CN105754752A - Method for giving gel property to detergent composition and high water content gel-type detergent composition - Google Patents
Method for giving gel property to detergent composition and high water content gel-type detergent composition Download PDFInfo
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- CN105754752A CN105754752A CN201610223840.3A CN201610223840A CN105754752A CN 105754752 A CN105754752 A CN 105754752A CN 201610223840 A CN201610223840 A CN 201610223840A CN 105754752 A CN105754752 A CN 105754752A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/43—Solvents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
- C11D1/10—Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/143—Sulfonic acid esters
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
- C11D1/721—End blocked ethers
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/90—Betaines
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
Abstract
The invention discloses a method for giving gel property to a detergent composition and a high water content gel-type detergent composition. The method contains 5-25% of amphoteric surfactant, wherein the amphoteric surfactant satisfies the following conditions: 1) the amphoteric surfactant is mixture of two or three selected from an amino acid type amphoteric surfactant, a betaine type surfactant and an imidazoline-type surfactant; 2) the amphoteric surfactant at least contains one amino acid type amphoteric surfactant. The method adopts a special amphoteric surfactant, so that the detergent composition has gel property and rapid dissolving property at the same time. The detergent composition does not adopt other gel-forming materials and only adopts the surfactant to form a gel structure.
Description
Technical field
The invention belongs to daily chemical products technical field, particularly to a kind of high water content composition of detergent being provided simultaneously with gel characteristic and rapid solution characteristic.
Background technology
The applied research of amino acid type surfactant starts from 19 century 70s, is mainly used in medicine and cosmetics anticorrosion, has good antiviral property.In recent years, amino acid type surfactant receives the concern of more and more Research Team because of its premium properties, and its application also expands further.Amino acid type surfactant can simply be divided into two classes by the difference of structure: 1) forms by being connected with each other by amido bond between fats a-amino acid；2) it is connected by alpha-amido, α-carboxyl or branched group by natural alpha-amino acid and long aliphatic chain and forms.That mainly study both at home and abroad at present and apply is the latter, and wherein, N-acyl group, O-acyl group, N-amino compounds and esters thereof are subject to the extensive attention of detergents and cosmetic industry because it has hypotoxicity and high biodegradability.
In daily use chemicals industry, the detergent for different purposes generally has different viscosity requirement.In general, house detergent is liquid detergent, liquid detergent, bath gel etc. such as, and its viscosity can between 200mPa s to 10000mPa s.Viscosity on the one hand meets actually used needs, as being easy to smear, wiping etc., also meets the affection need of consumer on the other hand.The detergent of gel state then can meet other function needs, as carried the detergent packaging etc. being not easy to trickle down because of collision, be easy to make unit dose in way.
At present, all big enterprises are mainly through adding various macromolecule thickener to form gel, such as Polyethylene Glycol, polysaccharide etc..Although macromolecule can solve gel problems, but product can be made to increase other defect, during such as low temperature, gel occurs；Easily there is metachromatism in high temperature；The foam characteristic of surfactant is suppressed；During cleaning, skinfeel is by polymeric impact, show sticky, cleaning dirty, residual sense is strong；High molecular high price ties up formulation cost space；Formed gel poorly water-soluble.Make a general survey of domestic and international open source literature, a kind of composition of detergent with gel characteristic, shear shinning characteristic and rapid solution characteristic does not still occur.
Summary of the invention
In order to overcome the shortcoming using macromolecule thickener to form gel, strengthen the water solublity of gel simultaneously, it is made to be applied to better in detergent, the invention provides a kind of method giving composition of detergent gel characteristic and its relevant high water content gel-type composition of detergent, the present inventor is surprisingly, give composition of detergent gel characteristic by composite realization of amphoteric surfactant, and this composition of detergent is also equipped with rapid solution characteristic.
The present invention adopts the following technical scheme that and realizes.
The present invention relates to a kind of composition of detergent with gel characteristic, shear shinning characteristic and rapid solution characteristic, it comprises:
1) zwitterionic surfactant of 5% to 25%；
2) other surfactants of 10% to 30%, other surfactants described are the mixture of a kind of in anion surfactant, nonionic surfactant or two kinds；
3) chelating agen of 0.01% to 5.0%；
4) cosolvent of 0.01% to 20%；
5) preservative of 0.01% to 2.0%；
6) water content is more than 60%.
High water content gel-type composition of detergent of the present invention, described zwitterionic surfactant meets the following conditions:
1) selected from amino acid type amphoteric surface active agent, the mixture of the two or three of betaine type amphoteric surfactant and Imidazoline Surfactants；
2) a kind of amino acid type amphoteric surface active agent is at least contained.
High water content gel-type composition of detergent of the present invention, described amino acid type amphoteric surface active agent is selected from one or more mixture of following compound:
1) N-fatty acyl group alanine derivatives；
2) N-fatty acyl group sarcosine derivative；
3) N-fatty acyl group glutamate derivatives；
Fatty acyl group is selected from the group of following structure: CnH2n+1, n is the positive integer of 8 to 22；Above-mentioned salt comprises cation, described cation selected from sodium ion, potassium ion, ammonium radical ion, organic amine ammonium root one or more mixture cationic.
