Tablet detergent
By embedding high amounts of enzyme and fabric softener preparations in solid form within the tablet detergent, the challenges of enzyme inactivation and lack of fabric softener are addressed, resulting in improved cleaning power, stability, and static removal.
Patent Information
- Application Number
- JP2024551911
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2022-12-21
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2042-12-21
AI Technical Summary
Current tablet detergents face challenges in maintaining cleaning power due to enzyme inactivation during the drying process and instability when exposed to air and humidity, leading to reduced effectiveness in removing protein and milk stains. Additionally, they lack fabric softener components, resulting in poor static removal and stability issues.
The development of a tablet detergent that embeds a high amount of enzyme preparation and fabric softener component in solid particle form, ensuring stability and preventing inactivation. This formulation includes a combination of water-soluble polymers, surfactants, enzyme preparations, fabric softener preparations, and foaming agents, which are continuously dried and molded to maintain stability and effectiveness.
The tablet detergent achieves enhanced cleaning power for protein and milk stains, improved stability against temperature and humidity, and effective static removal, making it suitable for both clothing and dishwasher use while maintaining long-term storage stability.
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Abstract
Description
[Technical field]
[0001] The present application relates to the technical field of detergents, and in particular to detergent tablets. [Background technology]
[0002] Solid, tablet-type detergents (tablet-type detergents) are increasingly favored and used by young consumers and business travelers due to their advantages such as high effective active ingredient content, concentration, storage, transportation, and portability. Although tablet-type detergents have the above advantages, they are not ideal in terms of cleaning power, which is of more concern to consumers, especially for stains such as protein and milk cake that are difficult to remove in daily life. Tablet-type detergents have very low moisture content, and therefore almost no moisture, due to the evaporation of moisture during the drying process, and are highly concentrated and portable, but due to the high temperature during drying, enzyme preparations with special functions will encounter high temperatures during the drying process, which will cause the inactivation of active ingredients, greatly weakening their cleaning ability and losing their original cleaning performance, and failing to remove protein and milk cake that are difficult to remove in daily life.
[0003] In addition, in the method of adding liquid enzyme preparations to tablet detergent by spraying and smearing, the liquid enzyme preparation itself contains a large amount of water and organic solvents, so if too much liquid enzyme preparation is added, not only will the tablet detergent itself, which is highly water-soluble, dissolve, but the tablet detergent will become sticky and soft, causing problems such as poor storage stability of the tablet detergent. In addition, in tablet detergents containing liquid enzyme preparations, the enzyme preparation is exposed to air and is easily affected by ambient temperature and humidity such as high temperature and humidity. Hyperacidic and hyperalkaline environments also easily inactivate enzyme-containing preparations. Therefore, current enzyme-containing tablet detergents have poor stability and are difficult to demonstrate high cleaning power, and there is still room for improvement.
[0004] In addition, existing tablet detergents do not contain fabric softeners, and fabric softeners must be added separately to remove static electricity from clothes, making laundry more complicated. If cationic fabric softeners are added directly to detergents, precipitation may occur due to mutual adsorption of different charges caused by prolonged contact with anionic surfactants in the detergent. As the functions of both are reduced, there is still no tablet detergent in the prior art that incorporates fabric softeners and maintains its cleaning and destaticizing functions. Summary of the Invention
[0005] In view of this, the present application provides a detergent tablet and a method for preparing the detergent tablet. A large amount of enzyme preparation is embedded in the detergent tablet of the present invention, which can ensure the stability of the enzyme preparation. At the same time, a softener component is embedded in the detergent tablet of the present invention, which makes the effect of the softener and the detergent component less susceptible to precipitation caused by mutual adsorption.
[0006] This application provides the following technical solutions: In a first embodiment, the present invention provides a detergent tablet comprising: 8 to 34 parts by weight of a water-soluble polymer; 14 to 50 parts by weight of a surfactant; 0.1 to 50 parts by weight of an enzyme preparation; 0.1 to 50 parts by weight of a fabric softener formulation; 1 to 10 parts by weight of a foam booster formulation; and 0 to 30 parts by weight of a molding aid, The enzyme formulation and fabric softener formulation are embedded onto the detergent tablet in the form of solid particles.
[0007] In some embodiments, the amount of water soluble polymer in the detergent tablet is preferably 9 to 33 parts by weight, 10 to 32 parts by weight, 11 to 31 parts by weight, 12 to 30 parts by weight, 13 to 29 parts by weight, 14 to 28 parts by weight, 15 to 27 parts by weight, 16 to 26 parts by weight, 17 to 25 parts by weight, 18 to 24 parts by weight, 19 to 23 parts by weight, 20 to 22 parts by weight, or 21 parts by weight, including any value and range therebetween.
[0008] In some embodiments, the amount of surfactant in the detergent tablet is preferably 16 to 48 parts by weight, 18 to 46 parts by weight, 20 to 44 parts by weight, 22 to 42 parts by weight, 24 to 40 parts by weight, 26 to 38 parts by weight, 28 to 36 parts by weight, 30 to 34 parts by weight, or 32 to 33 parts by weight, including any value and range therebetween.
[0009] In some embodiments, the amount of the enzyme formulation in the detergent tablet is preferably 0.5 to 50 parts by weight, 1 to 50 parts by weight, 2 to 48 parts by weight, 4 to 46 parts by weight, 6 to 44 parts by weight, 8 to 42 parts by weight, 10 to 40 parts by weight, 12 to 38 parts by weight, 14 to 36 parts by weight, 16 to 34 parts by weight, 18 to 32 parts by weight, 20 to 30 parts by weight, 22 to 28 parts by weight, 24 to 26 parts by weight, including any value and range therebetween.
[0010] In some embodiments, the amount of fabric softener formulation in the detergent tablet is preferably 0.5 to 50 parts by weight, 1 to 50 parts by weight, 2 to 48 parts by weight, 4 to 46 parts by weight, 6 to 44 parts by weight, 8 to 42 parts by weight, 10 to 40 parts by weight, 12 to 38 parts by weight, 14 to 36 parts by weight, 16 to 34 parts by weight, 18 to 32 parts by weight, 20 to 30 parts by weight, 22 to 28 parts by weight, 24 to 26 parts by weight, including any value and range therebetween.
