WO2002081612A1

WO2002081612A1 - Fabric softene compositions

Info

Publication number: WO2002081612A1
Application number: PCT/EP2002/003313
Authority: WO
Inventors: Harald Chrobaczek; Rainer Augart; Günther Tschida; Werner Stechele; Jürgen Uhl; Cornelia Scholz; Michael Geubtner; Rolf Moors; Petr Kvita; Barbara Weber; Mario Dubini
Original assignee: Ciba Specialty Chemicals Holding Inc.; Ciba Spezialitätenchemie Pfersee GmbH
Priority date: 2001-04-03
Filing date: 2002-03-25
Publication date: 2002-10-17

Abstract

The present invention relates to a fabric softener composition fo r the treatment of textile fibre materials in domestic applications, which softener composition comprises: A) a fabric softerner; and B) an aluminium salt of a polysilicic acid.

Description

Fabric softener compositions

The present invention relates to fabric softener compositions comprising a fabric softener and an aluminium salt of a polysilicic acid. Furthermore, the present invention relates to a method of use of the aluminium salt of a polysilicic acid to improve various properties of textile fibre materials in domestic applications.

New fabrics and clothes hang or drape in a manner which it is desirable to preserve for as long as possible in order to keep their "new" appearance. Similarly the textile has a feeling to the hand which it is also desirable to maintain. Unfortunately repeated laundering of cloth results in cumulative microscopic fibre damage resulting in increasing distortions to the fabric which require ironing to remove. Additionally, deposits on the cloth are exacerbated by the same damage and result in an increasing rough feel to the cloth.

Regular use of softener compositions in the laundering process are known to improve drape and the hand feel of fabrics by retarding the symptoms of fibre damage. However, there is a need to boost these effects without resorting to the use of excessive levels of softener which is impractical for reasons such as unacceptably high cost, fabric discolouration, waterproofing and a hand feel which may not be rough, yet is uncomfortable. Therefore there exists a need for compositions which provide fabrics with a "new looking" drape and a smooth feel.

Wrinkles in fabrics are caused by the bending and creasing of the textile material which places an external portion of a filament in a yarn under tension while the internal portion of that filament in the yarn is placed under compression. Particularly with cotton fabrics, the hydrogen bonding that occurs between the cellulose molecules contributes to keeping wrinkles in place. The wrinkling of fabric, in particular clothing, is therefore subject to the inherent tensional elastic deformation and recovery properties of the fibres which constitute the yarn and fabrics.

There is a demand for a quick fix which will help to diminish the labour involved in home laundering and/or the cost and time involved in dry cleaning or commercial laundering. This has brought additional pressure to bear on textile technologists to produce a product that will sufficiently reduce wrinkles in fabrics, especially clothing, and to produce a good appearance through a simple, convenient application of a product.

Another property which it would be desirable to impart is the reduction of wet soiling. Some wrinkle recovery treatments have the disadvantage that wet soiling is adversely effected. Hence, it is often also necessary to treat the textile material further to improve its wet soiling characteristics. It would therefore be desirable to find a process according to which wrinkle recovery as well as wet soiling is improved.

Needless to say, fabric materials currently on use both in the clothing use of people and in the industrial applications are in a very large part produced of synthetic fibers or traditional natural fibers. One of the largest differences between the properties of the synthetic and natural fibers is in the hydrophilicity-hydrophobicity behavior of them, the former fibers being of course outstandingly less hydrophilic than the latter. The remarkably small hydrophilicity of synthetic fibers sometimes causes serious problems not encountered in the use of natural fibers. For example, fabric materials made of synthetic fibers have a very poor capacity of water or sweat absorption, which is advantageous on one hand but disadvantageous on the other, so that wearers of clothes made of synthetic fibers unavoidably have an unpleasant feeling of heavy stuffiness especially when the clothes are underwears worn in contact with or in the proximity of the skin of the wearer in a hot and humid climate. Another serious problem caused by the poor hydrophilicity of synthetic fibers is the great accumulation of static electricity on the fibers causing unpleasantness to the wearer of clothes of synthetic fibers in such a charged condition. Many attempts have of course been proposed and practiced in the prior art to solve these problems by increasing the hydrophilicity of the fabric materials of synthetic fibers and also natural fibres. For example, the problem of poor water absorption of synthetic fibers can be mitigated by the mixed spinning or mixed weaving with water-absorptive natural fibers. The effectiveness of this method is, however, limited since too much amounts of the natural fibers mixed with the synthetic fibers to attain sufficient hydrophilicity of the fabric material naturally result in the loss of the advantages inherent to synthetic fibers. An alternative method is the treatment of the fabric material of synthetic fibers with a water-absorbent agent to impart hydrophilicity to the surface of the fibers. Extensive investigations have been and are being undertaken in this direction to propose various kinds of water-absorbent agents effective for a particular type of synthetic fibers. For example, the capacity of water absorption of polyester fibers, e.g. polyethylene terephthalate fibers, can be increased by the treatment with a water-soluble polyester resin. Unfortunately, such a method of the treatment of synthetic fibers with a water-soluble resin is defective in several respects of the poor durability of the effects obtained therewith and the adverse influences on the color fastness of dyed fabric materials in many cases.

As is well known, the pill formed on worn clothing markedly detracts from the appearance and feel of the clothing. The occurrence of pill is particularly a problem in the field of knitted materials, so that it has been greatly desired to seek measures for preventing the occurrence of pill on knitted fibre materials.