High water content gel-type composition of detergent of the present invention, described betaine type amphoteric surfactant is selected from any one in alkyl betaine, fatty acid amide glycine betaine, fattyamidopropyl betaine, fatty amide propyl hydroxypropyl sulfonated betaine or two or more mixture；Described Imidazoline Surfactants is selected from acetate alkyl sodium form imidazoline, fatty acid type imidazoline, any one or the two or more mixture in sulfonic acid type imidazoline.
High water content gel-type composition of detergent of the present invention, described anion surfactant is selected from: the mixture of any one or more in polyoxyethylenated alcohol sodium sulfate, fatty alcohol-polyoxyethylene ether carboxylic acid sodium, sodium alkyl sulfate, sodium alkyl benzene sulfonate, sodium alkyl sulfonate, α-sodium olefin sulfonate, methyl sodiosul foaliphatate, 2-Sulfosuccinic acid ester sodium salt.
Described polyoxyethylenated alcohol sodium sulfate, fatty alcohol alkyl chain is preferably the straight chained alkyl of 12 to 16 carbon atoms；The average adduct number of oxirane of alcohol ether is 1 to 3.
High water content gel-type composition of detergent of the present invention, described nonionic surfactant any one or two or more mixture in fatty alcohol-polyoxyethylene ether, collateralization fatty alcohol-polyoxyethylene ether, alkanolamide, alkyl-glucoside, sucrose ester, polyglyceryl fatty acid ester, the amine oxide.
High water content gel-type composition of detergent of the present invention, described cosolvent is the mixture of any one or more in ethanol, propylene glycol, glycerol；Described preservative is any one or two or more mixture in sodium benzoate, potassium sorbate, Methylisothiazolinone, phenoxyethanol.
High water content gel-type composition of detergent of the present invention, comprises light stabilizer, antioxidant, one or more mixture of essence further.
High water content gel-type composition of detergent of the present invention, it is substantially free of inorganic salt and macromolecule thickener.
The gel-type composition of detergent that the present invention relates to, when carrying out flow graph oscillation frequency sweep test (25 DEG C), loss modulus G " curve and storage modulus G ' curve intersection; low frequency range loss modulus G " higher than storage modulus G ', high frequency region storage modulus G ' is higher than loss modulus G ", G ' curve and G " range of strain that intersections of complex curve is corresponding is 101% to 102%；Said composition viscosity is at more than 130000mPa s, and when containing the container upside down of said composition, said composition will not natural flow in 5 minutes.
Described shear shinning characteristic, gel-type composition of detergent is 1s in shear rate-1Time, viscosity is more than 130000mPa s, and when shear rate increases to 10s-1Time, its viscosity is below 10000mPa s, and when shear rate continues to increase, its viscosity continues to reduce.
Described rapid solution characteristic, compositions is not stirred in the water of 25 DEG C with 0.2% concentration dilution, can dissolve voluntarily completely in 2 minutes.
High water content gel-type composition of detergent of the present invention has the advantage that and beneficial functional:
1, high water content gel-type composition of detergent of the present invention, compared with conventional conventional detergent compositions, it is not necessary to uses inorganic salt or macromolecule to form gel, and has the feature of green natural.
2, high water content gel-type composition of detergent of the present invention its be characterized in that it has selected suitable amphoteric surfactant composite, even if so that this detergent does not use macromolecule, System forming gel can also be promoted by the suitable pH value of adjustment, be different from traditional gel and generate means.While having saved thickening agent cost, owing to this composition of detergent with the addition of substantial amounts of amino acid type surfactant, almost non-toxic harmless, in use to human body skin as mild as a dove, and can effectively reduce other anion surfactants in formula to the stimulation of hand skin and residual, there is the feature of green natural.
3 it addition, this gel-type composition of detergent has good water solublity, is not stirred to dissolve completely voluntarily in 2 minutes with 0.2% concentration dilution in the water of 25 DEG C, and the dissolving of detergent in Actual laundering process will not be caused obstacle by gel state.
Accompanying drawing explanation
Fig. 1 be the composition of detergent of embodiment 1 different shearing forces under viscosity scanning curve, its rheometer test temperature is 25 DEG C, and shearing force ranges for 1s-1To 100s-1。
Fig. 2 is the oscillation frequency sweep curve of the composition of detergent of embodiment 1, and its rheometer test temperature is 25 DEG C, and strain sweep ranges for 10-2% to 103%.
Detailed description of the invention
The composite formation vermiculate glues of the preferred amphion of the present invention, obtained composition of detergent product has gel characteristic.Described special surface activating agent and auxiliary combination at least contain a kind of special amphoteric surfactant, are regulated by the combination of such special surface activating agent and system pH so that surfactant micellar easily changes from lameller micelles to vermiculate glues, form gel.
