CN115975739A - Detergent composition and stable laundry beads for use therein - Google Patents
Detergent composition and stable laundry beads for use therein Download PDFInfo
- Publication number
- CN115975739A CN115975739A CN202211586451.9A CN202211586451A CN115975739A CN 115975739 A CN115975739 A CN 115975739A CN 202211586451 A CN202211586451 A CN 202211586451A CN 115975739 A CN115975739 A CN 115975739A
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- CN
- China
- Prior art keywords
- detergent composition
- fatty acid
- boiling point
- water
- point solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000203 mixture Substances 0.000 title claims abstract description 147
- 239000003599 detergent Substances 0.000 title claims abstract description 97
- 239000011324 bead Substances 0.000 title claims abstract description 79
- -1 fatty acid salt Chemical class 0.000 claims abstract description 73
- 239000002904 solvent Substances 0.000 claims abstract description 63
- 238000009835 boiling Methods 0.000 claims abstract description 50
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 46
- 239000000194 fatty acid Substances 0.000 claims abstract description 46
- 229930195729 fatty acid Natural products 0.000 claims abstract description 46
- 150000001412 amines Chemical class 0.000 claims abstract description 32
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 17
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- 125000000217 alkyl group Chemical group 0.000 claims description 36
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 35
- 239000000047 product Substances 0.000 claims description 30
- 150000002191 fatty alcohols Chemical class 0.000 claims description 19
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 18
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 17
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 13
- 229920001519 homopolymer Polymers 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 claims description 12
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 11
- 229920001577 copolymer Polymers 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- 230000003472 neutralizing effect Effects 0.000 claims description 11
- 150000004665 fatty acids Chemical class 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 8
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 7
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 7
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- 102000004190 Enzymes Human genes 0.000 claims description 6
- 108090000790 Enzymes Proteins 0.000 claims description 6
- 239000003242 anti bacterial agent Substances 0.000 claims description 6
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- 230000002335 preservative effect Effects 0.000 claims description 6
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 6
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 6
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 6
- 229960001124 trientine Drugs 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 5
- 229940077388 benzenesulfonate Drugs 0.000 claims description 5
- 239000000686 essence Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 4
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 2
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 34
- 230000008859 change Effects 0.000 abstract description 21
- 238000005406 washing Methods 0.000 abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 11
- 238000009833 condensation Methods 0.000 abstract description 8
- 230000005494 condensation Effects 0.000 abstract description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 7
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005202 decontamination Methods 0.000 abstract description 3
- 230000003588 decontaminative effect Effects 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 25
- 238000001556 precipitation Methods 0.000 description 20
- 230000032683 aging Effects 0.000 description 17
- 238000013112 stability test Methods 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 11
- 239000004744 fabric Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000654 additive Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000004615 ingredient Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000002845 discoloration Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000007046 ethoxylation reaction Methods 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- UYZVDMGEEIRMSK-UHFFFAOYSA-N 3-propylheptan-1-ol Chemical compound CCCCC(CCC)CCO UYZVDMGEEIRMSK-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 229940088598 enzyme Drugs 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 4
- 108091005804 Peptidases Proteins 0.000 description 4
- 239000004365 Protease Substances 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229920001903 high density polyethylene Polymers 0.000 description 4
- 239000004700 high-density polyethylene Substances 0.000 description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 4
- 239000002304 perfume Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
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- 150000001768 cations Chemical group 0.000 description 3
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- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 3
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- 235000013162 Cocos nucifera Nutrition 0.000 description 2
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- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
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- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 1
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Landscapes
- Detergent Compositions (AREA)
Abstract
The invention discloses a detergent composition and a stable washing coagulated bead applied by the detergent composition, and relates to the technical field of daily chemical industry. The detergent composition comprises the following components in percentage by weight: 11-30% of high boiling point solvent A, 3-10% of low boiling point solvent B, 2-10% of organic amine neutralizer, 0-8% of fatty acid salt, 0.1-1% of reducing agent, 15-30% of nonionic surfactant, 15-40% of anionic surfactant and the balance of water. The stable laundry beads are made from a water-soluble film encapsulating a detergent composition. According to the invention, through effective compounding of the organic solvent and the fatty acid salt, the problem of color change of the high-content sulfonate surfactant after the washing condensation bead is aged can be effectively improved, and the content of the polyoxyethylene ether sulfate is increased in the presence of a reducing agent, so that solid particles can not be separated out from the surface of the washing condensation bead, and the washing condensation bead has excellent storage stability and decontamination performance.
Description
Technical Field
The invention belongs to the field of daily chemical industry, and particularly relates to a liquid detergent composition containing an organic amine neutralizer and suitable for water-soluble film encapsulation, and a stable laundry bead applied to the liquid detergent composition.
Background
Along with the acceleration of people's rhythm of life, the design that the pearl is put in because of its super concentrated content and single accurate ration to the laundry, convenient to use, energy-concerving and environment-protective, is favored by consumer more and more, and the market share of the pearl is fixed a lot and is also continuously increased.
The laundry beads are made of a colorless and transparent water-soluble film encapsulating the contents, and consumers can perceive the appearance, smell and the like more directly than traditional bottled detergent products. The change in the appearance of laundry beads can lead to a poor sensory experience for the consumer, and maintaining the storage stability of the laundry beads over an extended shelf life has been a particular concern in the industry.
In conventional liquid cleaning products, water is typically the primary solvent. Therefore, the raw materials are selected mainly in consideration of solubility in water, dispersibility, and the like. For laundry beads, the low water content limits the use of many of the original conventional materials, the most typical of which is the neutralizing agent. In traditional liquid detergent formulations, the neutralizing agent used primarily is sodium hydroxide or potassium hydroxide. An ionic salt formed by neutralizing a common anionic surfactant has low solubility in a low-water-content system, and a finally prepared composition has poor stability and is easy to generate the problems of turbidity, precipitation and the like. Although this problem can be solved to some extent by replacing some or all of the anionic surfactant with nonionic surfactant, zwitterionic surfactant, etc., it is apparent that the improvement of the neutralizing agent to retain the anionic surfactant is more desirable in terms of maintaining the detergency and other properties of the detergent, and therefore the laundry beads usually use an organic base instead of an inorganic base.
However, the addition of organic amine can react with aldehydes in the detergent composition or polyethylene water-soluble film to cause the composition to discolor, especially in a system with high content of sulfonate surfactant, and the discoloration is more serious. At present, reducing agents are mainly added into the composition to slow down color change, but the reducing agents can generate sulfate after being oxidized, the sulfate can be precipitated from a water-soluble film and recrystallized on the outer surface of a washing condensation bead after being saturated, the appearance of a product is seriously affected, and therefore the use of polyoxyethylene ether sulfate surfactants in the composition is limited.