[0011] In some embodiments, the amount of foam booster formulation in the detergent tablet is preferably 2 to 9 parts by weight, 3 to 8 parts by weight, 4 to 6 parts by weight, or 5 parts by weight, including any value and range therebetween.
[0012] In some embodiments, the amount of molding aid in the detergent tablet is preferably 1 to 28 parts by weight, 3 to 26 parts by weight, 5 to 24 parts by weight, 7 to 22 parts by weight, 9 to 20 parts by weight, 11 to 18 parts by weight, 13 to 16 parts by weight, or 14 to 15 parts by weight, including any value and range therebetween.
[0013] In some embodiments, the water-soluble polymer is one or more selected from polyvinyl alcohol, polyvinylpyrrolidone, gelatin, carrageenan, cross-linked polyacrylic acid, water-soluble polyacrylamide, polymers of vinyl acetate and vinyl alcohol, starch, dextrin, polysaccharides, cellulose, modified cellulose, and microcrystalline cellulose.
[0014] In some embodiments, the water soluble polymer comprises polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), hydroxypropylmethylcellulose (HPMC), and / or hydroxyethylcellulose (HEC).
[0015] In some embodiments, the polyvinyl alcohol may be unmodified or modified, e.g., carboxylated or sulfonated, or may be a copolymer of vinyl alcohol or vinyl ester monomers with one or more other monomers. Preferably, the PVA is partially or fully alcoholized or hydrolyzed. For example, the PVA may be about 40 to 100%, preferably about 50 to about 95%, and preferably about 80 to about 92% alcoholized or hydrolyzed. It is known that the degree of hydrolysis affects the temperature at which the PVA begins to dissolve in water; for example, 88% hydrolysis corresponds to a PVA solution that is soluble in cold water (i.e., room temperature), while 90% or more hydrolysis corresponds to a PVA solution that is soluble in warm water (hot water). The polyvinyl alcohol has an average molecular weight (MW) of 20,000 to 120,000 and an average degree of polymerization (DP) of 500 to 2,500, but more preferably has an average molecular weight (MW) of 25,000 to 100,000 and an average degree of polymerization (DP) of 550 to 2,000.
[0016] In some embodiments, the polyvinylpyrrolidone (PVP) may be prepared by methods such as bulk polymerization or solution polymerization using the monomer vinylpyrrolidone, and may be in the form of homopolymer, copolymer, and crosslinked polymer, as well as in the form of nonionic, cationic, or anionic. Preferably, it is either nonionic or anionic, or a combination thereof. In the present application, nonionic polyvinylpyrrolidone is more preferred. A composite of nonionic polyvinylpyrrolidone and PVA having an average molecular weight of 5,000 to 1,000,000 and a K value of 15 to 90 is preferred, while a composite of nonionic polyvinylpyrrolidone and PVA having an average molecular weight of 8,000 to 400,000 and a K value of 15 to 60 is more preferred.
[0017] In some embodiments, the aforementioned hydroxypropyl methylcellulose (HPMC) or / and hydroxyethyl cellulose (HEC) are synthetic or semi-synthetic inert viscoelastic polymers. By mixing and compounding with polyvinyl alcohol, it can play a protective role, thus promoting the film-forming properties of polyvinyl alcohol, reducing the amount of polyvinyl alcohol used, increasing the amount of surfactant used, improving the effective content in the concentrated performance of the product, and achieving the purpose of obtaining good cleaning effect with a small amount of product.
[0018] In some embodiments, the surfactant is a combination of one or two of an anionic surfactant and a nonionic surfactant.
[0019] In some embodiments, the surfactant is a composition comprising an anionic surfactant and a nonionic surfactant in a weight ratio of 10:1 to 10:6.
[0020] In some embodiments, the anionic surfactant may be selected from sulfate compounds obtained by sulfated olefins, such as alkylbenzenesulfonates and α-alkene sulfonates, and non-alkoxylated linear or branched alkyl (C6-C20) sulfates obtained by directly sulfating fatty acids and neutralizing them with alkali, such as dodecylbenzenesulfonate (LAS), α-olefinsulfonate (AOS), dodecyl sulfate (SLS), secondary alkane sulfonate (SAS) and fatty acid methyl ester sulfonate (MES), and may be selected from linear or branched (C6-C20) alkyl alkoxylated sulfates having a weight average alkoxylation degree ranging from 0.1 to 10, preferably linear or branched (C10-C16) alkyl ethoxylated sulfates having a degree of heavy homoalkoxylation ranging from about 1 to about 5, such as, but not limited to, dodecyl polyether sulfate (AES).
[0021] In some embodiments, the nonionic surfactant may be selected from alkyl alkoxylated alcohols (C6-C20) with a weight average degree of alkoxylation ranging from 5 to 15, including fatty alcohols, isomeric alcohol ethoxylates, polyoxyethylene ethers, alkylphenol ethoxylates, fatty acid polyoxyvinyl esters, oil ethoxylates, alkanol ethoxylates, ethylene oxide, propylene oxide, polyethers, polyol ester ethers, etc. Representative examples include, but are not limited to, fatty acid alcohol ethoxylates, polyoxyethylene alkyl phenyl ethers, polyoxyethylene alkyl ethers, polyoxyethylene polyoxypropylene block copolymers, polyethylene glycol fatty acid esters, polyoxyethylene sorbitan fatty acid esters, cocamide monomethylamine, cocamide dimethylamine, cocamide monoethanolamine, cocamide diethanolamine, fatty acid alkyl olamides, alkyl polyglucosides, methyl polyvinyl ethers, glucoside polyoxylates, fatty acid methyl ester ethoxylates, etc.
[0022] In some embodiments, the enzyme preparation is one or more selected from the group consisting of proteases, amylases, lipases, cellulases, mannanases, pectin lyases, papain, oxidoreductases, and glycohydrolases.
