CN114555771A - Antimicrobial particles - Google Patents

Antimicrobial particles Download PDF

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CN114555771A
CN114555771A CN202080072719.XA CN202080072719A CN114555771A CN 114555771 A CN114555771 A CN 114555771A CN 202080072719 A CN202080072719 A CN 202080072719A CN 114555771 A CN114555771 A CN 114555771A
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antimicrobial
particles
particle
perfume
composition
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阿马尼·达阿里纳·萨拉姆
克里斯廷·莱得里克·威廉姆斯
黛博拉·勒让德
井川阳子
赵璞
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Procter and Gamble Co
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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
    • C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
    • 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
    • C11D3/2068—Ethers
    • 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
    • C11D3/24—Organic compounds containing halogen
    • 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
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3707—Polyethers, e.g. polyalkyleneoxides
    • 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
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/12—Soft surfaces, e.g. textile

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Emergency Medicine (AREA)
  • Toxicology (AREA)
  • Dentistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Detergent Compositions (AREA)
  • Accessory Of Washing/Drying Machine, Commercial Washing/Drying Machine, Other Washing/Drying Machine (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention provides a composition comprising a plurality of antimicrobial particles, each of the plurality of antimicrobial particles comprising: (a) from 25% to 99% by total weight of the particle of a water-soluble carrier; and (b) a diphenyl ether antimicrobial agent, wherein each particle of the plurality of particles has a mass of about 1mg to about 1 g. Preferably, each of the antimicrobial particles further comprises a perfume. More preferably, the composition is a particulate laundry detergent composition comprising the plurality of antimicrobial particles in combination with a detergent particle.

Description

Antimicrobial particles
Technical Field
(through-the-wash) laundry additive in a laundering process and fabric treatment compositions comprising the same.
Background
In addition to the originally intended function, consumer products have evolved to address the needs of users for antimicrobial benefits. For example, users desire antimicrobial laundry detergent products that have an antimicrobial benefit to fabrics while cleaning the fabrics. Currently, various antimicrobial agents (e.g., diphenyl ethers) are known for use in consumer product formulations to deliver antimicrobial effects.
However, in the context of laundry detergents, achieving the desired efficiency of antimicrobial agents on fabrics is challenging. Specifically, during the wash cycle, most of the active ingredients (including the incorporated antimicrobial agents) are eventually washed away with the wash solution. Thus, only a small amount of the antimicrobial agent released by the laundry detergent may deposit onto the washed fabric. To compensate for this low deposition rate of the antimicrobial agent, manufacturers would have to increase the concentration of the antimicrobial agent in the laundry detergent product, which not only results in increased costs, but also environmental problems due to the increased amount of antimicrobial agent washed off during the laundry washing process and released into the environment.
In addition, certain antimicrobial agents (e.g., diphenyl ethers) are known for use in liquid laundry detergent formulations to deliver antimicrobial effects. However, in the context of solid, granular laundry detergent products, it has been found that such diphenyl ether antimicrobials, especially 4-4' -dichloro-2-hydroxydiphenyl ether (commonly known as "Dichlosan" or its trade name ") when provided at the same concentration levels as in liquid laundry detergent products"
Figure BDA0003598477860000011
HP100 ", as commercially available from BASF) has disappointing poor antimicrobial efficacy. To compensate for such poor antimicrobial efficacy, it is desirable to provide such antimicrobial agents in granular laundry detergent products at concentration levels significantly higher than liquid laundry detergent products, so that they become too costly to use to be practical.
Accordingly, there is a continuing need to improve the delivery efficiency and deposition rate of antimicrobial agents during laundry washing processes in order to maintain or improve the overall antimicrobial effect while minimizing its cost and environmental impact.
Disclosure of Invention
The present invention provides a composition comprising a plurality of antimicrobial particles, each of the plurality of antimicrobial particles comprising: (a) from 25% to 99% by total weight of the particle of a water-soluble carrier; and (b) a diphenyl ether antimicrobial agent, wherein each antimicrobial particle of the plurality of antimicrobial particles has a mass of from about 1mg to about 1 g.
When provided with the same amount of antimicrobial agent, the antimicrobial particles of the present invention can exhibit higher antimicrobial efficacy when formulated into a powder or liquid laundry detergent product as compared to when added to the powder or liquid laundry detergent product. Without being bound by any theory, it is believed that such antimicrobial particles provide a controlled/sustained release of the antimicrobial agent into the wash liquor during the wash process. This controlled/sustained release is particularly advantageous when the pH of the wash liquor is low during the later stages of the laundry washing process and certain antimicrobial agents (e.g. especially 4-4' -dichloro-2-hydroxydiphenyl ether) exhibit better fabric deposition at lower pH.
In addition, such antimicrobial particles of the present invention provide greater dosing flexibility to achieve more effective antimicrobial agent delivery when provided as a stand-alone fabric treatment product. Consumers may choose to dose more or less antimicrobial agent as desired, independent of the surfactant or other detersive active in the laundry detergent product. Consumers may also choose to add the antimicrobial particles of the present invention at a particular stage of the washing process, for example after washing or during the rinse cycle, to increase the rate of deposition of such antimicrobial agents on fabrics.
Still further, such antimicrobial particles of the present invention can be readily incorporated into particulate laundry detergent compositions which also contain detergent particles. Particulate laundry detergent compositions typically have a significantly higher equilibrium pH than liquid laundry detergent compositions, and such high pH environments do not benefit from deposition of certain antimicrobial agents as mentioned above. To address this problem, granular laundry detergent compositions can be reformulated to lower the equilibrium pH, but the cost and complexity associated with such reformulation is significant. Thus, the antimicrobial particles of the present invention provide a simple and more cost-effective alternative solution. Without being bound by any theory, it is believed that the water soluble carrier in such antimicrobial particles serves to separate the antimicrobial agent from the high PH environment of typical granular laundry detergent products, thereby improving the deposition rate of such antimicrobial agents.
Still further, when such antimicrobial particles contain perfume ingredients therein, improved freshness benefits and better malodor control benefits are surprisingly observed. Without being bound by any theory, it is believed that the antimicrobial agent in such particles interacts with the perfume ingredients to improve the release profile and deposition of such perfume ingredients (especially perfume microcapsules) on fabrics.
These and other aspects of the invention will become more apparent upon reading the following detailed description of the invention.
Detailed Description
The features and advantages of various embodiments of the present invention will become apparent from the following description, which includes examples intended to give a broad representation of specific embodiments of the invention. Various modifications will be apparent to those skilled in the art from this description and from practice of the invention. The scope of the invention is not intended to be limited to the particular forms disclosed, and the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the claims.
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Rather, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".
As used herein, terms such as "a" and "an" when used in a claim are understood to mean one or more of what is claimed or described. The terms "comprising," "including," and "including" are intended to be non-limiting.
The term "antimicrobial particle" refers to a particle comprising one or more antimicrobial agents in a water-soluble carrier.
The term "aspect ratio" refers to the ratio of the longest dimension of a perfume particle to its shortest dimension. For example, when such perfume particles have a hemispherical or compressed hemispherical shape, the aspect ratio is the ratio between the diameter of the bottom of the perfume particle and its height.
The term "particulate laundry detergent composition" refers to solid powdered or particulate laundry detergent compositions, preferably free-flowing powdered or particulate laundry detergent compositions, such as all-purpose or heavy-duty detergents for fabrics, and laundry auxiliaries such as bleach actives, rinse aids, additives or pretreatment products.
The term "detergent particle" refers to a particle comprising one or more detersive actives such as surfactants, builders, bleach actives, enzymes, polymers, chelants, softeners, suds suppressors, suds boosters, brighteners, dye transfer inhibitors and the like. Preferably, such detergent particles comprise one or more surfactants, especially anionic surfactants and/or nonionic surfactants.
The term "consisting essentially of …" means that the composition contains less than about 10%, preferably less than about 5%, of ingredients other than those listed.
Furthermore, the term "substantially free of means that the indicated material is present in an amount of from 0 wt% to about 1 wt%, preferably from 0 wt% to about 0.5 wt%, more preferably from 0 wt% to about 0.2 wt%. The term "substantially free" means that the indicated material is present in an amount of 0 wt% to about 0.1 wt%, preferably 0 wt% to about 0.01 wt%, more preferably it is not present at analytically detectable levels.