For a person skilled in the art, by reading the content of this disclosure, inventive feature, beneficial effect and advantage will become clear from.
Except as otherwise noted, all percentage ratios, mark and ratio are all by the total weight of the present composition.Except as otherwise noted, all giving the content of active substance about all wt of ingredients listed, therefore they are likely to the solvent or the by-product that comprise not included in commercially available material.Term " weight content " available symbols " % " represents herein.
Except as otherwise noted, there is the environment at 25 DEG C in all preparations and test in this article.
" include " herein, " comprising ", " containing ", " containing ", " having " or other variant be intended to non-enclosed including, do not distinguish between these terms.Term " comprises " and refers to and can add other step and composition not affecting final result.Term " comprise " also include term " by ... composition " and " substantially by ... form ".The compositions and methods of the invention/technique can comprise, consisting of be substantially made up of essential elements described herein and limit entry and arbitrary additional or optional composition described herein, component, step or limit entry.
" be substantially free of " herein, " without " or other variant be intended to non-enclosed not include, do not distinguish between these terms.Term " is substantially free of " and refers to that not interpolation or certain material addition are below 0.1% artificially.
Composition of detergent
The liquid detergent composition of the present invention includes fabric detergent compositions or tableware cleaning detergent compositions, is chosen in particular from the group of following composition: fabric detergent compositions, liquid hand dish washing detergent compositions, the automatic dishwashing detergent composition of liquid.
The composition of detergent of the present invention is contacted in water by the substrate (i.e. textile article and tableware) contacted with needs, thus by the greasiness removal of substrate surface, reaching the purpose of cleaning substrate surface.
Described fabric detergent compositions and tableware Cleasing compositions generally also comprise surfactant system and other common washing assisant such as viscosity modifier, enzyme preparation, spice etc..
Gel characteristic
Gel characteristic of the present invention refers to the fluid property that gel detergent system has, and its fluid property is different from general liquid detergent.The fluid property of liquid detergent can by viscosity, storage modulus G ' and loss modulus G " etc. parameter reflected.Storage modulus G ' is also called elastic modelling quantity, refers to that material is when deforming upon, and stores the size of energy due to elastic (reversible) deformation, reflects elastic properties of materials size.Loss modulus G " also known as viscous modulus, refer to that material is when deforming upon, the energy size of loss due to viscous deformation (irreversible), reflects tack of materials size.Storage modulus G ' is much larger than loss modulus G " time, material is mainly deformed elastically, so material list reveals the feature of elastomer.Loss modulus G " much larger than storage modulus G ' time, mainly there is viscous deformation in material, so material presents the feature of viscoid.Gel characteristic of the present invention refers to that the G ' numerical value of this inventive gel system is more than G "; demonstrate the feature of elastomer, be embodied in this invention composition of detergent more than viscosity 130000mPa s and when containing the container upside down of said composition said composition will not flow in 5 minutes.
Generally, when liquid detergent carries out the test of flow graph oscillation frequency sweep, at test zone internal loss modulus G " it is consistently greater than storage modulus G ', G " curve and G ' curve do not have intersection point, only shows the feature of viscoid.
Inventor have found that based on zwitterionic surfactant composite, described composition of detergent is made to obtain special fluid property after defining vermiculate glues structure, when using flow graph to carry out oscillation frequency sweep test (25 DEG C); G " curve and G ' curve intersection, low frequency range loss modulus G " higher than storage modulus G '; high frequency region storage modulus G ' is higher than loss modulus G ", namely under different strain rates, described composition of detergent can show the feature of viscoid and elastomer respectively.
Shear shinning characteristic
The gel-type composition of detergent that the present invention relates to is 1s in shear rate-1Time, viscosity is more than 130000mPa s, and when shear rate increases to 10s-1Time, its viscosity is below 10000mPa s, and when shear rate continues to increase, its viscosity continues to reduce.
Rapid solution characteristic
In the present invention, described rapid solution characteristic refers to that compositions is not stirred to dissolve voluntarily completely in 2 minutes with 0.2% concentration dilution in the water of 25 DEG C；
High water content
In the present invention, described high water content refers to that the water content of said composition is more than 60%；
Inorganic salt
Heretofore described salt is the relative molecular mass electrolyte less than 1000.The group of the anionic group of salt a kind of or composition in sulfate ion, chloride ion, nitrate ion, citrate ion, hydroxide ion, oxalate denominationby, sulfite ion, chloranion and hypochlorite ion；The cation group of salt comprises a kind of in lithium ion, sodium ion, potassium ion, rubidium ion, calcium ion, magnesium ion, ammonium radical ion or the group of composition, it is preferred to any one or the two or more mixture in sodium chloride, potassium chloride, sodium sulfate, ammonium chloride, calcium chloride, magnesium chloride and sodium citrate.