[0023] In some examples, the enzyme formulation may be a commercially available solid enzyme formulation such as solid phase isozymes from KDN Biotech Group (catalog number DX01: a complex of protease and cellulase), solid phase protease (catalog number 12.0T), solid phase cellulase (catalog number C2000), and solid phase cellulase from Novozymes (catalog number Careayme Premium 5000T, catalog number Celluclean 4500T, catalog number Celluclean 4500T), solid phase amylase (catalog number Stainzyme Plus Evity 12T), Savinase series of solid phase proteases (Savinase4.0T / Savinase6.0T / Savinase8.0T / Savinase12T / Savinase24T).
[0024] The enzyme preparation may be, for example, but is not limited to, alkaline protease coated particles and preparation methods thereof disclosed in Chinese Patent Publication No. CN102533708A, and enzyme particles prepared in a granular enzyme composition disclosed in Chinese Patent Publication No. CN105283534A.
[0025] In some embodiments, the particles of the enzyme preparation have an average particle size of 0.01 mm to 3.0 mm.
[0026] In some embodiments, the particles of the enzyme formulation have an average particle size of 0.05 mm to 2.8 mm, 0.1 mm to 2.5 mm, 0.1 mm to 2.0 mm, 0.5 mm to 2.0 mm, 1 mm to 2.0 mm, or 1.5 mm to 1.8 mm, including, but not limited to, any value and range therein.
[0027] In some embodiments, the fabric softener formulation comprises one or more of a cationic fabric softener, an anionic fabric softener, a nonionic fabric softener, an amphoteric quaternary ammonium salt fabric softener, a silicone fabric softener, polyethylene glycol / polypropylene glycol, and a molding aid.
[0028] In some embodiments, the particles of the fabric softener formulation have an average particle size of 0.01 mm to 3.0 mm.
[0029] In some embodiments, the particles of the fabric softener formulation have an average particle size of 0.05 mm to 2.8 mm, 0.1 mm to 2.5 mm, 0.1 mm to 2.0 mm, 0.5 mm to 2.0 mm, 1 mm to 2.0 mm, or 1.5 mm to 1.8 mm, including, but not limited to, any value and range therein.
[0030] In some embodiments, the fabric softener formulation comprises a cationic fabric softener, a polyethylene glycol / polypropylene glycol, and a molding aid.
[0031] In some embodiments, the fabric softener formulation comprises a cationic fabric softener, a silicone fabric softener, a polyethylene glycol / polypropylene glycol, and a molding aid.
[0032] In some embodiments, the softener formulation contains a cationic softener, a natural or synthetic cationic cellulose polymer softener, polyethylene glycol / polypropylene glycol, and a molding aid. The cationic softener may be one or more selected from alkyl dimethyl ammonium chloride, alkyl imidazoline salt, alkyl amide quaternary ammonium salt, and ester quaternary ammonium compound. The natural or synthetic cationic cellulose polymer softener is one or more selected from guar hydroxypropyltrimonium chloride, hydroxypropyl guar hydroxypropyltrimonium chloride, chitosan, polyquaternary ammonium salt-10, polyquaternary ammonium salt-6, polyquaternary ammonium salt-7, polyquaternary ammonium salt-39, and polyquaternary ammonium salt-6. Here, the polyquaternary ammonium salt series is preferably polyquaternary ammonium salt-10.
[0033] In some embodiments, the silicone softener is selected from one or more of dimethylsiloxane, polydimethylsiloxane, amino-modified polyorganosiloxane, polyether-modified siloxane, aminopolyether-modified siloxane, aminopolyether-modified siloxane, epoxypolyether-modified polysiloxane, and linear block polypolyether-modified siloxane.
[0034] In some embodiments, the shaping aid may be a water-soluble organic material, an insoluble organic material, an inorganic salt, etc. Specifically, the shaping aid is selected from one or more of bentonite, kaolin, sodium sulfate, neutral sodium silicate, sodium pyrophosphate, sodium borate, talc, silicon dioxide, 4A zeolite, and starch, cellulose, dextrin, and polysaccharides.
[0035] In some embodiments, the weight average molecular weight of the polyethylene glycol / polypropylene glycol is between 2,000 and 20,000.
[0036] In some embodiments, the weight average molecular weight of the polyethylene glycol / polypropylene glycol is from 3,000 to 20,000, 4,000 to 18,000, 5,000 to 15,000, 6,000 to 13,000, 7,000 to 12,000, 8,000 to 11,000, 9,000 to 10,000, including any value and range therebetween.
[0037] In some embodiments, the particles of the fabric softener formulation include: 3 to 60 parts by weight of polyethylene glycol / polypropylene glycol; 1 to 60 parts by weight of a cationic softener; or / and 1 to 10 parts by weight of a silicone softener; 1 to 90 parts by weight of bentonite; 1 to 50 parts by weight of starch; and 1 to 10 parts by weight of dextrin.
[0038] In some embodiments, the process may be selected from, but is not limited to, fluidized bed spray drying, pressure spray drying, pneumatic spray drying, vertical scraper film drying, turbulent tube drying, horizontal scraper film flash drying, and rotary drum drying.
[0039] In some embodiments, the foam booster formulation is selected from a mixture of anionic surfactants, zwitterionic surfactants, nonionic surfactants, and water, and more particularly, the foam booster formulation is a mixture of at least one of potassium lauryl alkanoate, triethanolamine salt of dodecylbenzenesulfonic acid, sodium laureth sulfate, polyoxyethylene alkyl ether phosphate triethanolamine salt, alkyl glycosides with carbon chains distributed in the range of (C8-C16), alkanolamides (C10-C16), fatty acid monoethanolamides and diethanolamides, cocamidopropyl hydroxysultaine, sodium alkylamide amphoacetate, and olefin (C12-C16) sulfonate with deionized or distilled water, and has a conductivity of <10 μs / cm.
[0040] In some embodiments, the foam booster formulation comprises: 1 to 4 parts by weight of potassium lauryl alkylate; 6 to 14 parts by weight of dodecylbenzenesulfonic acid TEA salt; 2 to 8 parts by weight of an olefin (C12-C16) sulfonate; 5 to 11 parts by weight of polyoxyethylene alkyl ether phosphate ester salt triethanolamine salt; 6 to 14 parts by weight of an alkyl glycoside; 2 to 6 parts by weight of cocamidopropyl hydroxysultaine, and 30 to 90 parts by weight of deionized water.
