PT94005B - Process for the preparation of a detergent composition comprising of coated particles - Google Patents

Abstract

Perfume particles comprise perfume dispersed within certain water-insoluble polymeric carrier materials and encapsulated in a protective shell by coating with a friable coating material. The coated particles allow for preservation and protection of perfumes which are susceptible to degradation or loss in storage and in harsh cleaning conditions. In use, the surface coating fractures and the underlying carrier/perfume particles efficiently deliver a large variety of perfume types to fabrics or other surfaces.

Description

The present invention relates to a process for the preparation of a detergent composition comprising perfumed coated particles comprising a perfume dispersed in a low molecular weight polymeric carrier material, insoluble in water and encapsulated with a friable coating. Such coated particles are useful, for example, in textile cleaning and conditioning compositions.

Mod. 71-10000 βχ. The present invention is based on the concept of controlled release of perfume, that is, the release of perfume at a time and under conditions that achieve the desired perfuming effect. In general, this is a very old idea and several processes to reach this end have been developed, from the simple idea of putting perfume on wax candles to the complex micro-encapsulation technology.

One of the concept aspects of controlled perfume release is to provide a slow release of perfume over an extended period of time.

This is usually achieved by mixing the perfume with a substance that, in essence, retains ”the perfume so that over time only small amounts of perfume are released. The use of polymeric substances of high molecular weight, with incorporated perfume to provide a controlled release of perfume over time, is known. See, for example, U.S. Patents 4,184,099, Lindauer et al, issued January 15, 1980; European Patent Application 0 028 118, Leenard, published on May 6, 1981;

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11. MJU 1991 and U.S. Patent 4,110,261, Nevland, issued August 29, 197θ 'which describe combining perfume with a controlled release medium and combining it in a solid product for cooling and air.

The textile laundry is also concerned with the controlled release of perfumes. The application of this concept allows to slow down and prevent the release of perfume over long periods of storage on shelves. This concept also allows to use much lower levels of perfume in the product, since much less perfume is used.

Preserving perfume during storage can be achieved in different ways. The perfume may be an integral part of the packaging for the composition. The perfume can be combined with the plastic used to make a bottle, or it can be mixed with a polymeric substance and the product used to coat a carton composition, as described in US Patent 4,540,721, Staller, issued in 10 September 1985 · In either case, the perfume is released over time from the polymer matrix.

perfume / controlled release agent can also coat the form of mixed particles in a washing composition. A process thought that can achieve this purpose is combining perfume with a water-insoluble polymer, forming into particles and additives to a composition for rinsing, as described in P _to try US 4 209 4l7, Whyte, issued on 24 June 1980; US Patent 4,339,356, Vhyte,

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issued on July 13, 1982; and U.S. Patent 3,576,760, Geuld et al., issued April 27, 1971.

The perfume can also be absorbed into a porous carrier material, which can be a polymeric material.

See, for example, Patent Publication UK2 066 839, Bares et al (applied for on behalf of Vyseka Skela Chemicko Technologika), published on 15 July 1981. These processes can also be used to mask unpleasant odors in a composition or to protect perfume from degradation due to rough components in a laundry composition. Such processes will provide these benefits only for dry powder or granular compositions because, as soon as the polymer is hydrated, the perfume is released. Thus, these processes provide benefits of perfumed fragrance when the product packaging is opened and the product is placed in the washing machine. While these benefits are desirable, it would be even more desirable to have a process that allows the application of undiluted, undissiped and unchanged perfume to the fabric and release of the perfume at the end of the washing process so that the fabric retains the desirable scented odor. .

Of course, one way to achieve this is to place the perfume in a product that goes directly into the dryer. In this way the perfume is applied directly to the fabric in the drying cycle. Such a method is described in both U.S. Patents 4,511,495, Melville, issued April 16, 1985 and U.S. 4,636,330, Melville, issued January 13, 1987. Both describe the formation of particulate perfume with a vehicle. These particles are formulated in a composition that is applied to textiles before they are put into the dryer or

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11. μι ψ90 »to be dried on the rope.

An even more desirable process for applying perfume to washed clothes would be one that would provide protection for the perfume throughout the washing process and thus release the perfume onto the fabric practically in its original state.

Such a process should allow the avoidance of dilution, degradation or loss of perfume during the washing cycle of the laundry process. This is achieved through the use of a system that releases the perfume in the drying process or later, after the perfume has been applied to the fabric. Avoiding the release of perfume during the washing process involves a very different and more difficult technology. Such protection must be stable, not only under conditions of high washing temperature, but also against degradation by water and other aggressive chemical agents of the washing process, such as bleaches, enzymes, surfactants, etc.

