Pouched compositions

ES 2 248 294 T3

DESCRIPTION

Compositions in the bag.

Technical field

The present invention relates to compositions in a bag having a compartment containing different components attached in different regions and to a process for making these bag compositions.

Background of the invention

Cleaning compositions currently exist in different product forms such as granules, liquids and tablets, each form presenting its corresponding advantages and disadvantages.

Recently, tablets have attracted renewed interest, mainly because they are easy for the consumer to handle and easy to dose ("unit dose") and have the additional advantage that they allow the incorporation of incompatible ingredients separated from each other, for example in different layers. This can reduce the contact area between these incompatible materials and thus reduce the possibility of any reaction between these materials.

However, to prepare shelf-stable tablets and to avoid tablet breakage during handling, the ingredients need to be compressed together and the use of binders is generally necessary to prevent the tablets from breaking. This can reduce its solubility and dispersibility, which is undesirable neither for the consumer nor from a performance standpoint.

Therefore, alternative forms or improved forms are required to provide user-friendly unit dose products whereby the different ingredients can be present separately from each other in an easy way (for example to reduce intimate contact and improve the stability of the ingredients. incompatible) without being pulverized or broken.

The inventors have now found a better way to provide improved products by solving the above problems, ie by incorporating a product in a bag in a specific way to meet the above requirements.

Bags containing particulate materials in water-soluble or dispersible containers are known (see EP-A-008910). Detergent bags are known in the art to be useful for providing unit dose compositions and for separating different ingredients from each other. For example, US-5,224,601 and EP-A-414,462 describe packages made with different compartments for different materials. However, this type of structure as well as other bags known in the art present problems and often require a complicated manufacturing process and a relatively large amount of material for the sheet.

The inventors have now found improved particulate bag compositions in which intimate contact with different components thereof is reduced without the need to compact them at the level of the tablets or make difficult structures, such as multiple separate compartments, to separate the different ingredients from each other. In the products of the invention, the different components of the compositions are hermetically packaged in different regions of one and the same compartment or bag, so that they are basically immobilized or fixed and remain so during handling and storage. However, since the components are still in powder or granular form and are not glued together as in tablets, dissolution or dispersion in water of the composition comprising these components is very rapid. Thus, better storage stability of incompatible ingredients such as enzymes and bleaches, minimal use of pouch material, and very good product release and performance are achieved.

In addition, improved processes are provided for forming the composition of the bag so that the components in the regions remain fixed or immobilized.

Summary of the invention

The present invention provides a composition in a bag, the composition comprising two or more particulate components and the bag comprising one or more water-disintegrable, water-soluble or water-dispersible compartments, whereby at least two of the components that are different from each other are present in one and the same compartment and each form a fixed region in said compartment.

The composition in a bag of the invention is prepared by a process comprising the steps of:

a) obtaining an open bag comprising an open compartment;

b) introducing a particulate component before at least one other different particulate component into the open compartment and / or introducing a particulate component into a different part of the open component than at least one other shaped component different particle; Y

ES 2 248 294 T3

c) then closing the open compartment so as to obtain a bag with a compartment (soluble in water or dispersible in water) comprising fixed regions of said components in the form of different particles.

The components are packaged so tightly that the regions are fixed, while the composition remains free-flowing (which can be seen when the bag is removed). This provides the advantages described above.

Typically this can be done by filling the open compartment to overflowing, using a stretchable and preferably elastic material for the compartment, using heat shrinkable material for the compartment, or filling and closing the open compartment under reduced pressure or even under vacuum.

The composition in the bag is preferably such that the bulk density of the composition after closing the compartment is 5% to 45% or even 35%, preferably 5% to 30% or even 10% to 25% higher than the average of the bulk density of the components before their introduction into the compartment.

Preferably, the bag as a whole is water soluble. Preferably the composition is a cleaning composition or a fabric care composition or a rinse additive composition.

The invention also provides processes for making the bag compositions of the invention, for example by the process described above and the preferred processes claimed and described below. A preferred process is such that a non-uniform thickness of the material in the compartment is obtained, which can provide a very rapid release of the product to the water or can help to control the release time of different components to the wash water.

Detailed description of the invention

Compositions and components thereof

The composition of the invention is present in a bag and is also referred to herein as a bag composition. The composition comprises at least two different particulate components. Generally, the particulate component is a powder, granules, extrudate, or flake.

As used herein, a "different" component means that the component has at least one different chemical property, for example that it has at least one different ingredient, than the other component (s), or that the component has at least one physical property. different than the other component (s). Typically, one component comprises one or more oxidizing ingredients and another component comprises one or more reducing ingredients or oxidizable ingredients. Examples are included below.

The particulate components are present in the compartment forming fixed or immobilized regions within this compartment.

The fixation of the regions limits the direct contact between the components of the composition, preferably it limits it only to the zone where the regions contact, without it being necessary to have separate compartment structures for each component.

Typically, regions are formed by introducing one particulate component into an open compartment prior to introducing another particulate component, such that layers of components are obtained, for example. Alternatively, or additionally, this can be accomplished by inserting a component into a different part of the open compartment.

Typically, the regions are fixed or immobilized by hermetically packaging the components together and checking that there is essentially no free headspace within the compartment that could allow movement of the powder. Typically, the hermetic packaging is such that the bulk density of the components after closing the compartment, and thus the bulk density of the compositions in the bag, is 5% to 45%, preferably 35%, preferably 5% or even 10% to 30% or even 25%, or it may be preferred to be 8% to 20% or even 15%, higher than the average bulk density of the components prior to their incorporation into the bag.