As used herein, all concentrations and ratios are by weight unless otherwise specified. All temperatures herein are in degrees Celsius (. degree. C.) unless otherwise indicated. All conditions herein are at 20 ℃ and atmospheric pressure unless otherwise specifically indicated. All polymer molecular weights are determined as weight average molecular weights unless otherwise specifically indicated.
Antimicrobial particles
The compositions of the present invention comprise a plurality of antimicrobial particles, each of the plurality of antimicrobial particles comprising: (a) from about 25% to about 99%, by total weight of the particle, of a water-soluble carrier; and (b) a diphenyl ether antimicrobial agent, wherein each antimicrobial particle of the plurality of antimicrobial particles has a mass of from about 1mg to about 1 g.
Preferably, each antimicrobial particle of the plurality of antimicrobial particles comprises from about 0.01% to about 3%, preferably from about 0.02% to about 2%, more preferably from about 0.05% to about 1%, most preferably from about 0.1% to about 0.5%, by total weight of said each antimicrobial particle, of said diphenyl ether antimicrobial agent.
The diphenyl ether antimicrobial agents of the present invention may be halogenated or non-halogenated, but are preferably halogenated. In a preferred embodiment, the diphenyl ether antimicrobial agent is a hydroxydiphenyl ether of formula (I):
Figure BDA0003598477860000041
wherein:
each Y is independently selected from chlorine, bromine or fluorine, preferably chlorine or bromine, more preferably chlorine,
each Z is independently selected from SO2H、NO2Or C1-C4An alkyl group, a carboxyl group,
r is 0, 1,2 or 3, preferably 1 or 2,
o is 0, 1,2 or 3, preferably 0, 1 or 2,
p is 0, 1 or 2, preferably 0,
m is 1 or 2, preferably 1, and
n is 0 or 1, preferably 0.
In the definition of formula (I) above, 0 means absent. For example, when p is 0, then Z is absent in formula (I). Each Y and each Z may be the same or different. In one embodiment, o is 1, r is 2, and Y is chloro or bromo. This embodiment may be: one chlorine atom is bonded to the benzene ring, whereas the bromine atom and the other chlorine atom are bonded to the other benzene ring; or a bromine atom is bonded to a benzene ring, whereas two chlorine atoms are bonded to other benzene rings.
More preferably, the diphenyl ether antimicrobial agent is selected from the group consisting of 4-4 ' -dichloro-2-hydroxydiphenyl ether, 2,4,4 ' -trichloro-2 ' -hydroxydiphenyl ether, and combinations thereof. Most preferably, the diphenyl ether antimicrobial agent is more preferably 4-4' -dichloro-2-hydroxydiphenyl ether.
In addition to the diphenyl ether antimicrobial agents disclosed above, other antimicrobial agents may be present, provided that these are present in amounts that do not cause formulation instability. Among the further useful antimicrobial agents are chelating agents which are particularly useful for reducing the resistance of gram negative bacteria in hard water. Acidic biocides may also be present.
In addition to the diphenyl ether antimicrobial agent described above, each antimicrobial particle of the plurality of antimicrobial particles of the present invention further comprises from about 25% to about 99%, preferably from about 30% to about 95%, more preferably from about 40% to about 94%, most preferably from about 50% to about 93%, by total weight of said each antimicrobial particle, of said water-soluble carrier.
The water-soluble carrier can be a material that dissolves in the wash liquor in a short period of time, for example in less than about 10 minutes. The water soluble carrier may be selected from the group consisting of water soluble inorganic alkali metal salts, water soluble alkaline earth metal salts, water soluble organic alkali metal salts, water soluble organic alkaline earth metal salts, water soluble carbohydrates, water soluble silicates, water soluble ureas, and any combination thereof.
The alkali metal salt may, for example, be selected from the group consisting of lithium, sodium and potassium salts, and any combination thereof. Useful alkali metal salts can be selected, for example, from alkali metal fluorides, alkali metal chlorides, alkali metal bromides, alkali metal iodides, alkali metal sulfates, alkali metal hydrogen sulfates, alkali metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates, alkali metal carbonates, alkali metal monohydrogen carbonates, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbates, and combinations thereof.
The alkali metal salt may be selected from the group consisting of sodium fluoride, sodium chloride, sodium bromide, sodium iodide, sodium sulfate, sodium bisulfate, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium carbonate, sodium bicarbonate, sodium acetate, sodium citrate, sodium lactate, sodium tartrate, sodium silicate, sodium ascorbate, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, potassium sulfate, potassium bisulfate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, potassium carbonate, potassium monohydrogen carbonate, potassium acetate, potassium citrate, potassium lactate, potassium tartrate, potassium silicate, potassium, ascorbic acid, and combinations thereof.
The alkaline earth metal salt may be selected from magnesium salts, calcium salts, and the like, and combinations thereof. The alkaline earth metal salt may be selected from the group consisting of alkali metal fluorides, alkali metal chlorides, alkali metal bromides, alkali metal iodides, alkali metal sulfates, alkali metal hydrogen sulfates, alkali metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates, alkali metal carbonates, alkali metal monohydrogen carbonates, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbates, and combinations thereof. The alkaline earth metal salt may be selected from the group consisting of magnesium fluoride, magnesium chloride, magnesium bromide, magnesium iodide, magnesium sulfate, magnesium phosphate, magnesium monohydrogen phosphate, magnesium dihydrogen phosphate, magnesium carbonate, magnesium monohydrogen carbonate, magnesium acetate, magnesium citrate, magnesium lactate, magnesium tartrate, magnesium silicate, magnesium ascorbate, calcium fluoride, calcium chloride, calcium bromide, calcium iodide, calcium sulfate, calcium phosphate, calcium monohydrogen phosphate, calcium dihydrogen phosphate, calcium carbonate, monohydrogen carbonate, calcium acetate, calcium citrate, calcium lactate, calcium tartrate, calcium silicate, calcium ascorbate, and combinations thereof.
Inorganic salts, such as inorganic alkali metal salts and inorganic alkaline earth metal salts, do not contain carbon. Organic salts, such as organic alkali metal salts and organic alkaline earth metal salts, contain carbon. The organic salt may be an alkali metal salt or an alkaline earth metal salt of sorbic acid (i.e., an ascorbate salt). The sorbate salt can be selected from the group consisting of sodium sorbate, potassium sorbate, magnesium sorbate, calcium sorbate, and combinations thereof.
The water soluble carrier may be or comprise a material selected from: water-soluble inorganic alkali metal salts, water-soluble organic alkali metal salts, water-soluble inorganic alkaline earth metal salts, water-soluble organic alkaline earth metal salts, water-soluble carbohydrates, water-soluble silicates, water-soluble urea, and combinations thereof. The water soluble carrier may be selected from the group consisting of sodium chloride, potassium chloride, calcium chloride, magnesium chloride, sodium sulfate, potassium sulfate, magnesium sulfate, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium acetate, potassium acetate, sodium citrate, potassium citrate, sodium tartrate, potassium tartrate, sodium potassium tartrate, calcium lactate, water glass, sodium silicate, potassium silicate, dextrose, fructose, galactose, isomalt, glucose, sucrose, raffinose, isomalt, xylitol, fructoses, brown sugar, and combinations thereof. In one embodiment, the water soluble carrier may be sodium chloride. In one embodiment, the water soluble carrier may be common salt.
The water soluble carrier may be or comprise a material selected from: sodium bicarbonate, sodium sulfate, sodium carbonate, sodium formate, calcium formate, sodium chloride, sucrose, maltodextrin, corn syrup solids, corn starch, wheat starch, rice starch, potato starch, tapioca starch, clay, silicates, citric acid carboxymethylcellulose, fatty acids, fatty alcohols, diglycerides of hydrogenated tallow, glycerol, and combinations thereof.
The water soluble carrier may be selected from the group consisting of water soluble organic alkali metal salts, water soluble inorganic alkaline earth metal salts, water soluble organic alkaline earth metal salts, water soluble carbohydrates, water soluble silicates, water soluble urea, starch, clay, water insoluble silicates, citric acid carboxymethyl cellulose, fatty acids, fatty alcohols, diglycerides of hydrogenated tallow, glycerol, polyethylene glycols, and combinations thereof.
The water soluble carrier may be selected from disaccharides, polysaccharides, silicates, zeolites, carbonates, sulfates, citrates, and combinations thereof.