Abrasion or friction induced wear in fabrics created by motion both during wear and in the laundering process is an important feature in the ageing of garments. This is evidenced by a progressive reduction in the mechanical strength of fabric measured by, for example, the tensile strength of a test strip. In extreme cases, this wear finally results in the actual teasing of cloth. Visually, areas of garments subjected to relatively extreme abrasion such as cuffs or collars can develop signs of wear which very obviously detract from the appearance of clothing.

It is known that the regular use of fabric softeners using various quaternary ammonium moieties can mitigate friction-induced wear (WO 97/36976). Without being bound by theory, it is believed that this is achieved by a lubrication of fibres and a consequent raising of the resistance of the cloth to abrasional wear and tear. Efforts to extend this protection by using higher levels of softener are impractical from both cost and technical perspectives. Accordingly, there is a need for additives or adjuncts to state of the art softener formulations which will boost their power to resist f rictional wear without the aforementioned drawbacks.

Surprisingly, it has been found that the use of aluminium salts of polysilicic acids in fabric softener compositions can improve the above properties.

Accordingly, the present invention relates to a fabric softener composition for the treatment of textile fibre materials in domestic applications, which softener composition comprises:

A) a fabric softener; and

B) an aluminium salt of a polysilicic acid. The aluminium salts of polysilicic acids used according to the present invention are known or can be prepared according to known methods. As to such preparations it is preferred that polysilicic acid is reacted with a basic aluminium chloride. Examples are basic aluminium hydroxyl chlorides, like AI₂(OH)₅CI. Usually the reaction is carried out in aqueous medium, at temperatures of from 20 to 100°C, especially 40 to 80°C. Furthermore, it is preferred that the reaction is carried out at a pH value of from 1 to 6, especially 2 to 5. The pH value can be adjusted by addition of an organic or anorganic acid. Organic acids, like acetic acid, are preferred.

It is advantageous, especially with respect to handling, to prepare the aluminium salts of polysilicic acids in the form of aqueous formulations. For this purpose the reaction product is mixed with water, wherein the aluminium salts of polysilicic acids are used in an amount of 0.1 to 60 % by weight, based on the total weight of the aqueous formulation. An amount of 5 to 60 % by weight, especially 10 to 60% by weight, is preferred. Highly preferred is an amount of 20 to 60 % by weight. The formulations preferably have a pH value of from 1 to 6, especially 1 to 5. Highly preferred is a pH value of from 2 to 4. The formulations can be stabilised with respect to the pH value by addition of common buffer systems, like acetic acid/sodium acetate.

Furthermore, the formulations can contain common additives. Examples are hydrotropic agents, like ε-caprolactam and urea.

In some cases it may be advantageous for the preparation of the aqueous formulation to add emulsifiers suitable for dispersing the aluminium salts of polysilicic acids. Examples for suitable emulsifiers include the following: i) Ethoxylates, such as alkyl ethoxylates, amine ethoxylates or amide ethoxylates. Alkyl ethoxylates include alcohol ethoxylates or isotridecyl ethoxylates. Preferred alcohol ethoxylates include nonionic fatty alcohol ethoxylates containing 2 to 55 ethylene oxide units. Preferred isotridecyl ethoxylates include nonionic isotridecyl ethoxylates containing 5 to 45 ethylene oxide units. Preferred amine ethoxylates include nonionic C10 to C20 alkyl amino ethoxylates containing 4 to 25 ethylene oxide units. Preferred amide ethoxylates include cationic fatty acid amide ethoxylates containing 2 to 25 ethylene oxide units. ii) Alkylammonium halides, preferably cationic quaternary ester alkylammonium halides or cationic aliphatic acid alkylamidotrialkylammonium methosulfates. iii) Ammonium salts, preferably cationic aliphatic quaternary ammonium chloride or sulfate.

Usually no emulsifiers need to be added to prepare the aqueous formulation of the aluminium salts of polysilicic acids.

Preferably, the aluminium salt of a polysilicic acid has a specific surface area of 20 to 800 m²/g, especially a specific surface area of 50 to 400 m²/g. Highly preferred is a specific surface area of 100 to 300 m²/g.

The determination of the specific surface area can, for example, be carried out according to G.W. Sears, Analytical Chem. 28, No. 12, pages 1981ff (1956).

Fabric softeners, especially hydrocarbon fabric softeners, suitable for use herein are selected from the following classes of compounds:

(i) Cationic quaternary ammonium salts. The counter ion of such cationic quaternary ammonium salts may be a halide, such as chloride or bromide, methyl sulphate, or other ions well known in the literature. Preferably the counter ion is methyl sulfate or any alkyl sulfate or any halide, methyl sulfate being most preferred for the dryer-added articles of the invention.

Examples of cationic quaternary ammonium salts include but are not limited to:

(1) Acyclic quaternary ammonium salts having at least two C₈ to C₃₀, preferably C₁₂ to C₂₂ alkyl or alkenyl chains, such as: ditallowdimethyl ammonium methylsulfate, di(hydrogenated tallow)dimethyl ammonium methylsulfate, distearyldimethyl ammonium methylsulfate, dicocodimethyl ammonium methylsulfate and the like. It is especially preferred if the fabric softening compound is a water insoluble quaternary ammonium material which comprises a compound having two C₁₂ to C₁₈ alkyl or alkenyl groups connected to the molecule via at least one ester link. It is more preferred if the quaternary ammonium material has two ester links present. An especially preferred ester-linked quaternary ammonium material for use in the invention can be represented by the formula:

wherein each Rn group is independently selected from Ci. to C₄ alkyl, hydroxyalkyl or C₂ to C alkenyl groups; T is either -O-C(O)- or -C(O)-O-, and wherein each Rι₂ group is independently selected from C₈ to C₂₈ alkyl or alkenyl groups; and e is an integer from 0 to 5.