[0041] In some embodiments, the foam booster formulation can be prepared by the following method: 60.5 parts by weight of deionized water / distilled water is added to a stirring vessel, and 2.5 parts by weight of potassium lauryl alkylate, 10 parts by weight of TEA salt of dodecylbenzenesulfonic acid, 5 parts by weight of olefin (C12-C16) sulfonic acid, 8 parts by weight of polyoxyethylene alkyl ether phosphate triethanolamine salt, 10 parts by weight of alkyl (C12-C16) glycoside, and 4 parts by weight of cocamidopropyl hydroxysulfobetaine are added in sequence, and stirred uniformly to dissolve, to obtain a foam booster formulation.
[0042] In some embodiments, the detergent tablet further contains one or more of dye inhibitors, fragrance essences, glycerin, propylene glycol, butylene glycol, pentylene glycol, mannitol, hydroxyethyl urea, glyceryl glucoside, tetrasodium glutamic acid diacetate, sodium bicarbonate, sodium iminodisuccinate, sodium polyaspartate, sodium polyepoxysuccinate, and trisodium methylglycine diacetate.
[0043] In some embodiments, the dye inhibitor is one or more selected from cationic dye inhibitors, nonionic dye inhibitors, and inorganic salt dye fixing agents. Specifically, the dye inhibitor is one or more of cationic dye inhibitors of imidazoline type, quaternary ammonium salt type, aliphatic polyamine derivatives, inorganic salts (e.g., bentonite) and celluloses, and nonionic dye inhibitors of polyvinylpyrrolidone, modified vinylpyrrolidone / vinimidazole copolymers. Preferably, the dye inhibitor is a mixture of polyvinylpyrrolidone and one or more of modified vinylpyrrolidone / vinimidazole copolymer, aliphatic polyamine derivative, and polyquaternary ammonium salt cellulose. More preferably, the dye inhibitor is a combination of polyvinylpyrrolidone and modified vinylpyrrolidone / vinimidazole copolymer (10:1-10).
[0044] In some embodiments, the detergent tablet further comprises a foaming accelerator with foaming function, which may be selected from inorganic foaming accelerators and organic foaming accelerators. The inorganic foaming accelerator may be any one or two mixtures of sodium carbonate and sodium bicarbonate.
[0045] In some examples, the enzyme preparations and fabric softener preparation particles of the present invention may appear as spheres, rods, plates, tubes, squares, rectangles, disks, stars, or thin slices of regular or irregular shapes.
[0046] In a second aspect, a method for preparing a detergent tablet is provided herein, comprising the steps of: 1) dissolving a water-soluble polymer in deionized water to be used as a solution of a film-forming sheet material for the manufacture of a tablet-type detergent; 2) adding surfactant, foaming agent, and / or molding aid in sequence, stirring and mixing uniformly, and then heating and drying to obtain a semi-solid sheet material; 3) distributing the enzyme preparation and the fabric softener preparation in solid particle form onto the semi-solid sheet material prepared in step 2) while continuously heating, drying and shaping to obtain a detergent tablet.
[0047] In summary, the present application includes at least one of the following beneficial technical effects: 1. The tablet detergent of the present application has a high content of enzyme preparations and fabric softener preparations, and has obvious advantages in cleaning power and static electricity removal ability. Due to the high enzyme content, it has excellent cleaning effect on proteins, milk scum, and blood stains that are difficult to remove in daily life, and can be used not only for clothes but also for washing dishes in a dishwasher. Due to the high content of fabric softener preparations, the tablet detergent of the present application can simultaneously achieve the dual effects of washing and softening clothes.
[0048] 2. This application uses a solid enzyme preparation that is not easily volatile and has stable performance characteristics. The solid enzyme preparation and the covered fabric softener component are added to the tablet-type detergent that is continuously dried by the mechanical device, so that the solid enzyme preparation and the covered fabric softener component can be added in the maximum amount at the same time as they are dried, so that the stability of the tablet-type detergent is not affected by temperature and humidity. This allows the solid enzyme preparation and the solid fabric softener preparation to be stably adsorbed by the dried tablet and meets the requirements for plastic-free packaging, reducing plastic pollution and making the product more in line with the requirements for environmental protection. In addition, the amount of the solid enzyme preparation and the covered solid fabric softener preparation can be flexibly controlled by adjusting the mechanical speed through frequency conversion, and the amount of addition can be flexibly set according to the object to be washed, making it suitable for large-scale production.
[0049] 3. The use of the combination of foam booster formulation and detergent ingredients increases the volume of the slurry during the tablet production process, reduces the density, makes the weight lighter, and the internal structure of the slurry becomes loose. The tablet detergent slurry can be dried quickly during the tablet production process, so that the effect of drying temperature on the stability of the solid enzyme formulation and the covered solid softener formulation is reduced and avoided. At the same time, the low density, light weight, and loose internal structure of the slurry not only makes it easy to add a large amount of enzyme formulation components to the continuously drying slurry, but also makes the solid enzyme formulation and solid softener formulation more firmly adsorbed by the sheet material after the moisture continues to evaporate, and is not easy to fall off, forming a stable detergent sheet material with strong cleaning power and softening ability.
[0050] 4. By simultaneously utilizing the properties of the foam booster formulation and the foaming agent to loosen the internal structure of the slurry, the molecular chains of the water-soluble polymer that forms the film are easily broken or easily unraveled in the slurry containing water, so that even when an auxiliary is added to the composition of the cleaning functional sheet material, the stability and non-shedding of the components of the cleaning particle composition and the solid-phase softener formulation are not affected. At the same time, the addition of the auxiliary not only makes the slurry easier to dry, but also helps to reduce the moisture content of the dried cleaning sheet material, and the low moisture content also helps to improve the storage stability of the tablet-type detergent.