A process that was developed to provide such benefits was that of perfume micro-encapsulation. Here the perfume comprises a capsule core that is completely coated with a material that can be polymeric. US Patents 4,144,184, Brain et al, issued on March 20, 1979 and US 4,234,627, Schilling, issued on November 18, 1980, describe the use of a resistant coating material which, in essence, prohibits the diffusion of perfume. The perfume is applied to the fabric by means of the micro-capsules and is released by breaking them that will occur with the manipulation of the fabric.

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Another process of applying the perfume involves providing the protection of the perfume throughout the washing cycle, with its release under conditions of high dryer temperature. US Patent 4,096,072, Drock et al, issued on June 20, 1978, describes a process for applying conditioning agents to useful fabrics through washing and drying scraps, using particles containing hydrogenated castor oil and the fatty salt of quaternary ammonia. Perfume can be incorporated into these particles. However, it is not clear whether the perfume thus incorporated is released in the washing cycle or, more desirably, transported in the particles to the dryer and released there, when the particles have softened.

US Patent 4 402 856, Schnoring et al, issued on September 6, 19θ3, describes a micro-encapsulation technique that involves the formulation of a shell material that will allow the perfume to diffuse out of the capsule only at a certain temperature . This allows the perfumed particles to be maintained during storage and then throughout the wash cycle.

The particles adhere to the fabric and are dragged to the dryer. The diffusion of the perfume out of the capsules therefore only occurs under the high temperature conditions of the dryer. These particles are made of gelatin, an anionic polymer and a hardening agent.

U.S. Patent 4,152,272, Young, issued May 1, 1979 »describes the incorporation of perfume into wax particles to protect the perfume during storage in dry compositions and during the laundry process. The perfume then diffuses through the wax matrix of the particles, to the fabric, under the high temperature conditions of the dryer.

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It is desirable to provide compositions comprising perfume particles which can be incorporated into liquid compositions, as well as dry powders or granules and provide long-term storage stability.

1? It is desirable to provide a process for applying a wide range of scented materials to fabrics or other surfaces, during a cleaning or conditioning process of fabrics or fibers.

It would be even more desirable to have a perfumed cleaning or conditioning composition that could provide a better odor to the product, improved perfume odor that was released during the washing process and a better intensity and perfume odor applied to the surface to be applied. be clean.

It would be particularly desirable to provide perfumed particles which are stable in liquid compositions, but which release their perfume when used.

The present invention relates to perfumed particles which have an average size, when coated, of less than about 350 microns (preferably an average size of not more than 150 microns; more preferably a range of 40-150 microns) comprising between about 5% ^and about 70% of a perfume dispersed in between about 30% and about 85% of water-insoluble polymeric carrier material with a molecular weight of between about 100 and about 30,000, a melting between about 37 ° C and about 190 ° C and a hardness value of between about 0.1 and about

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15, said particles having a friable coating on their outer surface. (By size we mean here the mean particle diameter for substantially spherical particles, or the size of the largest diameter or dimension in the non-spherical particles). Particle sizes greater than these may loosen more from the surface if they are deposited and do not provide a relative surface area large enough to release the perfume in the desired proportion. Likewise, particles larger than specified may be undesirably noticed on the surface to be treated. Particles located at the lower end of the boundaries tend to adhere well to the surface to be treated, but tend to release the perfume quite quickly.

Typically those particles are characterized by a coating that comprises up to 20% by weight of the perfumed particles. For general use in washing fabrics and conditioning compositions, the coating typically comprises between about 1% and about 10 ⁴ % by weight of the perfumed particles.

The preferred particles here are those in which the friable coating is substantially insoluble in water. Suitable coatings of this type can be prepared from aminoplast polymers, for example, the reaction products of an amine and an aldehyde. Typically friable coatings comprise, for example, the reaction products of an amine selected from urea and melamine and an aldehyde selected from formaldehyde, acetaldehyde or glutaraldehyde and mixtures of said amines and said aldehydes. Such friable coatings are described below.

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The perfumed coated particles described here are useful in situations where the coating of the particles is broken or worn (for example, in an automatic washing machine or laundry dryer) to release the particles which, in turn, release their perfume. Thus the coated particles are useful for typical cleaning compositions, including detergent surfactants, optional embedding agents and the like. The particles are also useful in conditioning compositions, comprised of fiber and tissue conditioning agents.

All percentages presented here are weighted, unless otherwise specified.

The present invention provides for the preservation, protection and distribution of perfumes contained in cleaning and conditioning compositions, over prolonged storage and during severe washing conditions. This is achieved by isolating the perfume in a carrier material in the form of small particles. The individual components of the invention will now be discussed in detail.