A second preferred type of quaternary ammonium material can be represented by the formula:

wherein Rn, e and R₁₂ are as defined above.

(2) Cyclic quaternary ammonium salts of the imidazolinium type such as di(hydrogenated tallow)dimethyl imidazolinium methylsulfate, 1-ethylene-bis(2-tallow-1 -methyl) imidazolinium methylsulfate and the like;

(3) Diamido quaternary ammonium salts such as: methyl-bis(hydrogenated tallow amidoethyl)-2-hydroxethyl ammonium methyl sulfate, methyl bi(tallowamidoethyl)-2- hydroxypropyl ammonium methylsulfate and the like;

(4) Biodegradable quaternary ammonium salts such as N,N-di(tallowoyl-oxy-ethyl)-N,N- dimethyl ammonium methyl sulfate and N,N-di(tallowoyl-oxy-propyl)-N,N-dimethyl ammonium methyl sulfate. Biodegradable quaternary ammonium salts are described, for example, in U.S. Patents 4,137,180, 4,767,547 and 4,789,491 incorporated by reference herein.

Preferred biodegradable quaternary ammonium salts include the biodegradable cationic diester compounds as described in U.S. Patent 4,137,180, herein incorporated by reference. (ii) Tertiary fatty amines having at least one and preferably two C8 to C30, preferably C12 to C22 alkyl chains. Examples include hardened tallow-di-methylamine and cyclic amines such as 1 -(hydrogenated tallow)amidoethyl-2-(hydrogenated tallow) imidazoline. Cyclic amines which may be employed for the compositions herein are described in U.S. Patent 4,806,255 incorporated by reference herein.

(iii) Carboxylic acids having 8 to 30 carbons atoms and one carboxylic group per molecule. The alkyl portion has 8 to 30, preferably 12 to 22 carbon atoms. The alkyl portion may be linear or branched, saturated or unsaturated, with linear saturated alkyl preferred. Stearic acid is a preferred fatty acid for use in the composition herein. Examples of these carboxylic acids are commercial grades of stearic acid and palmitic acid, and mixtures thereof which may contain small amounts of other acids.

(iv) Esters of polyhydric alcohols such as sorbitan esters or glycerol stearate. Sorbitan esters are the condensation products of sorbitol or iso-sorbitol with fatty acids such as stearic acid. Preferred sorbitan esters are monoalkyl. A common example of sorbitan ester is SPAN 60 (ICI) which is a mixture of sorbitan and isosorbide stearates.

(v) Fatty alcohols, ethoxylated fatty alcohols, alkyphenols, ethoxylated alkyphenols, ethoxylated fatty amines, ethoxylated monoglycerides and ethoxylated diglycerides.

(vi) Mineral oils, and polyols such as polyethylene glycol.

These softeners are more definitively described in U.S. Patent 4,134,838 the disclosure of which is incorporated by reference herein. Preferred fabric softeners for use herein are acyclic quaternary ammonium salts. Di(hydrogenated)tallowdimethyl ammonium methylsulfate is most widely used for dryer articles of this invention. Mixtures of the above mentioned fabric softeners may also be used.

The fabric softening composition employed in the present invention preferably contains about 0.1 to about 95 % by weight, based on the total weight of the fabric softening composition, of the fabric softening component. Preferred is an amount of 0.5 to 50 % by weight, especially an amount of 2 to 50 % by weight and most preferably an amount of 2 to 30 % by weight.

The amount of the aluminium salts of polysilicic acids in the fabric softening composition is preferably 0.005 to 10 % by weight, based on the total weight of the fabric softening composition. Preferred is an amount of 0.01 to 10 % by weight, especially an amount of 0.05 to 5 % by weight and most preferably an amount of 0.1 to 4 % by weight.

The fabric softening composition may also comprise additives which are customary for standard commercial fabric softening compositions, for example alcohols, such as ethanol, n-propanol, i-propanol, polyhydric alcohols, for example glycerol and propylene glycol; amphoteric and nonionic surfactants, for example carboxyl derivatives of imidazole, oxyethylated fatty alcohols, hydrogenated and ethoxylated castor oil, alkyl polyglycosides, for example decyl polyglucose and dodecylpolyglucose, fatty alcohols, fatty acid esters, fatty acids, ethoxylated fatty acid glycerides or fatty acid partial glycerides; also inorganic or organic salts, for example water-soluble potassium, sodium or magnesium salts, non- aqueous solvents, pH buffers, perfumes, dyes, hydrotropic agents, antifoams, anti redeposition agents, polymeric or other thickeners, enzymes, optical brighteners, antishrink agents, stain removers, germicides, fungicides, antioxidants and corrosion inhibitors.

Such additives are preferably used in an amount of 0 to 30 % by weight, based on the total weight of the fabric softening composition. Preferred is an amount of 0 to 20 % by weight, especially an amount of 0 to 10 % by weight and most preferably an amount of 0 to 5 % by weight.