[0051] 5. By utilizing the high molecular weight characteristics of polyethylene glycol / polypropylene glycol, the polyethylene glycol / polypropylene glycol and the covered cationic softener ingredient are slowly dissolved. Therefore, the interaction with the strong anionic detergent ingredient due to electrostatic adsorption and precipitation with each other in the first washing process is avoided. After the tablet containing the anionic detergent ingredient and the solid-phase enzyme preparation are first dissolved in the laundry, the polyethylene glycol / polypropylene glycol and the covered cationic softener ingredient begin to dissolve in the rinsing process, releasing the cationic softener ingredient to contact with the clothes. Not only can it quickly neutralize the anionic detergent residue on the clothes, but it can also quickly restore the softener to the clothes washed with the detergent. The effects of washing, cleaning, protecting and softening the clothes can be truly obtained. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0052] The technical solution of the present disclosure is described in further detail below with reference to the accompanying drawings and examples. The examples do not limit the present application, but are merely used to interpret the present application.
[0053] Unless otherwise stated, materials used in the examples are commercially available. If specific operational steps, experimental conditions, instruments or devices used are not shown in the examples, those skilled in the art can carry out operational steps, experimental conditions, instruments or devices routinely used in the art and are within the scope of this application.
[0054] Preparation Example Enzyme preparation particles The enzyme preparations used in the examples and comparative examples of this application are: Enzyme preparation A: solid-phase isozyme from KDN Biotech Group, catalog number DX01, which is a complex of protease and cellulase; Enzyme preparation B: solid-phase cellulase from Novozymes, catalog number: solid-phase protease Savinase 8.0T.
[0055] Preparation of fabric softener particles The preparation method of the softener preparation particles adopted in the examples and comparative examples of this application is as follows: add 40 kg of polyethylene glycol / polypropylene glycol into a heating and stirring kettle, heat it to a liquid state, add 40 kg of cationic softener and 5 kg of silicone softener, 45 kg of bentonite, 25 kg of starch, and 5 kg of dextrin in sequence, stir and mix uniformly, and obtain an irregular solid-phase softener preparation by extrusion cooling or spray drying.
[0056] Preparation of Foam Booster Formulation The foam booster preparation used in the examples and comparative examples of this application is prepared as follows: 60.5 kg of deionized water / distilled water is added to a stirring kettle, and 2.5 kg of potassium lauryl alkylate, 10 kg of TEA salt of dodecylbenzenesulfonic acid, 5 kg of olefin (C12-C16) sulfonic acid, 8 kg of polyoxyethylene alkyl ether phosphate triethanolamine salt, 10 kg of alkyl (C12-C16) glycoside, and 4 kg of cocamidopropyl hydroxysulfobetaine are added in sequence, and stirred and dissolved uniformly to obtain the foam booster preparation.
[0057] Working Example Example 1 The tablet detergent provided in this embodiment is It contains 8 kg of water-soluble polymers (specifically, 6 kg of PVA, 1 kg of PVP, and 1 kg of HPMC), 14 kg of surfactants (specifically, 12 kg of SDS and 2 kg of fatty alcohol polyoxyethylene ether AEO9), 2 kg of enzyme preparation, 2 kg of fabric softener preparation, 1 kg of foam booster preparation, 5 kg of molding aids, 0.1 kg of dye inhibitors, 1 kg of tetrasodium glutamic acid diacetate, 0.2 kg of fragrance essence, 0.2 kg of sodium bicarbonate, and 3 kg of glycerin.
[0058] The method for preparing the detergent tablets according to this embodiment is as follows. 1) Dissolve 8 kg of water-soluble polymer in 50 kg of deionized water, heat to 80℃-90℃, and stir uniformly to prepare a film-forming sheet material solution for tablet detergent. 2) 14 kg of surfactant, 1 kg of foam booster formulation component, 5 kg of molding aid (specifically starch / bentonite), 0.1 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.2 kg of fragrance essence, 0.2 kg of sodium bicarbonate, and 3 kg of glycerin are added in sequence, stirred and mixed uniformly, heated and dried to obtain a semi-solid sheet material. 3) 2 kg of the enzyme preparation in solid particle form prepared in Preparation Example and 2 kg of the fabric softener preparation in solid particle form are distributed onto the semi-solid sheet material prepared in 2) which is being continuously heated, and then dried and molded to obtain tablet-type detergent.
[0059] Examples 2 to 8 The detergent tablets of Examples 2 to 8 are prepared according to the composition of each detergent tablet of Table 1 and the method disclosed in Example 1.
[0060] Comparative Examples 1 to 2 and 5 to 6 According to the composition of each comparative example of detergent tablet in Table 2, the detergent tablets of Comparative Examples 1 to 2 and 5 to 6 are prepared according to the method disclosed in Example 1.
[0061] Comparative Example 3 The content of each component in this comparative example is shown in Table 2.
[0062] The method for preparing the tablet detergent according to this comparative example is as follows. 1) 29.5 kg of water-soluble polymer is dissolved in 60 kg of deionized water, heated to 80 to 90°C, stirred uniformly, and used as a solution of film-forming sheet material for manufacturing tablet-type detergent. 2) 39 kg of surfactant, 1 kg of foam booster formulation component, 10 kg of molding aid (especially starch / bentonite), 0.6 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.5 kg of fragrance essence, 0.7 kg of sodium bicarbonate, and 5 kg of glycerin are added in sequence, stirred and mixed uniformly, heated and dried to obtain a semi-solid sheet material. 3) 5 kg of the softener formulation in solid particle form is distributed onto a semi-solid sheet material which is continuously heated, dried and molded to obtain a solid sheet material. 4) Add 5 kg of fabric softener preparation to a mixture of an appropriate amount of glycerin and propylene glycol to dissolve, and stir thoroughly and uniformly to obtain a solution of enzyme preparation. Spray the solution of enzyme preparation onto a solid sheet material to obtain the tablet-type detergent.
[0063] Comparative Example 4 The content of each component in this comparative example is shown in Table 2.
[0064] The method for preparing the tablet detergent according to this comparative example is as follows. 1) 29.5 kg of water-soluble polymer is dissolved in 60 kg of deionized water, heated to 80 to 90°C, stirred uniformly, and used as a solution of film-forming sheet material for manufacturing tablet-type detergent. 2) Add 25 kg of the enzyme preparation to the water and dissolve it, then stir thoroughly and uniformly to obtain a solution of the enzyme preparation. 3) The solution of the enzyme preparation prepared in 2) is added to the solution of the film-forming sheet material prepared in 1), and 39 kg of surfactant, 1 kg of foaming agent preparation component, 10 kg of molding aid (specifically starch / bentonite), 0.6 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.5 kg of fragrance essence, 0.7 kg of sodium bicarbonate, and 5 kg of glycerin are added in sequence, stirred and mixed uniformly, heated and dried to obtain a semi-solid sheet material. 3) 5 kg of the fabric softener formulation in the form of solid particles is distributed onto the semi-solid sheet material prepared in 2) which is continuously heated, dried and molded to obtain the tablet-type detergent.
