阅读说明：本技术 包含增白剂的液体织物处理组合物 (Liquid fabric treatment composition comprising a whitening agent ) 是由 J·斯梅茨 C·E·A·朱斯 帕斯卡莱·克莱尔·扬尼克·凡斯廷温克尔 于 2019-08-14 设计创作，主要内容包括：本发明涉及液体织物处理组合物及其制备和使用方法。此类织物处理组合物包含有益剂胶囊、增白剂和季铵酯软化活性物质。此类织物处理组合物表现出改善的有益剂胶囊在织物上、尤其是棉织物上的沉积。(The present invention relates to liquid fabric treatment compositions and methods of making and using the same. Such fabric treatment compositions comprise benefit agent capsules, a whitening agent and a quaternary ammonium ester softening active. Such fabric treatment compositions exhibit improved deposition of benefit agent capsules onto fabrics, especially cotton fabrics.)

1. A liquid fabric treatment composition comprising, by weight of the composition:

a)0.1ppm to 200ppm of a benefit agent capsule, wherein the benefit agent capsule comprises a shell material encapsulating a core material, wherein the shell material is derived from polyvinyl alcohol and a shell component, wherein the shell component is selected from the list consisting of: polyacrylates, polyamines, melamine formaldehyde, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof; the core material comprises a benefit agent;

b)0.1 to 50ppm of a whitening agent selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof; and

c) from 10ppm to 2000ppm of a quaternary ammonium ester softening active.

2. A liquid fabric treatment composition according to claim 1, wherein the whitening agent is selected from the list consisting of:

and mixtures thereof, wherein M is a suitable cation, preferably M is H⁺Or Na⁺More preferably M is Na⁺(ii) a Preferably, the whitening agent is selected from the list consisting of:

and mixtures thereof; more preferably, the whitening agent isAnd/orMost preferably, the whitening agent is

3. A liquid fabric treatment composition according to any preceding claim, wherein polyvinyl alcohol is present at a level of from 0.01% to 20%, preferably from 0.05% to 10%, even more preferably from 0.1% to 5%, most preferably from 0.1% to 2% by weight of the benefit agent capsule.

4. A liquid fabric treatment composition according to any preceding claim, wherein the shell component is selected from the list consisting of: polyacrylates, polyamines, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof; preferably, the shell component is selected from the list consisting of: polyamines, polyureas, polyurethanes, polyacrylates, and mixtures thereof; more preferably, the shell component is selected from the group consisting of polyureas, polyacrylates, and mixtures thereof.

5. A liquid fabric treatment composition according to any preceding claim, wherein the level of brightener is from 0.5ppm to 30ppm, preferably from 1ppm to 20ppm, more preferably from 1ppm to 10ppm, most preferably from 1ppm to 5ppm by weight of the fabric treatment composition.

6. A liquid fabric treatment composition according to any preceding claim, wherein the polyvinyl alcohol has a degree of hydrolysis of from 70% to 99%, preferably from 75% to 98%, more preferably from 80% to 96%, most preferably from 82% to 96%.

7. A liquid fabric treatment composition according to any preceding claim, wherein the polyvinyl alcohol has a viscosity of from 2 to 150mpa.s, preferably from 3 to 70mpa.s, more preferably from 4 to 60mpa.s, most preferably from 5 to 55mpa.s, as a 4 wt% aqueous solution.

8. A liquid fabric treatment composition according to any preceding claim, wherein the weight ratio of polyvinyl alcohol to brightener is from 1/1 to 1/5000, preferably from 1/2 to 1/2000, more preferably from 1/5 to 1/1000, most preferably from 1/10 to 1/500.

9. A liquid fabric treatment composition according to any preceding claim, wherein the ratio of brightener to benefit agent capsules is from 50/1 to 1/500, more preferably from 10/1 to 1/250, most preferably from 5/1 to 1/100.

10. A liquid fabric treatment composition according to any preceding claim, wherein the quaternary ammonium ester softening active has the formula:

{R² _4-m-N⁺-[X-Y–R¹]_m}A^-

wherein:

m is 1,2 or 3, provided that the value of each m is the same;

each R¹Independently a hydrocarbyl or substituted hydrocarbyl group;

each R²Independently is C₁-C₃Alkyl or hydroxyalkyl radicals, preferably R²Selected from methyl, ethyl, propyl, hydroxyethyl, 2-hydroxypropyl, 1-methyl-2-hydroxyethyl, poly (C)_2-3Alkoxy), polyethoxy, benzyl;

each X is independently (CH)₂)n、CH₂-CH(CH₃) -or CH- (CH)₃)-CH₂-and

each n is independently 1,2, 3 or 4, preferably each n is 2;

each Y is independently-O- (O) C-or-C (O) -O-;

a-is independently selected from the group consisting of chloride, methosulfate, ethanesulfate, and sulfate, preferably a-is selected from the group consisting of chloride and methosulfate;

provided that when Y is-O- (O) C-, each R¹The total number of carbon atoms is from 11 to 21, preferably when Y is-O- (O) C-, each R¹The total amount of carbon is 11 to 19.

11. A liquid fabric treatment composition according to any preceding claim, wherein the quaternary ammonium ester softening active comprises fatty acid moieties comprising from 12 to 22 carbons, the quaternary ammonium ester being selected from the group consisting of:

a) bis- (2-hydroxypropyl) -dimethylammonium methylsulfate fatty acid ester;

b) isomers of bis- (2-hydroxypropyl) -dimethylammonium methylsulfate fatty acid esters;

c) n, N-bis (hydroxyethyl) -N, N-dimethylammonium chloride fatty acid ester;

d) n, N-bis (hydroxyethyl) -N, N-dimethylammonium methylsulfate fatty acid ester; and

e) n, N-tris (2-hydroxyethyl) -N-methylammonium methylsulfate fatty acid ester;

the fatty acid ester portion of the quaternary ammonium ester softening active is saturated or unsaturated, and substituted or unsubstituted.

12. A liquid fabric treatment composition according to any preceding claim, wherein quaternary ammonium ester softening active surfactant is present at a level of from 20ppm to 1000ppm, preferably from 50ppm to 500ppm, more preferably from 100ppm to 400ppm by weight of the fabric treatment composition.

13. A liquid fabric treatment composition according to any preceding claim, wherein benefit agent capsules are present in an amount of from 1ppm to 100ppm, preferably from 2ppm to 80ppm, more preferably from 3ppm to 50ppm by weight of the fabric treatment composition.