Macromolecule thickener
Macromolecule thickener of the present invention refers in particular to water miscible macromolecule thickening material, such as starch, gelatin, sodium alginate, guar gum, carapace glue, Radix Acaciae senegalis, xanthan gum, soybean glue, polyacrylamide, polyvinyl alcohol, polyvinylpyrrolidone, modified paraffin resin, carbomer, butadiene-styrene rubber etc..
PH scope
PH value is the method for expressing embodying certain solution or material acid-base value, the pH value of inventive gel type detergent combination directly affects its character, pH scope described herein refers to that inventive gel type composition of detergent can keep the acid-base value scope of its gel characteristic, shear shinning characteristic and rapid solution characteristic, the pH of described gel-type composition of detergent ranges for 4.0 to 8.0, it is preferable that pH ranges for 4.0 to 6.5.
Surfactant system
The surfactant system of the composition of detergent that the present invention relates to includes, but is not restricted to: anion surfactant, nonionic surfactant, cationic surfactant, the mixture that zwitterionic surfactant is a kind of and multiple.Preferred surfactant system comprises the mixture of anion surfactant and nonionic surfactant.
Zwitterionic surfactant
Content is mixture the 5% to 25% of zwitterionic surfactant, calculates with mixture total weight gauge.
Zwitterionic surfactant is selected from betaine type amphoteric surfactant, Imidazoline Surfactants, amino acid type surfactant；Include, but are not limited to: alkyl betaine, fatty acid amide glycine betaine, fattyamidopropyl betaine, fatty amide propyl hydroxypropyl sulfonated betaine, including acetate alkyl sodium form imidazoline, fatty acid type imidazoline, sulfonic acid type imidazoline；Alanine derivatives, glycine derivative etc..
Anion surfactant
Content is mixture the 10% to 30% of anion surfactant, calculates with mixture total weight gauge.
Anion surfactant is selected from sulfonate surfactant, carboxylate surfactant, one or more mixture of sulfated surfactant；It preferably is selected from alkylbenzenesulfonate, the alkyl sulfate of C8 to C18, the ethoxylated fatty alcohol sulfate of C8 to C18, alpha-alkene sulfonate, fatty acid alkyl ester sulfonate, the one of ethoxylized fatty alcohol ether carboxylate, and their mixture.
In some embodiments, the mixture of anion surfactant preferably comprises alkylbenzenesulfonate and derivant thereof.Described alkylbenzenesulfonate meets below formula:
Wherein R1 is carbon number is the alkyl of 6 to 24, M+For cation.R1 can be the alkyl of straight chain, it is possible to be the alkyl of side chain；Can be saturated alkyl, it is also possible to be the alkyl containing one or more unsaturated double-bonds.It is preferred that R1 is carbon number is the straight chained alkyl of 8 to 18.In some embodiments, the mixture of anion surfactant contains the aliphatic alcohol sulfate of ethoxylation.Ethoxylated fatty alcohol sulfate is the derivant of ethoxylate fatty alcohol, has below formula:
Wherein R1 is carbon number is the alkyl of 6 to 24；X is 0.5 to 30；Wherein M+For cation.R1 can be the alkyl of straight chain, it is also possible to be the alkyl of side chain；Can be saturated alkyl, it is also possible to be the alkyl containing one or more unsaturated double-bonds.Preferred R1 is carbon number is the straight chained alkyl of 8 to 18.X represents average ethoxylation degree, is 0.5 to 30, it is preferable that 0.5 to 10, and more preferably 0.5 to 3.
In some embodiments, containing alpha-alkene sulfonate, there is below formula:
Wherein a is 0 to 2, and R1 is carbon number is the alkyl of 6 to 24, it is preferable that R1 is carbon number is the alkyl of 8 to 18.Described anion surfactant can also comprise a kind of of alkyl sodium disulfonate or derivatives thereof and multiple mixture, it is preferable that alkyl diphenyl ether disulphonic acid sodium, suitable example is disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate salt.Fatty acid alkyl esters sulfate can also be contained, it is preferred to fatty acid methyl ester sulfate (MES), fatty acid carbon number preferably 8 to 18.Can also comprising sulfosuccinate, it is preferred to disodium alkyl polyoxyethylene sulfosuccinate, fatty alcohol carbon number preferably 8 to 18, average ethoxylation degree is preferably 2.0.
Nonionic surfactant
Content is mixture the 10% to 30% of nonionic surfactant, calculates with mixture total weight gauge.
Nonionic surfactant is selected from fatty alcohol alkoxy compound, APG, fatty acid alkoxylates, fatty acid ethoxylate, fatty acid alkyl alcohol amide, one or more mixture of ethoxylated sorbitan acid alcohol ester.