Patent US20210309948A discloses that the discoloration of a liquid detergent composition can be reduced by using a common reducing agent such as diallyl dimethyl ammonium chloride copolymer and sulfite, but still causes the problem of film-out deposition. Furthermore, the addition of the cationic polymer diallyldimethylammonium chloride copolymer results in a decrease in the solubility of the water-soluble film. Patent CN113980749A discloses a stable water-soluble film encapsulated liquid detergent composition, which also uses a nitrogen-containing compound in combination with a reducing agent such as sulfite, and although the overall stability of the detergent composition can be effectively improved, the introduced nitrogen-containing compound needs a sufficient amount of water to dissolve, and the cost of the composition is increased.
Disclosure of Invention
In order to solve the problems of the prior art, the present invention aims to provide a stable laundry bead, which is made by encapsulating a detergent composition with a water-soluble film, wherein the detergent composition can effectively improve the color change problem of the laundry bead with high content of sulfonate surfactant after aging through effective combination of an organic solvent and a fatty acid salt, and the increase of the content of polyoxyethylene ether sulfate in the presence of a reducing agent can not cause solid particles to be separated out from the surface of the laundry bead, so that the laundry bead has excellent storage stability and stain removal performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a detergent composition comprising the following components in percentage by weight: 11-30% of high boiling point solvent A, 3-10% of low boiling point solvent B, 2-10% of organic amine neutralizer, 0-8% of fatty acid salt, 0.1-1% of reducing agent, 15-30% of nonionic surfactant, 15-40% of anionic surfactant and the balance of water.
Further, the high boiling point solvent A is selected from one or more of glycerol, diethylene glycol, dipropylene glycol, polyethylene glycol and sorbitol. The high boiling point solvent A is present in the detergent composition in an amount of from 11 to 30% by weight, preferably from 14 to 25% by weight.
Further, the low-boiling point solvent B is selected from one or more of propylene glycol, ethylene glycol and dipropylene glycol methyl ether. The low boiling point solvent B is present in the detergent composition in an amount of 3 to 10% by weight, preferably 5 to 8% by weight.
Further, the organic amine neutralizer is one or more of ethanolamine, ethylenediamine and its coproducts and tetraalkylammonium hydroxide; the ethanolamine is selected from at least one of monoethanolamine, diethanolamine, triethanolamine and N-alkyl diethanolamine; the ethylene diamine and the co-product thereof are selected from at least one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
Preferably, the organic amine neutralizing agent is selected from one or more of monoethanolamine, diethanolamine, triethanolamine, and N-alkyl diethanolamine.
More preferably, the organic amine neutralizing agent is one or more selected from monoethanolamine and triethanolamine.
Further, the organic amine neutralizing agent is present in the liquid detergent composition in an amount of from 2 to 10% by weight. The organic amine neutralizing agent may adjust the pH of the composition to 7-8.
Further, the reducing agent is selected from one or more of thiosulfate, pyrosulfite, sulfite and bisulfite.
Preferably, the reducing agent is selected from one or a mixture of pyrosulfite, bisulfite and sodium sulfite.
Further, the content of the reducing agent in the liquid detergent composition is 0.1-1% by weight.
Further, the fatty acid salt is selected from one or more of C8-C18 fatty acid salt mixtures.
Preferably, the fatty acid salt is selected from the group consisting of oleate, laurate, cocoate, and mixtures of one or more of ethoxylated fatty alcohol ether carboxylates.
Further, the fatty acid salt is present in the liquid detergent composition in an amount of 0-8% by weight, preferably 2-6% by weight.
Further, the nonionic surfactant is selected from one or more of fatty alcohol alkoxylates, alkyl polyglycosides, fatty acid ester alkoxylates, fatty acid alkylolamides, fatty acid methyl ester ethoxylates and polyether surfactants.
Further, the content of the nonionic surfactant in the detergent composition is 15-30% by weight.
Further, the anionic surfactant is selected from one or more of alkyl benzene sulfonate of C6-C24, alkyl sulfate of C8-C18 and ethoxylated fatty alcohol sulfate of C8-C18; the alkyl benzene sulfonate is linear alkyl and branched alkyl, and may be saturated alkyl or alkyl with one or several unsaturated double bonds.
Preferably, the alkylbenzene sulfonate is dodecylbenzene sulfonate; the alkyl sulfate is dodecyl sulfate; the ethoxylated fatty alcohol sulfate is TexaponN70 from BASF.
Further, the anionic surfactant is present in the liquid detergent composition in an amount of from 10 to 40% by weight.
Further, the detergent composition also comprises 0-5% of other auxiliary agents; the other auxiliary agents are selected from at least one of chelating agent, enzyme preparation, preservative, polymer, inorganic salt, viscosity regulator, antibacterial agent, colorant, essence and pH regulator.
Further, the above detergent compositions can be encapsulated using a water-soluble film to make laundry beads.
A stable laundry bead comprising a water-soluble film and a detergent composition as described above; the water-soluble film encapsulates the detergent composition; the water-soluble film is one or a mixture of polyvinyl alcohol homopolymer and polyvinyl alcohol copolymer; the polyvinyl alcohol homopolymer is a hydrolysis product of a homopolymer of vinyl acetate; the polyvinyl alcohol copolymer is a hydrolysate of a copolymer of vinyl acetate and a second monomer, the second monomer is an acrylic monomer, and the second monomer accounts for 2 to 9 percent of the polyvinyl alcohol copolymer in mole percentage.
Further, the viscosity of the aqueous solution of the film with the mass percent of 4% is 10-25 centipoises.
The technical scheme described by the invention has the following beneficial effects:
1. the invention surprisingly discovers that the laundry beads prepared from the high-content sulfonate surfactant have stable color after aging, higher cost performance, better storage stability and better decontamination performance only by adding a single reducing agent.
2. The invention is characterized in that the washing coagulated beads prepared by the high-content sulfate surfactant through the effective combination of the organic solvent and the fatty acid salt have no precipitation outside the membrane after aging and have good storage stability.
Detailed Description
The features, benefits and advantages of the present invention will become apparent to those skilled in the art from a reading of the present disclosure.
All percentages, parts and ratios are based on the total weight of the composition of the present invention, unless otherwise specified. All weights as they pertain to listed ingredients are assigned to levels of active material and, therefore, do not include solvents or by-products that may be included in commercially available materials, unless otherwise specified. The term "percent by weight content" may be indicated herein by the symbol "%".
All molecular weights herein are weight average molecular weights expressed in daltons, unless otherwise indicated.