The perfumed particles of the present invention comprise perfume dispersed in certain carrier materials. The perfumed particles are coated with a friable coating material that breaks when used to release the perfumed particles which, in turn, release their perfume.

In the present context, the term perfume means any odorous material or any material

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11. UAI that act as a counter to bad smells. Generally, such materials are characterized by a vapor pressure higher than atmospheric pressure at ambient temperatures. The perfume or deodorizing materials employed herein will most often be liquid at room temperature, but can also be solid, such as the various camphor fragrances known in the art. A wide variety of chemicals are known for use in perfumery, including materials such as aldehydes, ketones, esters and the like. Most commonly, natural oils from plants and animals as well as exudates comprising complex mixtures of various with chemical components are known for use as perfumes and such materials can be used here. The perfumes indicated here can be relatively simple in their composition or comprise highly complex and sophisticated mixtures of natural and synthetic chemical components, all chosen to provide any desired odor.

The typical perfumes used here can comprise, for example, wood / earth bases containing exotic materials such as sandalwood oil, civet, patchouli oil and the like. These perfumes can be a light floral fragrance, for example, rose extract, violet extract and the like. Perfumes can be formulated to provide desirable fruit odors, for example lime / rudder, orange and the like. Suitable perfumes include musk ambreta, musky acetone, musky tibetine, musky xylol, aurantiol, ethyl vanillin and mixtures thereof.

Perfume materials are more fully described in SLArctander. Perfume Flavors and

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Chemicals. Vols I and II Aurthor. M _o ntclair, NJ and the Merck Index, 8 * Edition. Merck &. Ce., Inc. Rahway, NJ, both of which are incorporated herein by reference.

In summary, any chemically compatible material that gives off a pleasant odor or any other desirable odor can be used in the perfumed particles of the present invention to provide a desirable odor when applied to fabrics.

Perfumes that are normally solid in the present invention can also be used. These can be mixed with a blending agent such as a solvent prior to their incorporation into the particles, or they can be simply dissolved or incorporated, as long as the perfume does not sublimate or decompose when heated.

The invention also covers the use of materials that act as countermeasures to bad smells. These materials, although referred to as perfumes hereinafter, may not have a discernible odor themselves but may retain or reduce any unpleasant odors. Examples of suitable deodorants are described in U.S. Patent no. 3 102 101 issued on August 27, 1963, in favor of Hawley et al.

The perfumed particles of the present invention may even comprise perfumes that are not typically used to provide a fragrance to a surface, such as a fabric during the laundry process. Perfume materials that are very volatile, unstable or soluble in the special compositions that are used—

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Used to distribute the perfume, can be used in the present invention because the perfume is isolated from the composition in the particles. Scented materials that are not substantive to fabrics in the laundry process can also be used in the present invention, since the particles distribute the perfume to the surface of the fabric where it is released. Thus, the use of the present invention to provide a perfume to an enlarged surface is the type of perfumed materials that can be used.

Generally, the perfumed particles of the present invention will comprise between about 5% about 7%, preferably about 5% about 5% for perfume. The exact amount of perfume used in the particles will vary greatly, depending on the intensity of the fragrance particularly used and the desired odor effect.

The carrier materials for the perfumed particles must meet certain criteria to be useful in the present invention. Firstly, the carrier material must be insoluble in water and polymeric. In addition, the material should have a molecular weight between about 100 and about 30,000, preferably between about 500 and about 36,000. The molecular weight of the carrier material can be determined by any standard means. The material should also have a melting point of between about 37 ° C and about 190 ° C, typically 37 ° C to 130 ° C. This will prevent the particles from melting in storage or in the washing machine in laundry applications (the most desirable thing is to have a transport material that does not completely melt in an automatic dryer to avoid blocking the linen partition and excessive increase from the heat

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in the dryer). The melting point of the carrier material should also not be higher than a point where the perfume to be combined with it decomposes. The melting point of the carrier material is measured by what is called the drop melting point method. The American Society for Testing and Materials (ASTM) in Test Method D127-63 (re-approved in 1982, incorporated herein by reference). Briefly this process involves the following. The sample to be measured is deposited in a thermometer bulb by immersing a cold thermometer in the molten sample.

thermometer carrying the sample is then placed in a test tube and heated by means of a water bath until the sample melts and the first drop falls from the bulb of the thermometer. The average temperature at which the sample drops fall is the sample's drop melting point.