The water soluble carrier may be a water soluble polymer. The water-soluble polymer can be selected from polyvinyl alcohol (PVA), modified PVA; polyvinylpyrrolidone; PVA copolymers such as PVA/polyvinylpyrrolidone and PVA/polyvinylamine; partially hydrolyzed polyvinyl acetate; polyalkylene oxides such as ethylene oxide; polyethylene glycol; (ii) acrylamide; acrylic acid; cellulose, alkyl celluloses such as methyl cellulose, ethyl cellulose, and propyl cellulose; a cellulose ether; cellulose esters; a cellulose amide; polyvinyl acetate; polycarboxylic acids and salts; a polyamino acid or peptide; a polyamide; polyacrylamide; maleic/acrylic acid copolymers; polysaccharides, including starch, modified starch; gelatin; an alginate; xyloglucans, other hemicellulose polysaccharides including xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan and galactoglucomannan; natural gums such as pectin, xanthan gum, carrageenan, locust bean gum, gum arabic, tragacanth gum; and combinations thereof. In one embodiment, the polymer comprises: polyacrylates, especially sulfonated polyacrylates and water soluble acrylate copolymers; and alkylhydroxycelluloses such as methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, polymethacrylates. In another embodiment, the water soluble polymer may be selected from PVA; a PVA copolymer; hydroxypropylmethylcellulose (HPMC); and mixtures thereof.
The water soluble carrier may be selected from the group consisting of polyvinyl alcohol, modified polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl alcohol/polyvinyl amine, partially hydrolyzed polyvinyl acetate, polyalkylene oxide, polyethylene glycol, acrylamide, acrylic acid, cellulose, alkyl cellulose, methyl cellulose, ethyl cellulose, propyl cellulose, cellulose ether, cellulose ester, cellulose amide, polyvinyl acetate, polycarboxylic acids and salts, polyamino acids or peptides, polyamides, polyacrylamide, maleic/acrylic acid copolymers, polysaccharides, starch, modified starch, gelatin, alginate, xyloglucan, hemicelluloses, xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, galactoglucomannan, natural gum, pectin, xanthan gum, carrageenan, pectin, cellulose acetate, and/cellulose acetate, and/cellulose acetate, Locust bean gum, gum arabic, gum tragacanth, polyacrylates, sulfonated polyacrylates, water-soluble acrylate copolymers, alkyl hydroxy celluloses, methyl celluloses, sodium carboxymethyl cellulose, modified carboxymethyl celluloses, dextrins, ethyl celluloses, propyl celluloses, hydroxyethyl celluloses, hydroxypropyl methyl celluloses, maltodextrins, polymethacrylates, polyvinyl alcohol copolymers, hydroxypropyl methyl celluloses, and mixtures thereof.
The water soluble carrier may comprise a material selected from the group consisting of: formula H- (C)2H4O)x-(CH(CH3)CH2O)y-(C2H4O)zA polyalkylene polymer of-OH wherein x is from about 50 to about 300,y is from about 20 to about 100, and z is from about 10 to about 200; formula (C)2H4O)q-C(O)O-(CH2)r-CH3Wherein q is from about 20 to about 200, and r is from about 10 to about 30; formula HO- (C)2H4O)s-(CH2)t)-CH3Wherein s is from about 30 to about 250, and t is from about 10 to about 30; and mixtures thereof. Formula H- (C)2H4O)x-(CH(CH3)CH2O)y-(C2H4O)zThe polyalkylene polymer of-OH can be a block copolymer or a random copolymer, wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200.
The water soluble carrier may comprise: polyethylene glycol; formula H- (C)2H4O)x-(CH(CH3)CH2O)y-(C2H4O)zA polyalkylene polymer of-OH, wherein x is from about 50 to about 300; y is from about 20 to about 100, and z is from about 10 to about 200; formula (C)2H4O)q-C(O)O-(CH2)r-CH3Wherein q is from about 20 to about 200, and r is from about 10 to about 30; and formula HO- (C)2H4O)s-(CH2)t)-CH3Wherein s is from about 30 to about 250 and t is from about 10 to about 30.
The water soluble carrier may comprise from about 20% to about 80% by weight of the particle of the formula H- (C)2H4O)x-(CH(CH3)CH2O)y-(C2H4O)zA polyalkylene polymer of-OH, wherein x is from about 50 to about 300; y is from about 20 to about 100, and z is from about 10 to about 200.
The water soluble carrier may comprise from about 1% to about 20% by weight of the particle of formula (C)2H4O)q-C(O)O-(CH2)r-CH3Wherein q is from about 20 to about 200, and r is from about 10 to about 30.
Dissolving in waterThe sexual carrier may comprise from about 1% to about 10%, by weight of the particle, of the formula HO- (C)2H4O)s-(CH2)t)-CH3Wherein s is from about 30 to about 250 and t is from about 10 to about 30.
Preferably, the water soluble carrier may be selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxyalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, sodium sulfate, starch, and mixtures thereof. More preferably, the water soluble carrier may be polyethylene glycol (PEG). PEG may be a convenient material for preparing the particles because when the particles have the mass ranges disclosed herein, PEG may have sufficient water solubility to dissolve during the wash cycle. In addition, PEG can be easily processed in melt form. The melting initiation temperature of PEG can vary depending on the molecular weight of PEG. PEG is relatively low cost, can be formed in many different shapes and sizes, minimizes diffusion of unencapsulated perfume, and dissolves well in water. PEG has a variety of weight average molecular weights. In a particularly preferred embodiment of the invention, the water-soluble carrier is polyethylene glycol (PEG) characterized by a weight average molecular weight (Mw) of from about 1,000 daltons to about 20,000 daltons, preferably from about 1,500 daltons to about 15,000 daltons, more preferably from about 2,000 daltons to about 13,000 daltons. A particularly suitable PEG is commercially available from BASF under the trade name PLURIOL E8000 (which has a weight average molecular weight of 9000, even 8000 in the product name), although other PLURIOL products are also suitable.
Preferably, but not necessarily, each antimicrobial particle of the plurality of antimicrobial particles further comprises one or more perfume ingredients in an amount ranging from about 0.1% to about 30%, preferably from about 0.5% to about 20%, more preferably from about 1% to about 15%, by total weight of said each antimicrobial particle. It has been found that the incorporation of perfume ingredients into the antimicrobial particles of the present invention surprisingly and unexpectedly improves the freshness benefit and better malodor control benefit as compared to perfume ingredients that are not incorporated into any of the particles or perfume ingredients that are incorporated into particles containing a water soluble carrier but which are substantially free of antimicrobial agent. Without being bound by any theory, it is believed that the presence of the antimicrobial agent may interact with the perfume ingredients to improve the release profile and deposition of such perfume ingredients (especially perfume microcapsules) on fabrics.
The one or more perfumes are preferably selected from free perfumes, pro-perfumes, encapsulated perfumes (i.e., perfumes carried by a carrier material such as starch, cyclodextrin, silica, zeolite, or clay), perfume microcapsules, and combinations thereof. Preferably, the antimicrobial granules of the present invention contain Perfume Microcapsules (PMC), especially friable PMC. For the purposes of the present invention, the term "perfume microcapsule" or "PMC" covers both perfume microcapsules and perfume nanoparticles. In one embodiment, the PMC comprises a melamine/formaldehyde shell, which is commercially available from Appleton, Quest International, International Flavor & Fragrances, or other suitable sources. In a preferred embodiment, the PMC housing is coated with a polymer to enhance the ability of the PMC to adhere to the fabric. The antimicrobial particles of the present invention may comprise from about 0.1% to about 20%, preferably from about 1% to about 15%, more preferably from about 5% to about 10%, by total weight of each microbial particle in the antimicrobial particle, of perfume microcapsules. In a particularly preferred embodiment, each of the antimicrobial particles comprises a combination of free perfume and perfume microcapsules. More preferably, the weight ratio of free perfume to perfume microcapsule in each antimicrobial particle is in the range of from about 1:5 to about 20:1, preferably from about 1:2 to about 10:1, more preferably from about 1:1 to about 5:1, most preferably from about 1.5:1 to about 3: 1.