14. A process for preparing a liquid fabric treatment composition according to any preceding claim, comprising the steps of:

a. providing a composition comprising a whitening agent selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof;

b. mixing the composition comprising the whitening agent of step a) with an aqueous solution to form a diluted composition comprising the whitening agent;

c. providing a composition comprising a quaternary ammonium ester softening active and a benefit agent capsule;

d. mixing the composition of step c) comprising a quaternary ammonium ester softening active with the diluted composition of step b) comprising a brightener to form a liquid fabric treatment composition according to any one of the preceding claims.

15. Use of a liquid fabric treatment composition according to any preceding claim to increase the deposition of benefit agent capsules on fabric, preferably cotton fabric.

Technical Field

The present invention relates to fabric treatment compositions comprising benefit agent capsules and whitening agents, and methods of making and using the same.

Background

Liquid fabric treatment compositions for use in laundry washing processes provide benefits to fabrics delivered by benefit agents. One example of such a benefit is the maintenance of the bright appearance provided by the whitening agent. Other examples include softness (provided by softening actives) and pleasant odor provided by perfumes. One problem in the art is that many benefit agents, especially perfumes, are not deposited or rinsed off during fabric treatment. Since perfumes and other benefit agents are expensive components, encapsulation can be used to improve the delivery of benefit agents during use. Benefit agent capsules typically contain a benefit agent until the capsule breaks during use, thereby releasing the benefit agent. Thus, when the benefit agent capsules containing the perfume are broken, the perfume release provides a freshening benefit.

However, effective deposition of benefit agent capsules onto treated fabrics remains a challenge, particularly where the benefit agent capsules are contained in dilute fabric treatment compositions for treating fabrics. It has previously been determined that deposition aids can improve deposition of benefit agent capsules. However, the addition of deposition aids to fabric treatment compositions complicates the manufacturing process because it requires additional tanks and pumps, thus increasing costs.

Accordingly, there remains a need to provide a composition to improve the deposition of benefit agent capsules on fabrics to enhance the delivery of benefit agents, thereby providing longer lasting benefits during and after use of liquid fabric treatment compositions, while minimizing cost and formulation complexity. Applicants have discovered that some or all of the above-described needs may be met, at least in part, by an improved composition, as described below.

WO2016049456 a1 relates to capsule aggregates comprising two or more beneficial particles, each comprising an active and a polymeric material immobilizing the active; one or more binder polymers, each having a negatively charged or capable of negatively charged anionic chemical group; and one or more deposition polymers, each having a cationic chemical group that is or can be positively charged. WO201701385 relates to benefit agent capsules coated by a specific mixture of copolymers. US20170189283 a1 relates to microcapsule compositions comprising benefit agent capsules coated with a deposition protein, such as a protein-silanol copolymer, a protein-silane copolymer, a protein-siloxane copolymer, or a cationically modified protein.

Disclosure of Invention

The present invention relates to a fabric treatment composition comprising: a benefit agent capsule; a whitening agent selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof; and a quaternary ammonium ester softening active, wherein the benefit agent capsule comprises a shell material, wherein the shell material is derived from polyvinyl alcohol and a shell component, wherein the shell component is selected from the list consisting of: polyacrylates, polyamines, melamine formaldehyde, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof; the core material comprises a benefit agent.

The invention also relates to methods for making and using such fabric treatment compositions.

It is an object of the present invention to improve the deposition of benefit agent capsules on fabrics, especially cotton fabrics.

It is another object of the present invention to provide softness and bright color retention to the treated fabric.

Detailed Description

Definition of

As used herein, the term "fabric treatment composition" is a subset of cleaning and treatment compositions, which, unless otherwise indicated, includes multi-functional or "heavy-duty" detergents, especially cleaning detergents, in granular or powder form; multipurpose detergents in the form of liquids, gels or pastes, especially the so-called heavy-duty liquid types; liquid fine fabric detergents; liquid cleaning and disinfecting agents, fabric conditioning products (including softening and/or freshening), which may be in liquid, solid and/or dryer paper form; and cleaning adjuvants such as bleach additives and "stain-stick" or substrate-laden pretreatment-type products such as dryer paper, dry and wet wipes and pads, nonwoven substrates and sponges; as well as sprays and mists. All such products that are applicable may be in standard, concentrated or even highly concentrated form, even to the extent that such products may be non-aqueous in some way.

As used herein, articles such as "a" and "an" when used in a claim are understood to mean one or more of what is claimed or described.

As used herein, the terms "comprising," "including," and "containing" are intended to be non-limiting.

As used herein, the term "solid" includes granular, powder, bar, lentil, bead and tablet product forms.

As used herein, the term "fluid" includes liquid, gel, paste, slurry, and gaseous product forms.

Unless otherwise specified, all components or compositions are on average with respect to the active portion of that component or composition, and do not include impurities, such as residual solvents or by-products, that may be present in commercially available sources of such components or compositions.

All percentages and ratios are by weight unless otherwise indicated. All percentages and ratios are calculated based on the total composition, unless otherwise indicated.

It should be understood that every maximum numerical limitation given throughout this specification includes every lower numerical limitation, as if such lower numerical limitations were expressly written herein. Every minimum numerical limitation given throughout this specification will include every higher numerical limitation, as if such higher numerical limitations were expressly written herein. Every numerical range given throughout this specification will include every narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were all expressly written herein.

Fabric treatment composition

The liquid fabric treatment composition according to the present invention comprises by weight of the fabric treatment composition: 0.1ppm to 200ppm of a benefit agent capsule, wherein the benefit agent capsule comprises a shell material encapsulating a core material, wherein the shell material is derived from polyvinyl alcohol and a shell component, wherein the shell component is selected from the list consisting of: polyamines, melamine formaldehyde, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof; the core material comprises a benefit agent; 0.1 to 50ppm of a whitening agent selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof; and from 10ppm to 2000ppm of a quaternary ammonium ester softening active.

Whitening agent

The liquid fabric treatment composition comprises from 0.1ppm to 50ppm of a whitening agent selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof. It has surprisingly been found that the whitening agent provides improved deposition of benefit agent capsules, wherein the benefit agent capsules comprise a shell material encapsulating a core material, wherein the shell material is derived from polyvinyl alcohol and a shell component. Without being bound by theory, it is believed that deposition of benefit agent capsules is improved by the interaction between the polyvinyl alcohol and the whitening agent and quaternary ammonium ester softening active according to the present invention.