The polymeric material must also be of a special hardness. This hardness value can be measured using the standard test procedure for the penetration of needles into waxes: oil. ASTM D1321-86 Test Procedure (incorporated herein by reference). In short, this process involves first melting and then heating the sample to be tested to 17 ° C (30 ° F) above its freezing point. The sample is then poured into a container and cooled with air under controlled conditions. The sample is then conditioned to the test temperature in a water bath. Penetration is then measured with a penetrometer, which applies a standard needle to the sample for five seconds under a 100-gram load. The penetration or hardness value is the depth, in tenths of a millimeter, at which the normal needle

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malty penetrates the wax under these controlled and defined conditions. The hardness value of the carrier material must be between about 0.1 and about 15, preferably between 0.1 and 8, to be useful in the present invention.

This will allow the particles to have a hardness that optimizes the perfume preservation protection in the vehicle.

carrier material must also be inert as to perfume and relatively odorless. The material must allow the perfume to diffuse through it. The carrier material must also be of a type that melts without decomposition.

Non-limiting examples of such useful carrier materials include polyethylenes, polyamides, polystyrenes, polyisoprene, polycarbonates, polyesters, polyacrylates, vinyl polymers and polyurethanes and mixtures thereof, which meet the criteria described above, that is, which are soluble in water, have water a molecular weight between about 100 and about 30,000, have a melting point between about 37 ° C and 190 ° C and a hardness value between 0.1 and 15.

Highly preferred vehicles will have a hardness value of 0 1 to 8, typically 0.5; a molecular weight of 5,000 to 5,000 (typically 2,000); and a melting point of about 126 ° C - typically a polyethylene.

A carrier material that meets all of these specified criteria is sold under the POLYMAX 2000 brand by the Petrolite Specialty Polymers Group. This material is a polyethylene with a molecular weight of about 2,000, a melting point of about 126 ° C (259 ° F)

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and a hardness value (as measured above) at 25 ° C (77 ° F) of about 0.5. Another material that fulfills these criteria is POLYMAX 1000 (also sold by Petrolite Specialty Polymers Group). This material is also a polyethylene with a molecular weight of about 1000, a melting point of about 114 ° C (237 ° F) β has a hardness value at 25 ° C (77 ° E) of about 1, 0.

Another such material is POLYMAX 5θθ ·

It may be desirable to use a mixture of different carrier materials in the perfumed particles of the present invention, for example a mixture of polymeric material and a smaller amount of a waxy material. Examples of useful waxy materials include materials sold under the BOLER 1014, STARVAX 100 and VICTORY brands, all marketed by the Boler Petroluem Company. Such a mixture allows a better deposition property because the particles formed with it will have a more sticky surface. The combination of a large number of materials is possible and is intended to be covered by the present invention, provided that the final mixture of the vehicles meets the criteria indicated above.

The choice of vehicle to be used in the perfumed particles of the present invention will depend to some degree on the particular perfume to be used. Some perfumes will need a greater amount of protection than others and the vehicle to be used with them has to be chosen accordingly.

Generally, the perfumed particles used in the present invention will comprise between about 3θ $ © cer-1462237

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about 95%, preferably between about 5% and about 95% of carrier material. Here, too, this will vary with the type and quantity of the particular form of perfume used.

A typical process, perfume containing particles can be made as follows. The carrier material is first heated slowly to its melting point. The material is no longer heated beyond what is necessary to just melt the substance. The perfume is then quickly added, generally in the form of an oil or liquid, at room temperature, to the transport melt. The two are quickly mixed in a homogeneous mixture and then quickly cooled with liquid nitrogen (or with dry ice or any other means that quickly cool the mixture) until it has completely solidified. The solid material is then subdivided, usually by crushing or grinding, to produce particles of the desired average size. Other processes such as spray cooling or extrusion can also be used to subdivide the particles.

In order to better stabilize particularly volatile or delicate perfumes, it may be desirable to preload the perfume (i.e., mix the perfume) in silica gel or clay before combining with the carrier substance. Some perfumes that are not volatile will not require this special treatment because it would greatly inhibit their release of the carrier substance. Optimizing the rate at which the perfume is released from the vehicle is the goal and this optional additional step allows better control of the rate of some of the most volatile perfumes.

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The perfume-containing particles indicated above are encapsulated to provide a friable coating. This coating prevents the perfume from diffusing from the particles very easily during long periods of storage. In addition, the coating helps to preserve the original character of perfumes that have particularly volatile peaks. In addition, the coating helps to protect the scented particle from other ingredients present in the formulation to be scented.

The materials used here are friable and are designed to break when the scented formulation is used, thus releasing the scented particle.

The particles can be coated with more than one friable material to produce a particle that has more than one friable layer. They can be chosen from the different fragile coating materials to provide the necessary protection for the different perfumes, as long as one of the coating layers, usually the outer one, is friable.