The bulk density of a component prior to incorporation into the bag composition can be determined by the reverse cup method, as described in ISO 3424-1975-E. The average bulk density of the components prior to their incorporation into the compartment is calculated by first measuring the bulk density of each component according to ISO 3424 and then a weighted average is calculated based on the percentage by weight of the component in the final composition. For example, a bag consists of a compartment with a composition consisting of two components A and B. Component A is present in 40% by weight of the final composition. Component B is present in 60% by weight of the final composition. Component A has a bulk density according to the reverse cup method (measured according to ISO 3424) of 500 g / l. Component B has a bulk density

ES 2 248 294 T3 of 800 g / l (measured according to ISO 3424). The average bulk density of the composition before being incorporated into the bag is, therefore, ((500 x 0.4) + (800 x 0.6)) = 680 g / l.

The average bulk density of the bag composition, after the compartment is closed, can be determined by a volume displacement method.

A container with a wide neck and a detachable arm is filled with a solvent of known density, which should not affect the material in the compartment or the material in the form of a bag, down to the level of the collecting arm. The composition of the bag to be analyzed is accurately weighed and then immersed in the liquid, for example using a piece of fine metal wire. The amount of liquid that is displaced by the composition of the bag in the liquid leaves the container through the arm, which amount is carefully collected and weighed. The volume of this displaced liquid is easily calculated from the weight and the known density of the liquid. The density and volume displaced by the bag material (rather than the composition within the bag) can be measured or calculated. This can be deduced from the volume of liquid displaced as measured in the previous test. The density of the composition can then be calculated (errors associated with the use of the fine wire used to immerse the bag are minimal and are not taken into account). Depending on the material of the bag or compartment, a suitable liquid can be selected. For example, for a water soluble material like PVA, the preferred liquid is glycerol. Bags can contain microscopic pores in the film as a result of stretching so using a viscous solvent such as glycerol minimizes any errors due to leakage of liquid into the bag. Nonionic surfactants such as Neodol 235 are also useful.

Fixed region shaping and hermetic conditioning can be accomplished by increasing conditioning efficiency and reducing the space between component particles, for example by vibrating the components in the open compartment, allowing the components to settle over a period of time, slightly increasing the pressure, for example applying a pressure of up to 20 MPa, preferably up to 10 MPa or more preferably up to 5 MPa or even up to 2 MPa, if pressure is used, provided that the components and composition maintain free flow,

The bulk density of the component can be achieved by a compaction step. Typically, the particulate component is first placed in the open compartment and then pressure is exerted on said component causing the bulk density of said component to increase from 5% to 50%, preferably 10% or 15%. or 20%, and preferably 45% or 40% or 35% or 30%, of the original apparent density of the component before the compaction step.

The pressure can be exerted in the form of a solid body that is typically of a size and shape capable of fitting the opening of the open compartment. The solid body is capable of applying pressure on said component. Preferably, the solid body applies a pressure of up to 20 MPa, preferably up to 10 MPa or more preferably up to 5 MPa or even up to 2 MPa, to the particulate component.

To ensure a hermetic packaging of the components in the compartments, the particulate components are introduced, for example, into the open compartment (the preferred processes for this are described below) so that the open compartment is preferably almost completely filled , typically such that at least 95% of the volume of this form of open compartment, preferably at least 98% or even at least 100% of the open compartment shape is filled before closing said open compartment shape, or it may even be preferred that the shape is filled to overflowing with the components, i.e. the volume of the components is greater than 100% of the volume of the form, preferably greater than 105% or more preferably greater than 110% or even greater than 115%. In this case, closing the open compartment filled to 95% by volume or more ensures that only a very limited head space remains in the compartment after closing and therefore there is very limited movement of components in these compartments, that is, the regions formed by the components are fixed.

The composition in the bag of the present invention can, for example, be obtained by a process that involves

a) obtaining an open bag comprising an open compartment;

b) introducing a particulate component before at least one other particulate component into the open compartment and / or introducing a particulate component into a different part of the open component than at least one other particulate component particles; Y

c) then closing the open compartment so as to obtain a bag with a compartment comprising fixed regions of said particulate components.

In a preferred process, step c) of the above process can be carried out under reduced pressure, below atmospheric pressure, preferably applying vacuum, so that after filling and closing under reduced pressure or under vacuum, a compartment packaged in shape is obtained. hermetic.

ES 2 248 294 T3

The compartment is preferably formed from a stretchable material, preferably a film, preferably an elastic film, as described below. This is especially useful if the open compartment is filled completely or even overflowing and closed with a stretch film so that stretching the part of the film used to close the compartment and / or stretching the film in the open compartment you get airtight conditioning and fixed regions. Therefore, the use of an elastic material is preferred to ensure that tight conditioning is maintained over time.

Alternatively, the open compartment is rigid and in step b) the components are introduced into the open compartment such that at least 100%, preferably at least 105%, of the open compartment is occupied by the components, and then the compartment opened it is preferably closed with a stretchable material.

The shaping of fixed regions and hermetic conditioning can also be achieved by using a shrinkable material for the compartment, in which the surface area is reduced during or after closing the open compartment by contracting the material. A suitable material is, for example, a heat shrinkable material.

The shaping of the open compartment or the open form can be carried out by any known method. Preferred open shapes are prepared by introducing the material to form the compartment into a mold and then applying a vacuum to the mold so that the material takes the shape of the mold, a method also referred to as vacuum forming. Another preferred method is thermoforming to get the material to conform to the shape of the mold.

Introduction of the components can be done by any suitable method for introducing free-flowing materials into the mold.

Although the compartment comprises at least two particulate components, a liquid component can be added. It may be preferred to introduce a first particulate component into the open compartment first, then spray a small amount of liquid, typically 0.5% to 10% or even 1% to 5%, by weight of the primer. component, preferably water, and finally add the second component in the form of particles. In this way the regions can be even more fixed or immobilized.

The component comprises at least an amount of at least one particulate compound, but typically the component comprises at least two particulate compounds, preferably carefully mixed to form the component. As the components in the compartment of the bag are fixed in fixed regions, the interaction between the different components is reduced. This allows incompatible ingredients to be incorporated into a composition by separating these into fixed regions.