The fabric softener compositions are preferably in liquid aqueous form. The fabric softener compositions preferably contain a water content of 25 to 90% by weight based on the total weight of the composition. More preferably the water content is 50 to 90% by weight, especially 60 to 90 % by weight.

The fabric softener compositions preferably have a pH value from 2.0 to 9.0, especially 2.0 to 5.0. Preferred are fabric softener compositions which do not contain a substantial amount of a polyorganosiloxane.

The fabric softener compositions can, for example, be prepared as follows: Firstly, an aqueous formulation of the aluminium salt of a polysilicic acid is prepared as described above. The fabric softener composition according to the invention is usually, but not exclusively, prepared by firstly stirring the active substance, i.e. the hydrocarbon based fabric softening component, in the molten state into water, then, where required, adding further desired additives and, finally, after cooling, adding the formulation of the aluminium salt of a polysilicic acid. The fabric softener composition can, for example, also be prepared by mixing a preformulated fabric softener with an aqueous formulation of the aluminium salt of a polysilicic acid.

These fabric softener compositions are traditionally prepared as dispersions containing for example up to 30 % by weight of active material in water. They usually have a turbid appearance. However, alternative formulations usually containing actives at levels of 5 to 40 % along with solvents can be prepared as microemulsions which have a clear appearance (as to the solvents and the formulations see for example US-A-5,543,067 und WO-A- 98/17757). The aluminium salts of polysilicic acids of the present invention can be used for such compositions although it will be necessary to use them in microemulsion form to preserve the clear appearance of the fabric softener compositions which are microemulsions.

A highly preferred fabric softener composition according to the present invention is in liquid form and comprises:

A) 0.5 to 50 % by weight, based on the total weight of the composition, of the fabric softener;

B) 0.005 to 10 % by weight, based on the total weight of the composition, of the aluminium salt of a polysilicic acid;

C) 0 to 20 % by weight, based on the total weight of the composition, of customary additives; and

D) water to 100 %.

The fabric softener compositions can also be used in the form of tumble dryer sheet composition. In tumble dryer applications the compositions are usually incorporated into impregnates on non-woven sheets. However, other application forms are known to those skilled in the art.

The conditioning composition of the present invention may be coated onto a flexible substrate which carries a fabric conditioning amount of the composition and is capable of releasing the composition at dryer operating temperatures. The conditioning composition in turn has a preferred melting (or softening) point of about 25°C to about 150°C.

The fabric conditioning composition which may be employed in the invention is coated onto a dispensing means which effectively releases the fabric conditioning composition in a tumble dryer. Such dispensing means can be designed for single usage or for multiple uses. One such multi-use article comprises a sponge material releasably enclosing enough of the conditioning composition to effectively impart fabric softness during several drying cycles. This multi-use article can be made by filling a porous sponge with the composition. In use, the composition melts and leaches out through the pores of the sponge to soften and condition fabrics. Such a filled sponge can be used to treat several loads of fabrics in conventional dryers, and has the advantage that it can remain in the dryer after use and is not likely to be misplaced or lost.

Another article comprises a cloth or paper bag releasably enclosing the composition and sealed with a hardened plug of the mixture. The action and heat of the dryer opens the bag and releases the composition to perform its softening.

A highly preferred article comprises the inventive compositions releasably affixed to a flexible substrate such as a sheet of paper or woven or non-woven cloth substrate. When such an article is placed in an automatic laundry dryer, the heat, moisture, distribution forces and tumbling action of the dryer removes the composition from the substrate and deposits it on the fabrics.

The sheet conformation has several advantages. For example, effective amounts of the compositions for use in conventional dryers can be easily absorbed onto and into the sheet substrate by a simple dipping or padding process. Thus, the end user need not measure the amount of the composition necessary to obtain fabric softness and other benefits. Additionally, the flat configuration of the sheet provides a large surface area which results in efficient release and distribution of the materials onto fabrics by the tumbling action of the dryer.

The substrates used in the articles can have a dense, or more preferably, open or porous structure. Examples of suitable materials which can be used as substrates herein include paper, woven cloth, and non-woven cloth. The term "cloth" herein means a woven or non- woven substrate for the articles of manufacture, as distinguished from the term "fabric" which encompasses the clothing fabrics being dried in an automatic dryer.

It is known that most substances are able to absorb a liquid substance to some degree; however, the term "absorbent", as used herein, is intended to mean a substrate with an absorbent capacity (i.e., a parameter representing a substrates ability to take up and retain a liquid) from 4 to 12, preferably 5 to 7 times its weight of water.

If the substrate is a foamed plastics material, the absorbent capacity is preferably in the range of 15 to 22, but some special foams can have an absorbent capacity in the range from 4 to 12.

Determination of absorbent capacity values is made by using the capacity testing procedures described in U.S. Federal Specifications (UU-T-595b), modified as follows:

1. tap water is used instead of distilled water;

2. the specimen is immersed for 30 seconds instead of 3 minutes;

3. draining time is 15 seconds instead of 1 minute; and

4. the specimen is immediately weighed on a torsion balance having a pan with turned-up edges.

Absorbent capacity values are then calculated in accordance with the formula given in said Specification. Based on this test, one-ply, dense bleached paper (e.g., Kraft or bond having a basis weight of about 32 pounds per 3,000 square feet) has an absorbent capacity of 3.5 to 4; commercially available household one-ply towel paper has a value of 5 to 6; and commercially available two-ply household towelling paper has a value of 7 to about 9.5. Suitable materials which can be used as a substrate in the invention herein include, among others, sponges, paper, and woven and non-woven cloth, all having the necessary absorbency requirements defined above.

