WO2016099852A1

WO2016099852A1 - Fabric treatment composition

Info

Publication number: WO2016099852A1
Application number: PCT/US2015/063081
Authority: WO
Inventors: Lisa Grace FRENTZEL; Robert Richard Dykstra; Jaden Scott Zerhusen
Original assignee: The Procter & Gamble Company
Priority date: 2014-12-17
Filing date: 2015-12-01
Publication date: 2016-06-23
Also published as: US9347022B1; EP3204479B1; EP3204479A1

Abstract

A composition of a plurality of homogeneously structured particles. The particles include polyethylene glycol, perfume, and starch granules and each has a mass between about 0.95 mg and about 5 grams.

Description

FABRIC TREATMENT COMPOSITION

FIELD OF THE INVENTION

Composition for freshening laundry.

BACKGROUND OF THE INVENTION

There are a variety of particulate through the wash fabric treatment compositions available in the market. The objective of such products is to meet a consumer's desire for perfume bloom to occur during the wash or for delivering perfume to the articles that are washed or both. A common technical approach for delivering the desired benefit is to load a particulate carrier with perfume. The perfume can be one or both of encapsulated perfume and

unencapsulated perfume. Carriers including water soluble polymers, salt, and sugar can be used as the carrier material.

Typically, marketers of through the wash fabric treatment compositions market a plurality of different scent variants. To help the consumer discern various scent variants from one another when she is purchasing the product, each variant can be provided with a different color of particulate. The color is typically provided by a dye. Marketers of such products tend to prefer bright colors to invoke fruity fresh scents and rich light colors to invoke sophisticated scents.

The supply chain for large scale manufacturers of particulate through the wash fabric treatment compositions to deliver product to the shelves of retailers can be lengthy. This can occur because of the distance between the production facility and the end retailer, which may be on different continents. Further, to limit the risk of not being able to meet retail demand at a particular time, one or more of the manufacturer, distributor, and retailer may maintain inventory that can be tapped to meet and absorb fluctuations in the demand for the product.

As the particulate through the wash fabric treatment composition moves through the supply chain, the product can be exposed to harsh environmental conditions. Potentially detrimental environmental conditions to which the product is exposed include heat and moisture. Commonly, products are shipped via a container on a truck, rail car, or boat. These containers can be stored in the sun in hot climates for long durations. Temperatures inside the container can exceed 50 °C and can occur for many days.

For fabric treatment compositions that include perfume, the consequence of high temperature in the supply chain can be problematic with respect to the perfume benefits of the particulate through the wash. The degradation of polymeric materials can increase the rate of decomposition of perfume raw materials, resulting in a change in scent intensity of the fabric treatment composition at one or more consumer touch points, such as neat product odor, wet fabric odor, or dry fabric odor. In addition, some perfume raw materials may be more sensitive than others to degradation, resulting in a change in the character of the fabric treatment composition.

With these limitations in mind, there is a continuing unaddressed need for particulate fabric treatment compositions that have satisfactory perfume stability from the time of manufacture to the time of purchase by a consumer.

SUMMARY OF THE INVENTION

A composition comprising a plurality of particles, wherein said particles comprise: about 40% to about 95% by weight polyethylene glycol, wherein said polyethylene glycol has a weight average molecular weight from about 5000 to about 11000; about 0.1% to about 20% by weight perfume; and about 0.1% to about 50% by weight starch granules, wherein said starch granules have a dextrose equivalent from 0 to about 40, wherein said starch granules have a grain size of from about 1 μιη to about 500 μιη, and wherein said starch granules have a starch perfume load level of said perfume on said starch granules of from 0% to about 10% by weight of the starch granules; wherein said particles are substantially homogenously structured particles; and wherein each of said particles has a mass between about 0.95 mg to about 5 grams.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic of a pastillation apparatus.

FIG. 2 is a schematic of a particle.

DETAILED DESCRIPTION OF THE INVENTION

The particles of the fabric treatment composition may comprise more than about 40% by weight of the composition of polyethylene glycol. The particles of the fabric treatment composition may comprise about 40% to about 95% by weight of the particles of polyethylene glycol. The polyethylene glycol can have a weight average molecular weight from about 5000 to about 11000. The particles may further comprise from about 0.1% to about 20% by weight of the particles of perfume. The particles may further comprise from about 0.1% to about 50% by weight of the particles of starch granules. The starch granules can have a dextrose equivalent from 0 to about 40. The starch granules can have grain sizes of from about 1 μιη to about 500 μηι. The starch granules can have a perfume load level of the perfume on the starch granules of from 0% to about 10% by weight of the starch granules. The particles can be substantially homogeneously structured particles. Individually, the particles can have a mass between about 0.95 mg to about 5 grams. The perfume can be encapsulated perfume. The perfume can be unencapsulated perfume.

Polyethylene Glycol (PEG)

Polyethylene glycol (PEG) has a relatively low cost, may be formed into many different shapes and sizes, minimizes unencapsulated perfume diffusion, and dissolves well in water. PEG can be a suitable carrier for other substances delivered in the wash. PEG comes in various weight average molecular weights. A suitable weight average molecular weight range of PEG for the purposes of freshening laundry includes from 2,000 to about 13,000, from about 4,000 to about 12,000, alternatively from about 5,000 to about 11,000, alternatively from about 6,000 to about 10,000, alternatively from about 7,000 to about 9,000, alternatively combinations thereof. PEG is available from BASF, for example PLURIOL E 8000. The PEG can have a weight average molecular weight of 9000.

The particles of the fabric treatment composition can comprise about 40% or more by weight of the particles of PEG. The particles of the fabric treatment composition can comprise about 50% or more by weight of the particles of PEG. The particles of the fabric treatment composition can comprise about 60% or more by weight of the particles of PEG. The particles of the fabric treatment composition of the present invention may comprise from about 65% to about 99% by weight of the particles of PEG. The particles of the fabric treatment composition may comprise about 40% to about 95% by weight of the particles of PEG.