The composition of the present invention can be any composition in particulate form, in particular any powdery or granulated free-flowing composition that must be released into and be active therein.

Preferred compositions are beverages, edible compositions, pharmaceutical compositions, personal care compositions, cleaning compositions, fabric care or conditioning compositions; most preferably, the compositions of the present invention are cleaning compositions or fabric care compositions, preferably hard surface cleaners, more preferably laundry or dishwashing compositions, including detergents, pretreatment or soak compositions. or fabric conditioners and other rinse additives.

When used in cleaning compositions, the component can contain any active cleaning ingredient. Especially preferred are active ingredients such as surfactants, chelating agents, builders, enzymes, perfumes, bleaches, bleach activators, fabric softeners, fabric conditioners, antibacterial agents, effervescent sources, brighteners and photo-whiteners. The fabric care compositions preferably comprise at least one or more softeners, such as quaternary ammonium compounds and / or softening clays, and preferably additional agents such as anti-wrinkle aids, perfumes, chelators and polymers to preserve the integrity of the fabrics. tissues.

Generally, water is present at a level of 0% to 10%, more preferably 0.2% to 5% or even 0.2% to 3% or even 0.5% to 2%, by weight of the compartment, preferably the bag.

Typically, the composition comprises an amount of cleaning composition such that one or more compositions in the bag is or is sufficient for one wash.

Although the nature of the composition of the bag is such that it dissolves or disperses readily in water, it may be preferred that disintegrants such as effervescence sources, water-swellable polymers or clays are present in the bag itself or in the material itself. of the compartment and / or in the composition of the invention; in particular effervescent sources based on an organic acid and a carbonate source are useful. Suitable acids include citric acid, malic acid, maleic acid, and fumaric acid; suitable carbonate sources include sodium carbonate, bicarbonate and percarbonate salts. The preferred levels for the adjuvants of the

ES 2 248 294 T3 disintegration or the sources of effervescence or for both are from 0.05% to 15% or even from 0.2% to 10% or even from 0.3% to 5%, by weight of the composition of the bag.

In particular, for cleaning compositions it is beneficial that one component comprises at least one or more enzymes and another component comprises a peroxygen bleaching agent such as a percarbonate salt. The component containing the peroxygen bleaching agent is then enzyme-free, while the component comprising the enzyme may comprise a bleach activator but not a peroxygen bleaching agent.

It is also beneficial to include the bleaching agents, and in particular the peroxygen bleaching agent, in a component other than any hygroscopic material or anhydrous or hydratable material including excess dried materials, such as aluminosilicates, anhydrous salts or acids.

When the bag compositions are such that they have a visually distinguishable top side and bottom side and if the regions are layered, it may also be beneficial to include non-gelling detergent ingredients, such as water soluble acids and salts, in the bottom layer. including for example effervescent salts and acids such as carbonate salts and organic carboxylic acids such as citric acid, and in a higher or upper layer possible gelling ingredients such as anionic and non-ionic surfactants. Therefore, it is beneficial to include any peroxygen bleaching agent in the lower layer and any enzymes in the upper layer, if necessary. It has been found that when this bag composition is introduced into the wash solution through a dispensing device, in particular a dispensing drawer, faster and more complete release to the wash solution is achieved.

It may be beneficial to include any surfactant and bleach in the compartment so that it is released before any softener in the compartment or bag.

It may even be possible that some or all of the components are not pre-granulated, such as agglomerates, spray dried, extruded, prior to incorporation into the compartment, and that the component is a mixture of dry mixed powder ingredients or even raw materials. It may be preferable that, for example, less than 60%, or even less than 40% or even less than 20% of the component, is in the form of free-flowing pre-granules.

It has also been found to be beneficial for cleaning performance when the cleaning composition of the present invention or the compartment or bag material, preferably both the composition and said material, comprise one or more chelating agents, in particular chelating agents containing phosphonate and / or carboxylate, in particular EDDS, EDTA or HEDP.

It has also been found that the presence in the wash water of high levels of certain compartment or bag material dissolved with free hydroxy groups can adversely affect clay stain removal under certain wash conditions. Therefore, it is not only beneficial to use as little compartment material as possible and thus preferably use a bag with a single compartment, but it has also been found beneficial to incorporate a polyalkoxylated compound into the composition or material of the bag, preferably a polyalkoxylated alcohol, preferably with an average alcohol carbon chain length of 11 to 24, preferably 12 to 20 or even 14 to 18, and an average degree of alkoxylation of at least 20 or even at least 40 or even at least 70. Highly preferred percentages are 0.1% to 8%, or even 0.5 to 5% or even 0 8% to 3%, by weight of the composition of the bag of this compound and TAE80 is especially preferred.

The composition may also comprise liquid compounds, gels or solutions of compounds, for example nonionic surfactants in liquid or gel form, liquid fabric softeners, preferably contained in a separate compartment of the pouch.

Another preferred ingredient is a perhydrate bleach, such as percarbonate salts, especially the sodium salts, and / or an organic peroxyacid bleach precursor or activator compound. When the bag or compartment is formed from a material with free hydroxy groups, such as PVA, the preferred bleaching agent comprises a percarbonate salt and is preferably free of any perborate salt or borate salt. Borates and perborates have been found to interact with these hydroxy-containing materials and may reduce dissolution of the materials and may also reduce yield.

Preferred activators or precursors are imide-type alkyl percarboxylic precursor compounds including alkylene-, N, N'N¹ tetra acetylated diamines where the alkyl group contains 1 to 6 carbon atoms, especially those compounds where the alkyl group contains 1, 2 and 6 carbon atoms such as tetraacetyl ethylenediamine (TAED), 3,5,5-tri- Sodium methyl hexanoyloxybenzene sulfonate (iso-NOBS), sodium nonanoyloxybenzene sulfonate (NOBS), sodium acetoxybenzene sulfonate (ABS) and pentaacetyl glucose, but also amide substituted alkyl peroxyacid precursor compounds.

