant selected from at least one of anionic surfactant, nonionic surfactant and zwitterionic surfactant;
5% -95% of water and a polyalcohol solvent.
Preferably, the weight percentage of the surfactant is 20% -60%.
Further, the liquid detergent composition of the present invention further comprises 0.01% to 30% by weight of a co-additive comprising a viscosity modifier and a pH stabilizer. Typically, the fluidity of the composition is characterized by the kinetic viscosity, the kinetic viscosity of the liquid detergent composition of the present invention being 300 to 15000mpa.s, more particularly 30 to 5000mpa.s, even more particularly 200 to 5000mpa.s at 25 ℃. The liquid detergent composition of the present invention has a pH of 7.5 to 10.
Further, the auxiliary additive also comprises one or more of enzyme preparation, alkaline agent, preservative, anti-redeposition agent, functional polymer, chelating agent, fluorescent whitening agent and essence.
In some embodiments, the weight percentage of the surfactant in the liquid detergent composition is from 0.1% to 40%.
In some embodiments, the surfactant comprises the following components in weight percent: 1 to 30 percent of anionic surfactant, 1 to 30 percent of nonionic surfactant, 0 to 30 percent of zwitterionic surfactant and 0 to 30 percent of cationic surfactant.
In some embodiments, the liquid detergent composition of the present invention comprises, in weight percent:
0.1-5% of amphiphilic graft polymer;
5% -30% of a surfactant selected from at least one of anionic surfactant, nonionic surfactant and zwitterionic surfactant;
0.01-10% of an auxiliary agent selected from one or more of an enzyme preparation, an alkaline agent, a viscosity regulator, a pH stabilizer, a preservative, an anti-redeposition agent, a functional polymer, a chelating agent, a fluorescent whitening agent and essence; 5% -95% of water.
Amphiphilic graft polymers
The side chains of the amphiphilic graft polymer are formed via polymerization of the vinyl ester component (B) in the presence of the graft base (a).
Particularly suitable grafting bases (A) include:
(A1) Polyethylene glycol which may in particular be end-capped with C1-C25-alkyl groups at one or both end groups, but is preferably not etherified, and has an average molar mass Mn of preferably 1500 to 20000, more preferably 2500 to 15000.
(A2) Copolymers of ethylene oxide with propylene oxide and/or butylene oxide, said copolymers having an ethylene oxide content of at least 50% by weight, which likewise can be terminated, in particular at one or both end groups, by C1-C25-alkyl groups, but are preferably not etherified, and have an average molar mass Mm of preferably from 1500 to 20000, more preferably from 2500 to 15000
(A3) Chain-extended products having an average molar mass of 2500 to 20000, obtainable by reacting polyethylene glycols (A1) having an average molar mass Mn of 200 to 5000 or copolymers (A2) having an average molar mass Mn of 200 to 5000 with C2-C12-dicarboxylic acids or dicarboxylic esters or C6-C18-diisocyanates. The preferred grafting base (A) is polyethylene glycol (A1).
The vinyl ester component (B) may consist of (B1) vinyl acetate or vinyl propionate or a mixture of vinyl acetate and vinyl propionate, with vinyl acetate being particularly preferred as vinyl ester component (B). Or a vinyl ester component (B) formed by copolymerization of vinyl acetate and/or vinyl propionate (B1) with other ethylenically unsaturated monomers (B2), wherein the content by weight of the other ethylenically unsaturated monomers (B2) in the vinyl ester component (B) is not more than 30%. Suitable comonomers (B2) are, for example, monoethylenically unsaturated carboxylic and dicarboxylic acids and their derivatives, such as esters, amides and anhydrides, and styrene. It is of course also possible to use mixtures of different comonomers. Specific examples of comonomers include: (meth) acrylic acid, C1-C12-alkyl and hydroxy-C2-C12-alkyl (meth) acrylates, (meth) acrylamides, N-C1-C12-alkyl (meth) acrylamides, N-di (C1-C6-alkyl) (meth) acrylamides, maleic acid, maleic anhydride and mono (C1-C12-alkyl) maleates. Preferred monomers (B2) are C1-C8-alkyl (meth) acrylates and hydroxyethyl acrylate, particularly preferably C1-C4-alkyl (meth) acrylates.
More preferred monomers (B2) are methyl acrylate, ethyl acrylate, in particular n-butyl acrylate. When the preferred amphiphilic graft polymer contains the monomer (B2) as a constituent of the vinyl ester component (B), the content of (B2) in the graft polymer is preferably 0.5% to 20%, more preferably 1% to 15%, and most preferably 2% to 10%.
Due to the low content of ungrafted polyvinyl ester and the balanced ratio of components (a) and (B), the preferred amphiphilic graft polymer is soluble in water or in a water/alcohol mixture (e.g. 25% by weight of an aqueous diethylene glycol monobutyl ether solution). They have a significantly low cloud point, generally equal to or less than 95 ℃, preferably equal to or less than 85 ℃, and more preferably equal to or less than 75 ℃, for graft polymers soluble in water up to 50 ℃, and generally equal to or less than 90 ℃, preferably 45 ℃ to 85 ℃ for other graft polymers in 25 weight percent diethylene glycol monobutyl ether.
The most preferred amphiphilic graft polymer is a graft copolymer of a polyethylene glycol graft base and vinyl acetate side chains, e.g., conforming to the following structure;
the amphiphilic graft polymer of the present invention balances the degree of hydrophilicity and hydrophobicity of the polymer. Low grafting levels are required to ensure the overall solubility of the polymer in water. If the grafting ratio is too high, the polymer will become water insoluble and thus not uniformly dispersed in water. On the other hand, if the amount of ungrafted content is too low, the polymer will only be soluble in water and not be adsorbed in the polyester fabric.