In some embodiments, non-ionic surfactant mixture preferably comprises fatty alcohol alkoxy compound, and described fatty alcohol alkoxy compound has below general formula:
Described fatty alcohol alkoxy compound is fatty alcohol and epoxyalkane product of ring-opening polymerisation under base catalyst effect, substantially mixture.Fatty alcohol includes the isomery alcohol of straight chain alcohol or side chain.Alkoxy grp includes ethoxy group and propoxyl group group.The preferred carbon number of fatty alcohol is the fatty alcohol of 8 to 18, preferred alcohol includes, but are not limited to hexanol, capryl alcohol decanol, 2-ethylhexanol, 3-propyl enanthol, lauryl alcohol, different three decanol, tridecyl alcohol, tetradecanol, hexadecanol, Palmitoleyl alcohol, stearyl alcohol, isooctadecanol, oleyl alcohol, sub-oleyl alcohol, the one of linolenyl alcohol and mixture thereof.Average ethoxylation degree x preferably 2 to 12.Suitable example is SHELL company NEODOL series linear primary alcohol ethoxylate product, and DOW company ECOSURF.EH series ethoxylation and third aoxidizes 2-ethylhexanol product.
In some embodiments, non-ionic surfactant mixture preferably comprises APG, has below general formula:
Wherein, n is 6 to 24, and p is 1.1 to 3, it is preferable that n is 8 to 16.Suitable APG is BASF AG Glucopon series alkyl polyglucoside product such as.
Non-ionic surfactant mixture can contain fatty acid alkoxylates, it is preferable that from ethoxylation C8 to C18 fatty acid ester, and average ethoxylation degree is 2 to 10.Can containing ethoxylated sorbitan acid alcohol Arrcostab, alkyl carbon number is 6 to 18, and average ethoxyquin degree is 4 to 20；Suitable example is Corda company's T ween series of products.
Non-ionic surfactant mixture can contain fatty acid alkyl alcohol amide, and the carbon number of fatty acid is 6 to 24, it is possible to is the fatty acid of straight chain, it is also possible to is the fatty acid of side chain, it is possible to is saturated fatty acid, it is also possible to is undersaturated fatty acid；Alkylol number is 0 to 2.Preferred fatty acid carbon number is a glycollic amide of 8 to 18, diglycollic amide, and isopropanol amide, suitable example is cocoanut oil diethan olamide.
Non-ionic surfactant mixture can contain fatty acid methyl ester ethoxylate, and formula is as follows:
Wherein, n is 6 to 24；X is 2 to 20, it is preferable that n is 8 to 18, and x is 0.5 to 30.Preferred x is 4 to 10.Suitable example is LION company MEE product.Non-ionic surfactant mixture can contain polyether surfactant.Polyether surfactant is a kind of polymer, and containing the nonionic surfactant of oxidation ethylene and/or oxidation trimethylene repetitive, suitable example is BASF AG Pluronic series of products such as.
Optional member
The composition of detergent that the present invention relates to comprises additive optional as follows: the mixture of one or more compositions of alkaline agent, preservative, coloring agent, colour stabilizer and essence.
The composition of detergent that the present invention relates to can comprise one or more alkaline agents, and alkaline agent is selected from sodium hydroxide, potassium hydroxide, alkali carbonate, alkali-metal silicate.
In some embodiments, the composition of detergent that the present invention relates to preferably comprises preservative, and suitable example is phenoxy group alcohol, sodium benzoate；Isothiazolone and derivant thereof such as Methylisothiazolinone, methylchloroisothiazandnone, the one of BIT or its mixture.Preservative consumption is 0.001% to 5%, it is preferred to 0.01% to 2%.
In some embodiments, the composition of detergent that the present invention relates to contains coloring agent, and described coloring agent comprises dyestuff and pigment.Coloring agent comprise all in cleaning product application coloring agent, suitable example such as acid red G, basic fuchsin, Methanil Yellow G, Acid Light Yellow G, alkalescence egg yolk, direct fast blue B2RL, indigo-blue etc..
In some embodiments, the composition of detergent that the present invention relates to contains colour stabilizer.Colour stabilizer comprises all colour stabilizers can applied in cleaning product.
The composition of detergent that the present invention relates to preferably comprises spice, and described spice comprises all fragrance components being applicable to cleaning product.The spice used of the present invention can be natural origin, it is also possible to is the goods of chemosynthesis, or the mixture of the two.Suitable example such as Fructus Citri Limoniae, Flos Rosae Rugosae, jasmine, lavandula angustifolia, Citrus are fragrant, QINGXIANG, the Radix Aucklandiae etc..
Except above-mentioned optional member, the composition of detergent of the present invention also can comprise: water, organic solvent, cosolvent, solubilizing agent, structural agent, short infusion, foam inhibitor, fabric softener, anti-wrinkle agent etc. are various common and the additive of routine.These additives and associated method of use are all well-known to those skilled in the art, and the selection of its concrete type and consumption can be adjusted according to actual needs.
Preparation and using method
The composition of detergent of the present invention adopts various methods well-known to those skilled in the art to prepare.The preparation of described compositions can be undertaken by conventional means, specifically should according to component state in the solution and effect, and the stability of component selects suitable processing temperature and process time.