A highly preferred ingredient for use in the present invention is one or more enzymes. Preferred enzymes include lipases, cutinases, amylases, neutral and alkaline proteases, cellulases, endolases, esterases, pectinases, lactases.

ES 2 248 294 T3 and commercial peroxidases that are conventionally incorporated into detergent compositions. Suitable enzymes are discussed in US-3,519,570 and US-3,533,139. Preferred commercial protease enzymes include those sold under the brands Alcalase, Savinase, Primase, Durazym and Esperase by Novo Industries A / S (Denmark), those sold under the brands Maxatase, Maxacal and Maxapem by Gist-Brocades, those sold by Genencor International and those marketed under the Opticlean and Optimase brands by Solvay Enzymes. Preferred amylases include, for example, α-amylases obtained from a special strain of B. licheniformis, described in more detail in GB-1,269,839 (Novo). Suitable preferred commercial amylases include, for example, those sold by Gist-Brocades under the trade name Rapidase and those sold by Novo Industries A / S under the trade names Termamyl, Duramyl and BAN. Highly preferred amylase enzymes may be those described in WO 97/32961, WO95 / 26397 and WO96 / 23873. The lipase can be of fungal or bacterial origin and is obtained, for example, from a lipase-producing strain of Humicola sp., Thermomyces sp. or Pseudomonas sp., including Pseudomonas pseudoalcaligenes and Pseudomas fluorescens. Also useful in the present invention is a lipase from chemically or genetically modified mutants of these strains. A preferred lipase is derived from Pseudomonas pseudoalcaligenes, described in EP-B-0218272.

Another preferred lipase in the present invention is obtained by cloning the Humicola lanuginosa gene and expression of the gene in Aspergillus oryza, as a host, as described in EP-A-0258 068, which is marketed by Novo Industri A / S, Bagsvaerd , Denmark, with the brand name Lipolase. This lipase is also described in US 4,810,414, issued to Huge-Jensen et al. on March 7, 1989.

Anionic surfactants are also preferred, which include salts (including, for example, sodium, potassium, ammonium, and substituted ammonium salts such as monoethanolamine, diethanolamine, and triethanolamine salts) of sulfate, sulfonate, carboxylate, and sarcosinate-type anionic surfactants, preferably linear or branched alkylbenzene sulfonate, alkyl sulfates and alkyl ethoxylsulfates, isethionates, N-acyl taurates, methyl tauride fatty acid amides, alkylsuccinates and sulfosuccinates, sulfosuccinate monoesters (especially C monoesters₁₂-C₁₈saturated and unsaturated), sulfosuccinate diesters (especially C₆-C₁₄ saturated and unsaturated) and N-acyl sarcosinates. Most preferred is that when anionic surfactants are present, at least one alkyl sulfate surfactant is present, preferably a branched alkyl sulfate surfactant, preferably at a level of 1% to 20% or even 15% by weight of the composition.

Nonionic surfactants such as nonionic surfactants selected from the classes of the nonionic condensates of alkyl phenols, nonionic ethoxylated alcohols, nonionic ethoxylated / propoxylated fatty alcohols, ethoxylated / propoxylated condensates with nonionic propylene glycol are also preferred. non-ionic ethoxylated condensation compounds with propylene oxide / ethylenediamine addition compounds.

Cationic surfactants and softeners may also be present in the present invention, for example quaternary ammonium surfactants and softeners and choline ester surfactants.

Coloring agents such as iron oxides and hydroxides, azo dyes, natural dyes, may also be present in the composition or preferably in the compartment or in the pouch material, preferably they are present at levels of 0.001% to 10% or even 0.01 to 5% or even 0.05 to 1%, by weight of the bag composition.

In a preferred embodiment of the present invention, the composition in the bag comprises a first particulate component that forms a first fixed region in the compartment of the bag and comprises perfume, and a second particulate component that forms a second fixed region in the bag compartment and comprises a member selected from the group consisting of bleach, nonionic surfactant, polyethylene glycol with a molecular weight of 4000 or higher, enzyme and combinations thereof. Typically, the second component is free of perfume. In this preferred embodiment of the present invention, the perfume in the composition is more stable since it is contained in a fixed layer separated from the above ingredients that destabilize the perfume. This allows the perfume to remain stable in the composition comprising the perfume destabilizing ingredient.

Bag and compartment (s) thereof

The bag of the present invention has a closed structure, is made of the materials described herein, and encloses a volumetric space that comprises the composition. Thus, the bag can have any suitable shape, design or material to contain the composition before use, e.g. They do not allow release of the composition from the bag before the composition in the bag comes into contact with the water. The exact execution will depend, for example, on the type and amount of the composition in the bag, the number of compartments in the bag, and the characteristics required for the bag to contain, protect, and deliver or release the compositions.

The bag may be of such a size that it conveniently contains a unit dose amount of the composition of the present invention suitable for the required operation, for example when the composition is a detergent composition, this amount may be sufficient for one wash, or only a partial dose, to offer the consumer greater flexibility to vary the amount used, for example depending on the size and / or degree of soiling of the wash load.

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Preferably, the bag composition is formed in a mold with a round or flat bottom and rounded walls. Therefore, it is also preferred that the bag composition has a spheroid or more preferably cylindrical shape.

The bag has one or more compartments, where at least one contains at least two different particulate components. In a preferred embodiment, all of the particulate components are present in one and the same compartment of the bag and it may be preferred that the bag has only one compartment. This reduces the amount of material needed to form the compartment and bag. However, it may be preferred that one or more additional compartments for the liquid component are present in addition to the compartment comprising the two or more particulate components.