In preferred liquid fabric treatment compositions, the whitening agent is selected from the list consisting of:

and mixtures thereof, wherein M is a suitable cation, preferably M is H⁺Or Na⁺More preferably M is Na⁺(ii) a Preferably, the whitening agent is selected from the list consisting of:

and mixtures thereof;

more preferably, the whitening agent is

And/orMost preferably, the whitening agent is

Examples of suitable diaminostilbene whitening agents are available under the trade nameDMA-X、AMS-GX、DMA-X Conc、AMS Slurry 43、5BM-GX was supplied by BASF, by 3V Sigma as Optibrec and by Meghmani as Megawhite DMX-C. Examples of suitable biphenyl brighteners are available under the trade names:CBS, supplied by BASF; and Keyfluor^TMWhite ML, supplied by Milliken.

In preferred fabric treatment compositions, less than 1%, more preferably less than 0.01% of the total amount of whitening agent in the fabric treatment composition is encapsulated in benefit agent capsules according to the present invention. The unencapsulated brightener provides a bright appearance and improved benefit agent encapsulation deposition to the treated fabric.

In preferred fabric treatment compositions, the total level of whitening agent is from 0.5ppm to 30ppm, preferably from 1ppm to 20ppm, more preferably from 1ppm to 10ppm, most preferably from 1ppm to 5ppm by weight of the fabric treatment composition.

In preferred fabric treatment compositions, the ratio of whitening agent to benefit agent capsules is from 50/1 to 1/500, more preferably from 10/1 to 1/250, most preferably from 5/1 to 1/100.

Beneficial agent capsule

The liquid fabric treatment composition comprises from 0.1ppm to 200ppm benefit agent capsules comprising a core material and a shell material encapsulating the core material, wherein the shell material is derived from polyvinyl alcohol and a shell component, wherein the shell component is selected from the list consisting of: polyacrylates, polyamines, melamine formaldehyde, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof.

The level of benefit agent capsules may depend on the desired total level of free and encapsulated benefit agents in the fabric treatment composition. In preferred fabric treatment compositions, the benefit agent capsules are present in an amount of from 1ppm to 100ppm, preferably from 2ppm to 80ppm, more preferably from 3ppm to 50ppm by weight of the fabric treatment composition. Herein, "benefit agent capsule content" refers to the sum of shell material and core material.

In a preferred composition, the shell component is selected from the list consisting of: polyacrylates, polyamines, polyureas, polyurethanes, polysaccharides, modified polysaccharides, urea crosslinked with formaldehyde, urea crosslinked with glutaraldehyde, silica, sodium silicate, polyesters, polyacrylamides, and mixtures thereof; more preferably, the shell component is selected from the list consisting of: polyamines, polyureas, polyurethanes, polyacrylates, and mixtures thereof; even more preferably, the shell component is selected from the group consisting of polyureas, polyacrylates, and mixtures thereof; most preferably, the shell component is a polyacrylate.

The shell component may comprise from about 50% to about 100%, or from about 70% to about 100%, or from about 80% to about 100%, of the polyacrylate polymer. The polyacrylate may include a polyacrylate cross-linked polymer.

The shell material may comprise a material selected from the group consisting of: polyacrylates, polyethylene glycol acrylates, polyurethane acrylates, epoxy acrylates, polymethacrylates, polyethylene glycol methacrylates, polyurethane methacrylates, epoxy methacrylates, and mixtures thereof.

The shell material of the capsule may comprise a polymer derived from a substance comprising one or more multifunctional acrylate moieties. The multifunctional acrylate moiety may be selected from the group consisting of: trifunctional acrylates, tetrafunctional acrylates, pentafunctional acrylates, hexafunctional acrylates, heptafunctional acrylates, and mixtures thereof. The multifunctional acrylate moiety is preferably a hexafunctional acrylate. The shell material may comprise a polyacrylate comprising a moiety selected from the group consisting of: acrylate moieties, methacrylate moieties, amine acrylate moieties, amine methacrylate moieties, carboxylic acid acrylate moieties, carboxylic acid methacrylate moieties, and combinations thereof, preferably amine methacrylate or carboxylic acid acrylate moieties.

The shell material may comprise a material comprising one or more multifunctional acrylate and/or methacrylate moieties. The ratio of material comprising one or more multifunctional acrylate moieties to material comprising one or more methacrylate moieties may be from about-999: 1 to about 6:4, preferably from about 99:1 to about 8:1, more preferably from about 99:1 to about 8.5: 1.

In one aspect, the shell component is a polyurea or polyurethane. Capsules of shell components derived from polyurea or polyurethane may be prepared using one or more polyisocyanates and one or more crosslinkers.

Polyisocyanates are molecules having two or more isocyanate groups, i.e. O ═ C ═ N ", where the polyisocyanates can be aromatic, aliphatic, linear, branched or cyclic. In certain embodiments, the polyisocyanate contains an average of 2 to 4-N ═ C ═ O groups. In a particular embodiment, the polyisocyanate comprises at least three isocyanate functional groups. In certain embodiments, the polyisocyanate is water insoluble.

The polyisocyanate may be an aromatic or aliphatic polyisocyanate. The desired aromatic polyisocyanates each have a phenyl, tolyl, xylyl, naphthyl or diphenyl moiety or a combination thereof as the aromatic component. In certain embodiments, the aromatic polyisocyanate is polymeric methylene diphenyl diisocyanate ("PMDI"), polyisocyanurate of toluene diisocyanate, trimethylolpropane adduct of toluene diisocyanate, or trimethylolpropane adduct of xylylene diisocyanate.

Suitable aliphatic polyisocyanates include the trimer of hexamethylene diisocyanate, the trimer of isophorone diisocyanate or the biuret of hexamethylene diisocyanate. Further examples include those commercially available, such as BAYHYDUR N304 and BAYHYDUR N305, which are aliphatic water dispersible polyisocyanates based on hexamethylene diisocyanate; DESMODUR N3600, DESMODUR N3700, and DESMODUR N3900, which are low viscosity multifunctional aliphatic polyisocyanates based on hexamethylene diisocyanate; and DESMODUR 3600 and DESMODUR N100, which are aliphatic polyisocyanates based on hexamethylene diisocyanate, all available from Bayer Corporation (Pittsburgh, Pa.).