The individual particles containing perfume can also be agglomerated with the coating to provide larger particles that comprise a number of individual perfumed particles. This agglomerated material surrounding the particles provides an additional barrier to the diffusion of the perfume out of the particles. Such an approach also minimizes the surface area of free particles likely to scent diffusion. The proportion of the perfumed particles to the agglomerated material will vary widely, depending on the extent of the desired additional protection. It is

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The agglomeration approach can be particularly useful with very volatile perfumes or perfumes that are especially susceptible to degradation. The agglomeration of very small perfumed particles will also provide additional protection against premature perfume diffusion.

Agglomerating the particles in this way is useful to prevent the segregation of small perfumed particles from larger detergent granules, for example in a dry granular detergent product.

For cool coatings, the manufacturing process is based on applying coating as a kind of shell to the perfumed particles. For perfumed particles whose vehicle has a lower melting point than the melting point of the solvent used in the process, the process involves melting the perfume and the vehicle together and adding the molten mixture to a solvent solution of the shell material ”or a precursor maintained above the vehicle's melting temperature. The system is sufficiently agitated to form an emulsion of the vehicle / perfume of the desired liquid drop size in the ladle solution. The conditions necessary for depositing the encapsulation material are then established and the assembly is cooled to provide encapsulated solid particles with the desired friable pad. The insolubility of the shell in the water is established, either in the deposition phase, or by appropriate treatment before the isolation or use of the particles.

Although the process described here is a one-step cast / encapsulation drop process, it will become readily apparent to those skilled in the art.

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Various suitable encapsulation processes can be used, such as those reviewed in the Deary and Kondo books listed above. Depending on the materials used, the shell can provide hydrophilia or hydrophobia to the particles. Non-limiting examples of encapsulating materials and processes include arabic gum arabic concentrate deposited through a complex coacervation process, for example, US Patent 2,800,457, for hydrophilic shells and urea-formaldehyde deposited through a process of polycondensation, for example, US Patent 3 5 5 94 94, for hydrophobic shells.

The insolubility in water of the shell materials can be provided by crosslinking the gum arabic-gelatin coacervate with suitable aldehydes or other known gelatin hardeners after deposition. Polymerization of urea pre-condensate — formaldehyde during the encapsulation process provides insolubility in water.

The paste containing the perfumed particles can be used directly, for example, spray dried-1862237

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11. MAY 1990zVation with other components of the formulation, or they can be washed and separated and dried, if desired.

Perfume particles containing a hydrophilic coating deposited by complex coacervation are prepared as follows

Example 1

132 g of POLYMAX 5θθ (polyethylene with a molecular weight of 500) are heated in a beaker on a hot plate at about 100 ° C until only 44 g of perfume have been melted at room temperature are added to the molten POLYMAX 5OO and heating is maintained to bring this nuclear mixture back to 100 ° C.

The molten nuclear material is added to 400 g of a 5% aqueous gelatin solution (Sanafi A type, Bloora 275 resistance) maintained at 15-20 ° C above the core melting point in a 1-1 steel beaker and emulsified by stirring until a desired drop size of about 100 µm is reached. Then 200 g of 11% gum arabic solution is added and stirring is continued for about 30 minutes.

pH is reduced to about 4.2 by the dropwise addition of glacial acetic acid and the beaker contents are then poured into 1-1 of stirred water at room temperature. This solidifies the nuclear mixture with a concurrent deposition of gum arabic-gelatin coacervate.

coating is established by cooling the paste in ice water to about 5 ° C. A pas-1962237

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This can be used at that time, or the particle can be released from any coanervate not deposited in the slurry by adding about an equal volume of 10% sodium chloride and removing the capsules in a separating funnel. This can be repeated as many times as necessary to completely remove the free coacervate. The particles can be dried by filtration, washing the filter cake with water, then with inopiopañol, followed by drying in air, overnight, at 25 ° C.

The particles can be sieved to the desired size.

Example II

Perfumed particles with a coating less soluble in hydrophilic water can be prepared as follows.

A paste of perfumed particles containing a gum arabic-gelatin coating is prepared according to Example I. After cooling, the paste is allowed to warm to room temperature and 8.0 ml of aqueous glutaraldehyde solution are added with stirring to 25 $. The pH is raised to 5.1% by adding 2.5% aqueous sodium hydroxide solution and the slurry is stirred overnight.

The paste can be used at that time or separated as in Example 1. The glutaraldehyde treated coating can overcome a prolonged immersion in water at 60 ° C, while the untreated coatings are removed when heated to 50 ° C.

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Example III

Perfume particles containing a hydrophobic coating, insoluble in water, deposited by polycondensation, are prepared as follows.