The compartment of the bag has a closed structure, made of the materials described herein, which encloses a volumetric space comprising the components. Thus, the compartment is suitable to contain the particulate components prior to use, e.g. ie, without allowing the release of the components from the compartment before the composition in the bag comes into contact with the water. The compartment can be of any shape or design, depending on the type of material of the compartment, the type of the components or the composition, the intended use, the quantity of the components, etc. If more than one compartment is present, the compartments are joined or connected to each other by any means, for example sealed by heat sealing or wetting or glued with any known glue; Examples of these methods are described below.

Preferably, the compartment or preferably the bag as a whole is made of a material that is stretchable, as described herein. This, for example, facilitates the closure of the open compartment that is filled to more than 95% by volume or even 100% or even filled to overflow as described above. Furthermore, the material is preferably elastic to ensure tight conditioning and fixation of the regions during handling, e.g. For example, to ensure that no headspace (additional) is formed after the compartment is closed.

Preferred stretchable materials have a maximum degree of stretch of at least 150%, preferably at least 200% and more preferably at least 400%, which is determined by comparing the original length of a piece of material with the length of this piece of material. material just before rupture by stretching by applying a force of at least 1 Newton. Preferably the material is such that it has a degree of stretch as mentioned above, when a force of at least 2 Newton, or even at least 3 Newton is applied. Preferably it has this degree of stretch when a force is applied with the lower limits above, but not greater than 20 Newton, or even 12 Newton, or even 8 Newton. For example, a piece of film with a length of 10 cm, a width of 1 cm, and a thickness of 40 microns is stretched lengthwise with a force of 2.8 Newton and the tension is increased until it breaks. The degree of elongation just before break can be determined by continuously measuring the length to calculate the degree of stretch. For example, this piece of film with an original length of 10 cm can be stretched with a force of 2.8 Newton to 52 cm just before breaking and then has a maximum degree of stretch of 520%.

The force to stretch this piece of film (10 cm x 1 cm x 40 microns) to a degree of 200% should preferably be at least 1 Newton, preferably at least 2 Newton, more preferably at least 2.5 or even 3 Newton, and preferably not more than 20 Newton, preferably less than 12 Newton and most preferably less than 8 Newton. This in particular ensures that the elastic force remaining in the film after shaping is high enough to immobilize the powders within the bag but not high enough that the film cannot be adhered to a mold of reasonable depth by empty.

As is apparent from the definition herein, stretchable material is defined by a degree of stretch that has been measured when it is not present in the closed compartment. However, as mentioned above, the material preferably stretches when shaping the compartment. This can, for example, be observed if a grid is printed on the material, e.g. g., the film, before stretching, and then a compartment is formed with the component of this mesh material. It can be seen that the squares on the grid are elongated and therefore stretched.

The elasticity of the stretchable material in the compartment, and preferably the bag as a whole, can be defined as "springback". This can be determined by stretching the material, for example to a 200% elongation, as described above, and measuring the length of the material after the stretching force ceases. For example, a piece of film with a length of 10 cm, a width of 1 cm, and a thickness of 40 micrometers is stretched lengthwise to 20 cm (200% elongation) with a force of 2.8 Newtons (as in the previous case) and then the force ceases. The film recovers a length of 12 cm, which means an elastic recovery of 80%.

The elasticity of the bag material mentioned herein is the elasticity at the time the bag is manufactured. Prolonged stretching as, for example, typically occurs during bag storage will reduce the elasticity of the bag material due to deformation of the plastic. It is preferred that at the time of manufacturing the bag or the compartment thereof, the material of the compartment has

ES 2 248 294 T3 elasticity such that the elastic recovery is 20% to 100%, more preferably 50% or 60% or more preferably 75% or even 80% to 100%.

Thus, the material of the compartment and preferably the bag as a whole is stretched during shaping and / or closing of the compartment or the bag so that the resulting bag composition has a compartment or a bag that is at least partially stretched. . Typically and preferably, the degree of stretch is not uniform over the compartment or bag due to the shaping and closing process. For example, when a film is placed in a mold and an open compartment is formed by vacuum forming (and then filled with the components and closed), the part of the film at the base of the mold, the farthest from the closure points, it will stretch more than the top. Preferably, the elastic material that is furthest from the opening, e.g. For example, the material at the base of the mold will stretch more and be thinner than the material closer to the opening, eg. eg, at the top of the mold. Therefore, it may be preferred that the component that is to be released into the water first is comprised in a lower layer of the compartment and a component that is to be released into the water in a later stage is comprised in a later layer, closer to the part. compartment top. Alternatively, or additionally, it may be preferred that the less moisture-sensitive component is comprised in the lower layer of the compartment and a more moisture-sensitive component is comprised in a rear or upper layer.

As mentioned above, another advantage of the use of stretchable and preferably also elastic material is that the stretching action, when the compartment is shaped and / or when the compartment is closed, stretches the material of the compartment in a non-uniform way, obtaining a compartment and a bag with a non-uniform thickness. This allows to control the dissolution of the water-soluble bags of the present invention and, for example, the sequential release to water of the components of the composition in the bag.

Preferably, the material is stretched so that the variation in thickness in the compartment or bag formed with the stretched material is from 10% to 1000%, preferably from 20% to 600%, or even from 40% to 500% or even from 60% to 400%. This can be measured by any method such as using an appropriate micrometer. Material of the bag and compartment

Preferably, the composition is a composition that must be released into the water so that the bag and the compartment (s) thereof are designed so that at least one or more of the components is released at the time of delivery. addition to water or very shortly thereafter. Thus, it is preferred that the compartment and preferably the bag as a whole comprise a material that is water dispersible or more preferably water soluble.

It is especially preferred that at least one component is released into the water within 3 minutes, preferably even within 2 minutes or even within 1 minute, after contacting the bag composition with the water.

The preferred water dispersible material in the present invention has a dispersibility of at least 50%, preferably at least 75% or even at least 95%, as measured by the method described below using a glass filter with a maximum size of 50 micron pore.