Specific examples of wall monomer polyisocyanates include 1, 5-naphthylene diisocyanate, 4' -diphenylmethane diisocyanate (MDI), hydrogenated MDI (H12MDI), Xylylene Diisocyanate (XDI), tetramethylxylene diisocyanate (TMXDI), 4' -diphenyldimethylmethane diisocyanate, dialkyldiphenylmethane diisocyanates and tetraalkyldiphenylmethane diisocyanates, 4' -dibenzyl diisocyanate, 1, 3-phenylene diisocyanate, 1, 4-phenylene diisocyanate, isomers (optionally as a mixture) of Tolylene Diisocyanate (TDI), 1-methyl-2, 4-diisocyanatocyclohexane, 1, 6-diisocyanato-2, 2, 4-trimethylhexane, Toluene Diisocyanate (TDI), and mixtures thereof, 1, 6-diisocyanato-2, 4, 4-trimethylhexane, 1-isocyanatomethyl-3-isocyanato-1, 5, 5-trimethylcyclohexane, chlorinated and brominated diisocyanates, phosphorus-containing diisocyanates, 4,4' -diisocyanatophenylperfluoroethane, tetramethoxybutane 1, 4-diisocyanate, butane 1, 4-diisocyanate, hexane 1, 6-diisocyanate (HDI), dicyclohexylmethane diisocyanate, cyclohexane 1, 4-diisocyanate, ethylene diisocyanate, diisocyanatoethyl phthalate, and polyisocyanates having reactive halogen atoms, such as 1-chloromethylphenyl 2, 4-diisocyanate, 1-bromomethylphenyl 2, 6-diisocyanate and 3, 3-bischloromethyl ether 4,4' -diphenyl diisocyanate.

Other suitable commercially available polyisocyanates include LUPRANATE M20(PMDI, commercially available from BASF, containing 31.5% by weight of isocyanate groups "NCO"), wherein the average n is 0.7; PAPI 27(PMDI, commercially available from Dow Chemical, average molecular weight 340 and containing 31.4 wt% NCO) where the average n is 0.7; MONDUR MR (PMDI, containing 31 wt% or more NCO, commercially available from Bayer), wherein the average n is 0.8; MONDUR MR Light (PMDI, containing 31.8 wt% NCO, commercially available from Bayer), wherein the average n is 0.8; MONDUR 489(PMDI, commercially available from Bayer, containing 30 wt.% to 31.4 wt.% NCO) with an average n of 1.0; poly [ (phenylisocyanate) -co-formaldehyde ] (Aldrich Chemical, Milwaukee, Wis.), other isocyanate monomers such as DESMODUR N3200 (poly (hexamethylene diisocyanate), commercially available from Bayer) and TAKENATE D110-N (xylene diisocyanate adduct polymer, commercially available from Mitsui Chemicals (Rye Brook, n.y.), contains 11.5 wt.% NCO), DESMODUR L75 (a toluene diisocyanate-based polyisocyanate, commercially available from Bayer), DESMODUR IL (another toluene diisocyanate-based polyisocyanate, commercially available from Bayer) and DESMODUR (a polyisocyanurate of toluene diisocyanate).

Some suitable polyisocyanates have an average molecular weight ranging from 250Da to 1000Da, preferably from 275Da to 500 Da. Generally, the polyisocyanate concentration ranges from 0.1% to 10%, preferably from 0.1% to 8%, more preferably from 0.2% to 5%, even more preferably from 1.5% to 3.5%, all percentages being by weight of the capsule delivery system.

Crosslinkers suitable for use with the polyisocyanate each contain a plurality (i.e., two or more) of functional groups (e.g., -NH-, -NH2, and-OH) that can react with the polyisocyanate to form a polyurea or polyurethane. Examples include polyfunctional amines (e.g., polyamines) containing two or more amine groups, polyfunctional alcohols (e.g., polyols) containing two or more hydroxyl groups, epoxy crosslinkers, acrylate crosslinkers, and hybrid crosslinkers containing one or more amine groups and one or more hydroxyl groups.

The amine groups in the crosslinker include-NH 2 and R NH, R being substituted and unsubstituted C₁-C₂₀Alkyl radical, C₁-C₂₀Heteroalkyl group, C₁-C₂₀Cycloalkyl, 3-to 8-membered heterocycloalkyl, aryl, and heteroaryl.

Two such classes of polyamines include polyalkylene polyamines having the following structure:

wherein R is hydrogen or-CH₃(ii) a And m, n, x, y, and z are each independently integers from 0 to 2000 (e.g., 1,2, 3, 4, or 5).

Examples include ethylenediamine, 1, 3-diaminopropane, diethylenetriamine, triethylenetetramine, 1, 4-diaminobutane, hexaethylenediamine, hexamethylenediamine, pentaethylenehexamine, melamine, and the like.

Another class of polyamines are the following classes of polyalkylene polyamines:

wherein R is equal to hydrogen or-CH₃M is 1 to 5 and n is 1 to 5, for example, diethylenetriamine, triethylenetetramine and the like. Exemplary amines of this type also include diethylenetriamine, bis (3-aminopropyl) amine, bis (3-aminopropyl) ethylenediamine, bis (hexamethylene) triamine.

Another class of amines useful in the present invention are polyetheramines. They comprise primary amino groups attached to the ends of a polyether backbone. The polyether backbone is typically based on propylene oxide (P0), Ethylene Oxide (EO) or mixed P0/EQ. Based on the core structure, the ether amine can be a monoamine, diamine, or triamine. One example is:

exemplary polyetheramines include 2,2- (ethylenedioxy) -bis (ethylamine) and 4,7, 10-trioxa-1, 13-tridecanediamine.

Other suitable amines include, but are not limited to, tris (2-aminoethyl) amine, triethylenetetramine, N, N ' -bis (3-aminopropyl) -1, 3-propanediamine, tetraethylenepentamine, 1, 2-diaminopropane, 1, 2-diaminoethane, N, N, N ', N ' -tetrakis (2-hydroxyethyl) ethylenediamine, N, N, N ', N ' -tetrakis (2-hydroxypropyl) ethylenediamine, N, N, N ', N ' -tetrakis (3-aminopropyl) -1, 4-butanediamine, 3, 5-diamino-1, 2, 4-triazole, branched polyethyleneimines, 2, 4-diamino-6-hydroxypyrimidines, and 2,4, 6-triaminopyrimidines.