The using method of the composition of detergent of the present invention is well-known to those skilled in the art, typical using method is with undiluted mode or the mode that is diluted in water by concrete composition of detergent embodiment, contacting with the surface being washed object, then rinsing is washed the surface of object.Preferably, it is washed object between above-mentioned contact procedure and rinse step, carries out washing step.Washing step includes but not limited to clean and mechanical agitation.It is washed object and includes fabric and tableware.Described composition of detergent concentration in water is about 500ppm to 10000ppm, and water temperature is preferably 5 DEG C to about 60 DEG C.Water and the ratio being washed object are preferably from about 1:1 to about 20:1.
Without further describing, it is believed that those skilled in the art use the above can use the present invention to greatest extent.The following examples purpose is in that to be further described and show specific embodiments within the scope of the present invention.Therefore, embodiment is it should be understood that be used only for showing in more detail the present invention, and the content not limited the present invention in any way.
In following example, except as otherwise noted, all of content is all weight percentage, and the content about ingredients listed is the content through the active substance converted.
Embodiment 1
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 1 below:
The formula composition of the high water content gel-type composition of detergent of table 1 embodiment 1
| Raw material components | Role | Percentage by weight (%) |
| Myristoyl glutamate potassium | Surfactant | 7.0 |
| Dodecanamide propyl Folium hydrangeae strigosae alkali | Surfactant | 14.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 7.0 |
| Sodium olefin sulfonate | Surfactant | 2.0 |
| Fatty alcohol-polyoxyethylene ether-7 | Surfactant | 1.5 |
| Glycerol | Solvent | 5.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 1, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 4.5 to .2.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Embodiment 2
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 2 below:
The formula composition of the high water content gel-type composition of detergent of table 2 embodiment 2
| Raw material components | Role | Percentage by weight (%) |
| Oleoyl sodium glutamate | Surfactant | 7.0 |
| Cocamidopropyl propyl amide Folium hydrangeae strigosae alkali | Surfactant | 12.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 7.0 |
| Sodium olefin sulfonate | Surfactant | 2.0 |
| Fatty alcohol-polyoxyethylene ether-9 | Surfactant | 1.0 |
| Glycerol | Solvent | 5.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 2, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 4.6 to 5.1.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Embodiment 3
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 3 below:
The formula composition of the high water content gel-type composition of detergent of table 3 embodiment 3
| Raw material components | Role | Percentage by weight (%) |
| Sodium lauroyl sarcosine | Surfactant | 6.0 |
| Cocamidopropyl propyl amide Folium hydrangeae strigosae alkali | Surfactant | 12.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 8.0 |
| Sodium olefin sulfonate | Surfactant | 2.0 |
| Fatty alcohol-polyoxyethylene ether-9 | Surfactant | 0.8 |
| Glycerol | Solvent | 5.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 3, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 5.5 to 6.2.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Embodiment 4
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 4 below:
The formula composition of the high water content gel-type composition of detergent of table 4 embodiment 4
| Raw material components | Role | Percentage by weight (%) |
| Sodium lauroyl sarcosine | Surfactant | 2.0 |
| Cocamidopropyl propyl amide Folium hydrangeae strigosae alkali | Surfactant | 4.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 8.0 |
| Sodium olefin sulfonate | Surfactant | 1.5 |
| Fatty alcohol-polyoxyethylene ether-9 | Surfactant | 1.0 |
| Glycerol | Solvent | 1.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 4, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 5.5 to 6.2.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Embodiment 5
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 5 below:
The formula composition of the high water content gel-type composition of detergent of table 5 embodiment 5
| Raw material components | Role | Percentage by weight (%) |
| Sodium lauroyl sarcosine | Surfactant | 3.0 |
| Dodecanamide propyl Folium hydrangeae strigosae alkali | Surfactant | 6.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 10.0 |
| Sodium olefin sulfonate | Surfactant | 2.0 |
| Fatty alcohol-polyoxyethylene ether-7 | Surfactant | 0.8 |
| Glycerol | Solvent | 2.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 5, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 5.5 to 6.2.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Embodiment 6
A kind of high water content gel-type composition of detergent, comprises raw material components and the content of table 6 below:
The formula composition of the high water content gel-type composition of detergent of table 6 embodiment 6
| Raw material components | Role | Percentage by weight (%) |
| Sodium lauroyl glutamate | Surfactant | 4.0 |
| Cocamidopropyl propyl amide Folium hydrangeae strigosae alkali | Surfactant | 8.0 |
| Polyoxyethylenated alcohol sodium sulfate | Surfactant | 10.0 |
| Sodium olefin sulfonate | Surfactant | 0.2 |
| Fatty alcohol-polyoxyethylene ether-9 | Surfactant | 0.2 |
| Glycerol | Solvent | 1.0 |
| Disodiumedetate | Chelating agen | 0.1 |
| Sodium benzoate | Preservative | 0.2 |
| Methylisothiazolinone | Preservative | 0.04 |
| Deionized water | Solvent | Surplus (adds to 100%) |
According to the formulation content of table 6, first putting into deionized water and polyoxyethylenated alcohol sodium sulfate, put into other surfactants after stirring and dissolving, pH adjusts to 7.0 to 7.5, puts into chelating agen, preservative and other auxiliary agents, then by pH regulator to 5.5 to 6.2.Qualified products stand to basic non-foam, can fill be finished detergent composition.