More preferably, the material is water soluble and has a solubility of at least 50%, preferably at least 75% or even at least 95%, measured by the method described below using a glass filter with a pore size of 20 micrometers maximum.

Gravimetric method to determine the water solubility or water dispensability of the material in the compartment and / or bag:

10 grams ± 0.1 gram of material are added to a 400 ml beaker, the weight of which has been determined, and 245 ml ± 1 ml of distilled water are added. Stir vigorously on a magnetic stirrer set at 62.8 rad / s (600 rpm) for 30 minutes. The mixture is then filtered through a pleated qualitative sintered glass filter with the pore sizes defined above (max. 20 or 50 microns). The collected filtrate water is evaporated by any conventional method and the weight of the remaining polymer (which is the dissolved or dispersed fraction) is determined. The% solubility or dispensability can then be calculated.

Preferred materials are polymeric materials, preferably polymers that are formed into a film or sheet. The material in the form of a film can, for example, be obtained by casting, blow molding, extrusion or blow extrusion of the polymeric material, as is known in the art.

Preferred polymers, copolymers or derivatives thereof are selected from polyvinyl alcohol, polyvinylpyrrolidone, polyalkylene oxide, (modified) cellulose ethers, esters or amides, polycarboxylic acids and salts including polyacrylates, maleic acid copolymers / acrylic, polyamino acids or peptides, polyamides including polyacrylamide, polysaccharides including starch and gelatin, and natural gums such as xanthan gum and carrageenan gum. Preferably, the polymer is selected from polyacrylates and acrylate copolymers, including polymethacrylates, methyl cellulose, sodium carboxymethyl cellulose, dextrin, maltodextrin, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, most preferably polyvinyl alcohol / copolymers or hydroxypropyl methyl cellulose (HPMC).

ES 2 248 294 T3

The polymer can have any weight average molecular weight, preferably from about 1,000 to 1,000,000, or even 10,000 to 300,000, or even 15,000 to 200,000, or even 20,000 to 150,000.

Polymer blends can also be used. This can be especially beneficial in controlling the mechanical and / or dissolution properties of the compartment or bag depending on your application and needs. For example, it may be preferred that a mixture of polymers is present in the material of the compartment, whereby a polymeric material has a higher solubility in water than another polymeric material and / or a polymeric material has a higher mechanical strength than another polymeric material. The use of a mixture of polymers, with different weight average molecular weights, for example a mixture of PVA (or a copolymer thereof) and / or HPMC with a weight average molecular weight of 10,000 to 40,000, preferably around of 20,000, and of PVA (or copolymer thereof) and / or HPMC with a weight average molecular weight of about 100,000 to 300,000, preferably about 150,000.

Also useful are polymer blend compositions, for example those comprising a blend of hydrolytically degradable and water soluble polymers such as polylactide and polyvinyl alcohol that is made by mixing polylactide and polyvinyl alcohol, and typically comprising from 1% to 35% by weight of polylactide and about 65 to 99 by weight of polyvinyl alcohol, if the material is to be water-dispersible or water-soluble.

It may be preferred that the polymer present in the compartment material is 60% to 98% hydrolyzed, preferably 80% to 90%, to improve dissolution of the material.

Most preferred are materials that are water soluble, stretchable and elastic comprising PVA polymers having properties such as PVA films sold under the name M8630, by Chris-Craft Industrial Products of Gary, Indiana, USA.

Preferably, the level of a type polymer (eg commercial blend) in the film material, eg PVA polymer, is at least 60% by weight of the material or film, preferably at least 60% or even of at least 70% or even of at least 80 or 90%. The upper level is up to 100%, but is typically 99% or even 98% by weight.

The material of the present invention may comprise other additive ingredients in addition to the polymer or polymeric material. For example, it may be beneficial to add plasticizers, eg, glycerol, ethylene glycol, diethylene glycol, propylene glycol, sorbitol, and mixtures thereof, additional water, or disintegration aids. When the composition of the bag is a detergent composition, it may be useful if the material of the bag or compartment itself comprises a detergent additive to be supplied to the wash water, for example, polymeric organic agents to release soil, dispersants or inhibitors. dye transfer.

The material in the form of a film can be coated, preferably only on one side, by any coating method and with any coating agent, depending on the required properties; for example, it may be beneficial to coat the film so that the compartment or bag or composition therein is more stable during storage and / or less sensitive to moisture and / or acts as a better barrier against moisture.

A very useful way is to coat the material or film on one side with a coating that slows the dissolution of the film, before shaping the compartment and, therefore, before stretching the material or film. Then, by stretching the material or the film, the coating also stretches, resulting in cracks in the coating and / or an uneven distribution of the coating on the material and therefore on the compartment. This still guarantees stability against moisture during storage and the presence of cracks or uneven distribution still guarantees the necessary dissolution during use. Thus, it is possible to prepare a bag composition that is resistant to handling with wet fingers when gripped by the sides but continues to release product rapidly when immersed in water due to breakage of the film at the thinnest points.

Any coating material can be used, hydrophobic coatings or polymers with low water solubility, less than defined hereinbefore, being particularly useful.

The material of the compartment may be a shrinkable material, so that the surface area can be reduced during or after closing the open compartment by contraction of the material.

Preferably, the open compartment is closed with a piece of the same material as the material of the open compartment. The closure material, and preferably also the material of the open compartment or the shaping material, is preferably thermoplastic so that it can be closed by heat sealing. A thermoplastic coating can also be placed over the entire material or only in the areas where the sealed joints are to be made. The sealed joint can also be made by solvent welding or wetting sealing. Suitable heat sealable materials include polyvinyl alcohol, polyvinyl acetate, polyvinylpyrrolidone, polyethylene oxide, acrylic resins, and mixtures thereof, in particular polyvinyl alcohol.