Branched polyethyleneimines useful as crosslinking agents typically have a molecular weight of 200Da to 2,000,000Da (e.g., 800Da to 2,000,000Da, 2,000Da to 1,000,000Da, 10,000Da to 200,000Da, and 20,000Da to 100,000 Da).

Amphoteric amines, i.e., amines that can react as an acid as well as a base, are another class of amines useful in the present invention. Examples of amphoteric amines include proteins and amino acids such as gelatin, L-lysine, D-lysine, L-arginine, D-arginine, L-lysine monohydrochloride, D-lysine monohydrochloride, L-arginine monohydrochloride, D-arginine monohydrochloride, L-ornithine monohydrochloride, D-ornithine monohydrochloride, or mixtures thereof.

Guanamines and guanidine salts are another class of polyfunctional amines useful in the present invention. Exemplary guanamines and guanidine salts include, but are not limited to, 1, 3-diaminoguanidine monohydrochloride, 1-dimethylbiguanide hydrochloride, guanidine carbonate, and guanidine hydrochloride.

Commercially available examples of amines include JEFFAMINE EDR-148 (where n is 2), JEFFAMINE EDR-176 (where n is 3) (available from Huntsman) having the structure shown above. Other polyetheramines include the JEFFAMINE ED series, JEFFAMINE TRIAMINES, polyethyleneimines available from BASF (Ludwigshafen, Germany) on the LUPASOL scale (e.g., LUPASOL FG, LUPASOL G20 anhydrous, LUPASOL PR 8515, LUPASOL WF, LUPASOL FC, LUPASOL G20, LUPASOL G35, LUPASOL G100, LUPASOL G500, LUPASOL HF, LUPASOL PS, LUPASOL HEO 1, LUPASOL PNSO, LUPASOL PN6O, LUPASOL P0100, and LUPASOL SK). Other commercially available polyethyleneimines include EPOMIN P-1000, EPOMIN P-1050, EPOMIN RP18W, and EPOMIN PP-061, available from NIPPON SHOKUBA (N.Y). Polyvinylamines, such as those sold by BASF on the LUPAMINE scale, may also be used. A wide range of polyetheramines can be selected by those skilled in the art. In certain embodiments, the crosslinking agent is hexaethylenediamine, polyetheramine, or mixtures thereof.

The range of the polyfunctional amine, polyfunctional alcohol, or mixed crosslinker may vary from 0.1% to 10% (e.g., from 0.2% to 3%, 0.2% to 2%, 0.5% to 2%, or 0.5% to 1%) by weight of the capsule delivery system.

The capsules may comprise an emulsifier, wherein the emulsifier is preferably selected from anionic emulsifiers, nonionic emulsifiers, cationic emulsifiers or mixtures thereof, preferably nonionic emulsifiers.

The shell material of the capsule is derived from polyvinyl alcohol, preferably in an amount of from 0.01% to 20%, more preferably from 0.05% to 10%, even more preferably from 0.1% to 5%, most preferably from 0.1% to 2% by weight of the capsule. The polyvinyl alcohol may reside partially within the shell of the capsule and may reside partially on the outer surface of the shell. Preferably, the polyvinyl alcohol has at least one of the following properties, or a mixture thereof:

(i) a degree of hydrolysis of from 70% to 99%, preferably from 75% to 98%, more preferably from 80% to 96%, more preferably from 82% to 96%, most preferably from 86% to 94%;

(ii) a viscosity of from 2 to 150, preferably from 3 to 70, more preferably from 4 to 60, even more preferably from 5 to 55mPa.s in a 4% aqueous solution at 20 ℃.

In preferred fabric treatment compositions, the weight ratio of polyvinyl alcohol to brightener is from 1/1 to 1/5000, preferably from 1/2 to 1/2000, more preferably from 1/5 to 1/1000, most preferably from 1/10 to 1/500.

Suitable polyvinyl alcohol materials may be selected from Selvol 540PVA (Sekisui Specialty Chemicals, Dallas, TX), Mowiol 18-88 ═ Poval 18-88, Mowiol 3-83, Mowiol 4-98 ═ Poval 4-98(Kuraray), Poval KL-506 ═ Poval 6-77KL (Kuraray), Poval R-1130 ═ Poval 25-98R (Kuraray), Gohsenx K-434(Nippon Gohsei).

Perfume compositions are preferred encapsulated benefit agents that improve the odor of fabrics treated with fabric treatment compositions. The perfume composition comprises a perfume raw material. The encapsulated benefit agent may further comprise essential oils, malodor reducing agents, odor control agents, silicones, and combinations thereof.

Perfume raw materials are typically present in an amount of from 10% to 99%, preferably from 20% to 98%, more preferably from 70% to 96% by weight of the capsule.

The perfume composition may comprise from 2.5% to 30%, preferably from 5% to 30%, by weight of the perfume composition, of perfume raw materials characterized by a logP of less than 3.0 and a boiling point of less than 250 ℃.

The perfume composition may comprise from 5% to 30%, preferably from 7% to 25%, by weight of the perfume composition, of perfume raw materials characterized by a logP of less than 3.0 and a boiling point of greater than 250 ℃. The perfume composition may comprise from 35% to 60%, preferably from 40% to 55%, by weight of the perfume composition, of perfume raw materials characterized by a logP above 3.0 and a boiling point below 250 ℃. The perfume composition may comprise from 10% to 45%, preferably from 12% to 40%, by weight of the perfume composition, of perfume raw materials characterized by a logP above 3.0 and a boiling point above 250 ℃.

Preferably, the core further comprises a partitioning modifier. Suitable partitioning modifiers include vegetable oils, modified vegetable oils, propan-2-yl tetradecanoate, and mixtures thereof. The modified vegetable oil may be esterified and/or brominated. The vegetable oil comprises castor oil and/or soybean oil. The partitioning modifier may be propan-2-yl tetradecanoate. The partitioning modifier may be present in the core at a level of greater than 10%, or greater than 10% to about 80%, or greater than 20% to about 70%, or greater than 20% to about 60%, or about 30% to about 50%, based on the total weight of the core.