First, a urea-formaldehyde pre-condensate is formed by heating a mixture of 1662 g of 37% aqueous formaldehyde and 60-65 g of urea, adjusted to pH 8.0 with 0.53 g of tetraborate of sodium for 1 hour at 70 ° C and then adding 276.85g of water

429 ml of this pre-condensate and 142 ml of water are then stirred in a 1-1 steel reactor and 57 µl sodium chloride and 0.57g sodium carboxymethyl cellulose are added. Core components comprising 16.6 g of POLYMAX 500 vehicle and 60.7 ml of perfume are added and the reactor is heated to about 10 ° C above the melting point of the core. The agitation is adjusted to emulsify and keep the molten core at the desired drop size point and the pH of the content is adjusted to about 5.0 with diluted hydrochloric acid.

The reactor is then allowed to cool to room temperature with a gradual reduction in pH to 2.2 over a period of 2 hours. The reactor then has its temperature raised to 50 ° C for a further 2 hours, then it is cooled to room temperature, after which the pH is adjusted to 7.0 with a 10% sodium hydroxide solution.

The resulting paste, which contains a solid core of particles encapsulated with urea-formal-polymer-2162237

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dehyde can be used directly or isolated by separation, washing and air drying as needed.

The perfumed coated particles prepared previously can be used in all types of products where it is desirable to deposit fragrances on treated surfaces and where sufficient agitation or pressure is exerted to break the friable coating.

Typical examples of such products are laundry detergents and fabric softeners. The following illustrates the use of the compositions of the present invention in such products.

Laundry washing products comprise: a detergent surfactant; generally, one or more detergent extenders; optionally, various enzymes, bleaches, vehicles and the like, all well known in standard texts and very familiar to detergent formulators. Surfactants include soap, alkyl benzene sulfonates, ethoxylated alcohols, alkyl sulfates and the like.

Detergent-enhancing agents include various phosphates, zeolites, polycarboxylates and the like. U.S. Patents 3 · 9θ5 · 669, ^ -. 379,080 and U.605,609 can be referred to for typical listings of such ingredients.

Modern fabric softeners typically comprise one or more of quaternary ammonium, or imidazoline or imidazolinium compounds Fabric softeners (and antistatic agents) generally have one, or preferably two, alkyl substitutes ^ ΐ2 ”^ ΐ8 ^and ^ ° ^ ^{-3 or} three short chain alkyl groups. Again, these materials are conventional and well known to softener formulators.

Example IV

Granular laundry detergent as follows:

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Components C ^ alkylbenzene sodium sulfonate 7.5 C ^ sodium alkyl sulfate 7.5

C ^ (6.5) polyethoxylate ^to which 0 non-ethoxylated and 0 ethoxylated alcohol were extracted bottom 2.0 C ^ alkyltrimethyl ammonium chloride 1.0 Sodium tripolyphosphate 32.0 Sodium carbonate 10.0 Sodium perborate monohydrate 5.3 Sodium octanoyloxybenzene sulphate 5.8 Penta-acetate diethylene sodium triamine 0.5 Sodium sulfonate, HgO and traces Rest

The above composition is prepared using conventional means. The composition is combined with the perfumed particles of Example I. An amount of perfumed particles of Example I is combined with the detergent composition so that the detergent composition comprises about 0.3% perfume.

The particles can simply be mixed with the granule detergent. To avoid segregation-2362237

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perfume particles during packaging and delivery (due to their relatively smaller size compared to detergent granules), the particles can optionally be coated or agglomerated with a water-soluble coating material (on the coating) friable) before combining with the detergent granules. This can be achieved with a Schugi mixer (Flexomix 16o) in which a sufficient amount of a dextrin glue solution (2% dextrin, 3% water) is sprayed on the particles to result in scented particle clusters in the same size range as the other detergent granules.

perfume is protected from degradation, in the particles, by the bleach contained in the detergent composition during long periods of storage. When used in the washing process in an automatic washing machine, this detergent composition will provide a fragrant fragrance practically in its original state from the product, through the washing process and to the fabric.

A large number of perfumes can be used in the present composition, which would not otherwise be suitable for use in such laundry detergent compositions.