The graft polymer of polyvinyl acetate (PVAc) grafted onto poly L-glycol (PEG) is an amphiphilic polymer, and the polarity is mainly dependent on the ratio of polyethylene glycol as hydrophilic part to polyvinyl acetate as hydrophobic part, and the amount of their individual graft polymer chains. Higher amounts of vinyl acetate in the polymer make the polymer more nonpolar, while increasing the amount of PEG makes the polymer more polar.
The amphiphilic graft polymer preferably has a low degree of branching (degree of grafting). Based on the reaction mixture obtained, they have on average not more than 1 grafting site, preferably not more than 0.6 grafting site, more preferably not more than 0.5 grafting site, and most preferably not more than 0.4 grafting site per 50 alkylene oxide units. Based on the reaction mixture obtained, they contain on average preferably at least 0.05, in particular at least 0.1 grafting sites per 50 alkylene oxide units.
Preferably, the weight average molecular weight Mw of the amphiphilic graft polymer is 3000 to 100000, preferably 6000 to 45000, and more preferably 8000 to 30000.
Solvent system
Organic solvents include, but are not limited to, polyols. The polyol (or polyhydroxy alcohol) may be a linear or branched alcohol having two or more hydroxyl groups. Thus, diols in which two hydroxyl groups are attached to different carbon atoms in the aliphatic chain may also be used.
Suitable polyols include, but are not limited to, glycerol, propylene glycol, butylene glycol, pentylene glycol, xylitol, sorbitol, mannitol, diethylene glycol, triethylene glycol, erythritol, galactitol, or mixtures thereof.
The liquid detergent compositions of the present invention may comprise from 5% to 75% of one or more solvents, preferably from 7% to about 50%, more preferably from about 20% to about 30%.
Surface active agent
Surfactants for use in the detergent compositions of the present invention include anionic surfactants, nonionic surfactants, amphoteric surfactants or mixtures thereof.
Anionic surfactants
The total weight of the mixture of anionic surfactants is 0.01% to 30% of the total weight of the liquid detergent composition.
The anionic surfactant is selected from one or more of sulfonate surfactant, carboxylate surfactant and sulfate surfactant; preferably one or a mixture of several from alkylbenzene sulfonate, C8 to C18 alkyl sulfate, C8 to C18 ethoxylated fatty alcohol sulfate, d-olefin sulfonate, fatty acid alkyl ester sulfonate, ethoxylated fatty alcohol ether carboxylate.
In some embodiments, the mixture of anionic surfactants preferably contains alkylbenzene sulfonates and derivatives thereof. The alkylbenzene sulfonate salt satisfies the following general formula:
Wherein R is1 is an alkyl group having 6 to 24 carbon atoms, M + Is cationic. R is R 1 Alkyl groups which can be straight chain or branched chain; may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds. More preferably R 1 Is a straight-chain alkyl group having 8 to 18 carbon atoms.
Wherein R is 1 Is an alkyl group having 6 to 24 carbon atoms; x is 0.5 to 30; wherein M is + Is cationic. R is R 1 Alkyl groups which can be straight chain or branched chain; may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds. Preferably R 1 Is a straight-chain alkyl group having 8 to 18 carbon atoms. x represents an average degree of ethoxylation of from 0.5 to 30, preferably from 0.5 to 10, more preferably from 0.5 to 3.
In some embodiments, the mixture of anionic surfactants contains ethoxylated fatty alcohol sulfate. Ethoxylated fatty alcohol sulfates are derivatives of ethoxylated fatty alcohols having the general formula:
wherein R is 2 Is an alkyl group having 6 to 24 carbon atoms; x is 1 to 30; wherein M is + Is cationic. R is R 2 Alkyl which is linear or branched, saturated or contains one or more unsaturated double bonds, preferably linear alkyl having 8 to 18 carbon atoms. x represents an average degree of ethoxylation of from 1 to 30, preferably from 1 to 10, more preferably from 1 to 3.
In some embodiments, an alpha-olefin sulfonate is present having the general formula:
wherein y is 0 to 2, R 3 Is an alkyl group having 6 to 24 carbon atoms, preferably an alkyl group having 8 to 18 carbon atoms.
The anionic surfactant may also be selected from fatty acid alkyl ester sulphates, preferably fatty acid Methyl Ester Sulphates (MES), preferably having a fatty acid carbon number of 8 to 18. Sulfosuccinates, preferably fatty alcohol polyoxyethylene ether succinate monoester disodium salt, can also be included, the fatty alcohol carbon number is preferably 8 to 18, and the average ethoxylation degree is preferably 2.0.
The anionic surfactant may also comprise one or more mixtures of sodium alkyl disulfonate or derivatives thereof, preferably sodium alkyl diphenyl oxide disulfonate, a suitable example being sodium dodecyl diphenyl oxide disulfonate. Fatty acid alkyl ester sulfate, preferably fatty acid Methyl Ester Sulfate (MES), may also be included, the fatty acid carbon number preferably being 8 to 18. Sulfosuccinates, preferably fatty alcohol polyoxyethylene ether sulfosuccinic acid monoester disodium salt, can also be included, the fatty alcohol carbon number is preferably 8 to 18, and the average ethoxylation degree is preferably 2.0.