Preferably, but not necessarily, each antimicrobial particle of the plurality of antimicrobial particles further comprises a quaternary ammonium compound to provide additional fabric softening benefits. In particular, the quaternary ammonium compound deposits from the wash liquor onto the fibers of the fabric when released from the antimicrobial particles of the present invention during washing to provide a soft feel to the consumer. For example, each antimicrobial particle of the plurality of antimicrobial particles can comprise from about 5% to about 45%, preferably from about 10% to about 40%, more preferably from about 15% to about 35%, by total weight of the each antimicrobial particle, of a quaternary ammonium compound formed from a parent fatty acid compound having an iodine value of from about 18 to about 60, preferably from about 20 to about 60. Preferably, the quaternary ammonium compound is an ester quaternary ammonium compound, and more preferably is di- (tallowoyloxyethyl) -N, N-methylhydroxyethylammonium methylsulfate.
In addition to the quaternary ammonium compounds described above, the antimicrobial particles of the present invention may also contain a cationic polymer which serves to facilitate deposition of the quaternary ammonium compound onto the fabric and enhance its fabric softening properties. Each antimicrobial particle of the plurality of antimicrobial particles can comprise from about 0.5% to about 10%, preferably from about 1% to about 5%, by total weight of the each antimicrobial particle, of such cationic polymer. The cationic polymer is preferably a cationic polysaccharide, more preferably a polymeric quaternary ammonium salt of hydroxyethyl cellulose which has been reacted with an epoxide substituted with a trimethylammonium group. More preferably, the weight ratio of quaternary ammonium compound to cationic polymer in each particle may be in the range of about 3:1 to about 30:1, optionally about 5:1 to about 15:1, optionally about 5:1 to about 10:1, optionally about 8: 1. Without being bound by theory, the mass fraction of quaternary ammonium compound and the mass fraction of cationic polymer are balanced to obtain an adjunct effect from the cationic polymer to deposit satisfactory levels of quaternary ammonium compound onto the fabric being treated.
Each antimicrobial particle of the plurality of antimicrobial particles may further comprise from about 0.0001% to about 1%, preferably from about 0.001% to about 0.5%, more preferably from about 0.005% to about 0.1%, of one or more colorants by total weight of the each antimicrobial particle, in order to provide a visual cue that is pleasing to the consumer as an aesthetic appearance or highlights certain ingredients or benefits. The colorant may be selected from the group consisting of dyes, pigments, and combinations thereof. Preferably, the colorant imparts a color to the antimicrobial particles selected from the group consisting of blue, green, yellow, orange, pink, red, purple, gray, and the like.
The antimicrobial particles of the present invention may also contain water soluble or water dispersible fillers such as sodium chloride, sodium sulfate, sodium carbonate, sodium bicarbonate, sugars, starches, modified celluloses, silicas, zeolites, clays, and the like. Preferably, each particle may comprise from about 0.1% to about 7% clay by total weight of said each particle. More preferably, the clay is bentonite.
It is particularly preferred that the antimicrobial particles of the present invention are substantially or essentially free of surfactants, as the presence of such surfactants can accelerate the dissolution or dispersion of the antimicrobial particles in water and reduce their settling on the fabric, which is undesirable in the context of the present invention. More preferably, the antimicrobial particles of the present invention are substantially free or substantially free of any detersive active.
The antimicrobial particles of the present invention preferably comprise less than about 10%, optionally less than about 8%, optionally less than about 5%, optionally less than about 3%, of water by total weight of each of the antimicrobial particles. It is believed that water contents below or with these ranges provide more stable particles. The lower the mass fraction of water, the more stable the particles are considered.
Each antimicrobial particle of the invention has a mass of from about 1mg to about 1g, preferably from about 5mg to about 500mg, more preferably from about 10mg to about 250mg, most preferably from about 15mg to about 125 mg.
The granules may be formed into tablets, pills, spheres, and the like. They may have any shape selected from: spherical, hemispherical, compressed hemispherical, cylindrical, disk-shaped, circular, lentil-shaped, elliptical, cubic, rectangular, star-shaped, flower-shaped, and any combination thereof. Lentil refers to the shape of lentil. A compressed hemisphere refers to a shape corresponding to a hemisphere that is at least partially flat such that the curvature of the curved surface is on average less than the curvature of a hemisphere having the same radius. The compressed hemispherical grains can have an aspect ratio (i.e., the ratio of their bottom diameter to their height normal to the bottom) of about 2.0 to about 5, alternatively about 2.1 to about 4.5, alternatively about 2.2 to about 4. By elliptically-shaped particles is meant particles having a maximum dimension and a second dimension orthogonal to the maximum dimension, wherein the ratio of the maximum dimension to the second dimension is greater than about 1.2, preferably greater than about 1.5, more preferably greater than about 2. Preferably, the antimicrobial particles of the present invention have a hemispherical or compressed hemispherical shape.
Preferably, the antimicrobial particles are characterized by a longest dimension of from about 3mm to about 10mm, preferably from about 4mm to about 9mm, more preferably from about 5mm to about 8 mm; and/or an aspect ratio of about 1 to about 5, preferably about 1.5 to about 4, more preferably about 2 to about 4.
In a preferred, but not required, embodiment of the invention, the antimicrobial particles of the invention have a lower density than water, so that they can float on water and are more easily noticed by consumers during washing. For example, such antimicrobial particles can have a density in the range of from about 0.5g/cm3 to about 0.98g/cm3, preferably from about 0.7g/cm3 to about 0.95g/cm3, more preferably from about 0.8g/cm3 to about 0.9g/cm 3.
The plurality of antimicrobial particles of the present invention can have different shapes, sizes, masses, and/or densities.
Use of antimicrobial particles in a separate granular product
Many consumers prefer granular products, especially dust-free granules. The consumer can easily dose the granular product from the packaging directly into the washing machine or into a dosing compartment on the washing machine. Alternatively, the consumer may dose from the package into a measuring cup, which optionally provides one or more dosing indicia, and then dose the particles into a dosing compartment on the washing machine or directly into the drum. For products in which a measuring cup is used, granular products tend to be cleaner than liquid products.
A plurality of antimicrobial particles as mentioned above may be provided as separate granular products for fabric treatment in a washing process, which facilitates dosing into a washing machine for the consumer. The separate granular product may consist essentially of the antimicrobial particles of the invention, or it may contain other particles similar to the antimicrobial particles, such as perfume particles, softening particles, bleach particles, etc., which contain little or no surfactant or are of similar size to the antimicrobial particles. The separate granular product may be provided in a package separate from the package of the detergent composition. Having the antimicrobial particles in a package separate from the package of the detergent composition can be beneficial in that it allows the consumer to select the amount of antimicrobial agent to be dosed independently of the amount of detergent composition used. This can give consumers the opportunity to customize the amount of antimicrobial agent used, thereby customizing the resulting antimicrobial benefit based on their needs, which is a highly valuable consumer benefit.
Particulate laundry detergent product comprising antimicrobial particles
In a preferred, but not essential, embodiment of the invention, the antimicrobial particles of the invention are present in a particulate laundry detergent composition which also contains detergent particles. Preferably, a plurality of antimicrobial particles is present in the particulate laundry detergent composition as a minor portion, for example, in an amount of from about 0.05% to about 30%, preferably from about 0.1% to about 20%, more preferably from about 0.5% to about 15%, most preferably from about 1% to about 10%, by total weight of the particulate laundry detergent composition.
The particulate laundry detergent composition may comprise detergent particles in an amount ranging from about 10% to about 99.9%, preferably from about 20% to about 95%, more preferably from about 30% to about 90%, most preferably from about 40% to about 80%, by total weight of the particulate laundry detergent composition. The detergent particles of the present invention may comprise one or more detersive actives such as surfactants, builders, bleach actives, enzymes, polymers, chelants, softeners, suds suppressors, suds boosters, brighteners, dye transfer inhibitors and the like. The detergent particles may be spray-dried particles and/or agglomerated particles and/or extruded particles. Such detergent particles may be selected from: surfactant granules, including surfactant agglomerates, surfactant extrudates, surfactant needles, surfactant bars, surfactant flakes; polymer particles, such as cellulosic polymer particles, polyester particles, polyamine particles, terephthalic acid polymer particles, polyethylene glycol polymer particles; builder particles, such as sodium carbonate and sodium silicate co-builder particles, phosphate particles, zeolite particles, silicate particles, carbonate particles; filler particles, such as sulfate particles; dye transfer inhibitor particles; dye fixative particles; bleach particles, such as percarbonate particles, in particular coated percarbonate particles, such as percarbonate coated by carbonate, sulphate, silicate, borosilicate, or any combination thereof; perborate particles; bleach catalyst particles such as transition metal bleach catalyst particles or peroxyimine cation based bleach catalyst particles; preformed peracid particles, particularly coated preformed peracid particles; and a co-bleach particle of a bleach activator; a source of hydrogen peroxide and optionally a bleach catalyst; bleach activator particles such as sodium oxybenzenesulfonate bleach activator particles and tetraacetylethylenediamine bleach activator particles; chelant particles, such as chelant agglomerates; a hueing dye particle; a brightener particle; enzyme granules, such as protease granules, lipase granules, cellulase granules, amylase granules, mannanase granules, pectate lyase granules, xyloglucanase granules, bleaching enzyme granules, cutinase granules, and co-granulation of any of these enzymes; clay particles such as montmorillonite particles or particles of clay and silicone; flocculant particles, such as polyethylene oxide particles; wax particles, such as waxy agglomerates.