Alternatively, the particles can comprise from about 40% to about 80%, alternatively from about 45% to about 75%, alternatively from about 50% to about 70%, alternatively combinations thereof and any whole percentages or ranges of whole percentages within any of the aforementioned ranges, of PEG by weight of the particles.

The PEG can have a PEG perfume load level. The PEG perfume load level is the ratio of the mass of perfume in the PEG to the mass of PEG. To promote release of perfume, it can be desirable for the PEG perfume load level to be greater than the starch perfume load level discussed herein. The PEG perfume load level can be measured and compared to the starch perfume load level by 1) heating a sample of the fabric treatment composition containing PEG, perfume and starch granules above its melting point, 2) centrifuging the sample to separate the molten (liquid) PEG phase from the starch granules phase, 3) removing an equal weight portion of both phases, 4) diluting each phase with suitable level of methanol to enable measuring of the relative perfume levels of each phase via standard gas chromatograph and mass spectrometer techniques.

Balancing Agent

The particles of the fabric treatment composition described herein can comprise from about 0.1% to about 10% by weight of the particles of a balancing agent selected from the group consisting of glycerin, polypropylene glycol, isopropyl myristate, dipropylene glycol, 1,2 propanediol, PEG having a weight average molecular weight less than 2,000, and mixtures thereof. The balancing agent can be dipropylene glycol. As used herein, PEG having a weight average molecular weight less than 2,000 is a balancing agent. So, the balancing agent can be PEG having a weight average molecular weight less than 2000. PEG having a weight average molecular weight from 2,000 to about 13,000 is not a balancing agent. PEG having a weight average molecular weight from 2,000 to about 13,000 can be a major component of the particles.

The balancing agent for any of the particles disclosed herein can be selected from the group consisting of isopropyl myristate, dipropylene glycol, and mixtures thereof. Isopropyl myristate can be a suitable balancing agent at a level of about 4% by weight of the particles. Isopropyl myristate can be provided with the unencapsulated perfume.

The balancing agent can be polypropylene glycol. The balancing agent can be polypropylene glycol can have weight average molecular weight less than about 400, alternatively less than about 1,000, alternatively less than about 2,000, alternatively less than about 4,000.

It has been found that levels of PEG having a weight average molecular weight from about 2,000 to about 13,000 forming less than about 98% by weight of the particles can be desirable to provide for uniform formation of particles of a consumer desirable size via a rotoforming process. Optionally, the level of such PEG can be less than about 95% by weight of the particles, less than about 91% by weight of the particles, less than about 88% by weight of the particles, or less than about 80% by weight of the particles. Using a lower fraction of PEG can be desirable to reduce cost and to provide formula space for the inclusion of starch granules.

Some unencapsulated perfumes and perfume microcapsules have such intense scents that they can be overwhelming to consumers. Thus, for intense unencapsulated perfumes and/or perfume microcapsules, only a limited mass fraction of one or more of those components is needed to deliver the desired scent experience. In view that the desirable level of PEG can be less than about 91% by weight of the particles, if only a limited mass fraction of one or more of the unencapsulated perfume and/or perfume microcapsules is used, it may not be possible to produce particles having the desired size and shape, unless a balancing agent is provided in the composition. If an array of fabric treatment compositions is to be provided, the inability to provide for uniformity amongst the particles in the different scent variants across the array can be disconcerting to the consumer. Consumers tend to expect that the products of a single brand within a single category of goods will each have a similar look and feel as well as a similar function and efficacy.

The balancing agent should not interfere with the performance of the particles of the composition, for example by significantly altering the scent, color, or the dissolution profile of the particles. Further the balancing agent should have a suitably small effect on the melting point of the particles so that a variety of particles having different scent can be manufactured within a narrow range or even the same range of process settings. The balancing agent should also not interfere with the ability of the perfume microcapsules to become bound to the fabric being treated or the ability to be retained on the fabric during treatment or optional rinsing. The balancing agent should also not negatively interfere with the structural integrity of the perfume microcapsules, if present, that would lead to unwanted perfume leakage during product storage or an undesired modification of the perfume release profile when bound to the fabric. Balancing agents selected from the group consisting of glycerin, polypropylene glycol, isopropyl myristate, dipropylene glycol, 1 ,2 propanediol, PEG having a weight average molecular weight less than 2,000, and mixtures thereof are thought to not interfere with production of and performance of the particles of the composition. Since the balancing agent is offsetting having to include additional PEG to form particles having the desired size and shape, the balancing agent is desirably less expensive or at least cost-competitive with PEG, compatible with the process used to form the particles, easy to employ in the process used to form the particles, and readily available for supply in commercially viable quantities.

The balancing agent can also be practical in that it can allow the formulation of an array of fabric treatment compositions comprising particles that have similar, if not essentially the same, size, shape, and production characteristics and having a relatively narrow range of PEG levels. Having a narrow range of PEG levels can allow the manufacturer to use a single set of processing conditions to produce particles having different levels of unencapsulated perfume and/or encapsulated perfume, with the balance of the formula comprising the balancing agent, accounting for the inclusion of any dyes and/or formula minors.

For example, consider a first fabric treatment composition and a second fabric treatment composition, the particles of the first fabric treatment composition having a first unencapsulated perfume and the particles of the second fabric treatment composition having a second unencapsulated perfume. If the intensity of the first unencapsulated perfume is greater than the intensity of the second unencapsulated perfume, to have similar scent intensity of the unencapsulated perfume in the particles across the array of fabric treatment compositions, a lower level of first encapsulated can be offset with the balancing agent. This will allow the PEG levels for the particles of the two compositions to be within a narrow range so that the same manufacturing conditions can be used to produce the particles of both, or more, compositions. The balancing agent can be employed in a similar manner if the intensity of the perfume microcapsules or both the perfume microcapsules and unencapsulated perfumes are different between the particles of the compositions.

The particles of the fabric treatment compositions described herein can comprise from about 0.5% to about 5% by weight of the particles of a balancing agent selected from the group consisting of glycerin, polypropylene glycol, isopropyl myristate, dipropylene glycol, 1,2 propanediol, PEG having a weight average molecular weight less than 2,000, and mixtures thereof. The balancing agent for any of the compositions disclosed herein can be dipropylene glycol. The balancing agent for any of the compositions disclosed herein can be isopropyl myristate.