In some embodiments, the mixture of anionic surfactants contains a fatty acid salt. The fatty acid salt is formed by alkaline formation of fatty acid. The alkali agent which can be selected is monoethanolamine or triethanolamine. In the liquid detergent composition according to the present invention, the fatty acid salt is selected from metal salts of fatty acids having 10 to 20 carbon atoms, preferably linear alkyl fatty acids having 10 to 16 carbon atoms.
Nonionic surfactant
The total weight of the mixture of nonionic surfactants is 0.01 to 30% of the total weight of the liquid detergent composition. The nonionic surfactant is selected from one or more of fatty alcohol alkoxylate, alkyl polyglycoside, fatty acid alkoxylate, fatty acid ethoxylate, fatty acid alkyl alcohol amide, and ethoxylated sorbitan ester. In some embodiments, the nonionic surfactant mixture preferably contains a fatty alcohol alkoxylate having the general formula:
wherein n is 6 to 24; x is 0.5 to 30; y is 0 to 10.
The fatty alcohol alkoxylate is a product of ring-opening polymerization of fatty alcohol and alkylene oxide under the action of a basic catalyst, and thus is a mixture. Fatty alcohols include straight chain alcohols or branched chain isomeric alcohols. Alkoxy groups include ethoxy groups and propoxy groups. The fatty alcohol is preferably a C8 to C18 fatty alcohol, and preferred alcohols include, but are not limited to, one of hexanol, octanol, decanol, 2-ethyl hexanol, 3-propyl heptanol, lauryl alcohol, iso-tridecyl alcohol, tetradecyl alcohol, cetyl alcohol, palm oleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, linoleyl alcohol, linolenyl alcohol, and mixtures thereof. The average degree of ethoxylation x is preferably from 2 to 12. Preferred examples are the NEODOL series of linear fatty alcohol ethoxylate products from SHELL, the ECOSURFEH series of ethoxylated and propoxylated 2-ethyl hexanol products from DOW, the Lutensol XL series of ethoxylated and propoxylated 3-propyl heptanol products from BASF and the Lutensol XP series of ethoxylated 3-propyl heptanol products from BASF.
The nonionic surfactant mixture may contain fatty acid alkoxylates, preferably from ethoxylated C8 to C18 fatty acid esters, with an average degree of ethoxylation of from 2 to 10. May contain ethoxylated alkyl sorbitan esters having an alkyl carbon number of from 6 to 18 and an average degree of ethoxylation of from 4 to 20; a suitable example is the Corda company Tween series.
The nonionic surfactant mixture may comprise fatty acid alkyl alcohol amides having 6 to 24 carbon atoms, may be linear or branched, may be saturated or unsaturated; the number of alkyl alcohols is from 0 to 2. Preferably mono-and diethanolamides, isopropanol amides having a fatty acid carbon number of 8 to 18, suitable examples being coconut diethanolamide.
Other suitable surfactants include amphoteric surfactants. Suitable amphoteric surfactants for use herein include amidopropyl betaine and derivatives of aliphatic or heterocyclic secondary and tertiary amines in which the aliphatic moiety can be straight or branched chain and wherein one of the aliphatic substituents contains from 8 to 24 carbon atoms and at least one aliphatic substituent containing an anionic water-solubilizing group. Amphoteric surfactants, when present, typically comprise from 0.01% to 20% or from 0.5% to 10% of the liquid detergent compositions of the present invention.
Additive agent
The liquid detergent composition according to the invention comprises the following optional additives: the additive is one or more selected from viscosity regulator, pH stabilizer, enzyme preparation, alkali agent, antiseptic, antiredeposition agent, functional polymer, chelating agent, fluorescent whitening agent and essence.
Viscosity modifier
The liquid detergent compositions to which the present invention relates may comprise one or more viscosity modifiers to provide a suitable viscosity. Suitable viscosity modifiers are, for example, salts, polysaccharides, gums, short chain fatty alcohols, short chain fatty alcohol alkyl ethers. Suitable examples are sodium chloride, sodium formate, sodium acetate, ethanol, propylene glycol, sodium citrate, alkyl hydroxyalkyl cellulose ether, carrageenan, xanthan gum, polyacrylamide derivatives. The viscosity modifier is present in the liquid detergent composition in an amount of from 0.01% to 30.0%, further from 0.05% to 10.0%, and still further from 0.05% to 5.0%.
PH regulator
Including acidity and basicity modifiers. Wherein the acidity regulator is at least one of organic acid, inorganic acid and strong acid weak alkali salt, such as citric acid, succinic acid, benzoic acid, gallic acid, boric acid, preferably citric acid. The alkalinity regulator is selected from at least one of organic amine, hydroxide of alkali metal and carbonate of alkali metal, preferably sodium hydroxide.
Enzyme preparation
The detergent compositions to which the present invention relates may comprise one or more enzyme preparations to provide cleaning performance, fabric care and/or other benefits. The enzyme preparation is selected from the group consisting of:
proteases, alpha-amylases, cellulases, hemicellulases, phospholipases, esterases, lipases, peroxidases/oxidases, pectinases, lyases, mannanases, cutinases, reductases, xylanases, pullulanases, tannase, pentosanases, maltoglycans, arabinanases, beta-glucanases. Commonly used enzyme preparations are proteases, amylases, lipases, cutinases and/or cellulases. The enzyme preparation is present in an amount of 0.001% to 5%, further 0.01% to 2% of the detergent composition.