Preferably, such detergent particles are surfactant particles comprising from about 10% to about 90%, preferably from about 15% to about 80%, more preferably from about 20% to about 70%, by total weight of the detergent particle, of surfactant. More preferably, the surfactant is selected from the group consisting of anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, zwitterionic surfactants, and combinations thereof. Most preferably, the detergent particles of the present invention comprise anionic surfactant and/or nonionic surfactant.
The detergent particles of the present invention may be characterized by a median weight particle size (Dw50) of from about 250 μm to about 1000 μm, preferably from about 300 μm to about 950 μm, more preferably from about 400 μm to about 850 μm. Preferably, such detergent particles have a white or light-coloured appearance, while the antimicrobial particles have a blue, green, yellow, orange, pink, red, violet or grey colour, such that they visually form an contrast with the detergent particles.
In addition to the antimicrobial and detergent particles described above, the particulate laundry detergent composition of the present invention may comprise one or more detergent ingredients. Suitable detergent ingredients include: detersive surfactants including anionic detersive surfactant, nonionic detersive surfactant, cationic detersive surfactant, zwitterionic detersive surfactant, amphoteric detersive surfactant, and any combination thereof; polymers including carboxylate polymers, polyethylene glycol polymers, soil release polyester polymers such as terephthalic acid polymers, amine polymers, cellulose polymers, dye transfer inhibiting polymers, dye blocking polymers such as condensation oligomers produced by the condensation of imidazole and epichlorohydrin, optionally in a ratio of 1:4:1, hexamethylenediamine derivative polymers, and any combination thereof; builders including zeolites, phosphates, citrates, and any combinations thereof; buffers and alkalinity sources including carbonates and/or silicates; fillers, including sulfates and bio-packing materials; bleaching agents, including bleach activators, available oxygen sources, preformed peracids, bleach catalysts, reducing bleaches, and any combination thereof; a chelating agent; a photo-bleaching agent; a toner; a whitening agent; enzymes, including proteases, amylases, cellulases, lipases, xyloglucanases, pectate lyases, mannanases, bleaches, cutinases, and any combination thereof; fabric softeners, including clays, silicones, quaternary ammonium salt fabric softeners, and any combination thereof; flocculants such as polyethylene oxide; perfumes including starch encapsulated perfume accords, perfume microcapsules, perfume loaded zeolites, schiff base reaction products of ketone perfume raw materials and polyamines, blooming perfumes, and any combination thereof; aesthetic substances, including soap rings, layered aesthetic particles, gelatin beads, carbonate and/or sulfate speckles, colored clays, and any combination thereof: and any combination thereof.
In a preferred embodiment of the present invention, the particulate laundry detergent composition comprises one or more builders (excluding carbonates as described above) in an amount ranging from about 1 wt% to about 40 wt%, typically from 2 wt% to 25 wt%, or even from about 5 wt% to about 20 wt%, or from 8 wt% to 15 wt%, by total weight of such composition. As used herein, a builder refers to any ingredient or component that is capable of enhancing or improving the cleaning efficiency of a surfactant, for example by removing or reducing "free" calcium/magnesium ions in the wash solution, to "soften" or reduce the hardness of the wash liquor.
It is particularly desirable that such granular laundry detergent compositions have relatively low levels of phosphate builder, zeolite builder and silicate builder. Preferably, it comprises a total of up to 15 wt% phosphate builder, zeolite builder and silicate builder. More preferably, such granular laundry detergent compositions comprise from 0 wt% to about 5 wt% phosphate builder, from 0 wt% to about 5 wt% zeolite builder, and from 0 wt% to about 10 wt% silicate builder, with the total amount of these builders totaling no more than 10 wt% by total weight of the composition. Still more preferably, the granular laundry detergent composition comprises from 0 wt% to about 2 wt% phosphate builder, from 0 wt% to about 2 wt% zeolite builder, and from 0 wt% to about 2 wt% silicate builder, with the total amount of these builders totaling no more than 5 wt% by total weight of the composition. Most preferably, the granular laundry detergent composition comprises from 0 wt% to about 1 wt% of phosphate builder, from 0 wt% to about 1 wt% of zeolite builder, and from 0 wt% to about 1 wt% of silicate builder, with the total amount of these builders totaling no more than 2 wt% by total weight of the composition. The composition may also comprise one or more of any other supplementary builder, one or more chelating agent, or in general, be dissolved from the solution by, for example, chelation, complexation, precipitation, or ion exchangeAny substance in the liquor that removes calcium ions. In particular, the composition can comprise a calcium binding capacity of at least 50mg/g and a calcium binding constant log K Ca of at least 3.50 at a temperature of 25 ℃ and 0.1M ionic strength2+The substance of (1).
The granular laundry detergent composition of the present invention may comprise one or more solid carriers selected from the group consisting of sodium chloride, potassium chloride, sodium sulfate and potassium sulfate. In a preferred, but not required, embodiment, such particulate laundry detergent compositions comprise from about 20% to about 65% by weight sodium chloride and/or from about 20% to about 65% by weight sodium sulfate. When the particulate laundry detergent composition is in concentrated form, the total amount of sodium chloride and/or sodium sulfate in such compositions may, for example, total a total amount of from about 0 wt% to about 60 wt%.
Methods of using antimicrobial particles
The antimicrobial particles of the present invention are particularly useful for treating fabrics in a machine wash or hand wash setting to provide antimicrobial benefits and optionally improved fabric freshening benefits and malodor control benefits. The antimicrobial particles enable consumers to achieve antimicrobial benefits through washing, particularly a wash sub-cycle. By providing an antimicrobial benefit via the wash sub-cycle, the consumer need only dose the detergent composition and antimicrobial particles into a single location, such as a laundry tub, before or shortly after the washing machine is started.
A method for treating an article of clothing may include the step of providing an article of clothing in a washing machine. The laundry article is contacted with a composition comprising a plurality of antimicrobial particles disclosed herein during a wash sub-cycle of a washing machine. The particles may be dissolved in water provided as part of the wash sub-cycle to form a liquid. Dissolution of the particles may occur during the wash sub-cycle.
The washing machine has at least two basic sub-cycles within an operating cycle: a wash sub-cycle and a rinse sub-cycle. The wash sub-cycle of a washing machine is the cycle on the washing machine that begins when water is first added or partially added to fill the wash basin. The main purpose of the wash sub-cycle is to remove and/or loosen soil from the laundry articles and suspend the soil in the wash liquor. Typically, the wash liquid is drained at the end of the wash sub-cycle. The rinse sub-cycle of a washing machine occurs after the wash sub-cycle and has the primary purpose of rinsing soil and optionally some benefit agents brought to the wash sub-cycle by the laundry articles.
The method may optionally include the step of contacting the laundry article with a detergent composition comprising an anionic surfactant during a wash sub-cycle. Most consumers provide detergent compositions to the wash basin during the wash sub-cycle. The detergent composition may comprise anionic surfactants and optionally other benefit agents including, but not limited to, perfumes, bleaches, brighteners, shading dyes, enzymes, and the like. During the wash sub-cycle, the benefit agent provided with the detergent composition is contacted with or applied to a laundry article placed in the wash basin. Typically, the benefit agent of the detergent composition is dispersed in the wash liquor of water and benefit agent.