The preferred non-woven cloth substrates can generally be defined as adhesively bonded fibrous or filamentous products having a web or carded fiber structure (where the fiber strength is suitable to allow carding), or comprising fibrous mats in which the fibers or filaments are distributed haphazardly or in random array (i.e. an array of fibers is a carded web wherein partial orientation of the fibers is frequently present, as well as a completely haphazard distributional orientation), or substantially aligned. The fibers or filaments can be natural (e.g. wool, silk, jute, hemp, cotton, linen, sisal, or ramie) or synthetic (e.g. rayon, cellulose ester, polyvinyl derivatives, polyolefins, polyamides, or polyesters).

The preferred absorbent properties are particularly easy to obtain with non-woven cloths and are provided merely by building up the thickness of the cloth, i.e., by superimposing a plurality of carded webs or mats to a thickness adequate to obtain the necessary absorbent properties, or by allowing a sufficient thickness of the fibers to deposit on the screen. Any diameter or denier of the fiber (generally up to about 10 denier) can be used, inasmuch as it is the free space between each fiber that makes the thickness of the cloth directly related to the absorbent capacity of the cloth, and which, further, makes the non-woven cloth especially suitable for impregnation with a composition by means of intersectional or capillary action. Thus, any thickness necessary to obtain the required absorbent capacity can be used.

When the substrate for the composition is a non-woven cloth made from fibers deposited haphazardly or in random array on the screen, the articles exhibit excellent strength in all directions and are not prone to tear or separate when used in the automatic clothes dryer.

Preferably, the non-woven cloth is water-laid or air-laid and is made from cellulosic fibers, particularly from regenerated cellulose or rayon. Such non-woven cloth can be lubricated with any standard textile lubricant.

Preferably, the fibers are from 5 mm to 50 mm in length and are from 1.5 to 5 denier. Preferably, the fibers are at least partially orientated haphazardly, and are adhesively bonded together with a hydrophobic or substantially hydrophobic binder-resin. Preferably, the cloth comprises about 70% fiber and 30% binder resin polymer by weight and has a basis weight of from about 18 to 45 g per square meter.

In applying the fabric conditioning composition to the absorbent substrate, the amount impregnated into and/or coated onto the absorbent substrate is conveniently in the weight ratio range of from about 10:1 to 0.5:1 based on the ratio of total conditioning composition to dry, untreated substrate (fiber plus binder). Preferably, the amount of the conditioning composition ranges from about 5:1 to about 1 :1 , most preferably from about 3:1 to 1 :1 , by weight of the dry untreated substrate.

According to one preferred embodiment of the invention, the dryer sheet substrate is coated by being passed over a rotogravure applicator roll. In its passage over this roll, the sheet is coated with a thin, uniform layer of molten fabric softening composition contained in a rectangular pan at a level of about 15g per square yard. Passage for the substrate over a cooling roll then solidifies the molten softening composition to a solid. This type of applicator is used to obtain a uniform homogeneous coating across the sheet.

Following application of the liquefied composition, the articles are held at room temperature until the composition substantially solidifies. The resulting dry articles, prepared at the composition substrate ratios set forth above, remain flexible; the sheet articles are suitable for packaging in rolls. The sheet articles can optionally be slitted or punched to provide a non-blocking aspect at any convenient time if desired during the manufacturing process.

The fabric softener composition will be used after the textile fibre materials have been washed with a laundry detergent, which may be one of a broad range of detergent types. The tumble dryer sheet will be used after a laundering process. The textile fibre materials may be damp or dry.

The fabric softener composition may also be sprayed directly onto the fabrics, for example prior to or during the ironing or drying of the treated fabrics.

Examples of suitable textile fibre materials which can be treated with the fabric softener compositions are materials made of silk, wool, polyamide, acrylics or polyurethanes, and, in particular, cellulosic fibre materials of all types. Such fibre materials are, for example, natural cellulose fibres, such as cotton, linen, jute and hemp, and regenerated cellulose. Preference is given to textile fibre materials made of cotton. The fabric softener compositions are also suitable for hydroxyl-containing fibres which are present in mixed fabrics, for example mixtures of cotton with polyester fibres or polyamide fibres.

A further object of the present invention is a method of use for an aluminium salt of a polysilicic acid to improve drape and smoothness, wrinkle recovery, hydrophilicity, wet soiling, abrasion resistance and/or antipilling of textile fibre materials in domestic applications.

As to the aluminium salts of polysilicic acids the meanings and preferences given above apply.

According to this embodiment of the present invention the aluminium salt of a polysilicic acid can be used, for example, in a rinse step of a laundering operation, with or without presence of a fabric softener. It is self-evident that the aluminium salt of a polysilicic acid can be added as a part of the fabric softening agent, or a fabric softening agent and the aluminium salt of a polysilicic acid are added separately.

The aluminium salt of a polysilicic acid can also be used together with a detergent in a laundering operation. For this application conventional detergents can be used. The aluminium salts of polysilicic acids can be used as a part of the detergent, or the aluminium salts of polysilicic acids are added separately.

According to a further application the aluminium salts of polysilicic acids are sprayed onto the textile fibre material. This application can be carried out according to known methods. For this treatment aqueous formulations of the aluminium salts of poylsilicic acids can be used. In these formulations the aluminium salts of poylsilicic acids can have the same concentration as in the fabric softener composition.