The detergent compositions of the present invention may comprise from 0.001% to 10% by weight of the composition of an enzyme stabilizing system. The enzyme stabilizing system may be compatible with the detergent composition and may comprise one or more of calcium ions, boric acid, borax, propylene glycol, glycerol, and a mixture of one or more polyols. The weight and amount of enzyme stabilizing system is adjusted according to the form and composition of the detergent composition and the type of enzyme preparation.
Alkaline agent
The liquid detergent compositions according to the present invention may comprise one or more alkaline agents selected from the group consisting of sodium hydroxide, potassium hydroxide, alkali metal carbonates, alkali metal silicates and monoethanolamine. The alkaline agent is present in the liquid detergent composition in an amount of from 0.01% to 30.0%, further from 0.05% to 10.0%, and still further from 0.05% to 6.0%.
Preservative agent
In some embodiments, the liquid detergent compositions to which the present invention relates preferably comprise a preservative, suitable examples being phenoxy alcohol, sodium benzoate; isothiazolinones and derivatives thereof, such as methyl isothiazolinones, methyl chloroisothiazolinones, benzisothiazolinones or mixtures thereof. The preservative is used in an amount of 0.001% to 5%, further 0.01% to 2%.
Anti-redeposition agent
From the viewpoint of effectively improving the washing effect, the liquid detergent composition according to the present invention may contain an anti-redeposition agent. Anti-redeposition agents include, but are not limited to, mixtures of the following compounds:
cellulose derivatives such as carboxymethyl cellulose, ethyl hydroxyethyl cellulose, methyl cellulose; homopolymers and copolymers of vinylpyrrolidone, for example linear polyvinylpyrrolidone, copolymers of vinylpyrrolidone and vinyl acetate, copolymers of vinylpyrrolidone and vinylimidazole; polycarboxylates, such as polyacrylates, polyacrylic polymaleic acid copolymers, acrylic acid-acrylic ester-sulfonate copolymers. The antiredeposition agent is present in the liquid detergent composition in an amount of from 0.01% to 5%, further from 0.01% to 2%.
Functional polymers
The present invention relates to detergent compositions comprising one or more functional polymers comprising amphiphilic alkoxylated grease cleaning polymers, carboxylate polymers and/or modified carboxylate polymers, polycarboxylates and/or modified polycarboxylates.
The detergent compositions to which the present invention relates may comprise amphiphilic alkoxylated grease cleaning polymers having balanced hydrophilic and hydrophobic properties such that they remove grease particles from fabric surfaces or hard surfaces. One class of examples of such amphiphilic alkoxylated grease cleaning polymers include those comprising one or more core structures and a plurality of alkoxylated groups attached to the core structure, the core structure of which may be, but is not limited to, ethylene diamine, triethylenetetramine, tetraethylenepentamine, and the like, of the molecular formula H 2 N(C 2 H 4 NH) n H, the oxyalkylated groups of which may be, but are not limited to polyoxyethylene groups, polyoxypropylene groups and/or their block and/or random co-groups. The liquid detergent composition comprises 0-10.0% by weight of amphiphilic alkoxylated grease cleaning polymer, further 0.1-5.0% by weight of amphiphilic alkoxylated grease cleaning polymer, and further 0.5-2.0% by weight of amphiphilic alkoxylated grease cleaning polymer.
Chelating agent
The liquid detergent compositions of the present invention may comprise one or more metal ion chelating agents, including copper, iron and/or manganese chelating agents, and mixtures thereof. These chelating agents can reduce the concentration of free metal ions in the liquid detergent, thereby reducing the deactivation of the enzyme preparation by these metal ions, the catalytic decomposition of other components, etc. Useful chelating agents include aminocarboxylates, aminophosphonates, and the like, including but not limited to ethylenediamine tetraacetate (EDTA), nitrilotriacetate (NTA), diethylenetriamine pentaacetate (DTPA), alanine diacetate (MGDA), glutamate diacetate (GLDA) and/or ethylenediamine tetra (methylenephosphate) (EDTMPA), nitrilotris (methylenephosphate) (ATMP), diethylenetriamine penta (methylenephosphate) (DTPMP), hydroxy-ethane bisphosphonate (HEDP), and ethylenediamine disuccinate (EDDS), and mixtures thereof.
The liquid detergent composition according to the present invention comprises 0 to 20.0% by weight of the chelating agent, more preferably 0.1 to 5.0% by weight, still more preferably 0.5 to 2.0% by weight of the liquid detergent composition.
Fluorescent whitening agent
The use of fluorescent whitening agents in liquid detergent compositions is well known in the art and commercial fluorescent whitening agents are commercially available. Fluorescent whitening agents are present in the form of their alkali metal salts (most often sodium salts). Preferred fluorescent whitening agents include, but are not limited to: distyrylbiphenyl compounds. A suitable example is 4,4' -bis (sodium 2-sulfonate styryl) biphenyl, such as the product of BASF company CBS-X. The dosage of the fluorescent whitening agent is 0.01% -2% of the total amount of the composition, and further 0.01% -0.1%.
The liquid detergent compositions of the present invention may be flowable liquids or viscous liquids or gels, have good secondary detergency and are storage stable in alkaline environments.
Detailed Description
The polyester soil release polymer and liquid detergent compositions of the present invention are described in further detail below in conjunction with the specific examples.
The features, advantages and advantages of the present invention will become apparent to those skilled in the art from a reading of the present disclosure.
Preferably, the liquid detergent composition is a liquid laundry detergent composition or a liquid dish detergent composition, but preferably is a liquid laundry detergent composition. The liquid detergent composition may be aqueous or non-aqueous and may be anisotropic, isotropic or a combination thereof. As used herein, "water" means water added to the detergent composition as a separate component, excluding water introduced into the feed. The "solvent" does not comprise water added to the detergent composition as a separate component.