All formulations and tests herein occur in a 25 ℃ environment unless otherwise indicated.
The use of "including," "comprising," "containing," "having," or other variations thereof herein, is meant to encompass the non-exclusive inclusion, as such terms are not to be construed. The term "comprising" means that other steps and ingredients can be added that do not affect the end result. The term "comprising" also includes the terms "consisting of and" consisting essentially of "\82303030; and" comprising of "\8230". The compositions and methods/processes of the present invention comprise, consist of, and consist essentially of the essential elements and limitations described herein, as well as any of the additional or optional ingredients, components, steps, or limitations described herein. The term "free" as used herein means that the addition is not considered, and specifically means that the content is 0.01% by weight or less.
Washing condensing bead
The laundry beads comprise a water-soluble film that encapsulates a liquid composition in at least one compartment. The multi-compartment laundry beads can separate chemically incompatible ingredients or it may be desirable to release a portion of the ingredients earlier or later.
By laundry bead composition is meant a detergent composition in the liquid state. The composition can be encapsulated by a water-soluble film to form a laundry bead product, and the laundry bead product is diluted according to a certain proportion or directly contacted with a substrate (namely a fabric product, a hard surface and the like) to be contacted, so that stains on the surface of the substrate are removed, and the purpose of cleaning the surface of the substrate is achieved. The liquid laundry bead compositions typically also contain solvents, surfactant systems and other common detergency builders such as viscosity modifiers, enzyme preparations, perfumes and the like.
Water-soluble film
The water-soluble film is prepared from a water-soluble polymer prepared from monomers and then obtained by film-making equipment. The water-soluble polymer refers to one or a mixture of polyvinyl alcohol homopolymer and copolymer. The terms water-soluble film and water-soluble film are not distinguished in the present invention. The water-soluble film has a thickness of 65 microns to 90 microns.
The polyvinyl alcohol homopolymer is a hydrolysis product of a homopolymer of vinyl acetate and the polyvinyl alcohol copolymer is a hydrolysis product of a copolymer of vinyl acetate and a second monomer. The second monomer is one or more selected from acrylic acid, acrylate, methacrylic acid and methacrylate. The polyvinyl alcohol homopolymer or copolymer refers to a hydrolysis product of a homopolymer or copolymer of vinyl acetate, and the hydrolysis degree is 86-99%. The degree of hydrolysis was tested in section 2 of GB/T12010.2-2010 Plastic polyvinyl alcohol Material (PVAL): the determination of properties is described in detail, and the degree of hydrolysis is referred to as the degree of alcoholysis in this standard, and both meanings are consistent.
Method for preparing laundry beads
The laundry beads disclosed herein comprise at least one sealed chamber. Thus, the laundry beads may comprise a single cavity or multiple cavities. In embodiments comprising multiple cavities, each cavity can comprise the same and/or different compositions. In turn, the composition can take any suitable form, including but not limited to liquids, solids, and combinations thereof (e.g., solids suspended in a liquid). The cavities of the multi-cavity beads may have the same or different sizes and/or volumes.
The laundry beads of the present invention may be processed in three modes, vertical, horizontal and drum filling. Preferably, roller filling is adopted, the production efficiency is highest, and continuous production can be realized. Each row of rollers may contain a plurality of identically shaped mold cavities with the transition between the designed bottom interior wall and the side walls of the mold having a radius of curvature of 9.525 millimeters. The radius of curvature enables the die to impart rounded corners to the film package, forming a generally rectangular package shape and rounded transition to the bottom film surface. Holes are provided for the cavities along the bottom surface to draw a vacuum on the film and pull the film into the mold.
The bottom film is heated by a heating roller or infrared light before being vacuumized, so that the water-soluble film is softened and the next step of vacuumization is facilitated. The heating temperature is 60-90 ℃. The evacuation requires a negative pressure in the range of about 100 mbar to about 600 mbar, about 0.5 to about 1.5 seconds, to fully adhere the carrier film to the bottom surface of the mold.
The mask needs to pass through a wetting roller, the wetting agent can be water, a film composition or a plasticizer, and the control of the rotating speed of the wetting roller is very important and can influence the water covering amount and the sealing strength in the later period. And applying proper pressure in the sealing area to seal the upper film and the lower film to form a complete closed cavity. The film edges are then slit apart with a cutter to produce unit dose articles.
High boiling point solventA
The content of the high boiling point solvent A in the liquid detergent composition is 11-30% by weight, preferably 14-25% by weight.
The high boiling point solvent A is selected from one or more of glycerol, diethylene glycol, dipropylene glycol, polyethylene glycol and sorbitol. Suitable examples of the polyethylene glycol are PEG400.
The high-boiling-point solvent A is a solvent with the boiling point of more than or equal to 200 ℃ (101.3 kPa), and the solvent has low volatility in the bead product.
Low boiling point solventB
The content of the low-boiling point solvent B in the liquid detergent composition is 3-10% by weight, preferably 5-8% by weight.
The low-boiling-point solvent B is a solvent with the boiling point less than 200 ℃ (101.3 kPa). The low-boiling point solvent B is selected from one or a combination of more of propylene glycol, ethylene glycol and dipropylene glycol methyl ether.
The PVA film has certain permeability, and water, solvent, oxygen and the like easily penetrate through the film to influence the stability of contents. In the long-term storage process of the bead product, part of the solvent and water gradually volatilize, the composition proportion of the content is greatly changed, and after part of the solvent and water are lost, the content may have the phenomena of precipitation particles of sulfate and the like or gel layering and the like. The color yellowing of the coagulated beads is mainly caused by the oxidation of organic amine, oxygen easily penetrates through the film, and the oxidation of the organic amine is aggravated.
We have found that, surprisingly, controlling the organic solvents with different boiling points in a proper dosage range has a certain effect of alleviating the oxidation of organic amine and also has a good effect of inhibiting the precipitation of low-solubility sulfate and the like. Because the mechanism of relieving discoloration and improving the precipitation effect of particles on organic solvents with different boiling points is not clearly researched, the possible mechanism is presumed as follows: compared with the low-boiling-point solvent, the high-boiling-point solvent is less prone to volatilization through the PVA film in the long-term storage and aging process, and the organic amine is oxidized slowly in the specific high-boiling-point solvent and low-boiling-point solvent combination range, so that the color change is improved to a certain extent; and the high and low boiling point solvents within a specific dosage range have good binding capacity to free water, so that the free water in the contents is not easy to volatilize to a certain extent, and the granular substances of the sulfate with low solubility are not separated out or precipitated.
Organic amine neutralizer
The organic amine neutralizer of the invention has a weight percentage content of 2-10% in the liquid detergent composition.