Perfume

The particles of the fabric treatment composition of the present invention may comprise an unencapsulated perfume and/or perfume microcapsules. Perfumes are generally described in U.S. Patent No. 7,186,680 at column 10, line 56, to column 25, line 22. The particles of the fabric treatment composition can comprise unencapsulated perfume and can be essentially free of perfume carriers, such as a perfume microcapsule. Optionally, the particles of the fabric treatment composition comprise perfume carrier materials (and perfume contained therein). Examples of perfume carrier materials are described in U.S. Patent No. 7,186,680, column 25, line 23, to column 31, line 7. Specific examples of perfume carrier materials may include cyclodextrin and zeolites. For the compositions disclosed herein, it is not necessary that the particles of the fabric treatment composition comprise unencapsulated perfume at the time of manufacture. Rather, unencapsulated perfume at the time of manufacture can be an optional component. The starch can provide for perfume stability of unencapsulated perfume provided in the particle at the time of manufacture and unencapsulated perfume in the particle that might exist as a result of leakage from perfume microcapsules that are provided at the time of manufacture. Particles that are substantially free of or free of unencapsulated perfume at the time of manufacture can be desirable if consumers prefer to only have a limited exposure to a scent when dosing the particles of the fabric treatment composition. In absence of unencapsulated perfume at the time of manufacture, the limited exposure to scent might be provided by perfume leaking from encapsulated perfume in the particle after manufacture. A more significant scent experience can be provided after washing when the perfume microcapsules are deposited on the fabric and after the perfume from the microcapsules is released. Unencapsulated perfume can be desirable to provide scent to the particles so that the user of the particles experiences a pleasant smell when she dispenses the particles or opens a container containing the particles.

The particles can comprise about 0.1% to about 20%, alternatively about 1% to about 15%, alternatively 2% to about 10%, alternatively combinations thereof and any whole percentages within any of the aforementioned ranges, of perfume by weight of the particles of the fabric treatment composition. The perfume can be unencapsulated perfume and or encapsulated perfume.

The particles of the fabric treatment composition can comprise unencapsulated perfume and be free or essentially free of a perfume carrier. The particles of the fabric treatment composition may comprise about 0.1% to about 20%, alternatively about 1% to about 15%, alternatively 2% to about 10%, alternatively combinations thereof and any whole percentages within any of the aforementioned ranges, of unencapsulated perfume by weight of the particles of the fabric treatment composition.

The particles can comprise unencapsulated perfume and perfume microcapsules. The particles may comprise about 0.1% to about 20%, alternatively about 1% to about 15%, alternatively from about 2% to about 10%, alternatively combinations thereof and any whole percentages or ranges of whole percentages within any of the aforementioned ranges, of the unencapsulated perfume by weight of the particles. Such levels of unencapsulated perfume can be appropriate for any of the particles disclosed herein that have unencapsulated perfume. The particles can comprise unencapsulated perfume and perfume microcapsules but be free or essentially free of other perfume carriers. The particles can comprise unencapsulated perfume and perfume microcapsules and be free of other perfume carriers.

The particles of the fabric treatment compositions of the present invention can comprise encapsulated perfume. Encapsulated perfume can be provided as plurality of perfume microcapsules. A perfume microcapsule is perfume oil enclosed within a shell. The shell can have an average shell thickness less than the maximum dimension of the perfume core. The perfume microcapsules can be friable perfume microcapsules. The perfume microcapsules, if present, can be moisture activated perfume microcapsules.

The perfume microcapsules can comprise a melamine/formaldehyde shell. Perfume microcapsules may be obtained from Appleton, Quest International, or International Flavor & Fragrances, or other suitable source. The perfume microcapsule shell can be coated with polymer to enhance the ability of the perfume microcapsule to adhere to fabric. The perfume microcapsules can be those described in U.S. Patent Pub. 2008/0305982.

The particles can comprise about 0.1% to about 20%, alternatively about 1% to about

15%, alternatively about 2% to about 10%, alternatively combinations thereof and any whole percentages within any of the aforementioned ranges, of encapsulated perfume by weight of the particles of the fabric treatment composition.

The particles can comprise perfume microcapsules but be free of or essentially free of unencapsulated perfume. The particles may comprise about 0.1% to about 20%, alternatively about 1% to about 15%, alternatively about 2% to about 10%, alternatively combinations thereof and any whole percentages within any of the aforementioned ranges, of encapsulated perfume by weight of the particles of the fabric treatment composition. Starch Granules

The particles of the fabric treatment composition can comprise from about 0.1% to about 50% by weight of the particles of starch granules. Including starch granules in the particles can provide for improved perfume stability from the time of manufacture to the time of purchase as compared to particles that do not include starch granules. The particles of the fabric treatment composition can comprise from about 0.1 % to about 40% by weight of the particles of starch granules. The particles of the fabric treatment composition can comprise from about 0.1% to about 30% by weight of the particles of starch granules. The starch granules can be MELOJEL corn starch from Ingredion. The starch granules can be wheat, rice, potato, tapioca. The starch granules can be a polysaccharide material such as cellulose, xanthan gum, or gum arabic.

Starch is a polysaccharide consisting of a large number of glucose units joined by a glycosidic bond. It is produced by most green plants and can be found in large amounts in staple foods such as corn, wheat, rice and potatoes. One example is unmodified corn starch, such as Melojel corn starch from Ingredion.

The starch granules can have a dextrose equivalent from 0 to about 40. Dextrose equivalent is a characterization of the degree of hydrolyzation of the starch into simpler carbohydrates. The extent of conversion of starch is quantified by dextrose equivalent, which is roughly the fraction of glucosidic bonds that have been broken, or the degree of starch polymer hydrolysis, which is controlled by the hydrolysis reaction. It is a measure of reducing power, in the form of reducing sugars, compared to a dextrose standard of 100. The higher the dextrose equivalent, the greater the extent of starch hydrolysis. Fully hydrolyzed starch, or dextrose, has a dextrose equivalent of 100. Unmodified starch has a dextrose equivalent of 0. Maltodextrins are made by partial hydrolysis of corn starch with suitable acids and/or enzymes and have a dextrose equivalent of less than 20. Corn syrup solids and liquid corn syrups have a dextrose equivalent of greater than 20. The starch granules can have a dextrose equivalent from 0 to about 25.