Example V

Liquid fabric softener for use in an aqueous wash rinse bath as follows:

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Component - WEIGHT X Conditioner A 3.00 XX Softener B 5.00 HCl 0.29 Polydimethylsiloxane 0.15 Polyethylene glycol (4000) 0.30 Bronopol (Antimicrobial) 100 ppm Calcium chloride 30 ppm Dye 30 ppm

Coated Parfumed Particles *** 4.0

Water Rest »0 Softener A á r & och ₂ ch ₂ n ' ^, r (ch ₃ ) ₂ , Clonde each group R is in the range of C ^ -C ^ g alkyl» xThe Softener B is π ⁰

N N-CH _o CH _o 0-CR

V ²² c

I

R where each group R is in the range of C C-C ^ g alkyl xxx Particles prepared according to Example II. Size 100 microns; 5 $ of coat weight

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When used in a rinse bath of an automatic washing machine, the coating of the perfumed particles of Example V breaks and the particles provide a fragrance to the fabric to be treated

Example VI

Liquid laundry detergent composition as follows:

Component Weight

C4 linear sulfonic acid alkylbenzene 7.2

Polyethoxylated alkyl sulfuric acid (2.25) 10.8

C ^ ₂ polyethoxylate ₁₂ alcohol (6.5) m 6.5 C ^ ₂ alkyl trimethylammonium chloride 1.2 C ^ ₂ _ ^^ fatty acid 13.0 Oleic acid 2.0 Citric acid (anhydrous) 4.0 Diethylenetriamine pentacatic acid 0.23 Protease enzyme (2.0 AU / g) 0.75 Amylase enzyme (375 Am U / g) 0.16 TEPA-E, _, _q jk * 15—10 1.5 Monoethanolamine 2.0 (moles of alkanolamine) (0.033) Sodium ions 1.66 Potassium ions 2.65

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Propylene glycol

Ethanol

Formic acid

Calcium ion (0.94)

6.8

7.8

0.66

0.03

Residual components and water Rest to 100 pH at a concentration of 10 $ in water at 20 ° C (68 ° F) 8.65 * Monoethoxylated alcohol and alcohol removed ** 15-18 moles (avg) ethoxylated tetraethylene pentaimine ethylene oxide at each hydrogen point.

detergent is prepared by adding components, with continuous mixing, in the following order: pasty premix of alkylbenzene sulfonic acid, sodium hydroxide, propylene glycol and ethanol; premix in a paste of polyethoxylated alkyl sulfuric acid, sodium hydroxide and ethanol; pentacetic acid; polyethoxylated alcohol; premix of water, brighteners, alkanolamine and polyethoxylated alcohol; ethanol; sodium and potassium hydroxide, fatty acid, citric acid; formic acid and calcium; alkyl trimatilammonium chloride;

TEPA-E ^ g; pH adjustment to about 8.1 and rest of the components.

The above composition is combined with perfume containing particles prepared according to Example II, as follows. A quantity of the perfumed particles of Example II (average size in the range 40-150 microns; 5 ° ί coating) is carefully mixed in a detergent li-2762237

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II. 901990 liquid so that the detergent composition comprises about 0.3% perfume (about one liter of the detergent composition will comprise the perfumed particles).

f.

Example VIT

Softener composition of fibers or fabrics as follows:

C omponent Weight

Softener C * 37

TAMET ** 0.3

GMS ** 1.20

Phosphoric acid 0.023

Polydimethylsiloxane (350) 0.10

Glutaraldehyde 55θ PP ^m

Blue dye 10 ppm

Scented coated particles **** 3.0 * (R ^) ₂ (CH ^) ₂ N ⁺ , Br-, where rA is mixed C ^ ₂ C ^ g alkyl (i.e., seboalkyl ”).

** TAMET is seboalkyl N (CH ₂ CH ₂ 0H) ₂ .

*** is glyceryl monostearate.

Scented particles coated according to Example III, sieved to an average size of less than 150 cicons. Coating weight 3 ^>.

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It will be appreciated by those skilled in the art that the anions, X, used in any of the cationic fabric softeners indicated herein are routine matters for choice and that X may be, for example, chloride, bromide, methylsulfate and the like. Mixtures of fabric softeners as well as mixtures of anions can be used.

Example VIII

The detergent composition of E _x Example VI is modified using scented particles with cool cold coatings (melamine / urea / formaldehyde; 0.1 / 1 /, 1, 1 molar ratio; 3θθ microns in size) with coating weights of $ 1 and $ 20, respectively.

Example IX

Detergent bar composition prepared by gentle mixing (so as not to fracture the coating) of 2% by weight of the fragrant coated particles of Example I (7% coating »all particles passing through the 150 micron sieve) in a mixture of tallow soap at 99 »44 $ (Na salt) and formed on a bar in a cylindrical mold.

The compositions listed here can also be used in combination with abrasives. As is well known, abrasive cleaning products typically comprise 10% to 90% of an abrasive such as pumice, silica, calcium carbonate and the like. The scented coated particles used in such cleaning products are fractured, in use, to release their scent.

