CN1408004A - Water unstable foam - Google Patents

Abstract

An elastic article is provided which comprises a foam matrix formed from a polymeric material and a plasticiser, a stabilising agent and an active ingredient, such as a detergent active ingredient, typically to be delivered to an aqueous environment. Said elastic article provides a means to deliver an active ingredient to an aqueous environment, preferably the active ingredients being a detergent active ingredient, preferably enzymes, and the aqueous environment being the wash water.

Description

water unstable foam

field of invention

The present invention relates to foam components, generally particulate, comprising a matrix formed of a polymeric material and plasticizer, dissolving agents and active ingredients, such as detergent active ingredients, for release of the component generally into an aqueous environment.

Background of the invention

Compositions such as cleaning and personal care products, cosmetics and pharmaceuticals often include active ingredients that are to be released into water, or are required to be active in an aqueous environment. Most of these active ingredients are sensitive to humidity, temperature changes, light and/or air during storage.

Another problem with most of these active ingredients, especially enzymes, is that they tend to form dust during handling due to the physical forces acting directly on these active ingredients. Not only is waste material generated as a result, but the dust can also cause hygiene and health problems.

In order to solve these problems, studies have been conducted to protect active components with coating agents or sealants. The problem with most such coated particles is that during operation, these particles do not always exhibit sufficient impact resistance, and under the normal physical forces encountered during operation, these particle formation can produce Dust for hygiene and health concerns. Furthermore, these coated particles are not always readily soluble in aqueous environments, exhibiting poor solubility properties when in contact with water.

The inventors have discovered an improved method of protecting active ingredients and releasing these active ingredients into an aqueous environment. They have found that a particular foam component comprising a matrix formed of a polymeric material and a plasticizer is very resistant to impact forces and the active ingredients incorporated therein are protected from physical forces acting on said foam component . In addition, the inventors have discovered that when a dissolution aid is also incorporated into the foam component, the foam component readily dissolves or disintegrates upon contact with water, thereby releasing the active ingredient into the aqueous environment.

Therefore, the foam component of the present invention has good impact resistance, reduces breakage or abrasion during handling, reduces dust formation, and is easily dissolved when in contact with water. For example, enzyme-containing foam components, such as granules or beads, can be obtained that are safer and more efficient to handle and use. Furthermore, the components can be prepared such that they effectively release the active ingredients incorporated therein, such as enzymes, into the aqueous environment. The components of the present invention are stable to air under normal humidity storage conditions, but are unstable when in contact with water, thereby releasing the active ingredient. The foam component can be used in any product, especially in cleaning products, pharmaceuticals, personal care products, cosmetics and fabric care products.

Summary of the invention

The present invention provides a foam component comprising a polymeric material, a dissolution aid and a mixture of active ingredients, preferably active in an aqueous environment, which foam component is stable in contact with air and stable in contact with water unstable.

The dissolution aid improves the water solubility or water disintegration properties of the foam component.

Preferably, the dissolution aid for the foam component comprises a foaming system, a hydrotrope or a combination of both.

The invention also relates to a method of preparing the foam component.

The foam component is preferably obtained by a method comprising the steps of;

a) obtaining a polymer material;

b) chemically or physically introducing a gas into said polymer material;

c) contacting said polymeric material with an active ingredient prior to step b) and/or simultaneously with step b) and/or after step b);

d) prior to step b) and/or simultaneously with step b) and/or after step b), contacting said polymeric material with a dissolution aid; and

e) shaping the resulting polymeric material component;

If water is present, it is preferred to remove part of the water after or simultaneously with one or more steps a) to e).

In another embodiment of the present invention there is provided the use of foam components to deliver active ingredients, preferably detergent active ingredients, preferably enzymes, into an aqueous environment and the aqueous environment is preferably wash water.

Detailed description of the invention

foam component

The foam components of the present invention, also referred to herein as "components", comprise an active ingredient, a base and a dissolution aid. The active ingredient, base and dissolution aid will be described in detail below.

The components of the invention are preferably water-dispersible, water-decomposable or water-soluble. Preferred water-dispersible components of the present invention have a dispersibility of at least 50%, preferably at least 75%, or even at least 95%, as measured with a glass filter having a maximum pore size of 50 microns, as will be hereinafter described To illustrate; more preferred components of the present invention are water-soluble or water-decomposable, and have at least 50%, preferably at least 75%, or even at least 95% water-solubility or disintegratability, with a maximum pore size of 20 microns Glass filter measured, the method will be explained below, namely:

Determination of component water solubility in the present invention, the gravimetric analysis method of water decomposability or water dispersibility:

Add 50 grams ± 0.1 grams of components of the present invention into a 400 ml beaker whose weight has been determined, and add 245 ml ± 1 ml of distilled water. Stir vigorously with a magnetic stirrer set at 600 rpm for 30 minutes. The component mixture is then filtered through a folded qualitative sintered glass filter of pore size as defined above (up to 20 or 50 microns). The water in the collected filtrate is dried in a conventional manner, and the weight of the remaining components (which are dissolved, decomposed or dispersed parts) is measured. The percentage dissolved, disintegrated or dispersed can then be calculated.