[0065] Comparative Example 7 The content of each component in this comparative example is shown in Table 2.
[0066] The method for preparing the tablet detergent according to this comparative example is as follows. 1) 29.5 kg of water-soluble polymer is dissolved in 60 kg of deionized water, heated to 80 to 90°C, stirred uniformly, and used as a solution of film-forming sheet material for manufacturing tablet-type detergent. 2) 39 kg of surfactant, 1 kg of foam booster formulation component, 10 kg of molding aid (especially starch / bentonite), 0.6 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.5 kg of fragrance essence, 0.7 kg of sodium bicarbonate, and 5 kg of glycerin are added in sequence, stirred and mixed uniformly, heated and dried to obtain a semi-solid sheet material. 3) 25 kg of the enzyme preparation in the form of solid particles is distributed onto a semi-solid sheet material which is continuously heated, dried, molded and released to obtain a solid sheet material. 4) Add 5 kg of fabric softener preparation to the mixture of appropriate amount of glycerin, propylene glycol, and dissolve, and stir thoroughly and uniformly to obtain a solution of fabric softener preparation, and spray the solution of fabric softener preparation onto the solid sheet material to obtain the tablet-type detergent.
[0067] Comparative Example 8 The content of each component in this comparative example is shown in Table 2.
[0068] The method for preparing the tablet detergent according to this comparative example is as follows. 1) 29.5 kg of water-soluble polymer is dissolved in 60 kg of deionized water, heated to 80 to 90°C, stirred uniformly, and used as a solution of film-forming sheet material for manufacturing tablet-type detergent. 2) Add 5 kg of fabric softener preparation to water and dissolve, then stir thoroughly and uniformly to obtain a solution of fabric softener preparation. 3) The solution of the fabric softener preparation prepared in 2) is added to the solution of the film-forming sheet material prepared in 1), and 39 kg of surfactant, 1 kg of foam booster preparation components, 10 kg of molding aids (specifically starch / bentonite), 0.6 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.5 kg of fragrance essence, 0.7 kg of sodium bicarbonate, and 5 kg of glycerin are added in sequence, stirred and mixed uniformly, heated and dried to obtain a semi-solid sheet material. 4) 25 kg of the fabric softener formulation in the form of solid particles is distributed onto the semi-solid sheet material prepared in 2) which is continuously heated, dried and molded to obtain the tablet-type detergent.
[0069] Comparative Example 9 The content of each component in this comparative example is shown in Table 2. According to the method disclosed in Example 1, the tablet-type detergent of this comparative example is prepared.
[0070] Comparative Example 10 The content of each component in this comparative example is shown in Table 2.
[0071] The method for preparing the tablet detergent according to this comparative example is as follows. 1) 29.5 kg of water-soluble polymer is dissolved in 60 kg of deionized water, heated to 80 to 90°C, stirred uniformly, and used as a solution of film-forming sheet material for manufacturing tablet-type detergent. 2) 39 kg of surfactant, 1 kg of foam booster formulation components, 10 kg of molding aids (specifically starch / bentonite), 0.6 kg of dye inhibitor, 1 kg of tetrasodium glutamate diacetate, 0.5 kg of fragrance essence, 0.7 kg of sodium bicarbonate, and 5 kg of glycerin are added in sequence, stirred and mixed evenly, and 25 kg of a solid particle form enzyme formulation and 25 kg of a solid particle form softener formulation are added in sequence, stirred evenly, heated and dried to obtain a semi-solid sheet material.
[0072] Table 1. Composition of detergent tablets in Examples 1 to 8 [Table 1]
[0073] Table 2. Compositions of tablet detergents in Comparative Examples 1 to 10 [Table 2]
[0074] Performance test experiment 1. Stability of enzyme preparation particles and fabric softener preparation particles: After placing the tablet detergent in a test environment with a temperature of (25±2)℃ and humidity of (40±5)% for 48 hours, the tablet detergent was picked up by hand, turned over and rubbed appropriately to observe whether the enzyme preparation particles and fabric softener preparation particles on the tablet detergent fell off. The results are shown in Table 3.
[0075] 2. Moisture resistance and stability: Two tablets of detergent are stacked and placed in a test environment with a temperature of (25±2)℃ and humidity of (85±5)% for 24 hours. Then, the two tablets are separated to observe whether there is any adhesion between the tablets. The adhesion phenomenon can be divided into no adhesion, slight adhesion, and obvious adhesion. The results are shown in Table 3.
[0076] 3. Detergency test: According to the evaluation method of GB / T13174-2021 "Detergency and Circulation Washing Performance of Laundry Detergent", combined with the evaluation criteria of QB / T1224-2012 "Liquid Laundry Detergent", the test concentration of standard liquid detergent is 0.2%, and the test concentration of the sample is 0.013% (the test concentration is 1 / 15 of the standard liquid detergent).
[0077] 3.1 Whiteness measurement: The JB-01 soiled cloth, JB-02 soiled cloth, and JB-03 soiled cloth were cut into 6 cm × 6 cm size and combined into six groups with approximately the same average blackness for each type, and the samples from each group were used for the performance test of the same sample.
[0078] Using a whiteness meter, the whiteness values were read at 457 nm before and after cleaning, one by one. Before cleaning, two points were taken on the front and back of the sample (the two points on each side must be symmetrical in the center), and the whiteness values were measured, and the average value of the four measurements was taken as the whiteness F1 of the sample before cleaning. After cleaning, two points were taken on the front and back of the sample (the two points on each side must be symmetrical in the center), and the whiteness values were measured, and the average value of the four measurements was taken as the whiteness F2 of the sample after cleaning.