All percentages, fractions and ratios are by weight of the total composition of the present invention, unless otherwise specified. All weights as they pertain to listed ingredients are to the active level and, therefore, do not include solvents or by-products that may be included in commercially available materials, unless otherwise specified. The term "weight percent" may be expressed herein in terms of the symbol "%". All formulations and tests herein take place in an environment of 25 ℃, unless otherwise indicated.
The terms "comprising," "including," "containing," "having," or other variations thereof herein are intended to cover a non-closed inclusion, without distinguishing between them. The term "comprising" means that other steps and ingredients may be added that do not affect the end result. The term "comprising" also includes the terms "consisting of …" and "consisting essentially of …". The compositions and methods/processes of the present invention can comprise, consist of, and consist essentially of the essential elements and limitations described herein, as well as additional or optional ingredients, components, steps, or limitations of any of the embodiments described herein.
Liquid detergent composition
Liquid detergent composition refers to a detergent composition in a liquid state. The composition can be diluted according to a certain proportion or directly contacted with a substrate (namely fabric products, hard surfaces and the like) to be contacted, so that stains on the surface of the substrate are removed, and the aim of cleaning the surface of the substrate is fulfilled. The liquid detergent compositions also typically contain a surfactant system and other common detergency builders such as viscosity modifiers, enzyme preparations, perfumes and the like.
In one embodiment, the liquid detergent composition comprises, in weight percent, 0.01% to 5% of an amphiphilic graft soil release polymer and 1% to 10% of a fatty alcohol polyoxyethylene ether.
Further, the liquid detergent composition further comprises the following ingredients: 0.1-70% of a surfactant selected from at least one of anionic surfactant, nonionic surfactant and zwitterionic surfactant; fatty acid salt 0.1-30%; 0.01-30% of an auxiliary additive, wherein the auxiliary additive is at least one selected from a viscosity regulator, a pH regulator, an enzyme preparation, an alkaline agent, a preservative, a colorant, a solubilizer, an optical brightening agent, a color stabilizer and essence; and 5% -95% of water and a polyol solvent.
In this embodiment, the liquid detergent composition comprises, in weight percent: 0.1-10% of the polyester soil release polymer; 5% -30% of a surfactant, wherein the surfactant is at least one selected from anionic surfactant, nonionic surfactant and zwitterionic surfactant; fatty acid salt 0.5-5.0%; 0.01-10% of a washing auxiliary agent, wherein the auxiliary agent is at least one selected from viscosity regulator, pH regulator, enzyme preparation, alkaline agent, preservative, colorant, solubilizer, fluorescent whitening agent, color stabilizer and essence; and 5% -95% of water and a polyol solvent.
Stable liquid detergent composition
It is well known that the alkaline environment of detergents is prone to hydrolysis of the polyester soil release polymer, resulting in disruption of the polymer structure, thereby reducing the efficacy of the detergent. Under alkaline conditions, the ester groups in the polyester soil release polymer structure will form three parts, namely terephthalate, propylene glycol and polyethylene glycol after complete hydrolysis. The hydrolysis process requires the consumption of an equivalent amount of base to the ester groups, although the detergent composition typically contains a pH stabilizer, this will also have a significant effect on the pH of the composition. Second, the polyester soil release polymer is significantly different from the corresponding amounts of terephthalate, propylene glycol, polyethylene glycol and the like in terms of physical properties of the composition as a whole, such as viscosity, rheological properties, and the like. Terephthalate, propylene glycol, polyethylene glycol all reduce the viscosity of the composition slightly, but to a much lesser extent than polyester soil release polymers.
Thus, "stable" herein means that the physicochemical parameters of the liquid detergent composition, such as pH, viscosity, etc., do not change significantly after storage for a period of time under certain conditions. Since the value of the pH change depends on the amount of soil release polymer in the composition, the pH is hardly changed when the amount is small. However, even very small amounts of polyester soil release polymer hydrolyze, significantly changing the viscosity of the composition.
Preparation method
The liquid detergent compositions of the present invention are prepared by various methods well known to those skilled in the art. The formulation of the composition may be carried out by conventional means, in particular by selecting the appropriate processing temperature and processing time depending on the state and effect of the components in solution, and the stability of the components.
Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. The following examples are intended to further describe and demonstrate embodiments within the scope of the present invention. Accordingly, the examples should be construed as merely illustrative of the invention in greater detail and not limiting the invention in any way.
A process 1 for preparing a liquid detergent composition according to any one of the preceding claims comprising the steps of:
1) Adding deionized water and an alkaline agent into a preparation tank;
2) Stirring and heating, heating and saponifying fatty acid to obtain fatty acid salt, stirring until the fatty acid salt is completely dissolved, and adding an anionic surfactant;
3) After complete dissolution, adding the fatty alcohol alkoxylate, the nonionic surfactant and the amphoteric surfactant, and stirring until complete dissolution;
4) Stopping heating, adding the rest deionized water into the preparation tank, and cooling to below 40 ℃;
5) Adjusting the pH;
6) Adding additives such as preservative and the like, and stirring until the additives are completely dissolved;
7) Adjusting the viscosity;
8) Adding the amphiphilic graft polymer, and stirring uniformly.