The organic amine neutralizer is one or more of ethanolamine, ethylenediamine and its coproducts and tetraalkylammonium hydroxide. The ethanolamine is selected from at least one of monoethanolamine, diethanolamine, triethanolamine and N-alkyl diethanolamine; the ethylene diamine and the co-product thereof are selected from at least one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
Preferably, the organic amine neutralizing agent is selected from one or more mixtures of monoethanolamine, diethanolamine, triethanolamine or N-alkyl diethanolamine.
More preferably, the organic amine neutralizing agent is selected from one or more mixtures of monoethanolamine or triethanolamine.
Reducing agent
The reducing agent of the present invention is present in the liquid detergent composition in an amount of 0.1 to 1% by weight, preferably 0.2 to 0.6% by weight.
The reducing agent is selected from one or more of thiosulfate, pyrosulfite, sulfite and bisulfite. Preferably, the reducing agent is selected from one or more of pyrosulfite, bisulfite and sodium sulfite.
The cation part of the sulfite, thiosulfate, pyrosulfite and bisulfite is at least one of sodium ion, potassium ion, ammonium ion and ammonium ion formed by organic amine. In the ammonium ions formed by the organic amine, the organic amine is selected from one or more of ethanolamine, ethylenediamine and a coproduct thereof, and tetraalkylammonium hydroxide. The ethanolamine is selected from at least one of monoethanolamine, diethanolamine, triethanolamine and N-alkyl diethanolamine; the ethylene diamine and the co-product thereof are selected from at least one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
We have found that only mixtures of one or more of the above-mentioned sulfites, thiosulfates, pyrosulfites, bisulfites can impart enhanced stability properties to liquid detergent compositions. However, some sulfur-containing molecules other than those described in the present invention, such as dithionite and thiourea dioxide, cannot stabilize the liquid detergent composition, and may also adversely affect the odor.
Fatty acid salts
The fatty acid salts of the present invention are present in the liquid detergent composition in an amount of from 0 to 8% by weight, preferably from 2 to 6% by weight.
The fatty acid salt is selected from one or more of C8-C18 fatty acid salts. The alkyl chain segment may be a straight chain or branched chain, and may be a saturated alkyl group or an alkyl group containing one or more unsaturated double bonds. The fatty acid salt may be a single composition or a mixture of a plurality of fatty acid salts. Preferably, the fatty acid salt is selected from one or more of oleate, laurate, coconut oleate and ethoxylated fatty alcohol ether carboxylate. In the ethoxylated fatty alcohol ether carboxylate, the carbon number of the fatty alcohol is preferably 8 to 18, and the average degree of ethoxylation is preferably 2.0 to 10.
Anionic surfactants
The anionic surfactant of the present invention is present in the liquid detergent composition in an amount of from 15 to 40% by weight.
The anionic surfactant is selected from one or more of C6-C24 alkyl benzene sulfonate, C8-C18 alkyl sulfate, C8-C18 ethoxylated fatty alcohol sulfate and ethoxylated fatty alcohol ether carboxylate; the alkyl group may be a linear alkyl group and a branched alkyl group; the alkyl group may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds.
The cation part of the anionic surfactant is at least one selected from sodium ions, potassium ions, ammonium ions and ammonium ions formed by organic amine. Wherein in the ammonium ions formed by the organic amine, the organic amine is selected from one or more of ethanolamine, ethylenediamine and its coproduct, and tetraalkylammonium hydroxide. The ethanolamine is at least one selected from monoethanolamine, diethanolamine, triethanolamine and N-alkyl diethanolamine; the ethylene diamine and the co-product thereof are selected from at least one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
The alkyl benzene sulfonate has 6 to 24 carbon atoms in the alkyl group, and is selected from at least one of linear alkyl groups and branched alkyl groups; it may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds. In the technical scheme of the invention, the content of the alkylbenzene sulfonate is 10-28%. The alkylbenzene sulfonate content is calculated as the alkylbenzene sulfonate content.
The alkylbenzene sulfonate satisfies the following formula:
ra is C6-24 alkyl, M + Is a cationic moiety. A suitable example is dodecylbenzene sulfonate.
The ethoxylated fatty alcohol sulfate of the present invention is a derivative of an ethoxylate fatty alcohol having the following general formula:
R b is alkyl with 6-24 carbon atoms; x is 0.5-15; wherein M is + Is a cationic moiety. R is 1 The alkyl group may be a linear or branched alkyl group; it may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds. Preferably R b Is straight-chain alkyl with carbon number of 8-18. x represents an average degree of ethoxylation of from 0.5 to 15, preferably from 0.5 to 10, more preferably from 0.5 to 3. A suitable example is Texapon N70 from BASF.
The alkyl sulfate of the present invention may have a straight or branched alkyl chain segment, and may be a saturated alkyl group or an alkyl group having one or more unsaturated double bonds. The alkyl sulfate having 6 to 24 carbon atoms in the alkyl group is preferable, and the alkyl sulfate having 8 to 18 carbon atoms is more preferable. A suitable example is dodecyl sulfate.
In some embodiments, the alpha olefin sulfonate is included having the general formula:
a is 0-2, rc is C6-24 alkyl, preferably Rc is C8-18 alkyl.
The anionic surfactant mixture may also comprise one or more mixtures of alkyl disulfonates or derivatives thereof, preferably alkyl diphenyl oxide disulfonates, a suitable example being dodecyl diphenyl oxide disulfonate, dowfax series product from DOW. The composition also comprises sulfosuccinate, preferably fatty alcohol polyoxyethylene ether sulfosuccinic acid monoester disodium salt, the carbon number of the fatty alcohol is preferably 8-18, and the average ethoxylation degree is preferably 2.0.
Nonionic surfactant
The nonionic surfactant of the present invention is present in the liquid detergent composition in an amount of from 15 to 30% by weight.
The nonionic surfactant is selected from one or more of fatty alcohol alkoxylates, alkyl polyglycosides, fatty acid ester alkoxylates, fatty acid alkylolamides, fatty acid methyl ester ethoxylates and polyether surfactants.