[0079] The whiteness difference (F2-F1) of each sample before and after washing was calculated in a one-to-one correspondence manner, and the cleaning power was calculated separately for each sample group. According to the types of soiled fabric samples, the cleaning value R and cleaning ratio P of detergent for different types of soiled fabrics were determined, and the method is as follows:
[0080] 3.2 Calculation of cleaning value of soiled cloth The cleaning value of a certain type of soiled cloth is Ri=Σ(F2i-F1i) / n In the formula: i is the i-th type of soiled cloth sample, F1i is the spectral reflectance of the i-th type of soiled fabric sample before washing, %, F2i is the spectral reflectance of the i-th type of soiled fabric sample after washing, %, n is the effective content of each group of soiled fabric samples. The result is kept to one decimal place.
[0081] 3.3 Calculation of cleaning ratio for soiled cloth The cleaning ratio Pi=R3i / R0i for the i-th type of soiled cloth for a standard liquid detergent. In the formula, R0i is the cleaning value of standard liquid detergent, %, R3i is the cleaning value of the sample. The result is kept to one decimal place.
[0082] 3.4 Judging the cleaning power of detergents If Pi≧1.0, the judgment conclusion is “the cleaning power of the sample on the i-th type of soiled fabric is equal to or greater than that of the standard liquid detergent”, which is abbreviated as “cleaning power on the i-th type of soiled fabric is pass”.
[0083] If Pi<1.0, the judgment conclusion is "the cleaning power of the sample on the i-th type of soiled fabric is inferior to that of the standard liquid detergent", which is abbreviated as "the cleaning power on the i-th type of soiled fabric fails". The results are shown in Table 4.
[0084] 4. Antistatic performance test: According to QB / T4535-2013 fabric softener standard, the antistatic property of the tablet detergent is tested, and the surface resistivity logarithmic difference meter △lgρs ≧ 2.5 is passed. The results are shown in Table 4.
[0085] Table 3. Particle stability and humidity stability test results for tablet detergents prepared in the Examples and Comparative Examples [Table 3]
[0086] Table 4. Detergency and antistatic performance test results of tablet detergents prepared in the Examples and Comparative Examples [Table 4]
[0087] From the data in Table 4, it can be seen that with the increase in the content of the enzyme preparation, the cleaning ratios for JB-01-stained cloth, JB-02-stained cloth, and JB-03-stained cloth gradually increased, and the cleaning performance gradually improved. In Comparative Example 2, the content of the enzyme preparation was relatively large (70 kg), but compared with Example 8 (enzyme preparation content of 50 kg), the improvement in cleaning effect was not obvious. When the amount of enzyme preparation added was in the range of 0.1 to 50 kg, the cleaning effect increased with the content of the enzyme preparation, and the improvement in cleaning effect was obvious, and especially in the case of JB-02-stained cloth with a large amount of protein stains, the content of the enzyme preparation had a more significant effect on the cleaning power.
[0088] In Comparative Example 3, the enzyme preparation is prepared in a liquid form and then sprayed onto the solid detergent tablet. The cleaning ratio is only 2.52 for JB-02 soiled fabric, but the cleaning ratio is 3.95 for JB-02 soiled fabric in Example 1, which contains the same enzyme preparation content, and the cleaning effect is much worse than that of the detergent tablet using the enzyme preparation in particulate form. This is because the exposed liquid enzyme preparation is easily affected by the surrounding temperature and humidity, which affects the cleaning effect. In Comparative Example 4, the enzyme preparation in liquid form is directly mixed with other components of the detergent tablet, dried and molded, and the cleaning ratio is only 2.21 for JB-02 soiled fabric, but the cleaning ratio is 3.95 for JB-02 soiled fabric in Example 1, which contains the same enzyme preparation content, and the cleaning effect is much worse than that of the detergent tablet using the enzyme preparation in particulate form. This is because the liquid enzyme preparation is directly incorporated into the detergent tablet, and the enzyme is partially inactivated by the drying and molding process of the detergent tablet, which impairs the cleaning power of the detergent tablet.
[0089] In Comparative Examples 3 to 4, the enzyme preparation in liquid form was incorporated, and showed obvious adhesion in the stability tests of 24-hour humidity resistance and 48-hour humidity resistance. The stability performance of the tablet-type detergents in Examples 1 to 8 is all good.
[0090] As can be seen from the data in Table 4, the antistatic properties of the fabrics washed with the tablet detergent gradually increase with increasing content of fabric softener formulation. In Comparative Example 6, the amount of fabric softener particles is high (70 kg), and the antistatic properties are not significantly improved compared to the addition of 50 kg of fabric softener formulation in Example 7.
[0091] In Comparative Example 7, the softener is sprayed onto the semi-solid detergent tablet in liquid form, and as can be seen from the data in Table 4, the antistatic property of the fabric washed with the detergent tablet of Comparative Example 7 is only 2.0. Also, the detergency of the detergent tablet of Comparative Example 7 is significantly weaker than that of the detergent tablet containing the same amount of fabric softener formulation in Example 1. In Comparative Example 8, the softener is directly added in liquid form together with other ingredients, and as can be seen from the data in Table 4, the antistatic property of the fabric washed with the detergent tablet of Comparative Example 8 is only 2.0, which is unacceptable. Also, the detergency of the detergent tablet of Comparative Example 8 is significantly weaker than that of the detergent tablet containing the same amount of fabric softener formulation in Example 1. This is because the surfactants used in the examples of this application are anionic and nonionic surfactants, and the softener used contains a cationic surfactant. When the fabric softener formulation is incorporated by spraying or by directly mixing with other components of the tablet-type detergent, the fabric softener formulation may come into direct contact with the surfactant, and the cationic and anionic surfactants may electrostatically adsorb and precipitate, weakening the effectiveness of both. In Example 1, the high molecular weight characteristics of polyethylene glycol / polypropylene glycol are used to slowly dissolve the cationic fabric softener component coated with polyethylene glycol / polypropylene glycol. Thus, the interaction with the strong anionic detergent component due to electrostatic adsorption and precipitation with each other in the first washing step is avoided. After the tablet containing the anionic detergent component and the solid enzyme preparation are first dissolved in the laundry, the cationic fabric softener component coated with polyethylene glycol / polypropylene glycol begins to dissolve in the rinsing step, releasing the cationic fabric softener component to contact the clothes. Not only can it quickly neutralize the anionic detergent residue on the clothes, but it can also quickly restore the fabric softener on the clothes washed with the detergent. The effects of washing, cleaning, protecting and softening the clothes can be truly obtained.