ES 2 248 294 T3

Examples

Example 1

A piece of Chris-Craft M-8630 film, 38 microns thick, is placed on a mold and set. The mold consists of a cylindrical shape with a diameter of 45mm and a depth of 25mm. A 1mm thick film layer is present around the edge of the mold. The mold has some holes in its material to allow the application of a vacuum.

Vacuum is applied to stretch the film inside the mold and adhere the film to the inside surface of the mold. 20 g of a powdered detergent mixture comprising percarbonate salt and water soluble salts and organic acids, typically carbonate, citric acid and / or citrate salts, are poured into the mold. This powder mixture has a bulk density of 860 g / l before being poured into the mold. 20 g of a powdered detergent mixture comprising enzymes, bleach activator and surfactants are then poured into the mold. This powder mixture has a bulk density of 900 g / l before being poured into the mold.

The mold is filled 95% to 105%.

Then, a sheet of the same M-8630 film is placed on top of the mold with the powder and sealed to the first layer of film by applying an annular piece of flat metal with an internal diameter of 46 mm and this metal is heated moderate pressure on the rubber ring at the edge of the mold to heat seal the two pieces of film. The metal ring is typically heated to 140-146 ° C and applied for up to 5 seconds. The film is stretched during this process.

Next, the bulk density of the bag composition was measured by the method described above, resulting in 1020 g / l.

The bags manufactured by the previous method when immersed in 5 liters of water at 10 ° C released product within 10 seconds.

Example 2

A bilayer bag composition containing a detergent composition is prepared as follows:

A 38 micron piece of film is placed on a mold of the dimensions shown below and fixed so that the film is flush with the top of the mold.

Circular diameter of mold base: 28mm; circular diameter of the upper part of the mold: 37 mm; mold depth 18 mm.

Vacuum is applied to the film so that it is sucked into the mold and sticks to the sides of the mold. 11.75 grams of the next component (A) was poured into the mold film.

Component A

Enzymes 2.5%

Surfactant agglomerates 41.6%

Effervescent particle 6.9%

Defoamer particle 7.2%

Sodium carbonate 28.8%

Bleach activators 13.0%

This component has a bulk density of 725 g / l.

Then 2.5 grams of sodium percarbonate are added to component A. The sodium percarbonate has a bulk density of 1005 g / l. A second layer of 38 micron M-8630 film is then placed over the powder and mold and sealed with the first layer of film using a heat seal procedure similar to that described in Example 1.

The average bulk density of the bag composition before incorporation into the bag is therefore 774 g / l. After incorporation into the bag, the bulk density of the measured composition was 951 g / l, which represents an increase of 23%.

ES 2 248 294 T3

Example 3

A bilayer bag composition is prepared containing enzymes and sodium percarbonate.

The procedure described in Example 1 is used to prepare a bilayer bag composition consisting of 36 grams of sodium percarbonate and 4 grams of Termamyl 120 (supplied by Novo Industries). Sodium percarbonate forms the bottom layer and enzyme the top layer.

The composition of the monolayer bag is then prepared according to the procedure described in Example 1 by mixing the enzymes and the percarbonate in a homogeneous way.

Both bag compositions exhibit an 18% increase in density. In both cases the film on the bag is stretched.

Both types of bag compositions are then stored under elevated temperature and humidity conditions (32.2 ° C, ie 90 ° F, 80% relative humidity) without any external wrapping or packaging protection. The samples were taken after 48 hours and 96 hours of storage and the activities of the enzymes in both products were compared with each other. The enzyme activity in the monolayer bag after 48 hours is only about 30% of the enzyme activity in the bilayer bag composition; the enzyme activity in the monolayer bag after 96 hours is only about 20% of the enzyme activity in the bilayer bag composition.

This demonstrates the greatest stability during storage when fixed regions or layers are used to separate incompatible materials.

The following are detergent compositions that can also be suitably incorporated into a bag of the invention:

<td></td><td>TO</td><td>B</td><td>C</td><td>D</td><td>AND</td><td>F</td><td>G</td><td>H</td><td>I</td>

<td>First Top Coat: Spray Dried Granules</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>THE</td><td> 10,0</td><td> 10,0</td><td> 15,0</td><td> 5,0</td><td> 5,0</td><td> 10,0</td><td> -</td><td> -</td><td> -</td>

<td>TAS</td><td> -</td><td> 1,0</td><td> -</td><td></td><td></td><td></td><td> -</td><td> -</td><td> -</td>

<td>Branched or linear synthetic alkyl sulfate surfactant</td><td> -</td><td> -</td><td> 2,0</td><td> 5,0</td><td> 5,0</td><td></td><td> -</td><td> -</td><td> -</td>

<td>Cationic surfactant</td><td></td><td></td><td> 1,0</td><td> 1,0</td><td></td><td></td><td> -</td><td> -</td><td> -</td>

<td>DTPA, HEDP and / or EDDS</td><td> 0,3</td><td> 0,3</td><td> 0,5</td><td> 0,3</td><td></td><td></td><td> -</td><td> -</td><td> -</td>

<td>MgSO₄</td><td> 0,5</td><td> 0,5</td><td> 0,1</td><td> -</td><td></td><td></td><td> -</td><td> -</td><td> -</td>

<td>Sodium citrate</td><td> -</td><td> -</td><td> -</td><td> 3,0</td><td> 5,0</td><td> -</td><td> -</td><td> -</td><td></td>

<td>Sodium carbonate</td><td> 10,0</td><td> 7,0</td><td> 15,0</td><td></td><td></td><td> 10,0</td><td> -</td><td> -</td><td> -</td>

<td>Sodium sulfate</td><td> 5,0</td><td> 5,0</td><td> -</td><td> -</td><td> 5,0</td><td> 3,0</td><td> -</td><td> -</td><td> -</td>