Effect application test example
Visual inspection is tested
Composition of detergent of the present invention is clear gel, according to the concrete surfactant base used, it is possible to can slightly have faint yellow.Table 7 below is the visual inspection result that this invention composition of detergent is deposited 1 month under different temperatures.
Table 7 visual inspection the results list
| Composition of detergent title | -5℃ | 0℃ | 30℃ | 45℃ |
| Embodiment 1 | Clear | Clear | Clear | Clear |
| Embodiment 2 | Muddy | Clear | Clear | Clear |
| Embodiment 3 | Muddy | Clear | Clear | Clear |
| Embodiment 4 | Clear | Clear | Clear | Clear |
| Embodiment 5 | Clear | Clear | Clear | Clear |
| Embodiment 6 | Clear | Clear | Clear | Clear |
The fluid property test of composition of detergent gel
1, the viscosity scanning curve test under different shearing forces
Viscosity scanning curve such as Fig. 1 under the different shearing forces of the gel-type composition of detergent that embodiment 1 prepares.Wherein, rheometer test temperature is 25 DEG C, and shearing force ranges for 1s-1To 100s-1.It will be seen from figure 1 that be 1s in shear rate-1Time, viscosity is more than 130000mPa s, and when shear rate increases to 10s-1Time, its viscosity is below 10000mPa s, and when shear rate continues to increase, its viscosity continues to reduce.
2, loss modulus G " with the sweep test of storage modulus G '
The oscillation frequency sweep curve of the gel-type composition of detergent that embodiment 1 prepares is as shown in Figure 2.Wherein, oscillatory scanning test temperature is 25 DEG C, and frequency sweeping ranges is that strain sweep ranges for 10-2% to 103%.As can be seen from Figure 2, measuring in range of strain, loss modulus G " curve and storage modulus G ' curve intersection, low frequency range loss modulus G " higher than storage modulus G ', high frequency region storage modulus G ' is higher than loss modulus G ", G ' curve and G " range of strain corresponding to intersections of complex curve be all 101% to 102Between %.Be embodied in this invention composition of detergent more than viscosity 130000mPa s and when being loaded with the container upside down of said composition said composition will not flow in 5 minutes.
3, the water solublity test of composition of detergent gel
6 the embodiment composition of detergent of contrast test dissolution velocity in different temperatures water, it dissolves ratio unified is detergent concentration 0.2%, and period does not increase any mechanical agitation power, and its end value is dissolved completely in water with detergent, namely perusal is invariably tolerant for dissolving terminal, and result is in Table 8.
The water solublity test result list of table 8 composition of detergent gel
| Composition of detergent title | 2℃ | 10℃ | 25℃ | 45℃ |
| Embodiment 1 | 3min20s | 2min20s | 1min30s | 30s |
| Embodiment 2 | 6min50s | 3min50s | 1min57s | 54s |
| Embodiment 3 | 5min15s | 2min57s | 1min50s | 52s |
| Embodiment 4 | 2min10s | 1min40s | 59s | 20s |
| Embodiment 5 | 2min30s | 1min45s | 1min3s | 30s |
| Embodiment 6 | 2min32s | 1min43s | 1min | 31s |
Be can be seen that by the content of table 8, the composition of detergent of embodiment of the present invention 1-6 is respectively provided with good water solublity, 6 example composition all can be dissolved within 2 minutes and in water at nominal room temperature, and any mechanical agitation power need not be increased, therefore no matter said composition is applied in clothes washing or dishwashing detergent can meet rapidly-soluble requirement after in input water, washing process will not be caused obstacle.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is done any pro forma restriction, therefore it is every without departing from technical solution of the present invention content, according to any simple modification, equivalent variations and modification that above example is made by the technical spirit of the present invention, all still fall within the scope of technical solution of the present invention.
Claims (12)
1. the method giving composition of detergent gel characteristic, it is characterised in that comprise 5% to 25% zwitterionic surfactant；Described zwitterionic surfactant meets the following conditions:
1) selected from amino acid type amphoteric surface active agent, the mixture of the two or three of betaine type amphoteric surfactant and Imidazoline Surfactants；2) a kind of amino acid type amphoteric surface active agent is at least contained.
2. the method for imparting composition of detergent gel characteristic according to claim 1, it is characterized in that: described gel characteristic refers to that said composition viscosity is at more than 130000mPa s, and when containing the container upside down of said composition, said composition will not natural flow in 5 minutes.