During the wash sub-cycle, the wash basin may be filled or at least partially filled with water. The antimicrobial particles are soluble in water to form a wash liquor comprising a particulate component. Optionally, if a detergent composition is employed or if the antimicrobial particles are formulated into a granular laundry detergent composition, the wash liquor may comprise components of the detergent composition and components that dissolve the particles. The particles may be placed in the wash basin of a washing machine before the laundry article is placed in the wash basin of the washing machine. After the laundry article is placed in the wash basin of the washing machine, the particles may be placed in the wash basin of the washing machine. The particles may be placed in the wash basin before filling or partially filling the wash basin with water or after filling the wash basin with water has begun.
If the consumer uses the detergent composition to practice the method of treating a laundry article, the detergent composition and the particles may be provided in separate packages. For example, the detergent composition may be a liquid detergent composition provided from a bottle, pouch, water-soluble pouch, measuring cup, dosing ball or cartridge associated with a washing machine. The particles may be provided from individual packages, by way of non-limiting example from cartons, bottles, water-soluble pouches, measuring cups, pouches, and the like. If the detergent composition is in solid form such as a powder, a water-soluble fibrous substrate, a water-soluble sheet, a water-soluble film, a water-insoluble fibrous web carrying the solid detergent composition, the particle may have the solid form of the detergent composition. For example, the granules may be provided from a container containing a mixture of the solid detergent composition and the granules. Optionally, the particles may be provided by a pouch formed from a detergent composition which is a water-soluble fibrous substrate, a water-soluble sheet, a water-soluble film, a water-insoluble fibrous web carrying a solid detergent composition.
The laundry wash liquor used to dissolve the antimicrobial particles and treat the fabrics may have a pH value selected to best suit the fabrics to be cleaned in a broad range of pH spanning, for example, from about 5 to about 11, preferably from about 8 to about 10. The water temperature is preferably in the range of about 5 ℃ to about 100 ℃. The water to fabric ratio is typically from about 1:1 to about 30: 1. The wash liquor may comprise 40 litres or less of water, or 30 litres or less, or 20 litres or less, or 10 litres or less, or 8 litres or less, or even 6 litres or less of water. The wash liquor may comprise from above 0 litres to 15 litres, or 2 litres and to 12 litres, or even to 8 litres of water. In the case of diluted wash conditions, the wash liquor may comprise 150 litres or less of water, 100 litres or less of water, 60 litres or less of water, or 50 litres or less of water, especially for hand wash conditions, and may depend on the number of rinses.
Typically, from 0.01Kg to 2Kg of fabric per litre of wash liquor is dosed into the wash liquor. Typically, from 0.01Kg, or from 0.05Kg, or from 0.07Kg, or from 0.10Kg, or from 0.15Kg, or from 0.20Kg, or from 0.25Kg, to 1.8Kg, or to 1.6Kg, or to 1.5Kg, or to 1.3Kg, or to 1.1Kg, or to 0.9Kg, or to 0.7Kg, or to 0.5Kg of fabric per litre of wash liquor is dosed into the wash liquor.
Preparation of antimicrobial particles
For carriers that can be conveniently processed as a melt, a rotational molding process can be used. The mixture of molten carrier and other materials constituting the particles is prepared, for example, in a batch or continuous mixing process. The molten mixture may be pumped to a rotary molder, such as Sandvik ROTOFORM 3000 having a 750mm wide, 10m long ribbon. The rotary molding apparatus may have a rotating cylinder. The cylinders may have 2mm diameter holes arranged at a pitch of 10mm in the transverse direction and at a pitch of 9.35mm in the longitudinal direction. The cylinder may be positioned about 3mm above the belt. The belt speed and the rotational speed of the cylinder may be set to about 10 m/min. The molten mixture may pass through holes in the rotating cylinder and be deposited on a moving conveyor disposed below the rotating cylinder.
The molten mixture may be cooled on a moving conveyor to form a plurality of solid particles. Cooling may be provided by ambient cooling. Optionally, cooling may be provided by spraying the underside of the conveyor with water at ambient temperature or cooling water.
Once the pellets have developed sufficient viscosity, the pellets may be transferred from the conveyor to downstream processing equipment of the conveyor for further processing and/or packaging.
Optionally, the particles may have a gaseous content. Such occlusions of gas (e.g., air) may help the particles dissolve more quickly in the wash. By way of non-limiting example, occlusion of the gas may be provided by injecting the gas into the molten precursor material and milling the mixture.
Other methods may also be used to prepare the particles. For example, granulation or pressure agglomeration may be a suitable method. In granulation, the precursor material containing the particulate component material is compacted and homogenized by a rotating mixing tool and granulated to form granules. For precursor materials that are substantially free of water, particles of various particle sizes can be prepared.
In pressure agglomeration, a precursor material of the component material comprising the particles is compacted and plasticized under pressure and shear forces, homogenized, and then discharged from a pressure agglomerator via a forming/shaping process. Pressure agglomeration techniques include extrusion, roller compaction, granulation, and tableting.
The precursor material comprising the particulate component material may be delivered to a planetary roller extruder or a twin screw extruder having co-rotating or counter-rotating screws. The barrel and extrusion granulation head may be heated to the desired extrusion temperature. The precursor material comprising the particulate component material may be compacted under pressure, plasticized, extruded in strands through a porous extrusion die in the extruder head, and sized using a cutting blade. The pore size of the extrusion head may be selected to provide particles of an appropriate size. The extruded particles may be shaped using a pelletizer to provide particles having a spherical shape.
Optionally, the extrusion and compression steps may be performed in a low pressure extruder, such as a flat die pelletizing press available from Amandus Kahl, Reinbek, Germany. Optionally, the extrusion and compression steps may be carried out in a low pressure extruder, such as the BEXTRUDER available from Hosokawa Alpine Aktiengesellschaft, Augsburg, Germany.
Roller compaction may be used to prepare the particles. In a roll press, a precursor material comprising a particulate component material is introduced between two rolls and rolled under pressure between the two rolls to form a dense sheet. The rollers provide high linear pressure on the precursor material. The rollers may be heated or cooled as desired, depending on the processing characteristics of the precursor material. The dense sheet is broken into small pieces by cutting. The pellets may be further formed, for example, by using a pelletizer.
Test method
The following techniques must be used to determine the characteristics of the perfume particles, detergent particles and particulate laundry detergent compositions of the present invention so that the invention described and claimed herein can be fully understood.
Test 1: antimicrobial testing
The antimicrobial efficacy of the sample particulate laundry detergent composition was measured as follows:
each defined sample of the granular laundry detergent composition to be tested (e.g., 15.29g) was dissolved in 1L of water having a water hardness level of 342 mg/L. Such water is obtained by passing 0.034g CaCl2And 0.139g MgCl2·6H2O is formed by dissolving in 1L Deionized (DI) water. By magnetic forceThe agitator mixes the solution for about 4 minutes and then dispenses 265ml of such solution into the exposed chamber of the washing drum as described in the laundry detergent sterilization test method promulgated by the japanese detergent and soap equity exchange commission.
In addition, the stainless steel mandrel was made from a single continuous stainless steel wire having a diameter of about 1/16 inches, which was bent to form 3 horizontally extending segments each about 2 inches long, connected by 2 vertical segments about 2 inches long. The mandrel serves as a carrier for wrapping the fabric ballast.
Approximately 300 grams of cotton fabric was then scoured by boiling for one hour in 3L of distilled or DI water containing about 1.5 grams of sodium carbonate and about 1.5 grams of a non-ionic wetting agent. The fabric was then rinsed in boiling water and then in cold water until all visible traces of foam formed by the wetting agent were removed. The fabric was then drained and air dried at ambient temperature for at least 24 hours. The scoured and dried fabric was then cut into strips each having a width of about 2 inches and weighing about 15 ± 0.1 g. A piece of such cotton fabric strip is then taken and one of its ends is fixed to the outer horizontal extension of the stainless steel mandrel. The strip of cotton fabric is wrapped around the three horizontal extensions of the mandrel with sufficient tension for about 12 to 13 turns until the entire strip of fabric is wrapped onto the mandrel. Staples or pins may be used to secure the loose ends of the fabric strip. The fabric wrapped mandrel may then be sterilized in a separate exposure chamber of the washing drum described above, or separately from the exposure chamber. The fabric wrapped around the mandrel and the exposure chamber should both be dry prior to placing the mandrel into the exposure chamber.