The components of the present invention are generally used to deliver active substances into an aqueous environment. The components of the present invention, preferably their matrix, are therefore unstable when in contact with water. When this occurs, the active ingredient(s) or part of the active ingredient(s) present in the composition are released into a liquid, preferably an aqueous environment such as water. Preferably the ingredient or part of the ingredient is denatured, decomposed, preferably dispersed or dissolved in a liquid, preferably in an aqueous environment, more preferably in water. Rapid release of the active ingredient into water may be preferred whereby the ingredient disperses or dissolves quickly; preferably the ingredient is at least 10% by weight of the ingredient within 30 minutes after contact with water, or more preferably at least 30% or even at least 50%, or even at least 70%, or even at least 90% dissolved or dispersed (introduced into water at a concentration of 1% by weight). It may even be preferred that this occurs within 20 minutes, or even within 10 minutes, or even within 5 minutes of contacting the component with water. Solubility or dispersibility can be measured by the method described above to determine the dissolution, decomposition or dispersibility of the ingredients in the present invention.

A preferred component is a change in the total volume of the components compared to the initial total volume, preferably a reduction of at least 10%, for example at a temperature of 25° C., when ^{1 cm} of the above components are added to 100 ml of demineralized water while at 200 rpm As measured while stirring at 5 min at high speed. It is preferred that such a change in total volume, or reduction, be at least 20%, or even at least 40%, or even at least 60%, or even at least 90%, or even about 100%, for example because it may be preferable for substantially all components to be quickly Decomposes, disperses or preferably dissolves in water.

This can be measured by any method known in the art, in particular by the following method of the present invention (secondary immersion method):

The resulting 1 cm ^fraction was introduced into a 100 ml microvolume test cylinder filled with 50 ml ± 0.1 ml of organic inert solvent. Where acetone does not denature and/or does not react with the polymeric material of the component matrix of the invention, for example when the polymeric material is PVA, for example acetone may be used. It has been found that other neutral organic media can be used depending on the properties of the substance; the inert solvent can make the component basically not dissolved, dispersed, decomposed or denatured by the solvent.

The cylinder is airtight and is left to stand for 1 minute, whereby the solvent penetrates the entire composition. The change in volume is measured and recorded as the original volume V _i of the foam sample. The components are then removed from the solvent and left to dry in air to evaporate the solvent.

The components were then placed in a 250ml beaker filled with 100ml of demineralized water, kept at 25°C, and stirred for 5 minutes at a speed of 200rpm with the help of a magnetic stirrer. If there is residue, use a 60mm mesh copper filter to filter out the component sample residue, and place it in an oven at a certain temperature for a period of time, thereby removing residual moisture. The dried residual components were reintroduced into the measuring cylinder in which the volume of acetone had been adjusted to 50 ml.

The increase in total volume is detected and recorded as the final volume V _f of the fraction. Then the reduction ΔV of the total volume of the component sample is: $\%\mathrm{\ΔV}=\frac{V}{\mathrm{Vi}}*100$

The component preferably has a relative density p ^* of 0.01 to 0.95, more preferably 0.05 to 0.9, or even 0.1 to 0.8, or even 0.3 to 0.7. The relative density is the ratio of the density (ρ ^* ) of the component to the sum (ρ _s ) of the densities of all parts of bulk material used to form the component.

The foam components preferred for use in the present invention are air stable or stable in contact with air, which means that the bulk volume of the component or its matrix remains substantially unchanged when exposed to air. Specifically this means that the components are stored for 24 hours in an open beaker (9 cm diameter, without any protective baffles) in an incubator under controlled environmental conditions (humidity = RH60%, temperature = 25°C) , the component preferably retains 75% to 125%, even 90% to 110%, or even 95% to 100% of its bulk volume. Preferably the component retains preferably 75% to 125%, even 90% to 110%, or even 95% to 100% of its bulk volume at a humidity of 80% and under the above storage conditions.