Furthermore, it is also possible to use the aluminium salts of polysilicic acids in a pre-soak application, wherein usually before the laundering process the textiles to be treated are pre- soaked in an aqueous bath containing the aluminium salts of polysilicic acids. For this treatment aqueous formulations of the aluminium salts of poylsilicic acids can be used. In these formulations the aluminium salts of polysilicic acids can have the same concentration as in the fabric softener composition.

The present invention helps remove wrinkles from fabrics, including clothing, dry cleanable fabrics and draperies, without the need for ironing. The present invention can be used on washed clothing, which is damp or dry, to relax wrinkles and give clothes a ready to wear look that is demanded by today's consumer. The present invention also essentially eliminates the need for touch up ironing usually associated with closet, drawer, and suitcase storage of garments.

When ironing is desired however, the present invention can also act as an excellent ironing aid. When used as an ironing aid, the aluminium salts of polysilicic acids produce a crisp, smooth appearance similar to that of spray starch ironing aids without the dry residue or flaking that occurs with typical spray starch ironing aids. It appears that recognition of improved "ease of ironing" can arise from a combination of at least three factors, namely fewer wrinkles to be removed, wrinkles more easily removed (e.g. with less weight upon the iron), or more completely removed, and less effort required to slide the iron along the fabric.

An additional benefit of the aluminium salts of polysilicic acids is an in-wear wrinkle control benefit. The present invention can help to prevent future wrinkles from forming in the fabric even after the fabric has been through a wash cycle, or a tumble drying process.

A better understanding of the present invention and of its many advantages will be had by referring to the following Examples, given by way of illustration. The percentages given in the examples are percentages by weight.

Example 1 a) Preparation of Formulation A (aluminium salt of polysilicic acid)

120 parts of an aqueous solution of AI₂(OH)₅CI-2-3 H₂O (50 %) and 25 parts of acetic acid

(60 %) are added to 340 parts of water under stirring. Stirring is continued and 390 parts of polysilicic acid (30 %, colloidal solution, specific surface area of 200 m²/g) are added. The reaction mixture is heated to a temperature of 63°C and stirred for further 105 minutes. Then

60 parts of urea, 63 parts of sodium chloride and 9 parts of sodium acetate 3-hydrate are added and stirring is continued for 20 minutes at a temperature of 63°C. After cooling to room temperature 105 parts of water are added. The resulting formulation has a pH value of 2.8 to 3.8. In the following this formulation is designated as Formulation A.

b) Preparation of Formulation B (aluminium salt of polysilicic acid)

120 parts of an aqueous solution of AI₂(OH)₅CI-2-3 H₂O (50 %) and 25 parts of acetic acid (60 %) are added to 340 parts of water under stirring. Stirring is continued and 390 parts of polysilicic acid (30 %, colloidal solution, specific surface area of 100 m²/g) are added. The reaction mixture is heated to a temperature of 63°C and stirred for further 105 minutes. Then 60 parts of e-caprolactam , 63 parts of sodium chloride and 9 parts of sodium acetate 3- hydrate are added and stirring is continued for 20 minutes at a temperature of 63°C. After cooling to room temperature 105 parts of water are added. The resulting formulation has a pH value of 2.8 to 3.8. In the following this formulation is designated as Formulation B.

c) Preparation of the fabric softener composition

The fabric softener compositions are prepared by using the procedure described below. This type of fabric softener composition is normally known under the name of "triple strength" or "triple fold" formula.

75 g of water is heated to 40°C. 15 g of the molten fabric softener di-(palmcarboxyethyl)- hydroxyethyl-methylammonium-methosulfate (or Rewoquat WE 38 DPG available from Witco) is added to the heated water under stirring and the mixture is stirred for 1 hour at 40°C. Afterwards the aqueous softener solution is cooled down to below 30°C while stirring. When the solution cools down 0.1 g of magnesium chloride is added and the pH is adjusted to 3.2 with 0.1 N hydrochloric acid. The formulation is then filled up with water to 100 g.

Then 3 g of Formulation A prepared as given above under a) (or 3 g of Formulation B prepared as given above under b)) are added to 100 g of the fabric softener composition prepared as given above. The fabric softener composition has a pH value of 3.2.

As a reference, a further fabric softener composition is prepared as given above, but without addition of the aqueous formulation of the aluminium salt of a polysilicic acid. This rinse conditioner formulation has a pH value of 3.2. Table 1 (fabric softener compositions used in the application test for 1 kg wash load)

Example 2 (Reduction of micro creases on cotton (prior to ironing))

The formulated fabric softener compositions (see Table 1 ) are applied according to the following procedure:

Woven cotton swatches of size of 50 cm by 40 cm are washed together with ballast material (cotton and cotton/polyester) in a AEG Oeko Lavamat 73729 washing machine maintaining the washing temperature at 40°C . The total fabric load of 1 kg is washed for 15 minutes with 33 g of ECE Color Fastness Test Detergent 77 (Formulation January 1977, according to ISO 105-CO6). The rinse conditioner formulation as described in Table 1 is applied in the last rinse cycle at 20°C. After rinsing with the formulation the textile swatches are dried on a washing line at ambient temperature.

Evaluation of micro creases

The creasing (surface smoothness) of the dried swatches is evaluated according to the

AATCC-Standard method Nr. 124. Five persons evaluate the creases of the cotton swatches against the AATCC THREE DIMENSIONAL Smoothness Appearance Replicas. On the evaluation scale a number of 1 means very strong creasing, whereas 5 means almost no creasing. Table 2 (Results of the evaluation of creases on cotton by AATCC method prior to ironing)

These above results show a marked improvement in crease recovery for the textile fabric material treated with compositions of the present invention.