Preferably, the capsules have a volume weighted average particle size of from 0.5 microns to 100 microns, preferably from 1 micron to 60 microns, even more preferably from 5 microns to 45 microns.

For example, polyacrylate benefit agent capsules are available from Encapsys (825East Wisconsin Ave, Appleton, WI 54911) and can be made with, for example, perfume as a benefit agent as follows: a first oil phase consisting of 37.5g of perfume, 0.2g of t-butylaminoethyl methacrylate and 0.2g of beta-hydroxyethyl acrylate was mixed for about 1 hour, then 18g of CN975(Sartomer, Exter, Pa.) was added. The solutions are mixed until needed later in the process.

A second oil phase consisting of 65g of perfume oil, 84g of isopropyl myristate, 1g of 2,2 '-azobis (2-methylbutyronitrile) and 0.8g of 4,4' -azobis [ 4-cyanovaleric acid ] was added to a jacketed steel reactor. The reactor was maintained at 35 ℃ and the oil solution was mixed with a 2 "flat blade mixer at 500 rpm. A nitrogen blanket was applied to the reactor at a flow rate of 300 cc/min. The solution was heated to 70 ℃ over 45 minutes and held at 70 ℃ for 45 minutes, after which it was cooled to 50 ℃ over 75 minutes. At 50 ℃, the first oil phase was added and the combined oils were mixed for an additional 10 minutes at 50 ℃.

An aqueous phase containing 85g of Selvol 540PVA (Sekisui Specialty Chemicals, Dallas, TX) as 5% solids, 268g of water, 1.2g of 4,4 '-azobis [ 4-cyanovaleric acid ] and 1.1g of 21.5% NaOH was prepared and mixed until the 4,4' -azobis [ 4-cyanovaleric acid ] was dissolved.

Once the oil phase temperature was reduced to 50 ℃, mixing was stopped and the water phase was added to the mixed oil. High shear agitation was applied to produce an emulsion with the desired dimensional characteristics (1900rpm for 60 minutes).

The temperature was raised to 75 ℃ over 30 minutes, held at 75 ℃ for 4 hours, raised to 95 ℃ over 30 minutes, and held at 95 ℃ for 6 hours.

Quaternary ammonium ester softening actives

The liquid fabric treatment composition of the present invention comprises from 10ppm to 2000ppm, preferably from 20ppm to 1000ppm, more preferably from 50ppm to 500ppm, most preferably from 100ppm to 400ppm of a quaternary ammonium ester softening active (fabric softening active, "FSA"). The level of quaternary ammonium ester softening active may depend on the desired concentration of total softening active as well as the presence or absence of other softening actives.

Without being bound by theory, applicants believe that the deposition of benefit agent capsules, particularly the affinity for cotton fabrics, is improved by at least partially coating the benefit agent capsules.

Preferably, the parent fatty acid from which the quaternary ammonium fabric softening active is formed has an iodine value of from 5 to 60, more preferably from 10 to 45, even more preferably from 15 to 40. Without being bound by theory, a lower melting point is obtained when the parent fatty acid from which the quaternary ammonium fabric softening active is formed is at least partially unsaturated, rendering the FSA easier to process. Especially di-unsaturated fatty acids, can easily process FSA.

Suitable quaternary ammonium ester softening actives include, but are not limited to, materials selected from the group consisting of: mono-esterquat, di-esterquat, tri-esterquat and mixtures thereof. Preferably, the monoester quaternary ammonium softening compounds are present in an amount of from 2.0% to 40.0%, the diester quaternary ammonium softening compounds are present in an amount of from 40.0% to 98.0%, and the triester quaternary ammonium softening compounds are present in an amount of from 0.0% to 25.0%, by weight of the total quaternary ammonium ester softening active.

The quaternary ammonium ester softening active may comprise a compound of the formula:

{R² _(4-m)-N+-[X-Y–R¹]_m}A-

wherein:

m is 1,2 or 3, provided that the value of each m is the same;

each R¹Independently a hydrocarbyl or branched hydrocarbyl group, preferably R¹Is straight chain, more preferably R¹Is a linear alkyl chain that is partially unsaturated;

each R²Independently is C₁-C₃Alkyl or hydroxyalkyl radicals, preferably R²Selected from methyl, ethyl, propyl, hydroxyethyl, 2-hydroxypropyl, 1-methyl-2-hydroxyethyl, poly (C)_2-3-alkoxy), polyethoxy, benzyl;

each X is independently- (CH)₂)_n-、-CH₂-CH(CH₃) -or-CH (CH)₃)-CH₂-, and

each n is independently 1,2, 3 or 4, preferably each n is 2;

each Y is independently-O- (O) C-or-C (O) -O-;

a-is independently selected from the group consisting of chloride, methosulfate and ethanesulfate, preferably a-is selected from the group consisting of chloride and methosulfate;

provided that when Y is-O- (O) C-, each R¹The total number of carbons is 11 to 21, preferably 11 to 19.

In preferred liquid fabric treatment compositions, the quaternary ammonium ester softening active comprises fatty acid moieties having from 12 to 22 carbons, the quaternary ammonium ester being selected from the group consisting of:

a) bis- (2-hydroxypropyl) -dimethylammonium methylsulfate fatty acid ester;

b) isomers of bis- (2-hydroxypropyl) -dimethylammonium methylsulfate fatty acid esters;

c) n, N-bis (hydroxyethyl) -N, N-dimethylammonium chloride fatty acid ester;

d) n, N-bis (hydroxyethyl) -N, N-dimethylammonium methylsulfate fatty acid ester; and

e) n, N-tris (2-hydroxyethyl) -N-methylammonium methylsulfate fatty acid ester;

the fatty acid ester portion of the quaternary ammonium ester softening active is saturated or unsaturated, and substituted or unsubstituted.

Examples of suitable quaternary ammonium ester softening actives are commercially available from KAO Chemicals under the trade names Tetranyl AT-1 and Tetranyl AT-7590, from Evonik under the trade names Rewoquat WE16DPG, Rewoquat WE18, Rewoquat WE20, Rewoquat WE28 and Rewoquat 38DPG, from Stepan under the trade names Stepatex GA90, Stepatex VR90, Stepatex VK90, Stepancatex VA90, Stepancatex DC90, Stepancatex VL 90A.