3. the method for imparting composition of detergent gel characteristic according to claim 1, it is characterised in that: the described amino acid type amphoteric ionic surface active agent mixture of any one or more in N-fatty acyl group alanine salt, N-fatty acyl sarcosinates and N-fatty acyl group glutamate, Glu；Fatty acyl group is selected from the group of following structure:
CnH2n+1, n is the positive integer of 8 to 22；
Above-mentioned salt comprises cation, described cation selected from sodium ion, potassium ion, ammonium radical ion, organic amine ammonium root one or more mixture cationic.
4. the method for imparting composition of detergent gel characteristic according to claim 1, it is characterised in that: described betaine type amphoteric surfactant is selected from any one in alkyl betaine, fatty acid amide glycine betaine, fattyamidopropyl betaine, fatty amide propyl hydroxypropyl sulfonated betaine or two or more mixture；Described Imidazoline Surfactants is selected from any one in acetate alkyl sodium form imidazoline, fatty acid type imidazoline, sulfonic acid type imidazoline or two or more mixture.
5. a high water content gel-type composition of detergent, it is characterised in that it comprises:
1) zwitterionic surfactant of 5% to 25%；
2) other surfactants of 10% to 30%, other surfactants described are the mixture of at least one in anion surfactant, nonionic surfactant or two kinds；
3) chelating agen of 0.01% to 5.0%；
4) cosolvent of 0.01% to 20%；
5) preservative of 0.01% to 2.0%；
6) water content is more than 60%.
6. high water content gel-type composition of detergent according to claim 5, it is characterised in that: described zwitterionic surfactant meets the following conditions:
1) selected from amino acid type amphoteric surface active agent, two or more mixture of betaine type amphoteric surfactant and Imidazoline Surfactants；
2) a kind of amino acid type amphoteric surface active agent is at least contained.
7. high water content gel-type composition of detergent according to claim 6, it is characterised in that: the described amino acid type amphoteric surface active agent mixture of any one or more in N-fatty acyl group alanine derivatives, N-fatty acyl group sarcosine derivative and N-fatty acyl group glutamate derivatives；
Fatty acyl group is selected from the group of following structure: CnH2n+1, n is the positive integer of 8 to 22；
Above-mentioned salt comprises cation, described cation selected from sodium ion, potassium ion, ammonium radical ion, organic amine ammonium root one or more mixture cationic.
8. high water content gel-type composition of detergent according to claim 6, it is characterised in that: described betaine type amphoteric surfactant is selected from any one in alkyl betaine, fatty acid amide glycine betaine, fattyamidopropyl betaine, fatty amide propyl hydroxypropyl sulfonated betaine or two or more mixture；Described Imidazoline Surfactants is selected from any one in acetate alkyl sodium form imidazoline, fatty acid type imidazoline, sulfonic acid type imidazoline or two or more mixture.
9. high water content gel-type composition of detergent according to claim 5, it is characterised in that: the described anion surfactant mixture of any one or more in polyoxyethylenated alcohol sodium sulfate, fatty alcohol-polyoxyethylene ether carboxylic acid sodium, sodium alkyl sulfate, sodium alkyl benzene sulfonate, sodium alkyl sulfonate, α-sodium olefin sulfonate, methyl sodiosul foaliphatate, 2-Sulfosuccinic acid ester sodium salt；Fatty alcohol alkyl chain is preferably the straight chained alkyl of 12 to 16 carbon atoms；The average adduct number of oxirane of alcohol ether is 1 to 3；
Described nonionic surfactant any one or two or more mixture in fatty alcohol-polyoxyethylene ether, collateralization fatty alcohol-polyoxyethylene ether, alkanolamide, alkyl-glucoside, sucrose ester, polyglyceryl fatty acid ester, the amine oxide.
10. high water content gel-type composition of detergent according to claim 5, it is characterised in that: described cosolvent is the mixture of any one or more in ethanol, propylene glycol, glycerol；Described preservative is any one or two or more mixture in sodium benzoate, potassium sorbate, Methylisothiazolinone, phenoxyethanol.
11. high water content gel-type composition of detergent according to claim 5, it is characterised in that: it further comprises one or more the mixture in light stabilizer, antioxidant, essence；And said composition is substantially free of inorganic salt and macromolecule thickener.
12. high water content gel-type composition of detergent according to claim 5, it is characterized in that: when carrying out flow graph oscillation frequency sweep test (25 DEG C), loss modulus G " curve and storage modulus G ' curve intersection; low frequency range loss modulus G " higher than storage modulus G ', high frequency region storage modulus G ' is higher than loss modulus G ", G ' curve and G " range of strain that intersections of complex curve is corresponding is 101% to 102%；Said composition viscosity is at more than 130000mPa s, and when containing the container upside down of said composition, said composition will not natural flow in 5 minutes.
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| CN111233009A (en) * | 2020-02-28 | 2020-06-05 | 山东丽波日化股份有限公司 | Heavy alkali filter aid and preparation method thereof |
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| WO2023116697A1 (en) * | 2021-12-21 | 2023-06-29 | 青岛海尔洗衣机有限公司 | Washing machine |
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