Example 3 (Reduction of micro creases on cotton (after ironing))

The textile swatches (cotton woven) from Example 2 are divided in 2 parts and one of it (with a size of 20 cm to 40cm) is slightly rewetted with 6.5 ml water (fine sprayed over the textile surface) and ironed without pressure for 60 seconds at 160°C.

The micro creases of the ironed swatches are evaluated according AATCC-Standard method Nr. 124 as described in Example 2.

Table 3 (Results of the evaluation of creases on cotton by AATCC method after ironing)

These results show that microcreases can be removed significantly better by ironing when the textile fabric material is treated with compositions of the present invention.

Example 4 (Reduction of micro creases on cotton/polyester (prior to ironing))

The formulated rinse conditioners (see Table 1 ) are applied according to the following procedure:

Woven cotton/polyester swatches of size of 50 cm by 40 cm are washed and rinsed according to procedure described in Example 2. Evaluation of micro creases

The creasing (surface smoothness) of the dried swatches is evaluated according to procedure described in Example 2.

Table 4 (Results of the evaluation of creases on cotton/polyester by AATCC method prior to ironing)

The above results show an improvement in surface smoothness for the textile fabric material treated with compositions of the present invention.

Example 5 (Reduction of micro creases on cotton/polyester (after ironing))

The textile swatches (cotton/polyester woven) from Example 2 are divided in 2 parts and one of it (with a size of 20 cm to 40cm) is slightly rewetted with 6.5 ml water (fine sprayed over the textile surface) and ironed without pressure for 60 seconds at 160°C.

Table 5 (Results of the evaluation of creases on cotton/polyester by AATCC method after ironing)

These results show that surface smoothness is significantly improved by ironing when the textile fabric material is treated with compositions of the present invention. Example 6 (Reduction of wet soiling of cotton)

Treatment of the textile material

Woven cotton swatches of size of 50 cm by 40 cm are washed together with ballast material (cotton and cotton/polyester) in a AEG Oeko Lavamat 73729 washing machine maintaining the washing temperature at 40°C. The total fabric load of 1 kg is washed for 15 minutes with 33 g of ECE Color Fastness Test Detergent 77 (Formulation January 1977, according to ISO 105-CO6). The rinse conditioner formulation as described in Table 1 is applied in the last rinse cycle at 20°C. After rinsing with the formulation the textile swatches are dried on a washing line at ambient temperature.

Soiling procedure

The treated swatches are cut to 5g pieces and then "soiled" for 20 minutes in a Linitest apparatus at 80°C with a solution of

0.1 g/l Carbon black (Corax N765)

0.3 g/l Nonionic Surfactant (Dobanol 91-10)

(Liquor ratio 50:1)

The soiled swatches are rinsed 30 seconds with tap water, spun and dried on a line at 60°C.

Washing out of soil

In a third step the soiled textile swatches are washed in a Linitest apparatus for 20 minutes with 3 g/l ECE Detergent at 80°C using a liquor ratio of 50:1. The washed swatches are rinsed for 30 seconds with tap water, spun and dried on a line at 60°C.

Evaluation of Wet Soiling

The lightness value Y measured with a Datacolor Spectraphotometer SF 500 is taken as a measure for the amount of soil deposited on the textile. Decreasing values of Y mean higher soil deposits on the textile.

The lightness value Y is measured after soiling of the swatches with carbon black and after washing out of the soil. Table 6 (Results of lightness value measurements after soiling of the cotton swatches)

(Y value prior to soiling = 93.5)

The results in Table 6 show an improved wet soil behaviour (less staining) of the textile fabric material treated with compositions of the present invention.

Table 7 (Results after wash out of soil)

Results in Table 7 demonstrate that besides reduced wet soiling the treated textile release in a wash process the soil more readily compared to untreated materials.

Example 7 (Reduction of wet soiling of cotton/polyester)

In this example cotton/polyester 66/34 woven: 85 g/m2, bleached, with resin finishing is treated, soiled and the soiled washed out according to the procedure described in Example 6. The evaluation of wet soiling is described in Example 6. Table 8 (Results of lightness value measurements after soiling of the treated polyester/cotton swatches)

(Y value prior to soiling = 92.5)

Results in Table 8 show that an improved wet soil behaviour (less staining) of polyester/cotton fabric material can be achieved when treated with compositions of the present invention.

In a washing process treated polyester/cotton fabric releases soil more readily than untreated fabric (Results in Table 9).

Table 9 {Results after wash out of soil)

These results (Table 9) show an improvement in wet soil release for the textile fabric material treated with compositions of the present invention.

Example 8 Hydrophilicity

The formulated rinse conditioners (see Table 1) are applied according to the following procedure:

Evaluation of Hydrophilicity

The water absorption of fabrics treated with the test samples is measured by the wicking test. Test strips are fixed to a frame and dipped about 1 mm deep in a colored aqueous solution. The rise of water in the strips is measured after twenty minutes. Water absorption of fabrics treated with rinse conditioner formulations from Table 1 are compared. The average values of four parallel measurements are given in Table 10.

Table 10

These results show an improved hydrophilicity of the textile fabric material treated with compositions of the present invention.