Adjuvant materials

The fabric treatment composition may comprise additional ingredients, such as those selected from the group consisting of: polymeric deposition aids, organic builders and/or chelating agents, enzymes, enzyme stabilizers, shading dyes, particulate matter, cleaning polymers, external structurants and mixtures thereof.

Polymeric deposition aid: the base mix may comprise from 0.1% to 7%, more preferably from 0.2% to 3% of a polymeric deposition aid. As used herein, "polymeric deposition aid" refers to any cationic polymer or combination of cationic polymers that significantly enhances the deposition of fabric care benefit agents onto fabrics during laundering. Suitable polymeric deposition aids may comprise cationic polysaccharides and/or copolymers. As used herein, "benefit agent" refers to any material that can provide fabric care benefits. Non-limiting examples of fabric care benefit agents include: silicone derivatives, oily sugar derivatives, dispersed polyolefins, polymer latexes, cationic surfactants, and combinations thereof. Preferably, the deposition aid is a cationic polymer or an amphoteric polymer. The cationic charge density of the polymer is preferably in the range of 0.05 to 6 meq/g. The charge density is calculated by dividing the number of net charges per repeat unit by the molecular weight of the repeat unit. In one embodiment, the charge density varies from 0.1 meq/g to 3 meq/g. The positive charge may be located on the backbone of the polymer or on a side chain of the polymer.

Organic builders and/or chelating agents: the base mixture may comprise from 0.6% to 10%, preferably from 2% to 7% by weight of one or more organic builders and/or chelating agents. Suitable organic builders and/or chelating agents are selected from the group consisting of: MEA citrate, citric acid, aminoalkylene poly (alkylene phosphonates), alkali metal ethane 1-hydroxy bisphosphonates, and nitrilotrimethylene phosphonates, diethylenetriamine penta (methylene phosphonic acid) (DTPMP), ethylenediamine tetra (methylene phosphonic acid) (DDTMP), hexamethylenediamine tetra (methylene phosphonic acid), hydroxy-ethylene-1, 1-diphosphonic acid (HEDP), hydroxyethane dimethylene phosphonic acid, ethylenediamine disuccinic acid (EDDS), ethylenediamine tetraacetic acid (EDTA), hydroxyethyl ethylenediamine triacetic acid (HEDTA), nitrilotriacetic acid (NTA), Methyl Glycine Diacetate (MGDA), iminodisuccinic acid (IDS), hydroxyethyliminodisuccinic acid (HIDS), hydroxyethyliminodiacetic acid (HEIDA), glycine diacetate (GLDA), diethylenetriamine pentaacetic acid (DTPA), Catecholsulfonates such as tiron (tm) and mixtures thereof.

Toning dye: hueing dyes, shading dyes or fabric hueing or hueing agents are laundry aids which may be used in the fluid laundry detergent composition. The long history of these materials in laundry washing has originated from the use of "laundry bluing agents" years ago. Recent developments have included the use of sulfonated phthalocyanine dyes having a zinc or aluminum central atom; and, more recently, a wide variety of other blue and/or violet dyes have been used for their hueing or coloring effect. See, e.g., WO 2009/087524a1, WO2009/087034a1, and references therein. The fluid laundry detergent compositions herein typically comprise from 0.00003 wt% to 0.1 wt%, from 0.00008 wt% to 0.05 wt% or even from 0.0001 wt% to 0.04 wt% of fabric hueing agent.

Particulate matter: suitable particulate materials are clays, suds suppressors, microcapsules (e.g. with encapsulated ingredients such as perfume), bleaching agents and enzymes in encapsulated form; or aesthetic aids such as pearlizing agents, pigment particles, mica, and the like. Particularly preferred particulate materials are microcapsules, especially perfume microcapsules. Microcapsules are typically formed by at least partially, preferably completely, surrounding the benefit agent with a wall material. Preferably, the microcapsules are perfume microcapsules, wherein the benefit agent comprises one or more perfume raw materials. Suitable amounts are from 0.0001% to 5% or from 0.1% to 1% by weight of the fabric treatment composition.

Spice: suitable perfumes are known in the art and are typically incorporated at levels of from 0.001% to 10%, preferably from 0.01% to 5%, more preferably from 0.1% to 3% by weight.

Cleaning polymer: suitable cleaning polymers provide a wide range of surface and fabric soil cleaning and/or soil suspension. Any suitable cleaning polymer may be used. Useful cleaning polymers are described in USPN 2009/0124528a 1. Non-limiting examples of useful classes of cleaning polymers include: an amphiphilic alkoxylated grease cleaning polymer; clay soil cleaning polymers; a soil release polymer; and soil-suspending polymers.

Process for preparing a liquid fabric treatment composition

The process for preparing a liquid fabric treatment composition according to the invention comprises the steps of:

a. providing a composition comprising a whitening agent selected from the list consisting of:

diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof;

b. mixing the composition comprising the whitening agent of step a) with an aqueous solution to form a diluted composition comprising the whitening agent;

c. providing a composition comprising a quaternary ammonium ester softening active and a benefit agent capsule;

d. mixing the composition of step c) comprising the quaternary ammonium ester softening active and the benefit agent capsules with the diluted composition of step b) comprising the whitening agent.

Use of liquid fabric treatment compositions

Applicants have surprisingly found that the whitening agent in the liquid fabric treatment composition according to the present invention, selected from the list consisting of: diaminostilbene whitening agents, biphenyl whitening agents, and mixtures thereof. Without being bound by theory, applicants believe that improved benefit agent capsule deposition, particularly affinity for cotton fabrics, results from the interaction between the brightener and the polyvinyl alcohol and quaternary ammonium ester fabric softening actives of the benefit agent capsules, even in relatively dilute liquid fabric treatment compositions.

Method

Method for treating fabric

A mini washer model 1001 (which is a small washer simulator with a U.S. top-loading design) is used to treat fabrics. For each set, the mini-washer tube was loaded with 100g of fabric comprising 20g of knitted polyester (supplied by WFK) and 80g of knitted cotton (supplied by WFK). 4 non-whitened cotton wool tracer (supplied by WFK) of size 4cm by 4cm were also added for headspace analysis. 3L of tap water at 40 ℃ and 14.7g of liquid detergent composition were added to each tube. The fabrics were treated with the liquid detergent in a mini-washer tube for 45 minutes to simulate the main wash of a washing machine. After 45 minutes, the fabric was centrifuged for 5 minutes while the water was spun off. After the main wash, the fabrics were treated with a liquid fabric treatment composition comprising a quaternary ammonium ester softening active, benefit agent capsules and a whitening agent during 7 at 25 ℃. After 7 minutes, the fabric was centrifuged again for 12 minutes. The cotton fabric was taken out and hung dry at night. The next day, the dried fabric was analyzed as follows to determine the headspace concentration above the treated fabric.