A process 2 for preparing a liquid detergent composition according to any of the preceding claims comprising the steps of:
1) Adding deionized water and an organic solvent into a preparation tank;
2) Stirring, adding an alkaline agent and fatty acid to saponify into fatty acid salt, stirring until the fatty acid salt is completely dissolved, and adding an anionic surfactant;
3) After the temperature is reduced to below 40 ℃, adding nonionic surfactant and amphoteric surfactant, and stirring until the nonionic surfactant and the amphoteric surfactant are completely dissolved;
4) Adjusting the pH;
5) Adding the amphiphilic graft polymer, enzyme preparation, essence, pigment and other additives, and stirring until the amphiphilic graft polymer and the additives are completely dissolved;
6) Adding the balance of deionized water, and stirring uniformly.
The liquid detergent composition prepared by the 2 methods has high storage stability and excellent detergency.
Secondary decontamination
The secondary soil release is to deposit specific components in the composition on the fabric after the fabric is washed for the first time by the detergent composition, and then to test the soil release performance after the second time of washing.
Viscosity of the mixture
The property of a liquid that, when flowing, creates internal friction between its molecules is called the viscosity of the liquid. The amount of tackiness is expressed as viscosity. Viscosity is a measure of the viscosity of a fluid and is an indication of the fluid flow force versus its internal friction phenomena. The higher the viscosity, the higher the internal friction, and the higher the molecular weight, the more hydrocarbon bonds, and the greater the force.
The viscosity is generally divided into: dynamic viscosity, kinematic viscosity, conditional viscosity. Dynamic viscosity refers to: the liquid layer per unit area per unit distance is used to generate the force required per unit flow rate. In the international system of units, the dynamic viscosity unit is pa.s, and the dynamic viscosity characterizes the internal friction coefficient of the viscosity of a liquid; the kinematic viscosity is the ratio of the dynamic viscosity of the fluid to the density ρ of the fluid at the same temperature. Conditional viscosity: refers to the viscosity in terms of conditional units measured using different specific viscometers.
Typically, the viscosity of a liquid detergent is characterized by the dynamic viscosity, and a rotational viscometer is typically used to measure the viscosity of the liquid detergent. The viscosity referred to in the present invention is the dynamic viscosity, and the viscosity of the composition at 25 ℃ + -0.1 ℃ is measured as a viscosity number using a rotational viscometer.
Viscosity of surfactant solution
When the concentration of surfactant in water is higher than its critical micelle concentration, aggregates can spontaneously form, and the structure and morphology of the aggregates determine the physical properties of the aqueous surfactant solution, such as viscosity. With the increase of the concentration of the surfactant, spherical micelles, rod-like micelles, linear micelles, and liquid crystal structures such as lamellar micelles, hexagonal phase micelles, etc. are gradually formed. As the micelle volume becomes larger, the morphology changes from zero dimension (spherical), one dimension (rod-like, linear) to two dimension, three dimension, and the friction between micelles becomes stronger and stronger, which is manifested by the increase of the viscosity of the aqueous surfactant solution.
Not only can the concentration change of the surfactant influence the micelle form and the viscosity thereof, but also inorganic salts, small molecular alcohols, high molecular polymers and the like can obviously change the aggregation form of the surfactant, thereby influencing the viscosity thereof. In general, for anionic surfactants, the presence of inorganic salts can compress the electric double layer of the micelle, forcing the micelle morphology to change from spherical to rod-like or even linear, resulting in an increase in the viscosity of the surfactant solution. While certain high molecular polymers, especially hydrophobically modified polymers, change the morphology of the strands of the gum, resulting in viscosity changes, as surfactants more readily form micelles centered on the hydrophobic block.
The amphiphilic polymer has hydrophobic segments of polyester and hydrophilic segments of polyether, and can cause a drastic change in viscosity upon addition of surfactant solution. When surfactant solution with a rod-like micelle structure is added, micelle rearrangement is induced to form spherical micelle with smaller structure, so that solution viscosity is obviously reduced. Hydrolysis of the soil release polymer, which results in a change in the amphiphilicity of the polymer, releases the surfactant which is accumulated, and the rod-like micelles are formed again. Thus, to characterize the stability of the polyester soil release polymer, the present invention employs a heat storage viscosity change rate, when the heat storage viscosity change rate of the liquid detergent composition is less than 20%, it is believed that the polyester soil release polymer does not undergo significant structural changes.
The method for testing the viscosity change rate comprises the following steps: samples were stored in a high temperature (45 ℃ ±1 ℃) incubator, after 4 weeks of storage, the viscosity values of the two samples at 25 ℃ ±0.1 ℃ were determined and calculated as follows:
thermal storage viscosity difference = high temperature storage sample viscosity-normal temperature storage sample viscosity;
heat storage viscosity change rate = heat storage viscosity difference/normal temperature storage sample viscosity.
In the examples below, all amounts are by weight unless otherwise indicated, and the amounts for the listed ingredients are the amounts of the active material converted.
In the examples, the following abbreviations will be used and have the indicated functions.
KOH: and (3) preparing fatty acid salt and alkaline agent by saponification of the neutralized fatty acid with potassium hydroxide.
NaOH: and (3) sodium hydroxide, neutralizing fatty acid and saponifying to prepare fatty acid salt and alkaline agent.
LAS: linear alkyl sodium sulfonate with 10-13 carbon atoms and anionic surfactant.
AES: ethoxylated fatty alcohol sulfate, fatty alcohol with 12-14 carbon atoms, average ethoxylation degree of 2 and anionic surfactant.
MES: fatty acid methyl ester sulfate, fatty acid C8-18, anionic surfactant.
AEO9: fatty alcohol polyoxyethylene ether, average degree of ethoxylation is 9, nonionic surfactant.