Example 9 (Antipilling)

Textile swatches are washed in a washing machine, rinsed and dried. The antipilling properties are evaluated after 1 wash/rinse-cycle.

The textile used is: Cotton knit: 163 g/m2, bleached with resin finishing

Cotton knit swatches of size of 50 cm by 40 cm are washed together with ballast material (cotton and cotton/polyester) in a AEG Oeko Lavamat 73729 washing machine maintaining the washing temperature at 40°C . The total fabric load of 1 kg is washed for 15 minutes with 33 g of ECE Color Fastness Test Detergent 77 (Formulation January 1977, according to ISO 105-CO6). The rinse conditioner formulation as described in Table 1 is applied in the last rinse cycle at 20°C. After rinsing with the formulation the textile swatches are dried on a washing line at ambient temperature.

Evaluation of the pilling

The pilling of the treated swatches is tested and evaluated according to a method described under point 3 (SN 198525, 1990). A number of 1 is assigned to a very strong pilling, a number of 5 reflects no or very slight pilling.

The following results (evaluated after 125, 250 and 500 rotations) have been found :

Table 11 (Results of pilling tests)

These results show a markedly improvement resistance to pilling when textile fabric material is treated with compositions of the present invention.

Example 10 (Abrasion resistance (Cotton))

Woven cotton swatches of size of 50 cm by 40 cm are washed together with ballast material (cotton and cotton/polyester) in a AEG Oeko Lavamat 73729 washing machine maintaining the washing temperature at 40°C. The total fabric load of 1 kg is washed for 15 minutes with 33 g of ECE Color Fastness Test Detergent 77 (Formulation January 1977, according to ISO 105-CO6). The rinse conditioner formulation as described in Table 1 is applied in the last rinse cycle at 20°C. After rinsing with the formulation the textile swatches are dried on a washing line at ambient temperature. Evaluation of the Abrasion Resistance

The testing and evaluation of the abrasion resistance is done as described under point 3 (SN 198529, 1990) of the Martindale method. The greater the number of rotations the fibre can tolerate, the greater is the abrasion resistance of the fibre.

The following results (evaluated until the fibres broke) have been found :

Table 12 (Results of abrasion tests)

These results show that treatment of textile fabric material with compositions of the present invention improves markedly the abrasion resistance of the textile.

Example 11 (Abrasion resistance (Polyester/Cotton))

Woven Cotton/Polyester swatches of size of 50 cm by 40 cm are washed and rinsed according to procedure described in Example 2.

Evaluation of the Abrasion Resistance

The testing and evaluation of the abrasion resistance is done as described in Example 10. The following results (evaluated until the fibres broke) have been found : Table 13 (Results of abrasion tests)

In the experiments the following textiles have been used:

Cotton woven: 120 g/m2, bleached Cotton/Polyester 66/34 woven: 85 g/m2, bleached. Cotton knit: 163 g/m2, bleached

All 3 textiles were finished with a resin according to Oekotex Standard 100:

30 g/l of modified dimethyloldihydroxyethylene urea ( 70% active material)

9 g/l Magnesiumchloride (with 6 H₂O) padding with a pick-up of approximately 80%

Drying at about 110 - 120°C in a oven followed by a 4 minute curing step at 145°C.

Claims

WHAT IS CLAIMED IS:

1. A fabric softener composition for the treatment of textile fibre materials in domestic applications, which softener composition comprises:

A) a fabric softener; and

B) an aluminium salt of a polysilicic acid.

2. A fabric softener composition according to claim 1 , wherein the aluminium salt of a polysilicic acid has a specific surface area of 50 to 400 m /g .

3. A fabric softener composition according to claim 1 or 2, wherein the aluminium salt of a polysilicic acid has a specific surface are of 100 to 300 m²/g.

4. A fabric softener composition according to claim 3, wherein the aluminium salt of a polysilicic acid is prepared by reaction of polysilicic acid with a basic aluminium chloride.

5. A fabric softener composition according to any of claims 1 to 4, which contains 0.005 to 10 % by weight of the aluminium salt of a polysilic acid, based on the total weight of the softener composition.

6. A fabric softener composition according to any of claims 1 to 5, which contains 0.5 to 50 % by weight of the fabric softener, based on the total weight of the softener composition.

7. A fabric softener composition according to any of claims 1 to 6 which is in liquid form and comprises:

D) water to 100 %.

8. A fabric softener composition according to any of claims 1 to 7, wherein the fabric softener composition is prepared by mixing a preformulated fabric softener with an emulsion comprising the aluminium salt of a polysilicic acid.

9. A fabric softener composition according to any of claims 1 to 7 which is present as a tumble dryer sheet composition.

10. A fabric softener composition according to any of claims 1 to 9 which composition contains no substantial amount of a polyorganosiloxane.

11. A method of use for an aluminium salt of a polysilicic acid to improve drape and smoothness, wrinkle recovery, hydrophilicity, wet soiling, abrasion resistance and/or antipilling of textile fibre materials in domestic applications.

12. A method of use according to claim 11 wherein the aluminium salt of a polysilicic acid is used in a rinse step of a laundering operation.

13. A method of use according to claim 11 wherein the aluminium salt of a polysilicic acid is used together with a fabric softener.

14. A method of use according to claim 11 wherein the aluminium salt of a polysilicic acid is used together with a detergent in a laundering operation.

15. A method of use according to claim 11 wherein the aluminium salt of a polysilicic acid is sprayed onto the textile fibre material.