Method for determining headspace concentration above a treated fabric

The dried non-whitened cotton tracer was analyzed by the fast headspace GC/MS (gas chromatography mass spectrometry) method. A 4 x 4cm aliquot of the cotton tracer was transferred to a 25mL headspace vial. The fabric samples were equilibrated at 75 ℃ for 10 minutes. The headspace above the fabric was sampled for 5 minutes via the SPME (50/30 μm DVB/Carboxen/PDMS) method. The SPME fiber was then immediately thermally desorbed into the GC. Analytes were analyzed by fast GC/MS in full scan mode. Ion extractions of specific masses of PRMs were used to calculate the total HS response and perfume headspace composition above the test group.

Method for measuring viscosity of polyvinyl alcohol solution

The viscosity was measured using a Brookfield LV series viscometer or equivalent and was measured at 4.00% +/-0.05% solids.

a. A solid solution of 4.00% +/-0.05% polyvinyl alcohol was prepared.

Weigh 500mL beaker and stirrer. The weight was recorded. A16.00 +/-0.01 gram sample of polyvinyl alcohol was added to the beaker. Approximately 350mL to 375mL of deionized water was added to the beaker and the solution was stirred. The beaker was placed in a hot water bath with a lid. Stirring at moderate speed for 45 minutes to 1 hour, or until the polyvinyl alcohol is completely dissolved. The agitator was turned off. The beaker was cooled to about 20 ℃.

The final weight of the beaker was calculated as follows:

final weight ═ weight of empty beaker and stirrer) + (solid% in decimal x 400)

Example (b): weight of the empty beaker and stirrer was 125.0 g

Polyvinyl alcohol (sample) 97.50% solids or 0.9750 (as decimal)

Final weight 125.0+ (0.9750 × 400) 515.0 g

The top load balance was zeroed and a beaker of polyvinyl alcohol solution and a propeller were placed on top of it. Deionized water was added to bring the weight to the calculated final weight of 515.0 grams.

The solids content of the sample must be 4.00+ 0.05% to measure viscosity.

b. Measurement of viscosity

Samples of 4% polyvinyl alcohol solution were dispensed into the chamber of the viscometer, the spindle was inserted and attached to the viscometer. Sample Adapter (SSA) with chamber SC4-13RPY, Ultralow adapter. Mandrels SC4-18 and 00. The sample was allowed to equilibrate at a temperature of 20 ℃. The viscometer was started and the steady state viscosity value was recorded.

The viscosity was reported as <13cP to 0.01cP, 13cP to 100cP to 0.1 cP; viscosities in excess of 100cP are reported to the nearest 1 cP.

If the calculated solution solids content is 4.00+ -0.05%, no correction for the measured viscosity is necessary. Otherwise, the following formula is used to correct the measured viscosity of the solution solids deviation.

Log_eCorrected viscosity ═ _e(Log measurement of viscosity)

(percent solids) × (0.2060) + (0.1759)

Corrected viscosity 2.718282 (logarithm of corrected viscosity)

Examples

The polyacrylate spice capsules were prepared as follows: a first oil phase consisting of 37.5g of perfume, 0.2g of t-butylaminoethyl methacrylate and 0.2g of beta-hydroxyethyl acrylate was mixed for about 1 hour, then 18g of CN975(Sartomer, Exter, Pa.) was added. The solutions are mixed until needed later in the process.

A second oil phase consisting of 65g of perfume oil, 84g of isopropyl myristate, 1g of 2,2 '-azobis (2-methylbutyronitrile) and 0.8g of 4,4' -azobis [ 4-cyanovaleric acid ] was added to a jacketed steel reactor. The reactor was maintained at 35 ℃ and the oil solution was mixed with a 2 "flat blade mixer at 500 rpm. A nitrogen blanket was applied to the reactor at a flow rate of 300 cc/min. The solution was heated to 70 ℃ over 45 minutes and held at 70 ℃ for 45 minutes, after which it was cooled to 50 ℃ over 75 minutes. At 50 ℃, the first oil phase was added and the combined oils were mixed for an additional 10 minutes at 50 ℃.

An aqueous phase containing 85g of Selvol 540PVA (Sekisui Specialty Chemicals, Dallas, TX) as 5% solids, 268g of water, 1.2g of 4,4 '-azobis [ 4-cyanovaleric acid ] and 1.1g of 21.5% NaOH was prepared and mixed until the 4,4' -azobis [ 4-cyanovaleric acid ] was dissolved.

Once the oil phase temperature was reduced to 50 ℃, mixing was stopped and the water phase was added to the mixed oil. High shear agitation was applied to produce an emulsion with the desired dimensional characteristics (1900rpm for 60 minutes).

The temperature was raised to 75 ℃ over 30 minutes, held at 75 ℃ for 4 hours, raised to 95 ℃ over 30 minutes, and held at 95 ℃ for 6 hours.

Fabrics were treated according to the method described in the method section using liquid fabric treatment compositions examples 1 to 2. The whitening agent 15 was added to example 2 using a premix. The brightener 15 premix was made by mixing together the brightener 15, diethylene glycol, and monoethanolamine in a plastic beaker with a blade mixer.

Brightener 15 corresponds to the formula

The premix is made to enable a uniform distribution of the whitening agent. The detailed compositions of the fabric treatment compositions (examples 1 to 2) are provided in table 1.

Table 1: composition details of comparative example 1 and inventive example 2。

1N, N-bis (hydroxyethyl) -N, N-dimethylammonium chloride fatty acid ester. The iodine value of the parent fatty acid of this material was about 20.

The material from Evonik contains impurities in the form of free fatty acids, impurities in the form of monoesters of N, N-bis (hydroxyethyl) -N, N-dimethylammonium chloride fatty acid esters, and impurities in the form of fatty acid esters of N, N-bis (hydroxyethyl) -N-methylamine.

The headspace above the dry treated cotton fabric showed an increase from 129nmol/L to 154 nmol/L. This increase was determined to be significant at a 90% confidence level using student's t-test.

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".