[0092] In Comparative Examples 7 to 8, a liquid fabric softener formulation was incorporated, and in the stability test, clear adhesion was observed in the 24-hour humidity stability and 48-hour humidity stability tests.
[0093] In Comparative Example 9, no foam booster is added, and the overall structure of the tablet detergent is relatively compact and not loose enough, so that a large number of enzyme preparation particles and softener particles fall off, and the detergency and antistatic properties are much weaker than those of Example 5, which contains a foam booster but has the same other composition. This is because the foam booster loosens the internal structure of the slurry, making the molecular chains of the water-soluble polymer that forms the film easily break or easily break apart in the slurry containing water, so that even when an auxiliary is added to the tablet detergent composition, it does not affect the stability and non-falling of the components of the cleaning particle composition and the solid softener formulation.
[0094] In Comparative Example 10, the enzyme preparation particles and the fabric softener preparation particles were directly mixed with other components of the tablet detergent to prepare a tablet detergent in which the enzyme preparation particles and the fabric softener preparation particles were completely embedded in the tablet detergent. The composition of the tablet detergent in Comparative Example 10 is exactly the same as that in Example 5, and the only difference is the position of the enzyme preparation particles and the fabric softener preparation particles in the tablet detergent. In Example 5, the particles are embedded on the tablet detergent, and in Comparative Example 10, the particles are uniformly embedded inside the tablet detergent. From the test results of the cleaning power and antistatic performance in Table 4, it can be seen that the cleaning power and antistatic performance of the tablet detergent in Comparative Example 10 are both poor. This is because the enzyme preparation particles and the fabric softener preparation particles are arranged on the surface of the tablet detergent, so that the particles come into contact with water more quickly and dissolve quickly, so that the cleaning effect and antistatic effect can be exerted more quickly. In Comparative Example 10, the particles are uniformly embedded in the detergent tablet, and the detergent tablet needs to be dissolved as a whole before releasing the enzyme and fabric softener particles, after which the enzyme and fabric softener particles come into contact with water to exert their cleaning and antistatic effects. In the quick mode of the washing machine, the advantage of the enzyme and fabric softener particles embedded in the detergent tablet is even more obvious.
[0095] It should be noted that the specific examples are merely an interpretation of the present application and are not limitations on the present application. After reading this specification, a person skilled in the art may, if necessary, modify the examples without inventive step, provided that such modifications are within the scope of the claims of the present application and are protected by the Patent Law.
Claims
1. In tablet detergents, 8 to 34 parts by weight of a water-soluble polymer; 14 to 50 parts by weight of a surfactant; 0.1 to 50 parts by weight of an enzyme preparation; 0.1 to 50 parts by weight of a fabric softener formulation; 1 to 10 parts by weight of a foam booster formulation; and 0 to 30 parts by weight of a molding aid; A detergent tablet, characterized in that the enzyme preparation and the fabric softener preparation are embedded in the detergent tablet in the form of solid particles.
2. 2. The tablet-type detergent according to claim 1, wherein the water-soluble polymer is one or more selected from the group consisting of polyvinyl alcohol, polyvinylpyrrolidone, gelatin, carrageenan, cross-linked polyacrylic acid, water-soluble polyacrylamide, polymers of vinyl acetate and vinyl alcohol, starch, dextrin, polysaccharides, cellulose, modified cellulose, and microcrystalline cellulose.
3. 2. The detergent tablet according to claim 1, wherein the surfactant is one or a combination of two of anionic surfactants and nonionic surfactants.
4. 2. The tablet-type detergent according to claim 1, wherein the enzyme preparation is one or more selected from the group consisting of protease, amylase, lipase, cellulase, mannanase, pectin lyase, papain, oxidoreductase, and carbohydrate hydrolase.
5. 2. The detergent tablet according to claim 1, wherein the average particle size of the enzyme preparation is from 0.01 mm to 3.0 mm.
6. 2. The tablet-type detergent according to claim 1, wherein the fabric softener formulation contains one or more of a cationic fabric softener, an anionic fabric softener, a nonionic fabric softener, an amphoteric quaternary ammonium salt fabric softener, and a silicone fabric softener, polyethylene glycol / polypropylene glycol, and a molding aid.
7. The fabric softener formulation comprises: 3 to 60 parts by weight of polyethylene glycol / polypropylene glycol; and / or 1 to 60 parts by weight of a cationic softener 1 to 10 parts by weight of a silicone softener; 1 to 90 parts by weight of bentonite; 1 to 50 parts by weight of starch; 2. The tablet-type detergent according to claim 1, further comprising 1 to 10 parts by weight of dextrin.
8. The foam booster formulation comprises: 1 to 4 parts by weight of potassium lauryl alkylate; 6 to 14 parts by weight of dodecylbenzenesulfonic acid TEA salt; 2 to 8 parts by weight of an olefin (C12-C16) sulfonate; 5 to 11 parts by weight of polyoxyethylene alkyl ether phosphate ester salt triethanolamine salt; 6 to 14 parts by weight of an alkyl glycoside; 2 to 6 parts by weight of cocamidopropyl hydroxysultaine, 2. The detergent tablet according to claim 1, further comprising 30 to 90 parts by weight of deionized water.
9. 2. The detergent tablet of claim 1, further comprising one or more of a dye inhibitor, a fragrance essence, glycerin, propylene glycol, butylene glycol, pentylene glycol, mannitol, hydroxyethyl urea, glyceryl glucoside, tetrasodium glutamic acid diacetate, sodium bicarbonate, sodium iminodisuccinate, sodium polyaspartate, sodium polyepoxysuccinate, and trisodium methylglycine diacetate.
10. 2. The tablet-type detergent according to claim 1, wherein the water-soluble polymer contains polyvinyl alcohol, polyvinylpyrrolidone, hydroxypropylmethylcellulose and / or hydroxyethylcellulose.
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