TO-7: and the average ethoxylation degree of the isomeric tridecanol polyoxyethylene ether is 7, and the nonionic surfactant.
XP-80: 2-propyl heptanol polyoxyethylene ether, the average degree of ethoxylation is 8, nonionic surfactant.
XL-80: 2-propylheptanol ethoxylated and propoxylated polyoxyethylene ether, average degree of ethoxylation of 8, nonionic surfactant.
LAB (LAB): lauramidopropyl betaine, zwitterionic surfactant.
MEE: fatty acid methyl ester ethoxylate, fatty acid carbon number is 6-24, average degree of ethoxylation is 0.5-30, nonionic surfactant.
PAA: : sodium salt of acrylic acid homopolymer, polycarboxylate. Acusol 445N, a product of Dow Chemical company.
EPEI: polyethyleneimine (mw=600), polyester soil release polymer with 20 ethoxylate groups per-NH.
HP22: polyethylene vinyl ester grafted polyethylene oxide copolymer, product of BASF company, brandHP22。
PG 101: polyethylene vinyl ester grafted polyethylene oxide copolymer, product of BASF company, brandPG101。
TH-20: polyester polyether polymer, trademark TEXCARE SRN-100, of Clariance;
protease: alkaline protease, product of Novozymes company under the trade name Savinase Ultra 16XL.
Preservative: methyl isothiazolinone and chloromethyl isothiazolinone mixtures.
Examples and comparative examples
The liquid detergent compositions of examples 1-5 and the liquid detergent compositions of comparative examples 1-5 herein were prepared according to the ingredients shown in Table 1, i.e., weight percentages.
TABLE 1 liquid detergent compositions A-J
Secondary quick detergency test
1. Pre-washing by a decontamination machine:
the polyester white cloth was cut into square cloth pieces (7×7 cm), and pre-washed with reference to a soil-release washing test method in national standard (determination of detergency and cycle washing performance of a detergent for GBT 131742008 clothing) under the following conditions:
1) Adopting a vertical decontamination machine, wherein each cylinder adopts 4 pieces of polyester white cloth dirt cloth;
2) The washing time is 20min, and the washing temperature is 30 DEG C
3) The washing concentration was 0.2%, i.e. 2g of detergent per jar, 1L of hard water;
4) After the washing is finished, the dirty cloth is fished out, the cloth of each cylinder is respectively put in a rinsing device for rinsing 1 time (1.5L of tap water is used for rinsing), and the cloth is thrown 15 times; dehydrating once, and throwing 15 times; placing the materials together in a 45-degree oven for drying, and naturally airing at room temperature for about 60 minutes or overnight;
2. preparation and aging of the sewage cloth:
1) Dripping oil stain on the pre-washed and dried white cloth, wherein the oil stain consumption is about 0.3g, which is equivalent to about 10 drops of a disposable straw; two parallel samples were made for each oil stain.
2) After oil stains are dripped, the dirty cloth is horizontally placed on a tray, and the dirty cloth is aged overnight.
3. Washing machine
The reference national standard (determination of detergency and cycle washing performance of a detergent for GBT 131742008 clothing) was made by the following method:
1) A vertical decontamination machine is adopted, and each cylinder adopts 2 pieces of dirt cloth; the washing time was 5min and the washing temperature was 30 ℃.
2) The washing concentration of the detergent compositions A-H was 0.2%, i.e. 2g of detergent was used per jar, 1L of hard water was used; the washing concentration of the detergent compositions I-P was 0.07%, i.e., 0.7g of detergent per jar, with 1L of hard water.
3) After the washing is finished, the dirty cloth is fished out, rinsed for 1 time respectively (1.5L of tap water is used for each), and thrown 15 times; dewatering once, and throwing 15 times. The whiteness of the cloth was tested with a WSD-3U fluorescent whiteness meter.
Secondary quick detergency= (whiteness after washing of detergent composition-whiteness after washing of reference sample)/whiteness after washing of reference sample
Storage appearance stability test
High temperature stability: after the composition is bottled and sealed, the composition is placed in an environment of 45+/-1 ℃ and kept at constant temperature for 4 weeks, the temperature is restored to the room temperature of 25+/-5 ℃, and the composition is not layered or precipitated, so that the high-temperature stability is qualified.
Low temperature stability: after the composition is bottled and sealed, the composition is placed in an environment of 0+/-2 ℃ and kept at constant temperature for 4 weeks, and then taken out for immediate observation. The composition has no delamination or precipitation, and is qualified in low-temperature stability.
Freeze thawing cycle stability: placing in the environment of-15 ℃ to-20 ℃ for 24 hours at constant temperature, taking out, placing in the environment of 25+/-5 ℃ for 24 hours at room temperature for one cycle, continuously circulating four times, and observing the state of the composition each time. The composition has no layering or precipitation, and is qualified in freeze-thawing cycle stability.
Stability at normal temperature: after the composition is bottled and sealed, the composition is placed in a room temperature environment (20 ℃ -30 ℃), and after the composition is placed for 4 weeks, the composition is not layered or precipitated, and the stability at normal temperature is qualified. The heat storage viscosity change rate was calculated as follows:
thermal storage viscosity change rate= (high temperature sample viscosity-low temperature sample viscosity)/low temperature sample viscosity
The viscosity measurement method comprises the following steps: LVDV-II+Pro type digital viscometer of Brookfield.
The test results are shown in Table 2.