Starch granules and granules of starch derivatives having a dextrose equivalent from 0 to about 40 are thought to be able to provide a perfume stability benefit and are easily formulated into the particles of the fabric treatment composition. More particularly, starch granules and granular starch derivatives having a dextrose equivalent from 0 to about 25 can provide a perfume stability benefit. Such starch granules are thought to be easily formulated into the particles of the fabric treatment composition. Starch granules having a dextrose equivalent of about 0 can be practical. The benefits of such starch granules are thought to include less negative environmental impact, they may be easier to process in a melt as they may not thicken the melt as much, may be readily available in particles sizes within a desirable range, and may not swell as much as hydrolyzed starch granules. MELOJEL available from INGREDION, Bridgewater, New Jersey, United States of America can be practical.

Starch granules may also help to reduce or control perfume distortion that might occur in particles having both encapsulated perfume and unencapsulated perfume. Unencapsulated perfume may degrade at a different rate than encapsulated perfume. This can lead to a time- dependent distortion in the scent of the particles. The inclusion of starch can help to slow down the perfume distortion of the unencapsulated perfume or unencapsulated perfume that has leaked from the perfume microcapsules.

Granular starch derivatives having a dextrose equivalent between about 25 and about 40 may be more difficult to employ in formulations. Without being bound by theory, it is thought that higher dextrose equivalent starch granules can form particle networks that can lead to unwanted gelling or viscosity growth in the PEG hot melt. Higher dextrose equivalent may also reduce the desired improvement in perfume stability. Without being bound by theory, it is thought that increased starch hydrolysis and higher dextrose equivalent leads to materials that are less capable of slowing unwanted autoxidation reactions as compared to starch granules having lower hydrolysis and lower dextrose equivalent.

The dextrose equivalent of the starch granules is measured using the method of ISO 5377:1981.

To evaluate the ability to process melts into particles, melts having different starch components were prepared. The melts were formed of 67.17% by weight PEG having a weight average molecular weight of 8000, 1.08% by weight dipropylene glycol, 7.50% by weight unencapsulated perfume, 4.04% by weight perfume microcapsules (1.13% by weight active perfume microcapsules), 0.20% by weight dye (5% by weight active), 20.00% by weight starch material as set forth in Table 1, and 0.01% by weight butylated hydroxytoluene.

To make the melts, molten PEG was loaded into a mixing vessel having temperature control to keep the batch materials at about 80 °C during mixing. The individual remaining components of the mixture were mixed into the PEG serially with the mixture being observed to be homogeneous prior to introducing an additional component to the melt.

An attempt was made to spread the mixture into molds having a hemispherical shape having a diameter of about 5 mm and a height of about 2.5 mm. After cooling and hardening of melts that could be formed into the molds, the resulting particles were removed from the mold. The character of processing for each such melt prepared is summarized in Table 1 with the character of processing being descriptive of whether particles could be formed or not. Table 1. Character of processing of a melt consisting of 67.17% by weight PEG having a weight average molecular weight of 8000, 1.08% by weight dipropylene glycol, 7.50% by weight unencapsulated perfume, 4.04% by weight perfume microcapsules, 0.20% by weight dye (5% by weight active), 20.00% by weight starch material, and 0.01% by weight butylated

hydroxytoluene.

To further evaluate the ability to process melts into particles, melts having a starch weight percentage of 10.00% were prepared. Melts were formed of 77.24% by weight PEG having a weight average molecular weight of 8000, 8.20% by weight unencapsulated perfume, 4.41% by weight perfume microcapsules, 0.14% by weight dye (5% by weight active), 0.01% by weight butylated hydroxytoluene, and 10.00% by weight starch material as set forth in Table 2. The character of processing for each such melt prepared is summarized in Table 2. Table 2. Character of processing of a melt consisting of 77.24% by weight PEG having a weight average molecular weight of 8000, 8.20% by weight unencapsulated perfume, 4.41% by weight perfume microcapsules, 0.14% by weight dye (5% by weight active), 0.01% by weight butylated hydroxytoluene, and 10.00% by weight starch material.

For both the 10% by weight starch granules and the 20% by weight starch material, particles we able to be formed when the starch had a dextrose equivalents between 0 and 25.

To evaluate the improvement in perfume stability obtained by including starch granules in the particles, two formulations were compared. The control formula was 87.36% by weight PEG having a weight average molecular weight of 8000, 0.01% by weight butylated hydroxytoluene, 0.85% by weight dipropylene glycol, 7.50% by weight unencapsulated perfume, 4.04% by weight perfume microcapsules, and 0.24% by weight dye (5% by weight active). The test formula was 65.52% by weight PEG having a weight average molecular weight of 8000, 0.01% by weight butylated hydroxytoluene, 0.85% by weight dipropylene glycol, 7.50% by weight unencapsulated perfume, 4.04% by weight perfume microcapsules, 0.24% by weight dye (5% by weight active), and 21.84% by weight starch granules.

The particles were formed in the same manner as that described previously with respect to evaluating the character of processing melts. After forming particles, specimens of each formulation were stored at 35 °C for one year. Perfume was extracted from the control formula without starch and the test formula having starch and the mass of the perfume raw materials was measured using gas chromatography and mass spectrometry. The results reported in Table 3 are normalized against the mass of the respective perfume raw material in the control formula after storage. So, for example, the mass of octanal in the formula having starch granules was 2.1 times greater than the mass of octanal in the formula without starch granules. Table 3. Normalized mass of perfume raw materials in particles after 1 year of storage.

Without being bound by theory, it is thought that including starch in the particles improves perfume stability during storage. As shown in Table 3, after one year of storage, particles having starch granules tend to have a greater mass of most of the listed perfume raw materials than particles that do not have starch granules.