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Example X

Abrasive cleaner as follows:

Component Floor Sodium greasy sulfate 1.0 Calcium carbonate U0.0 Pumice (passed through a 60 micron sieve) 45.0 Sodium sulfate 10.0 + Scented coated particles 3.0 Trisodium chlorinated phosphate 1.0 »According Example III; 10 $ coating; particles through the 100 micron sieve.

The composition of E _x emplo X is prepared by gently mixing the ingredients dry.

It will be appreciated by the formulator that the weight (or thickness) of the functional friable linings can be adjusted according to the intended use. For example, even relatively thick coatings, they will break and release their perfume under the conditions of European washing machines, which can involve washing times of many minutes, high temperature and considerable agitation. By contrast, the condition of American washing machines is shorter and smoother, so that less coating material can be used. For fabric softeners, stirring and stirring times are generally shorter than for washing.

Claims (15)

-claims1 *. —Process for the preparation of a detergent composition, in the form of a bar, optionally consisting of one or more detergent surfactants, one or more formers and a perfumed ingredient, characterized by the fact that said perfumed ingredient comprises particles perfumes made up of between 5% θ 70% of a perfume dispersed in between 30% and 95% of a polymeric vehicle material, insoluble in water, with a molecular weight of between 100 and 30,000, a melting point of between o 37 C and 190 C and a hardness value of between 0.1 and 15, said particles having a friable coating on their outer surfaces and said coated particles having an average size of less than 350 microns, preferably not greater than 150 micorons. 2". Process according to claim 1, characterized in that the friable coating is an aminopJaptic polymer 3 *. Process according to claim 2, characterized in that the coating is the product of the reaction of an amine selected from urea and melamine, or · mixtures thereof and the aldehyde is chosen from formal, dehyde, acetaldehyde, glutaraldehyde or mixtures thereof. Process according to claim 3, characterized in that the carrier material is selected from the group consisting of polyethylene, polyamides, polystyrene polyisoprene, polycarbonate, polyester, polyacrylate,. vinyl polymers, polyurethanes and mixtures thereof. 3162237 Case 3965 r 5 *. Process according to claim 4, characterized in that the carrier material comprises polyethylene. 6 *. Process according to claim 1, characterized in that said composition also comprises an abrasive. Mod. 71 · 20,000 «χ. - 8/90 7 *. -Process according to the previous claims, characterized in that in the perfumed particles coated with an average size, when coated, less than 350 microns, preferably not greater than 150 j microns, more preferably 40 4 150 microns, which buy end of 5 $ © 70 $ of a perfume, said perfume is dispersed in between 30 $ and 95 $ of a polymeric material material insoluble in water, with a molecular weight of between 100 15 and 30,000, a melting point of between 37 ° C and 190 ° C and a hardness value of between 0.1 and 15, said particles having a friable coating, practically insoluble in water, on their outer surfaces. 8 *. Process according to claim 7 * characterized in that the coating on the particles comprises up to 20% by weight of the perfumed particles. 9. The process according to claim 7, characterized in that the coating on the particles consists of an aminoplastic polymer. 10 *. Process according to claim 9, characterized in that in the particles the coating consists of the reaction product of an amine chosen from urea and melamine and an aldehyde selected from formaldehyde, acetaldehyde and glutaradehyde and mixtures of said amines and aldehydes . 11 *. - Process according to claim 10, characterized by the fact that in the particles the carrier material is chosen from the group consisting of polyethylenes, polyamides, polystyrenes, polyisoprene, polycarbonates, polyesters, polyacrylates, vinyl polymers, polyurethanes -3262237 Case 3965 and its mixtures. Mod. 71 · 20,000 βχ. - 90 / Οβ 12 *. Process according to claim 10, characterized in that in the particles the carrier material comprises polyethylene. 13>. Process for preparing a fabric softener according to the preceding claims, characterized in that it comprises one or more fabric or fiber or anti-static softening agents, and contains perfumed particles according to claim 7 14>. Process for preparing a softener composition according to claim 13, characterized in that the perfumed particles have a friable aminoplastic polymer coating. 15 *. Process according to claim 14, characterized in that the coating is the product of the reaction of an amine selected from urea and melamine, or mixtures thereof, and the aldehyde is selected from among maldehyde, acetaldehyde, glutaraldehyde or their mixtures. l6 *. Process according to claim 15, characterized in that the carrier material is selected from the group consisting of polyethylenes, polyamides, polystyrene, polyisoprene, piicarbonates, polyesters, polyacrylates, vinyl polymers, polyurethanes and mixtures thereof. * Process according to claim 16, characterized in that the carrier material ± comprises polyethylene.