The fatty alcohol alkoxylates have the general formula:
wherein n is 6-24; x is 0.5-30 and y is 0-10.
n is 6 to 24; x is 0.5 to 30 and 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 an alkaline catalyst, and is basically a mixture. The fatty alcohol includes a straight chain alcohol or a branched chain isomeric alcohol. Alkoxy groups include ethoxy and propoxy groups. The fatty alcohol is preferably a fatty alcohol having a carbon number of 8-18, and the preferred alcohols include, but are not limited to, one of hexanol, octanol, decanol, 2-ethylhexanol, 3-propylheptanol, lauryl alcohol, isodecanol, tridecanol, tetradecanol, hexadecanol, palmitolein, 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. Suitable examples are: fatty alcohol polyoxyethylene ether (9), i.e., AEO9; NEODOL series linear fatty alcohol ethoxylate products from SHELL corporation; the DOW company ECOSURF EH series ethoxylated and propoxylated 2-ethyl hexanol products; the products of the BASF company Lutensol XL series of ethoxylated and propoxylated 3-propylheptanols; the BASF company Lutensol XP series ethoxylated 3-propyl heptanol products, and the like.
The alkyl polyglycoside has the following general formula:
wherein n is 6 to 24 and p is 1.1 to 3.n is preferably from 8 to 16. Suitable alkyl glycosides are, for example, those of the G1ucopon series available from BASF.
The fatty acid ester alkoxylate is one or more selected from ethoxylated C8-C18 fatty acid esters with an average degree of ethoxylation of 2-10. May contain an ethoxylated alkyl sorbitan ester having an alkyl carbon number of 6 to 18 and an average degree of ethoxylation of 4 to 20; a suitable example is the Corda Tween series of products.
The fatty acid alkylolamide has fatty acid with carbon number of 6-24, and can be linear fatty acid, branched fatty acid, saturated fatty acid or unsaturated fatty acid; the number of alkyl alcohols is 0-2. Preferred are monoethanolamide, diethanolamide, isopropanolamide of fatty acid having a carbon number of 8-18, and suitable examples are coconut diethanolamide.
The fatty acid methyl ester ethoxylate has the following general formula:
wherein n is 6-24; x is 0.5-30. Preferably, n is 8 to 18 and x is 2 to 20. More preferably x is 4 to 10. A suitable example is the LION company MEE product.
The polyether surfactant is a block polymer having surface activity, and is a nonionic surfactant obtained by addition polymerization of ethylene oxide or propylene oxide with an initiator, and suitable examples thereof are those of Pluronic series produced by BASF corporation.
Other auxiliaries
Other auxiliary agents involved in the invention comprise one or more of enzyme preparation, acid-base modifier, essence, preservative, antibacterial agent, polymer and chelating agent.
Enzyme preparation
One or more enzyme preparations may be included in the detergent compositions of the present invention to enhance the soil release properties of the product as well as to provide other benefits to fabric care. The enzyme preparation is at least one selected from protease, alpha-amylase, cellulase, hemicellulase, phospholipase, esterase, lipase, peroxidase/oxidase, pectinase, lyase, mannanase, cutinase, reductase, xylanase, pullulanase, tannase, pentosanase, maltose, arabinase and beta-glucanase, and is preferably protease. Suitable proteases include, but are not limited to, savinase16L, savinase Ultra16XL, savinase event 16L, progress Uno 101L, progress Uno 100L from Novin, effect P150 from DuPont, preferenzP200, preferenzP300, lavergy 104L, 104LS from Bass. The content of the enzyme preparation is 0.001% -5%, preferably 0.01% -2% of the total weight of the detergent composition.
Acid-base regulator
The pH regulator comprises an acidity regulator and an alkalinity regulator. Wherein, the acidity regulator is selected from organic acid, inorganic acid and strong acid and weak base salt which are well known in the daily chemical product industry, preferably citric acid, succinic acid and boric acid, and more preferably citric acid. Alkalinity regulators, i.e., organic amines. The organic amine is at least one of ethanolamine, ethylenediamine and its coproduct, and tetraalkylammonium hydroxide. The ethanolamine is at least one selected from monoethanolamine, diethanolamine, triethanolamine and N-alkyl diethanolamine; the ethylenediamine and its coproduct are selected from at least one of diethylenetriamine, triethylenetetramine and tetraethylenepentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
Essence
The detergent compositions to which the present invention relates may contain perfume, which perfume comprises all perfume ingredients suitable for use in laundry products.
Preservative agent
The detergent compositions according to the invention may contain a preservative to provide preservative properties to the liquid formulation, the preservative being present in an amount of from 10ppm to 500ppm and being selected from the group consisting of 1, 2-benzisothiazolin-3-one, 2-methylisothiazolin-3-one, 5-chloro-2-methylisothiazolin-3-one, phenoxyethanol, DMDMH, and mixtures thereof.
Antibacterial agent
The detergent compositions of the present invention may further comprise an anti-bacterial agent. The antibacterial agent is at least one selected from hypochlorous acid and salts thereof, parachloro-m-xylenol, parachloro-m-cresol, hydroxy-dichloro-diphenyl ether, hydroxy-trichloro-diphenyl ether, triclocarban, o-phenylphenol, dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, didecyl dimethyl ammonium chloride, polyhexamethylene biguanide hydrochloride, 1-hexadecyl pyridinium chloride, zinc pyrithione and pyridone ethanolamine salt.
Polymer and method of making same
The polymer of the invention comprises: salts of homopolymers of acrylic acid; salts of copolymers of acrylic acid; cellulose derivatives such as carboxymethyl cellulose, ethyl hydroxyethyl cellulose, methyl cellulose; homopolymers and copolymers of vinylpyrrolidone, such as copolymers of linear polyvinylpyrrolidone, N-vinylpyrrolidone and vinyl acetate; polyethyleneimine derivatives, for example ethoxylated polyethyleneimine, polyethylene terephthalate and derivatives thereof, polyethylene glycol and derivatives thereof. The polymers impart soil redeposition resistance to the detergent composition and/or promote soil release from the surface of the substrate and/or enhance the appearance of the detergent composition.
Chelating agents
The chelating agent is selected from one or more of citrate, glutamic acid diacetate, methyl glycine diacetate, ethylene diamine tetraacetic acid salt, cyclohexanediamine tetraacetate, ethylene glycol diethyl ether diamine tetraacetate, ethylene diamine tetrapropionate, diethylene triamine pentaacetate, triethylene tetramine hexaacetate and 2-hydroxyethyl ethylene diamine triacetate. The cation of the salt of the chelating agent may be selected from sodium ions, lithium ions, ammonium ions formed from organic amines.
In addition to the above ingredients, the detergent compositions of the present invention may contain various conventional and customary additives such as cosolvents, solubilizers, structurants, foaming agents, defoamers, fabric softeners, bleaching systems, anti-wrinkle agents, and the like. These additives and the associated methods of use are well known to those skilled in the art, and the particular type and amount of such additives can be selected and adjusted to the particular needs.