The starch granules can have a grain size between about 1 μιη and about 500 μιη. The starch granules can have a grain size between about 1 μιη and about 200 μιη. The starch granules can have a grain size between about 1 μιη and about 30 μιη. Without being bound by theory, it is thought that smaller grain sizes of starch granules are associated with improved stability of the perfume in the particles.

The starch granules can have a starch perfume load level of from 0% to about 10% by weight of the starch granules. The starch perfume load level is the ratio of the mass of perfume absorbed to the starch granules to the mass of the starch granules. The starch granules can have a starch perfume load level of from 0% to about 5% by weight of the starch granules. The starch granules can have a starch perfume load level of from 0% to about 2% by weight of the starch granules. The starch granules can have a starch perfume load level of from 0% to about 1% by weight of the starch granules. Prior to manufacture of the composition, the starch granules can be substantially free or free from unencapsulated perfume. A starch that is not hydrophobic ally or cationically modified or modified with moieties that significantly improve the ability of the starch to self-emulsify perfume can be practical. The PEG perfume load level can be measured and compared to the starch perfume load level by 1) heating a sample of the fabric treatment composition containing PEG, perfume and starch granules above its melting point, 2) centrifuging the sample to separate the molten (liquid) PEG phase from the starch phase, 3) removing an equal weight portion of both phases, 4) diluting each phase with suitable level of methanol to enable measuring of the relative perfume levels of each phase via standard gas chromatograph and mass spectrometer techniques.

The PEG perfume load level can be greater than the starch perfume load level. The PEG perfume load level can be more than about 1.3 times the starch perfume load level. The PEG perfume load level can be more than about 2 times the starch perfume load level. The PEG perfume load level can be more than about 4 times the starch perfume load level. The PEG perfume load level can be more than about 6 times the starch perfume load level. The PEG perfume load level can be more than about 10 times the starch perfume load level. Higher ratios of the PEG perfume load level to the starch perfume load level are thought to provide for improved release of the perfume contained in the particles.

By maintaining a relatively low level of perfume loading on the starch granules, the perfume provided in the particles can be more freely available for the consumer to experience. Starch can have a tendency to restrain from release perfumes that are typically used in laundry applications. Thus, having a limited amount of perfume fixed with the starch granules can be desirable to promote perfume bloom and provide for scent of the particles at the point of purchase.

Dye

The particles may comprise dye. The dye may include those dyes that are typically used in laundry detergent or fabric softeners. The fabric treatment composition may comprise less than about 0.1%, alternatively about 0.001% to about 0.1%, alternatively about 0.01% to about 0.02%, alternatively combinations thereof and any hundredths of percent or ranges of hundredths of percent within any of the aforementioned ranges, of dye by weight of the particles of fabric treatment composition. Examples of suitable dyes include, but are not limited to, LIQUITINT PINK AM, AQUA AS CYAN 15, and VIOLET FL, available from Milliken Chemical.

Employing a dye can be practical to help the user differentiate between particles having differing scents. Free of Laundry Actives and Softeners

The fabric treatment composition may be substantially free or even free of laundry active and/or fabric softener actives. The particles of the fabric treatment composition may be substantially free or even free of laundry active and/or fabric softener actives. To reduce costs and avoid formulation compatibility issues, particles that are free or substantially free of laundry actives and/or fabric softener actives can be practical. The particles can comprise less than about 3% by weight of the particles, alternatively less than about 2% by weight of the particles, alternatively less than about 1% by weight of the particles, alternatively less than about 0.1% by weight of the particles, alternatively are about free, alternatively free of laundry actives and/or fabric softener actives or combinations thereof. A laundry active includes: detergent surfactants, detergent builders, bleaching agents, enzymes, mixtures thereof, and the like. It is appreciated that a non-detersive level of surfactant may be used to help solubilize perfume contained in the particles. Particles

Particles may be formed by processes including those disclosed in U.S. Patents 5,013,498 and 5,770,235. Particles can be practically formed by processing a melt of the composition that subsequently forms the particles. The melt of the particles of the present invention may be prepared in either batch or continuous mode. In batch mode, molten PEG is loaded into a mixing vessel having temperature control. Starch granules, if present, can then be added and mixed with PEG until the mixture is substantially homogeneous. Balancing agent, if present, can then be added and mixed until the mixture is substantially homogeneous. Perfume can be added to the PEG. The mixture can be mixed until the mixture is substantially homogeneous. Encapsulated perfume, if present, can be added and mixed until the mixture is substantially homogeneous. Dye, if present, can then be added to the vessel and the components are further mixed for a period of time until the entire mixture is substantially homogeneous. In continuous mode, molten PEG is mixed with starch granules, if present, unencapsulated perfume, if present, and perfume microcapsules, if present, in an in-line mixer such as a static mixer or a high shear mixer and the resulting substantially homogeneous mixture is then used to make the particles. Balancing agent, if present, perfume microcapsules, if present, and unencapsulated perfume, if present, can be added to PEG in any order or simultaneously and dye can be added at a step prior to making the particles or any other suitable time. The particles can be made according to the following process. Molten PEG can be provided. Starch granules can be premixed with the PEG prior to forming the melt, for example to simplify material handling and or minimize the number of tanks required to manufacture the particles. Starch granules can be mixed with the PEG. Perfume can be mixed with the PEG. Together, the molten PEG, starch granules, and perfume can form a melt. The melt can be formed into particles. Optionally, perfume microcapsules can be mixed with the PEG. The particles can be formed by passing the melt through small openings. The particles can be formed by depositing the melt in a mold. The particles can be formed by spraying the melt onto a chilled surface. The chilled surface can be a chilled drum. The chilled drum can be a rotating chilled drum.