TABLE 2 Secondary fast detergency, hot storage viscosity Change Rate and storage appearance stability of liquid detergent compositions A-J for washing polyester cloths
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The above table shows a detergent composition system with low surfactant content and high water content, the combined secondary quick detergency of the amphiphilic graft polymer HP22 and the fatty alcohol-polyoxyethylene ether XL-80 adopted in examples 1-5 is more than 35%, the heat storage viscosity change rate is less than 20%, and the storage stability is qualified. Comparative examples 1-3 are combinations of HP22 or XL-80 alone, and the results show that although stability is acceptable, detergency is inferior to example 1, demonstrating the synergistic effect of HP22 and the nonionic surfactant XL-80. Comparative examples 4 and 5 are detergent compositions with the addition of XL-80 and polyester soil release polymer TH-20 at levels of 0.5% and 2% and still less than 0.1% of the combination of HP22 and XL-80 with secondary quick detergency and poor heat storage stability.
The liquid detergent compositions of examples 6-9 and the liquid detergent compositions of comparative examples 6-9 herein were prepared according to the ingredients shown in Table 3, i.e., weight percentages.
TABLE 3 detergent compositions K-R
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The whiteness value, secondary quick detergency, heat storage viscosity change rate, storage appearance stability and the like of the washed polyester cloths of the detergent compositions I to R were tested, and the results are shown in table 4.
Table 4 whiteness value, secondary quick detergency, heat storage viscosity change rate and storage appearance stability of the washed polyester fabrics with the detergent compositions I to R
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The above table shows a detergent composition system with high surfactant content and low water content, and the combination of the amphiphilic graft polymer HP22 and the fatty alcohol-polyoxyethylene ether XP-80 used in examples 6-9 still shows more excellent detergency. And the change rate of the heat storage viscosity is less than 20%, and the storage stability is qualified. Comparative example 9 the combined soil release effect of the polyester polyether soil release polymers TH20 and XP-80 was far less than the detergent compositions of examples 6-9.
Liquid detergent compositions of examples 10-13 herein were prepared according to the ingredients shown in Table 5, i.e., weight percent.
TABLE 5 liquid detergent compositions S-Z
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The whiteness value, secondary quick detergency, heat storage viscosity change rate, storage appearance stability and the like of the washed polyester cloths of the detergent compositions S to Z were tested, and the results are shown in table 6.
TABLE 6 Secondary fast detergency, hot storage viscosity Change Rate and storage appearance stability of liquid detergent compositions s-Z washed polyester cloths
| Example 10 | Example 11 | Example 12 | Example 13 | |
| Composition and method for producing the same | S | T | w | v |
| Whiteness value | 56.3 | 56.78 | 57.22 | 57.63 |
| Viscosity mPas | 479.6 | 452.1 | 437.2 | 401.4 |
| Secondary quick detergency/% | 38.6 | 39.9 | 40.9 | 41.9 |
| Thermal storage viscosity change rate/% | 1.5 | 2.3 | 4.5 | 8.7 |
| High temperature stability | Qualified product | Qualified product | Qualified product | Qualified product |
| Low temperature stability | Qualified product | Qualified product | Qualified product | Qualified product |
| Freeze thawing cycle stability | Qualified product | Qualified product | Qualified product | Qualified product |
| Stability at ordinary temperature | Qualified product | Qualified product | Qualified product | Qualified product |
The above table shows a high pH detergent composition system, and in examples 10-13, the combined secondary quick detergency of the amphiphilic graft polymer PG101 and the fatty alcohol-polyoxyethylene ether TO-7 is more than 35%, the heat storage viscosity change rate is less than 20%, and the storage stability is qualified.
Embodiments of the present invention are illustrated in the following examples and comparative examples, which are illustrative of embodiments according to the present invention, although the present invention is not intended to be limited by these examples and comparative examples.
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Unless otherwise indicated, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40mm" is intended to mean "about 40mm".
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (4)
1. The liquid detergent composition containing the amphiphilic graft polymer is characterized by comprising 0.1-5% of the amphiphilic graft polymer and 1-10% of fatty alcohol polyoxyethylene ether by weight percent; the composition also comprises the following components: 0.1-70% of surfactant, 5-95% of water and a polyalcohol solvent; the surfactant is at least one selected from anionic surfactant, nonionic surfactant and zwitterionic surfactant;
the amphiphilic graft polymer is a graft copolymer of a polyethylene glycol graft substrate and an ethyl acetate side chain, and has the structural characteristics shown in a formula (I):
in the formula (I), n ranges from 50 to 55, and the weight average molecular weight Mw of the amphiphilic graft polymer ranges from 25000 to 30000; the amphiphilic graft polymer has a low degree of branching, having an average of no more than 1 grafting site per 50 alkylene oxide units, at least 0.05 grafting sites;
The fatty alcohol-polyoxyethylene ether has the structural characteristics shown in the formula (II):
in the formula (II), n is 8 to 18; x is 6 to 12; y is 0 to 20; the fatty alcohol in the fatty alcohol polyoxyethylene ether is an isomeric alcohol.
2. The liquid detergent composition according to claim 1, wherein the weight percentage of the surfactant is 20-60%.
3. The liquid detergent composition according to claim 2, further comprising 0.01-30% by weight of a co-additive; the viscosity of the liquid detergent composition is 200 mPa.s-5000 mPa.s at 25 ℃ and the pH is 7.5-10.
4. A liquid detergent composition according to claim 3, wherein the co-additive comprises one or more of an enzyme preparation, an alkaline agent, a preservative, a functional polymer, a chelating agent, an optical brightening agent and a perfume.
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