Process for preparing detergent composition
The laundry bead compositions of the present invention are prepared by various methods well known to those skilled in the art. The preparation of the compositions can be carried out by conventional means, with suitable processing temperatures and processing times being selected with regard to the state and action 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. The examples are therefore to be understood as merely illustrative of the invention in more detail and not as limiting the content of the invention in any way.
A process for making a detergent composition comprising the steps of:
1) Mixing water, a high boiling point solvent A, a low boiling point solvent B and an organic amine neutralizer;
2) Adding an anionic surfactant, mixing until the solution is clear, and cooling by using chilled water;
3) When the temperature is reduced to 40-50 ℃, adding the nonionic surfactant, and mixing until the mixture is completely dissolved;
4) Adjusting the pH value to 7-8;
6) Adding other auxiliary agents, and stirring until the auxiliary agents are completely dissolved;
7) Adding the rest of deionized water, and uniformly stirring.
Storage stability of detergent compositions
High-temperature stability: after the composition is bottled and sealed, the composition is placed in an environment with the temperature of 45 +/-1 ℃, is kept at the constant temperature for 4 weeks, and then is restored to the room temperature of 25 +/-5 ℃, the composition does not have layering or precipitation, and the high-temperature stability is qualified.
Low-temperature stability: the composition is bottled, sealed, placed in an environment of 0 +/-2 ℃, placed at constant temperature for 4 weeks, taken out and immediately observed. The composition has no demixing or precipitation separation, and is qualified in low-temperature stability.
Freeze-thaw cycle stability: placing the mixture in an environment with the temperature of between 15 ℃ below zero and 20 ℃ below zero, taking out the mixture after placing the mixture for 24 hours at constant temperature, and placing the mixture in an environment with the temperature of 25 +/-5 ℃ at room temperature for 24 hours, wherein the circulation is once and four times continuously, and the state of the composition is observed every time. The composition has no demixing or precipitation separation, and is qualified in freeze-thaw cycle stability.
And (3) normal temperature stability: after the composition is bottled and sealed, the composition is placed in a room temperature environment (20-30 ℃) for 4 weeks, no layering or precipitation is generated on the composition, and the stability at normal temperature is qualified.
Storage stability of laundry beads
High-temperature precipitation stability: the washing coagulated beads are placed in a constant-temperature air-blast oven environment at 45 +/-1 ℃ for 2 weeks with no particles or powder precipitation and no leakage outside the film, and the stability is qualified when the particles are precipitated at high temperature.
High temperature and high humidity stability: the laundry beads were sealed in a high density polyethylene (HDEP) bag and stored at 45 + -1 deg.C and 70% -80% relative humidity for 8 weeks. And then taking out the membrane from the constant temperature and humidity box to test the color change, the precipitation outside the membrane and the dissolution performance.
Laundry bead color change test and color change rate rating assessment
The outer membrane of the washing condensation bead is cut, the content is taken out, the color change of the content before and after high-temperature and high-humidity treatment is tested by a color difference meter, and the color change rate (Y) of the content is calculated according to the following formula (1).
Y = Db2-Db1 (1), Y: a rate of change of color of the contents;
db1: db value (yellow-blue color value) of the liquid detergent composition of unit dose before high-temperature and high-humidity aging treatment;
db2: db value (yellow-blue value) of the liquid detergent composition of unit dose after high-temperature and high-humidity aging treatment;
and (3) high-temperature high-humidity aging treatment: the laundry beads were sealed in a high density polyethylene (HDEP) bag and stored at 45 + -1 deg.C and 70% -80% relative humidity for 8 weeks.
TABLE 1 color Change rating of coagulated bead Contents after high temperature and humidity aging treatment
Test of the solubility of laundry beads
The solubility of the laundry beads according to the invention is the dissolution in 1 litre of water. 1 washing beads are placed in a beaker, and the beads are stirred and dissolved in the beaker for a period of time, and then the stirring is stopped. All the solution and the residue in the beaker were immediately filtered through a 60 mesh screen and the dissolution performance was rated according to the residue on the screen within 1 minute.
In the present invention, the time during which the beads are stirred and dissolved in the beaker is referred to as the dissolution time. For beads that were not aged, the dissolution time was 5 minutes. For pouches subjected to aging treatment, the dissolution time was 10 minutes.
The dissolution performance rating is shown in table 4. Dissolution performance was determined visually, with a rating of 1 representing complete dissolution and a rating of 4 representing no dissolution.
TABLE 2 evaluation of dissolution Properties
Detergency testing method
Detergency in the present invention refers to the ability of a fabric detergent composition to remove various stains. The test was carried out according to the method of the national standard GB/T13174-2008. Three dirty cloths, namely carbon black, protein and sebum, are adopted, and a WSD-3U fluorescence whiteness meter is used for measuring the whiteness W1 of the three dirty cloths before washing. Hard water with the hardness of 250ppm is prepared according to the GB/T13174-2008 standard, and one-time washing is completed by adopting an RHLQ type vertical decontamination machine, wherein the addition amount of a detergent is 2g/L in a common type, and the concentration type is 0.7g/L. Washing time is 20min, washing temperature is 30 ℃, stirring speed is 120r/min, washed dirty cloth is rinsed and dried, whiteness W2 of washed cloth pieces is tested by a whiteness meter, and a whiteness difference delta W calculation method is as the following formula (2):
Δ W = W2-W1 (2), where W2 is the post-wash whiteness and W1 is the pre-wash whiteness.
And (3) comparing the detergency of the sample detergent with that of the national standard detergent to obtain a P value, wherein the formula is as follows:
p = [ Delta ] W sample/[ Delta ] W standard (3), wherein the [ Delta ] W sample is the whiteness difference of the dirty cloth before and after cleaning by the sample detergent, and the [ Delta ] W standard is the whiteness difference of the dirty cloth before and after cleaning by the national standard detergent.
Evaluation criteria for detergency
A P value < 1 indicates that the detergent composition has a lower detergency than the control, and a P value > 1 indicates that the detergent composition has a higher detergency than the control. The larger the P value, the stronger the detergency of the detergent composition. When the P value is more than or equal to 1.10, the detergent composition has good washing and stain removal performance.
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. The examples are therefore to be understood as merely illustrative of the invention in more detail and not as limiting the content of the invention in any way.
In the following examples, all amounts are by weight unless otherwise indicated, and the amounts of the listed ingredients are converted to active material amounts.
In the following examples, the following components were used.
Glycerol, belonging to the class of high-boiling solvents a.
Polyethylene glycol 400, belonging to the class of high boiling point solvents a.
Dipropylene glycol, belonging to the class of high boiling solvents a.
Propylene glycol, belonging to the class of low boiling solvents B.
Ethylene glycol, belonging to the class of low boiling solvents B.