The particles may be formed into different shapes including tablets, pills, spheres, and the like. A particle can have a shape selected from the group consisting of spherical, hemispherical, compressed hemispherical, lentil shaped, and oblong. Lentil shaped refers to the shape of a lentil bean. Compressed hemispherical refers to a shape corresponding to a hemisphere that is at least partially flattened such that the curvature of the curved surface is less, on average, than the curvature of a hemisphere having the same radius. A compressed hemispherical particle can have a ratio of height to diameter of from about 0.01 to about 0.4, alternatively from about 0.1 to about 0.4, alternatively from about 0.2 to about 0.3. Oblong shaped refers to a shape having a maximum dimension and a maximum secondary dimension orthogonal to the maximum dimension, wherein the ratio of maximum dimension to the maximum secondary dimension is greater than about 1.2. An oblong shape can have a ratio of maximum dimension to maximum secondary dimension greater than about 1.5. An oblong shape can have a ratio of maximum dimension to maximum secondary dimension greater than about 2. Oblong shaped particles can have a maximum dimension from about 2 mm to about 15 mm and a maximum secondary dimension of from about 2 mm to about 10 mm. Oblong shaped particles can have a maximum dimension from about 2 mm to about 10 mm and a maximum secondary dimension of from about 2 mm to about 7 mm. Oblong shaped particles can have a maximum dimension from about 2 mm to about 6 mm and a maximum secondary dimension of from about 2 mm to about 4 mm.

Particles 30 having an oblong shape can be indicative of suitable particle making conditions. For particles 30 produced from a melt, an oblong shape can be an indication that suitable processing conditions are being employed with respect to one or more of temperature of the melt, conveyor surface speed, conveyor surface temperature, or other process condition. When a melt from which particles 30 are prepared is at a sufficiently high temperature, the melt will tend to flow and a surface of the yet to be formed particle 30 will spread out in the machine direction of the conveyor surface after the melt is deposited on the conveyor surface. If the temperature of the melt is too low, forming substantially uniformly shaped particles 30 can be challenging.

Optionally, for any of the formulations disclosed herein, individual particles 30 can have a mass from about 0.95 mg to about 5 g, alternatively from about 0.95 mg to about 2 g, alternatively from about 10 mg to about 1 g, alternatively from about 10 mg to about 500 mg, alternatively from about 10 mg to about 250 mg, alternatively from about 0.95 mg to about 125 mg, alternatively combinations thereof and any whole numbers or ranges of whole numbers of mg within any of the aforementioned ranges. In a plurality of particles 30, individual particles 30 can have a shape selected from the group consisting of spherical, hemispherical, compressed hemispherical, lentil shaped, and oblong.

An individual particle 30 may have a volume from about 0.003 cm³ to about 5 cm³. An individual particle 30 may have a volume from about 0.003 cm³ to about 1 cm³. An individual particle 30 may have a volume from about 0.003 cm³ to about 0.5 cm³. An individual particle 30 may have a volume from about 0.003 cm³ to about 0.2 cm³. An individual particle 30 may have a volume from about 0.003 cm³ to about 0.15 cm³. Smaller particles 30 are thought to provide for better packing of the particles in a container and faster dissolution in the wash.

The composition can comprise particles 30 that are retained on a number 10 sieve as specified by ASTM International, ASTM Ell - 13. The composition can comprise particles 30 wherein more than about 50% by weight of the particles 30 are retained on a number 10 sieve as specified by ASTM International, ASTM Ell - 13. The composition can comprise particles 30 wherein more than about 70% by weight of the particles 30 are retained on a number 10 sieve as specified by ASTM International, ASTM Ell - 13. The composition can comprise particles 30 wherein more than about 90% by weight of the particles 30 are retained on a number 10 sieve as specified by ASTM International, ASTM Ell - 13. It can be desirable to provide particles 30 sized as such because particles retained on a number 10 sieve me be easier to handle than smaller particles.

Without being bound by theory the inclusion of starch in the particles 30 can reduce perfume degradation in the particles 30 associated with autoxidation of the perfume carried in the particles 30. Without being bound by theory, it is thought that the benefit associated with including starch increases with decreasing size of the particles 30. The composition can comprise particles 30 that pass a sieve having a nominal sieve opening size of 22.6 mm. The composition can comprise particles 30 that pass a sieve having a nominal sieve opening size of 22.6 mm and are retained on a sieve having a nominal sieve opening size of 0.841 mm. Particles 30 having a size such that they are retained on a sieve having a nominal opening size of 22.6 mm may tend to have a dissolution time that is too great for a common wash cycle. Particles 30 having a size such that they pass a sieve having a nominal sieve opening size of 0.841 mm may be too small to conveniently handle. Particles 30 having a size within the aforesaid bounds may represent an appropriate balance between dissolution time and ease of particle 30 handling.

A plurality of particles 30 may collectively comprise a dose for dosing to a laundry washing machine or laundry wash basin. A single dose of the particles 30 may comprise from about 1 g to about 27 g.

A single dose of the particles 30 may comprise from about 5 g to about 27 g, alternatively from about 13 g to about 27 g, alternatively from about 14 g to about 20 g, alternatively from about 15 g to about 19 g, alternatively from about 18 g to about 19 g, alternatively combinations thereof and any whole numbers of grams or ranges of whole numbers of grams within any of the aforementioned ranges. The individual particles 30 forming the plurality of particles that can make up the dose can have a mass from about 0.95 mg to about 5 g. The plurality of particles 30 can be made up of particles 30 having different size, shape, and/or mass. The particles 30 in a dose can each have a maximum dimension less than about 15 mm. Each of the particles 30 in a dose can have a maximum dimension less than about 1 cm.

The particles 30 may be manufactured by a pastillation process. A schematic of a pastillation apparatus 100 is illustrated in FIG. 1. The steps of manufacturing according to such process can comprise providing the desired formulation as a viscous material 50. The viscous material 50 can comprise or consists of any of the formulations disclosed herein.