The fabric wrapped mandrel was then placed into the exposed chamber of a wash drum containing 265ml of the above wash solution. The exposed chamber was then stirred at about 60rpm for about 20 minutes. After stirring for 20 minutes, the fabric-wrapped mandrel was centrifuged for about 2 minutes and the wash solution was discarded. 265ml of fresh hard water as described above was then dispensed into the same exposure chamber to rinse the fabric wrapped mandrel. The exposed chamber was stirred at the same stirring speed for an additional 3 minutes, then the fabric-wrapped mandrel was again spin-dried for about 2 minutes, and then the rinse solution was discarded. The fabric wrapped mandrel was rinsed and again centrifugally dried according to the same procedure as described above.
Next, the cotton fabric strips were removed from the mandrel and air dried overnight at ambient temperature. The dried strips of cotton fabric were then cut into 2cm x 2cm square pieces and 10 pieces of such cotton fabric were stacked together to form a test sample weighing about 0.40 ± 0.05 g.
Such test samples were then subjected to the bacterial activity evaluation method as described in section 8.1 of the Japanese Industrial Standard (JIS) L1902-2015 standard, while the bacterial count was calculated according to section 8.1.4.5.2 (instead of calculating the amount of ATP as described in section 8.1.4.5.3).
And (3) testing 2: dissolution Rate test
Dissolution rate testing is used to measure the dissolution rate of particles.
The test was performed by adding 400ml of deionized water to a 400ml clear glass beaker at room temperature (25 ℃) and then dispersing about 1 gram of the test particles into the deionized water. A stopwatch was used to count the total time required before the particles were completely dissolved.
And (3) testing: aspect ratio of particles
For non-spherical particles, the longest and shortest dimensions of the particle can be measured by using a vernier caliper. To reduce the variation in data, typically 10 particles can be measured and then the average result used. Particle aspect ratio herein is calculated using the following formula: aspect ratio is longest dimension/shortest dimension.
And (4) testing: perfume bloom and fabric freshness test
The improved perfume body and fabric freshness benefits were demonstrated using a dissolution Head-Space Count test. The test is similar in many respects to the conditions that may occur when a consumer treats her laundry with particles.
In the dissolution headspace count test method, the particles to be tested are placed in distilled water and the amount of Perfume Raw Material (PRM) in the air transferred to the headspace above the water at various points in time is measured as a count. Measurement of the lysis headspace counts was performed using a 7100Ultra Fast GC analyzer MicroSense5 ZNOSE (available from Electronic Sensor Technology, new bury Park, calif., USA) with accompanying software MicroSense version 5.37. The instrument system is a miniature high-speed gas chromatograph containing gas chromatographic sensors, pneumatic controls and supporting electronics. Gas chromatography sensors are based on 6-port valves and ovens, pre-concentration traps, short gas chromatography columns and surface acoustic wave detectors. The laptop-based system controller operates the system, analyzes the data, and provides a user interface. A complete instruction for ZNOSE can be found in the 7100Ultra Fast GC Analyzer operating Manual MicroSense 5. To perform the dissolution headspace count test, ZNOSE was set to the following settings: 5ps2a1b — 35(DBS chromatography column); 1 second pump sampling time; 0.5 second data collection; the column temperature ranges from 40 ℃ to 180 ℃ and ramps up at a rate of 5 ℃/5 cc; and the surface acoustic wave detector is set to 35 deg.c. A total of 20g of 25 ℃ Deionized (DI) water was added to a clean 40ml sample vial (such as VWR scientific catalog number EP 140-40C). A total of 0.040g of test particles or 0.040g portion of test particles was added to 20g of water in the sample bottle to provide a sample of test particulate material at a concentration of 2.0mg/mL in DI water. After the addition of the test particulate material, a 3mm thick PTFE silicone septum was secured to the sample bottle and immediately a ZNOSE injection needle was inserted into the headspace of the sample bottle along with a separate needle attached to the carbon filter. The ZNOSE measurement was performed every 90 seconds and continued at ambient temperature between 22 ℃ and 27 ℃ for at least 45 minutes without any agitation of the sample or the bottle. The headspace count for each PRM was recorded at each 90 second measurement time point. The dissolution headspace count reported for a given time point is the sum of the counts of all PRMs detected in the headspace at that time point.
The dissolved headspace count is a function of the concentration in the headspace of the particular perfume raw material under consideration. A higher headspace count is associated with a higher concentration of perfume in the headspace.
Examples
The examples herein are intended to illustrate the invention, but are not intended to limit or define the scope of the invention.
Example 1: antimicrobial particles
The following are exemplary antimicrobial particles a-E according to the present invention:
TABLE 1
Figure BDA0003598477860000211
Figure BDA0003598477860000221
1Under the trade name of
Figure BDA0003598477860000222
HP100 is supplied by BASF and contains 30% of 4-4' -dichloro-2-hydroxydiphenyl ether active in 1, 2-propanediol solution. Concentrations provided herein are pure activity levels, not feedstock levels.
2C18 unsaturated DEEHMAMS (diethyl hydroxyethylmethylammonium methylsulfate), available from EVONIK, had an iodine value of about 42.
3Polymer PK, available from Dow Chemical, is a cationic hydroxyethyl cellulose having a weight average molecular weight of 400kDa, a charge density of 0.18 and an average weight percentage of nitrogen/anhydroglucose repeat units of 0.28%.
Example 2: antimicrobial particles in granular laundry detergent products
The antimicrobial particles of the invention from example 1 were incorporated into the following granular laundry detergent products of formulations I-V:
TABLE 2
Ingredient (wt%) I II III IV
C11-C13Linear alkyl benzene sulphonate (LAS) 9.5 13 5.4 13
C with EO 7-912-C15Ethoxylated alcohols 1.3 1.1 2.4 1
Soap 0.1 0.1 10 0.5
C12-C14Alkyl sulfates - 5 0.3
Methyl Ester Sulfonate (MES) 4.4 - - -
Zeolite 8 2 9 1.5
Bleaching agent 0.5 - 0 2
Polymer and method of making same 1 1 1.1 2
Enzyme 0.3 0.3 0.7 0.2
Whitening agent 0.1 0.2 0.1 0.3
Carbonate salt 3.5 24 11 20.5
Silicates of acid or alkali 6 10 8 5
Citric acid 0.7 - - -
Sulfuric acid esters/salts 61.4 44.1 43.6 50.4
Antimicrobial beads1 2 2 2 2
Others (e.g. perfumes, aesthetic substances, etc.) Proper amount of Proper amount of Proper amount of Proper amount of
1Any one of the antimicrobial beads of the invention a-E from example 1 or mixtures thereof.
Example 3: comparative testing demonstrated higher deposition rates of antimicrobial agents when incorporated into antimicrobial beads
A sample of the invention comprising the antimicrobial particles of the invention (sample a) is provided. A comparative sample (sample B) comprising particles (without antimicrobial agent) and antimicrobial agent alone (not incorporated into the particles) is also provided.
Specifically, sample A contained 13.5 grams of antimicrobial particles consisting of 13.42 grams of PEG9000 and 0.08 grams
Figure BDA0003598477860000231
HP100 is formed. The antimicrobial particles in sample a were prepared by the following steps:
pre-melting the PEG9000 material in a 75 ℃ oven overnight;
weigh the molten PEG9000 material into a 250mL beaker;
weigh 4-4' -dichloro-2-hydroxydiphenyl ether biocide into the same beaker;
place the beaker in a water bath at 85 ℃;
mix the contents of the beaker with a blender (4-blade stirrer) at 250RPM for 10 minutes;
transferring the mixture into a bead mold;
keeping the mould at room temperature, allowing the mixture in the mould to cool and solidify; and
collecting the cured antimicrobial beads from the mold.
Sample B contained separately 13.42 grams of PEG9000 particles and 0.08 grams
Figure BDA0003598477860000232
HP 100. The PEG9000 particles in sample B were formed by the following steps:
pre-melting the PEG9000 material in a 75 ℃ oven overnight;
preheating the mould and the scraper in an oven at 75 ℃;
transfer of molten PEG9000 material into a preheated mold;
keeping the mold at room temperature so that the molten PEG9000 material in the mold cools and solidifies;
the cured PEG9000 beads were collected from the mold.