Sodium metabisulfite, belonging to the class of reducing agents.
Sodium bisulfite, a reducing agent.
Sodium sulfite, belonging to the class of reducing agents.
Linear alkyl benzene sulphonic acid, abbreviated as LAH, belongs to the class of anionic surfactant precursors.
Ethoxylated fatty alcohol sulfates, AES for short, belong to the class of anionic surfactants.
Dodecanoic acid, belonging to the class of fatty acid salt precursors.
Myristic acid, belonging to the class of fatty acid salt precursors.
Oleic acid, belonging to the class of fatty acid salt precursors.
Fatty alcohol polyoxyethylene ether (9), AEO9 for short, belongs to the class of nonionic surfactants and fatty alcohol alkoxylates. Ethoxylated and propoxylated 3-propylheptanol, called Lutensol XL for short, belongs to the class of nonionic surfactants, fatty alcohol alkoxylates.
Ethoxylated 3-propylheptanol, called Lutensol XP for short, belongs to the class of nonionic surfactants, fatty alcohol alkoxylates.
Monoethanolamine belongs to the category of organic amine neutralizer.
Triethanolamine, belonging to the category of organic amine neutralizers.
Deionized water, which belongs to the category of solvents.
Sodium citrate belongs to the category of other auxiliary agents.
Protease: the category of the additive is other additives.
Essence: the category of the additive is other additives.
Pigment: the category of the additive is other additives.
Examples and comparative examples
The following examples are illustrative and comparative of the present invention and are not intended to limit the present invention.
The respective components of examples 1 to 6 and comparative examples 1 to 20 were prepared into detergent compositions according to the above-mentioned preparation methods of detergent compositions by weight percent, the detergent compositions were coated into laundry beads according to the preparation methods of laundry beads, and the detergent compositions and the laundry beads were respectively subjected to storage stability tests according to the methods described above. Tables 3, 5 and 7 show the contents of the components in the detergent compositions of examples 1 to 6 and comparative examples 1 to 20 in percentage by weight. Tables 4, 5 and 6 show the results of the storage stability tests of the detergent compositions and the laundry beads prepared in examples 1 to 6 and comparative examples 1 to 20.
TABLE 3 compositions of detergent compositions A-J
TABLE 4 storage stability of detergent compositions A-J and laundry beads
From the above-mentioned results of stability tests in tables 3 to 4, in examples 1,2, 5 and 6, respectively, and comparative examples 1 to 4, it was found that when the content of the fatty acid salt is in the range described in the technical solution of the present invention, but the content of the organic solvent is not in the range described in the technical solution of the present invention, for example, the high boiling point solvent a is lower than the value in the technical solution of the present invention, and the low boiling point solvent B is used in an amount higher than the value in the technical solution of the present invention (comparative examples 1 to 4), although the storage stability of the detergent compositions G to J is acceptable, the corresponding laundry beads show the phenomenon of particulate matter precipitation at high temperatures, that is, the stability of precipitation at high temperatures is not acceptable. Meanwhile, the color change rate grade of the content after high-temperature high-humidity aging is obviously poor, particularly for the composition G-I with high sulfonic acid content (more than 20%), the color change rate Db value of the content of the condensed beads is more than 15, the phenomenon of serious discoloration occurs, and the composition cannot pass the high-temperature high-humidity stability test. And the results of comparative example 2 and comparative example 3 show that, in the case of cleaning compositions H and I having a high AES content, the sulfate in AES is further caused to precipitate out of the film as particles, and the stability at high temperature and high humidity cannot be passed.
TABLE 5 compositions of detergent compositions K to Q
TABLE 6 storage stability of detergent compositions K-Q and laundry beads
In comparison with example 5, although the content of the fatty acid salt of the washing composition of comparative example 5 is within the range of the present invention, the content of the high boiling point solvent A is out of the range of the present invention, and the content of the low boiling point solvent B is lower than the range of the present invention, the low temperature and freeze-thaw cycle stability thereof shows a delamination phenomenon, the storage stability of the detergent composition is not satisfactory, and also the color change rate of the content is deteriorated, the content leakage phenomenon out of the coagulated bead film and the film insolubilization phenomenon, i.e., the high temperature and high humidity stability cannot be passed after the aging at high temperature and high humidity are occurred.
In comparison with example 5, comparative example 6, in which the content of the fatty acid salt is within the range of the present invention, but the content of the high boiling point solvent a is out of the range of the present invention, and the content of the low boiling point solvent B is higher than the range of the present invention, although the storage stability of the detergent composition and the high temperature precipitation stability of the laundry beading can be passed, the high temperature stability of the beading cannot be passed, and the deterioration of the color change rate of the content and the insolubilization of the film also occur.
The results of comparative example 7, compared to example 1, show that when the contents of both the high boiling point solvent a and the low boiling point solvent B are below the ranges of the present invention, storage stability by the detergent composition and storage stability of the laundry beads are not achieved even if the content of the fatty acid salt is within the ranges of the present invention.
The results of the above analyses of comparative examples 1 to 7 show that: when the content of the fatty acid salt is within the range of the present invention and the amounts of the high boiling point solvent a and the low boiling point solvent B are out of the range of the technical solution of the present invention, the storage stability of the detergent composition and the storage stability of the laundry beads are adversely affected to various degrees, respectively.
Comparative examples 8 and 9 were compared with examples 1 and 5, respectively, and it was found that the fatty acid salt and the low boiling point solvent B were within the range of the present invention, but when the high boiling point solvent a was higher or lower than the range, the storage stability test of the detergent composition was passed, but the storage stability test of the laundry beads was not passed, and the color change rate Db after the high temperature and high humidity aging of the contents was significantly increased, and the discoloration was more serious. When the high boiling point solvent a is less than the range value, a phenomenon of particle precipitation at high temperature is caused, and when it is more than the range value, a phenomenon of precipitation outside the film and remarkable deterioration of film solubility is caused.
Whereas comparative analysis of the results of stability tests according to comparative examples 10 to 11 and examples 2 and 5 showed that both the fatty acid salt and the high boiling point solvent A were within the range of the present invention, and that when the low boiling point solvent B was below the value of the range (comparative example 10), neither the storage stability of the detergent composition nor the storage stability of the laundry beads passed; when the low boiling point solvent is higher than the value of the range (comparative example 11), although the storage stability of the detergent composition can be passed, it also causes bad results of off-specification discoloration and poor water solubility of the film after high temperature and high humidity aging of the laundry beads.