The viscous material 50 can comprise: more than about 40% by weight of the viscous material 50 of PEG (optionally about 40% to about 95% by weight of the viscous material 50 of PEG), wherein the PEG has a weight average molecular weight from about 5000 to about 11000; from about 0.1% to about 20% by weight of the viscous material 50 of perfume; and from about 0.1% to about 50% by weight of the viscous material 50 of starch granules, wherein said starch granules have a dextrose equivalent from 0 to about 40, wherein the starch granules have a grain size between about 1 μιη to about 500 μιη, and wherein the starch granules have a perfume load level of said perfume on the starch of less than about 10% by weight of the starch granules; wherein the viscous material 50 is formed into a plurality of particles 30, each of the particles 30 having a continuous phase of the PEG; wherein each of the particles 30 have a mass between about 0.95 mg to about 5 grams. The starch granules provided in manufacture can be substantially free from perfume. The viscous material 50 can be provided at a processing temperature less than about 20 degrees Celsius above the onset of solidification temperature as determined by differential scanning calorimetry.

The perfume microcapsules can be added as a slurry to the PEG and unencapsulated perfume to form the viscous material 50. The perfume microcapsules can be added as a powder to the PEG and unencapsulated perfume to form the viscous material 50. The viscous material 50 can be passed through small openings 10 and onto a moving conveyor surface 20 upon which the viscous material 50 is cooled below the glass transition temperature to form a plurality of particles 30. As illustrated in FIG. 1, the small openings 10 can be on a rotatable pastillation roll 5. Viscous material 50 can be distributed to the small openings 10 by a viscous material distributor 40. Particles can be formed on a ROTOFORMER, available from Sandvik Materials Technology, such as a Sandvik Rotoform 3000 having a 750 mm wide 10 m long belt. The cylinder of such rotoformer can have 2 mm diameter apertures set at 10 mm pitch in the cross machine direction and 9.35 mm in the machine direction. The cylinder of such rotoformer can be set 3 mm above the belt. The belt speed and rotational speed of the rotoformer can be 10 m/min. The melt can be fed to such rotoformer at 3.1 kg/min from a mixer and be at a temperature of about 50 °C.

Each of the particles 30 can be substantially homogeneously structured. A substantially homogenously structured particle 30 is a particle in which the component materials forming the particle 30 are substantially homogeneously mixed with one another. A substantially homogeneously structure particle 30 need not be perfectly homogeneous. There may be variations in the degree of homogeneity that is within limits of mixing processes used by those skilled in the art in commercial applications. Each of the particles 30 can have a continuous phase of the PEG. Each of the particles 30 can be a continuous phase of a mixture of the component materials forming the particle. So, for instance, if the particles comprise component materials A, B, and C, the particles 30 can be a continuous phase of a mixture A, B, and C. The same can be said for any number of component materials forming the particles 30, by way of nonlimiting example, three, four, five, or more component materials.

A homogeneously structured particle 30 is not a particle that has a core and coating, the particle being discrete from other particles having the same structure. A homogeneously structured particle 30 can be non-mechanically separable. That is, the component materials forming the homogeneously structured particle 30 may not be mechanically separated, for instance by a knife or fine pick. When the particles 30 are taken together as the composition, the composition can be substantially free from or even free from coated inclusions.

Homogeneously structured particles 30 can be substantially free or free from inclusions having a size greater than about 500 μιη. Homogeneously structured particles 30 can be substantially free from or free from inclusions having a size greater than about 200 μιη.

Homogeneously structured particles 30 can be substantially free from or free from inclusions having a size greater than about 100 μιη. Without being bound by theory, an abundance of large inclusions may be undesirable because they might interfere with the dissolution of the particle 30 in the wash or leave visually perceptible residue on the articles being washed.

As used herein, size refers to the maximum dimension. A cross section of a

homogeneously structured particle 30 does not reveal an overall structure of the particle to be a core and coating. M&M'S candy marketed by Mars, Incorporated, which is a chocolate core having a sugar coating, is not a homogeneously structured particle. In the case of M&M'S candy, the chocolate core and coating are mechanically separable. A chocolate covered raisin is similarly not a homogeneously structured particle. A homogeneously structured particle 30 is not a coated particle.

A schematic of a substantially homogeneous structured particle 30 is shown in Fig. 2. As shown in Fig. 2, the perfume 110 can be substantially randomly dispersed in the PEG 120. The perfume 110 can be unencapsulated perfume and or perfume microcapsules. The starch granules 130 can be substantially randomly dispersed in the PEG 120 as well. As shown in Fig. 2, a substantially homogeneously structured particle 30 is not a particle having a core and coating arrangement. Rather, the constituent components of the formula are substantially

homogeneously mixed with one another. Without being bound by theory, substantially homogeneous structured particles 30 are thought to possibly be less capital intense to produce and the processes to produce such particles 30 are thought to result in more uniform particles which are more acceptable to the consumer.

The particles 30 can have a substantially flat base 140. The particles 30 can have a flat base 140. The particles 30 can have a flat or substantially flat base 140. A flat base 140 or substantially flat base 140 can be beneficial because it can provide visual indicia of suitable processing conditions with respect to one or more of temperature of the melt, conveyor surface speed, conveyor surface temperature, or other process condition. When a melt from which particles 30 are prepared is at a sufficiently high temperature, the melt will tend to flow and a surface of the yet to be formed particle 30 will conform to the surface of the conveyor surface. If the temperature of the melt is too low, forming uniformly shaped particles 30 can be challenging.

The particles 30 can have a substantially circular flat base 140. The substantially circular flat base 140 can have a diameter between about 1 mm and about 12 mm. The substantially circular flat base 140 can have a diameter between about 2 mm and about 8 mm. The substantially circular flat base 140 can have a diameter between about 4 mm and about 6 mm.

The composition comprising a plurality of particles 30 can be as follows with the numbers in brackets corresponding to how the composition may be described and claimed: [1] A composition comprising a plurality of particles (30), wherein said particles comprise: 40% to 95% by weight of said particles of polyethylene glycol (120), wherein said polyethylene glycol has a weight average molecular weight from 5000 to 11000; 0.1% to 20% by weight of said particles of perfume (110); and 0.1% to 50% by weight of said particles of starch granules (130), wherein said starch granules have a dextrose equivalent from 0 to 40, wherein said starch granules have a grain size of from 1 μιη to 500 μιη, and wherein said starch granules have a starch perfume load level of said perfume on said starch granules of from 0% to 10% by weight of the starch granules; wherein said particles are substantially homogenous ly structured particles; and wherein each of said particles has a mass between 0.95 mg to 5 grams. [2] The composition according to [1], wherein said particles are substantially free from inclusions having a size greater than 500 μιη. [3] The composition according to [1] or [2], wherein said starch granules have a dextrose equivalent from 0 to 25. [4] The composition according to any one of [1] through [3], wherein said starch granules have a grain size of from 1 μιη to 200 μιη. [5] The composition according to any one of [1] through [4], wherein said polyethylene glycol has a polyethylene glycol perfume load level of said perfume on said polyethylene glycol, wherein said polyethylene glycol perfume load level is greater than said starch perfume load level. [6] The composition according to any one of [1] through [5], wherein said particles further comprise dye.