The fabric was then treated with sample a and sample B, respectively, according to the following wash conditions:
a washing machine: haier Dual activation TLA 1466
And (3) washing circulation: 2 min dissolution/10 min soaking/15 min washing/4 min rinsing/2 centrifugal drying
Load capacity: a total of 1.7kg, comprised 4 pieces of CW98 (cotton) (New Cotton: New polyester 8:2)
Hardness: 9gpg Ca Mg 4:1
HMI：Fe:Cu:Mn 6:1:4
Water temperature: 25 deg.C
Four (4) pieces of CW98 cotton (10x10cm) from each wash were hung dry and sent for deposition analysis of 4-4' -dichloro-2-hydroxydiphenyl ether.
Specifically, 4-4' -dichloro-2-hydroxydiphenyl ether was extracted from the fabric by using methanol with the aid of ASE (accelerated solvent extraction). Approximately 3g of fabric was accurately weighed and filled into a steel ASE tube, after which the extraction protocol was run at 100 ℃ and 2000psi for 5 minutes using methanol as the extraction solvent. The extracted contents were collected and transferred to a 25ml flask, and were made to volume with methanol, after which an injection sample was prepared by further diluting 25 times by adding 50:50 methanol: water.
The injected samples were then subjected to gradient reverse phase High Performance Liquid Chromatography (HPLC) separation on a C18 column and quantified by tandem mass spectrometry (MS/MS) operating under Multiple Reaction Monitoring (MRM) conditions in negative mode. The LC-MS/MS test was performed by injecting 5ul of the injected sample, thereby separating the injected sample on a Waters Acquity UPLC C18 chromatographic column with a gradient from 70% mobile phase a (1% aqueous formic acid)/30% mobile phase B (0.1% formic acid in methanol) to 5% mobile phase a/95% mobile phase B in 3 minutes, and maintaining the final gradient for another 3 minutes. Antimicrobial agent 4-4' -dichloro-2-hydroxydiphenyl ether was detected in negative MRM mode. Ion pairs of m/z 253>142 are used for quantitative conversion, while ion pairs of m/z 253>125 are used for identification.
Standard standards of a standard substrate in the range of 0.5g/ml to 500ng/ml were injected to establish a calibration curve. Weighting using calibration curves (1/x)2) The secondary regression determines the concentration of 4-4' -dichloro-2-hydroxydiphenyl ether in the injected sample by an inverse algorithm.
The results of the deposition of 4-4' -dichloro-2-hydroxydiphenyl ether on the fabrics treated with sample a and sample B are as follows:
TABLE 3
Figure BDA0003598477860000241
The above results show that 4-4' -dichloro-2-hydroxydiphenyl ether, when incorporated into particles, has a significantly higher deposition rate than when added alone.
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Rather, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".
Each document cited herein, including any cross referenced or related patent or patent application and any patent application or patent to which this application claims priority or its benefits, is hereby incorporated by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with any disclosure of the invention or the claims herein or that it alone, or in combination with any one or more of the references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.
While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims (11)

1. A composition comprising a plurality of antimicrobial particles, each of the plurality of antimicrobial particles comprising:
a) from 25% to 99% by total weight of the particle of a water-soluble carrier; and
b) a diphenyl ether antimicrobial agent which is capable of inhibiting the growth of microorganisms,
wherein each antimicrobial particle of the plurality of antimicrobial particles has a mass of 1mg to 1 g.
2. The composition of claim 1, wherein each antimicrobial particle of the plurality of antimicrobial particles comprises from 0.01% to 3%, preferably from 0.02% to 2%, more preferably from 0.05% to 1%, most preferably from 0.1% to 0.5%, by total weight of said each antimicrobial particle, of the diphenyl ether antimicrobial agent; wherein the diphenyl ether antimicrobial agent is preferably selected from the group consisting of 4-4 ' -dichloro-2-hydroxydiphenyl ether, 2,4,4 ' -trichloro-2 ' -hydroxydiphenyl ether, and combinations thereof; and wherein the diphenyl ether antimicrobial agent is more preferably 4-4' -dichloro-2-hydroxydiphenyl ether.
3. The composition of any one of the preceding claims, wherein each antimicrobial particle of the plurality of antimicrobial particles comprises from 30% to 95%, more preferably from 40% to 94%, most preferably from 50% to 93%, by total weight of the each antimicrobial particle, of the water-soluble carrier; wherein the water-soluble carrier is preferably a water-soluble polymer; wherein the water soluble carrier is preferably selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxyalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, sodium sulfate, starch, and combinations thereof; wherein the water soluble carrier is most preferably a polyethylene glycol characterized by a weight average molecular weight (Mw) of 1,000 to 20,000 daltons, preferably 1,500 to 15,000 daltons, more preferably 2,000 to 13,000 daltons.
4. The composition of any one of the preceding claims, wherein each antimicrobial particle of the plurality of antimicrobial particles further comprises from 0.1% to 30%, preferably from 0.5% to 20%, more preferably from 1% to 15%, by total weight of said each antimicrobial particle, of a perfume; wherein
The perfume is preferably selected from the group consisting of free perfume, pro-perfume, encapsulated perfume, perfume micro-capsules, and combinations thereof; wherein the perfume more preferably comprises a combination of free perfume and perfume microcapsules; wherein most preferably the weight ratio of free perfume to perfume microcapsule in each antimicrobial particle is from 1:5 to 20:1, preferably from 1:2 to 10:1, more preferably from 1:1 to 5:1, most preferably from 1.5:1 to 3: 1.
5. The composition of any preceding claim, wherein each antimicrobial particle of the plurality of antimicrobial particles further comprises from 5% to 45%, preferably from 10% to 40%, more preferably from 15% to 35%, by total weight of the each antimicrobial particle, of a quaternary ammonium compound formed from a parent fatty acid compound having an iodine value of from 18 to 60, preferably from 20 to 60; wherein the quaternary ammonium compound is preferably an ester quaternary ammonium compound; wherein the quaternary ammonium compound is more preferably bis- (tallowoyloxyethyl) -N, N-methylhydroxyethylammonium methylsulfate.
6. The composition of claim 5, wherein each antimicrobial particle of the plurality of antimicrobial particles further comprises from 0.5% to 10%, preferably from 1% to 5%, by total weight of the each antimicrobial particle, of a cationic polymer; wherein the cationic polymer is preferably a cationic polysaccharide; wherein the cationic polymer is more preferably a polymeric quaternary ammonium salt of hydroxyethyl cellulose which has been reacted with an epoxide substituted with a trimethylammonium group.
7. The composition of any preceding claim, wherein each antimicrobial particle of the plurality of antimicrobial particles further comprises from 0.0001% to 1%, preferably from 0.001% to 0.5%, more preferably from 0.005% to 0.1%, of a colorant, by total weight of the each antimicrobial particle; wherein preferably the colorant is selected from the group consisting of dyes, pigments, and combinations thereof.
8. The composition of any one of the preceding claims, wherein each antimicrobial particle of the plurality of antimicrobial particles is characterized by:
i) a shape selected from: spherical, hemispherical, compressed hemispherical, cylindrical, disk-shaped, circular, lentil-shaped, elliptical, cubic, rectangular, star-shaped, flower-shaped, and combinations thereof; wherein preferably each of said perfume particles has a hemispherical or compressed hemispherical shape; and/or
ii) a longest dimension of 3mm to 10mm, preferably 4mm to 9mm, more preferably 5mm to 8 mm; and/or
iii) an aspect ratio of 1 to 5, preferably 1.5 to 4, more preferably 2 to 4; and/or
iv) at 0.5g/cm3To 0.98g/cm3Preferably 0.7g/cm3To 0.95g/cm3More preferably 0.8g/cm3To 0.9g/cm3Density within the range.
9. The composition according to any preceding claims, wherein the composition is a particulate laundry detergent composition; wherein the plurality of antimicrobial particles is preferably present in the particulate laundry detergent composition in an amount in the range of from 0.05% to 30%, preferably from 0.1% to 20%, more preferably from 0.5% to 15%, most preferably from 1% to 10% by total weight of the particulate laundry detergent composition.
10. The composition according to claim 9, wherein the particulate laundry detergent composition further comprises from 10% to 99.9%, preferably from 20% to 95%, more preferably from 30% to 90%, most preferably from 40% to 80% of detergent particles; wherein each of the detergent particles preferably comprises from 10 wt% to 90 wt% of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, zwitterionic surfactants, and combinations thereof.
11. A method for treating an article of clothing, the method comprising the steps of:
a) providing an article of clothing in a washing machine; and
b) contacting the article of clothing with the composition of any of the preceding claims during a wash sub-cycle of the washing machine.
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