TABLE 7 compositions of detergent compositions R to Z
TABLE 8 storage stability of detergent compositions R-Z and laundry beads
The stability test results of comparative examples 12 to 14 show that when the high boiling point solvent a and the low boiling point solvent B are both within the range of the present invention and the amount of the fatty acid salt is out of the range, the color change rate Db of the content after the high temperature and high humidity aging of the laundry beads is significantly increased compared to examples 6, 1 and 5, respectively, and the discoloration is severe, i.e., the high temperature and high humidity stability test cannot be passed. Particularly, in comparative example 12 having a high sulfonic acid content and a high AES content, the precipitation of particulate matter outside the membrane was also caused during aging at high temperature and high humidity, as compared with example 6, and the low temperature stability test of the detergent composition failed.
The above comparative examples illustrate that: the amount of the fatty acid salt has a non-negligible effect on the storage stability of the detergent composition and the storage stability of the laundry beads, and the storage stability of the laundry beads at high temperature and high humidity can be improved only by controlling the amount within the technical scheme of the present invention.
The stability results of comparative examples 15-17 compared to examples 1, 4, and 5 demonstrate that the storage stability of the detergent composition and the storage stability of the laundry beads failed when any of the high boiling point solvent a, the low boiling point solvent B, and the fatty acid salt were outside the scope of the protocol of the present invention.
The comparison of the stability performance results of the above examples and comparative examples shows that the organic solvent and fatty acid salt of the present invention can effectively improve the storage stability of detergent compositions and laundry beads by compounding in a specific dosage range; particularly, the problem of color change of the washing condensation beads of the high-content sulfonate surfactant after aging can be effectively solved; and the content of polyoxyethylene ether sulfate in the washing condensation bead can be increased without causing solid particles to be separated out from the surface of the washing condensation bead.
The stability test result of comparative example 18, compared to example 6, shows that the content color change rate Db without the reducing agent is 23.4, and the content color change rate is poor in grade, which is not favorable for high temperature and high temperature stability. The results of the stability tests of comparative examples 19 to 20 show that, when the reducing agent according to the invention is not used, but sodium dithionite and thiourea dioxide are used in equal weight percentages, they lead to a strong pungent odor of the contents, while thiourea dioxide also leads to the precipitation of particles and the storage stability is not passed.
The stability performance results of the above comparative examples illustrate that: a single reducing agent can stabilize the color of laundry beads prepared from high levels of sulfonate surfactants after aging, increasing the level of polyoxyethylene ether sulfate in the presence of the reducing agent of the present invention does not result in the precipitation of solid particles on the surface of the laundry beads, and does not impart enhanced stability to liquid detergent compositions and laundry beads when the reducing agent of the present invention is not employed.
(2) Detergency test
The above examples 1-6 were tested as described according to the foregoing detergency test method and the results are shown in Table 9.
Table 9 detergency test results of examples 1 to 6
| Sample numbering | P value of carbon black stained cloth | P value of protein stain cloth | P value of sebum stain cloth |
| Example 1 | 1.10 | 2.42 | 1.29 |
| Practice ofExample 2 | 1.13 | 3.61 | 1.16 |
| Example 3 | 1.15 | 3.06 | 1.26 |
| Example 4 | 1.18 | 3.54 | 1.39 |
| Example 5 | 1.16 | 3.47 | 1.35 |
| Example 6 | 1.13 | 3.58 | 1.27 |
As can be seen from the comparison of the results of the detergency tests in table 9, examples 1 to 6 provided by the present invention have good detergency performance in washing, in addition to the long-term storage stability, and all pass the detergency test.
The technical contents of the present invention are further illustrated by the examples, so as to facilitate the reader to understand more easily, but the embodiments of the present invention are not limited thereto, and any technical extension or re-creation made by the present invention is protected by the present invention.
Claims (10)
1. A detergent composition, characterized by comprising the following components in percentage by weight: 11-30% of high boiling point solvent A, 3-10% of low boiling point solvent B, 2-10% of organic amine neutralizer, 0-8% of fatty acid salt, 0.1-1% of reducing agent, 15-30% of nonionic surfactant, 15-40% of anionic surfactant and the balance of water; the high boiling point solvent A is one or a combination of glycerol, dipropylene glycol, polyethylene glycol and sorbitol; the low-boiling point solvent B is one or a combination of propylene glycol, ethylene glycol and dipropylene glycol methyl ether.
2. The detergent composition as claimed in claim 1, wherein the fatty acid salt is selected from one or more of C8-C18 fatty acid salts.
3. A detergent composition as claimed in claim 1, wherein said organic amine neutralizing agent is selected from one or more of the group consisting of ethanolamine, ethylenediamine and its co-products, and tetraalkylammonium hydroxide.
4. A detergent composition according to claim 3, wherein said ethanolamine is selected from at least one of monoethanolamine, diethanolamine, triethanolamine, N-alkyl diethanolamine; the ethylene diamine and the co-product thereof are selected from at least one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the tetraalkylammonium hydroxide is at least one selected from the group consisting of tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
5. A detergent composition according to claim 1, wherein said reducing agent is selected from the group consisting of one or more of thiosulfate, metabisulfite, sulfite and bisulfite.
6. The detergent composition according to claim 1, wherein the nonionic surfactant is selected from the group consisting of one or more of fatty alcohol alkoxylates, alkyl polyglycosides, fatty acid ester alkoxylates, fatty acid alkylolamides, fatty acid methyl ester ethoxylates, and polyether surfactants.
7. The detergent composition as claimed in claim 1, wherein the anionic surfactant is selected from one or more of alkyl benzene sulfonate of C6-C24, alkyl sulfate of C8-C18, and ethoxylated fatty alcohol sulfate of C8-C18.
8. A detergent composition according to claim 1, further comprising 0-5% of other adjunct agents; the other auxiliary agents are selected from at least one of chelating agent, enzyme preparation, preservative, polymer, inorganic salt, viscosity regulator, antibacterial agent, colorant, essence and pH regulator.
9. A stable laundry bead comprising a water-soluble film and a detergent composition according to any of claims 1-8; the water-soluble film encapsulates the detergent composition; the water-soluble film is one or a mixture of polyvinyl alcohol homopolymer and polyvinyl alcohol copolymer; the polyvinyl alcohol homopolymer is a hydrolysis product of a homopolymer of vinyl acetate; the polyvinyl alcohol copolymer is a hydrolysate of a copolymer of vinyl acetate and a second monomer, the second monomer is an acrylic monomer, and the second monomer accounts for 2 to 9 mole percent of the polyvinyl alcohol copolymer.
10. The stable laundry bead set forth in claim 9 wherein said water-soluble film is present in an amount of about 4% by weight; the viscosity of the aqueous solution is 10-25 centipoises.
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