<td>Sodium silicate 1,6R</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 2,0</td><td> -</td><td> -</td><td> -</td><td></td>

<td>Zeolite A</td><td> 16,0</td><td> 18,0</td><td> 20,0</td><td> 20,0</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td>

<td>SKS-6</td><td> -</td><td> -</td><td> -</td><td> 3,0</td><td> 5,0</td><td> -</td><td> -</td><td> -</td><td> -</td>

<td>Polyacrylic and / or polymaleic acid polymer, or salt</td><td> 1,0</td><td> 2,0</td><td> 11,0</td><td> -</td><td> -</td><td> 2,0</td><td> -</td><td> -</td><td> -</td>

<td>PEG 4000</td><td> -</td><td> 2,0</td><td> -</td><td> 1,0</td><td> -</td><td> 1,0</td><td> -</td><td> -</td><td> -</td>

<td>Rinse aid</td><td> 0,05</td><td> 0,05</td><td> 0,05</td><td> -</td><td> 0,05</td><td> -</td><td> -</td><td> -</td><td> -</td>

<td>Silicone oil</td><td> 0,01</td><td> 0,01</td><td> 0,01</td><td> -</td><td> -</td><td> 0,01</td><td> -</td><td> -</td><td> -</td>

ES 2 248 294 T3 (Continued)

<td></td><td>TO</td><td>B</td><td>C</td><td>D</td><td>AND</td><td>F</td><td>G</td><td>H</td><td>I</td>

<td>Effervescent granule with 50% citric acid and 50% sodium carbonate</td><td> 10</td><td> 7,0</td><td>^-</td><td>^-</td><td>^-</td><td>^-</td><td>^-</td><td>^-</td><td>^-</td>

<td>Middle layer: Chipboard</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>THE</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> -</td><td> 2,0</td><td> 2,0</td><td> -</td>

<td>Branched or linear synthetic alkyl sulfate surfactant</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 4,0</td><td> 4.0</td>

<td>Ethoxylated alkyl sulfate surfactant</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 1,0</td><td> 0,5</td>

<td>Carbonate</td><td></td><td></td><td> -</td><td> -</td><td> 4,0</td><td> 1,0</td><td> 1,0</td><td> 1,0</td><td> -</td>

<td>Sodium citrate</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 5,0</td>

<td>Citric acid</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> 4,0</td><td> -</td><td> 1,0</td><td> 1,0</td>

<td>SRP</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> 1,0</td><td> 1,0</td><td> 0,2</td><td> -</td>

<td>Zeolite A</td><td></td><td></td><td> -</td><td> -</td><td> -</td><td> 15,0</td><td> 26,0</td><td> 15,0</td><td> 16,0</td>

<td>PEG</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 4,0</td><td> -</td><td> -</td>

<td>Chipboard SKS-6 / LAS</td><td> 6,0</td><td> 10,0</td><td> -</td><td> -</td><td> 9,0</td><td> 6,0</td><td> -</td><td> 7,0</td><td> 10,0</td>

<td>Non-ionic surfactant</td><td> -</td><td> 2,0</td><td> 1,0</td><td> -</td><td> 5,0</td><td> 0,5</td><td> -</td><td> 0,7</td><td> -</td>

<td>Enzymes (cellulase, amylase, protease, lipase)</td><td> 1,3</td><td> 0,3</td><td> 0,5</td><td> 0,5</td><td> 0,8</td><td> 2,0</td><td> 0,5</td><td> 0,16</td><td> 0,2</td>

<td>Fragrance</td><td> 1,0</td><td> 0,5</td><td> 1,1</td><td> 0,8</td><td> 0,3</td><td> 0,5</td><td> 0,3</td><td> 0,5</td><td> -</td>

<td>Citrate / citric acid</td><td> -</td><td> -</td><td> 20,0</td><td> 4,0</td><td> -</td><td> 5,0</td><td> 15,0</td><td> -</td><td> 5,0</td>

<td>Photobleaching</td><td> 0,02</td><td> 0,02</td><td> 0,02</td><td> 0,1</td><td> 0,05</td><td> -</td><td> 0,3</td><td> -</td><td> 0,03</td>

<td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>Bottom layer: Particulate components for dry addition</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>

<td>Effervescent granule (as above)</td><td> -</td><td> 4,0</td><td> 10,0</td><td> 4,0</td><td> 25</td><td> 8,0</td><td> 12,0</td><td> 2,0</td><td> 4,0</td>

<td>TAED</td><td> 2,5</td><td> -</td><td> -</td><td> 1,5</td><td> 2,5</td><td> 6,5</td><td> -</td><td> 1,5</td><td> -</td>

<td>MBAS</td><td> -</td><td> -</td><td> -</td><td> 8,0</td><td> -</td><td> -</td><td> 8,0</td><td> -</td><td> 4,0</td>

<td>LAS (flakes)</td><td> 10,0</td><td> 10,0</td><td> -</td><td> -</td><td> -</td><td> -</td><td> -</td><td> 8,0</td><td> -</td>

<td>Sodium percarbonate</td><td> 15,0</td><td> -</td><td> -</td><td> 10,0</td><td> 15,0</td><td> 5,0</td><td> -</td><td> 11,0</td><td> -</td>

<td>Speck</td><td> -</td><td> -</td><td> -</td><td> 0,3</td><td> 0,05</td><td> 0,1</td><td> -</td><td> -</td><td> -</td>

<td>Suds suppressor</td><td> 1,0</td><td> 0,6</td><td> 0,3</td><td> -</td><td> 0,10</td><td> 0,5</td><td> 1,0</td><td> 0,3</td><td> 1,2</td>

<td>Soap</td><td> 0,5</td><td> 0,2</td><td> 0,3</td><td> 3,0</td><td> 0,5</td><td> -</td><td> -</td><td> 0,3</td><td> -</td>

<td>Loads up to 100%</td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td><td></td>