[7] The composition according to any one of [1] through [6], wherein said perfume comprises encapsulated perfume. [8] The composition according to any one of [1] through [7], wherein said perfume comprises unencapsulated perfume. [9] The composition according to any one of [1] through [8], wherein said starch granules are unmodified starch. [10] The composition according to any one of [1] through [9], wherein said particles are substantially free from inclusions having a size greater than 200 μιη. [11] The composition according to any one of [1] through [10], wherein said particles are substantially free from inclusions having a size greater than 100 μηι. [12] The composition according to any one of [1] through [11], wherein said starch granules have a grain size of from 1 μιη to 30 μιη. [13] The composition according to any one of [1] through [12], wherein said particles have a flat or substantially flat base. [14] The composition according to any one of [1] through [13], wherein said particles are in a dose of from 1 g to 27 g. [15] The composition according to any one of [1] through [14], wherein said particles are retained on an ASTM El 1-13 number 20 sieve.

The particles 30 can be made according to the following process, with the numbers in brackets corresponding to how the process may be described and claimed: [1] A process for forming particles (30) comprising the steps of: forming a melt by: providing molten polyethylene glycol; providing starch granules and mixing the starch granules with said polyethylene glycol; and providing perfume and mixing the perfume with said polyethylene glycol; and forming the melt into particles. [2] The process according to [1], wherein said particles are formed by passing said melt through small openings. [3] The process according to [1], wherein said particles are formed by depositing said melt into a mold. [4] The process according to [1], wherein said particles are formed by spraying said melt onto a chilled surface. [5] The process according to any one of [1] through [4], wherein said perfume comprises encapsulated perfume.

[6] The process according to any one of [1] through [5], wherein said particles are substantially free from inclusions having a size greater than 500 μιη. [7] The process according to any one of [1] through [6], wherein said starch granules have a grain size of from 1 μιη to 200 μιη. [8] The process according to any one of [1] through [7], wherein said polyethylene glycol has a polyethylene glycol perfume load level of said perfume on said polyethylene glycol, wherein said polyethylene glycol perfume load level is greater than said starch perfume load level. [9] The process according to any one of [1] through [8], wherein said particles are substantially free from inclusions having a size greater than 100 μιη. [10] The process according to any one of [1] through [9], wherein said starch granules have a grain size of from 1 μιη to 30 μιη. [11] The process according to any one of [1] through [10], wherein said particles have a flat or substantially flat base. [12] The process according to any one of [1] through [11], wherein said particles are retained on an ASTM El 1-13 number 20 sieve.

The particles can be made according to the following process. Molten PEG can be provided. Starch granules can be mixed with the PEG. Perfume can be mixed with the PEG. Together, the molten PEG, starch granules, and perfume can form a melt. The melt can be formed into particles. Optionally, perfume microcapsules can be mixed with the PEG. The particles can be formed by passing the melt through small openings. The particles can be formed by depositing the melt into a mold. The particles can be formed by spraying the melt onto a chilled surface.

The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm."

Every document cited herein, including any cross referenced or related patent or application, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.

While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims

CLAIMS What is claimed is:

1. A composition comprising a plurality of particles (30), wherein said particles comprise:

40% to 95% by weight polyethylene glycol (120), wherein said polyethylene glycol has a weight average molecular weight from 5000 to 11000;

0.1% to 20% by weight perfume (110); and

0.1% to 50% by weight starch granules (130), wherein said starch granules have a dextrose equivalent from 0 to 40, wherein said starch granules have a grain size of from 1 μιη to 500 μιη, and wherein said starch granules have a starch perfume load level of said perfume on said starch granules of from 0% to 10% by weight of said starch granules; wherein said particles are substantially homogenously structured particles; and wherein each of said particles has a mass between 0.95 mg to 5 grams.

2. The composition according to Claim 1, wherein said particles are substantially free from inclusions having a size greater than 500 μιη.

3. The composition according to Claim 1 or Claim 2, wherein said starch granules have a dextrose equivalent from 0 to 25.

4. The composition according to any one of the preceding claims, wherein said starch granules have a grain size of from 1 μιη to 200 μιη.

5. The composition according to any one of the preceding claims, wherein said polyethylene glycol has a polyethylene glycol perfume load level of said perfume on said polyethylene glycol, wherein said polyethylene glycol perfume load level is greater than said starch perfume load level.

6. The composition according to any one of the preceding claims, wherein said starch granules have a dextrose equivalent of zero.

7. The composition according to any one of the preceding claims, wherein said perfume comprises encapsulated perfume.

8. The composition according to any one of the preceding claims, wherein said perfume comprises unencapsulated perfume.

9. The composition according to any one of the preceding claims, wherein said starch granules are unmodified starch.

10. The composition according to any one of the preceding claims, wherein said particles are substantially free from inclusions having a size greater than 200 μιη.

11. The composition according to any one of the preceding claims, wherein said particles are substantially free from inclusions having a size greater than 100 μιη.

12. The composition according to any one of the preceding claims, wherein said starch granules have a grain size of from 1 μιη to 30 μιη.

13. The composition according to any one of the preceding claims, wherein said particles have a substantially flat base (140).

14. The composition according to any one of the preceding claims, wherein said particles are in a dose of from 1 g to 27 g.

15. The composition according to any one of the preceding claims, wherein said particles are retained on an ASTM El 1-13 number 20 sieve.