The change in bulk volume can be measured by any conventional method. Particularly useful is a digital image recording system with a digital camera connected to a personal computer itself equipped with calibrated image analysis software. The resulting ¹ cm sample of the components was introduced into an open beaker with a diameter of 9 cm and stored under the above conditions for 24 hours. After 24 hours, all three-dimensional dimensions were measured with an image analysis recording system. The measurement for each sample was repeated three times, and the change in the average bulk volume expressed in % was calculated.

Preferred components are such that when in the form of particles having an average particle size of 2000 microns or less, these particles still retain 75% to 125% of their bulk volume, even 90% to 110%, or even 95% to 100%. This can be measured, for example, by placing 20 g of such granules, or granules comprising more than 500 granule weights, into a volumetric beaker with a diameter of 9 cm. The bottom of the beaker was tapped slightly until the particles redistributed themselves in a stable position with a level upper surface. Measure the volume. The open beaker with these pellets was then carefully placed in an incubator and kept at the desired %RH and temperature set for 24 hours. After 24 hours, the bulk volume was measured and the change in bulk volume expressed in % was calculated.

The component preferably comprises (expressed by weight) at least 1%, more preferably from 5% to 70%, more preferably at least 10%, more preferably from 15% or even 20% or even 25% to 50% by weight of the component One (or more) active ingredients.

This component preferably comprises (expressed by weight) 10% to 99%, more preferably at least 20% or even 30% to 99%, more preferably from 20% or 30% to 90% to 80% matrix.

The component comprises (expressed by weight) at least 1%, more preferably from 5% or from 10%, or from 15%, or from 20% to 50%, or to 40%, or to 30%, or to 25% dissolution aids.

matrix

The matrix of the components of the present invention, referred to herein as the "matrix", is formed from a polymeric material and a plasticizer. The polymeric material and the plasticizer will be described in more detail below.

The ratio of plasticizer and polymer material in the matrix is preferably 1 to 100, more preferably 1 to 70 or 1 to 50, more preferably 1 to 30 or even 1 to 20, depending on the ratio of plasticizer and polymer material used. type. For example when the polymeric material comprises PVA and the plasticizer comprises glycerol or a glycerol derivative and optionally water, the ratio is preferably in the vicinity of 1:15 to 1:8, with a preferred ratio of about 10:1.

The matrix of the invention may further comprise active ingredients of the components of the invention and/or dissolution aids of the components of the invention. The active ingredient and the dissolution aid will be described in detail below. Crosslinking agents may also be added to suitably modify the properties of the matrix or final component. Borates may be useful for the substrates of the invention.

The matrix of the invention preferably has a glass transition temperature (Tg) below 50°C, preferably below 40°C, preferably below 20°C or even below 10°C or even below 0°C. Preferably the Tg of the matrix of the invention is above -20°C or even -10°C.

When matrix Tg is used herein, it refers to the Tg of the matrix present in the component, so the matrix may be a mixture of polymeric material and plasticizer alone, or polymeric material, plasticizer, active ingredient and/or dissolution aids, and in any case additional components (eg stabilizers, thickening aids, fillers, lubricants, etc. as described below) may optionally be present.

The Tg used in the present invention is as defined in the textbook "Dynamic Mechanical Analysis" (page 53, page 57 Figure 3.11c), which is when the material (matrix) changes from the glass state to the rubber state, that is, the segments obtain sufficient mobility with each other The temperature at which the flow takes place.

The Tg of the matrix of the composition of the invention can be measured with a Perkin-Elmer DMA 7e apparatus, following the instructions in the operating manual for the apparatus, to produce a curve as described in Figures 3-11 on page 57 of the book Dynamic Mechanical Analysis. The Tg measured with this device is the logarithm of temperature or frequency between the glass and the "leathery region", as defined in that text.

The matrix, and preferably the components as a whole, have particular elasticity and flexibility due to their particular glass transition temperature. Specifically, this means that the matrix and components can reversibly deform, absorbing the energy of an impact or force such that the component or matrix retains substantially its original shape after a physical force has been attacked and applied to said components bulk volume.

Elasticity can be defined by the modulus of elasticity of the matrix, or even of the components, while the modulus of elasticity can be defined by Young's modulus. The modulus can be calculated using mechanical tests of tension or stress known in the art, for example with a Perkin-Elmer DMA 7e apparatus, following the manufacturer's protocol at a specific % static tension range, i.e. 10-40% static tension Take measurements. This represents the maximum tension that can be applied during normal production or operation. Therefore, the modulus of elasticity defined in the present invention is the maximum modulus measured with the device in the static tension range of 10-40%. For example, a 1 cm ³ -sized matrix (or component) can be used when testing with the device.

The substrates of the present invention typically have less than 4GN·m ^-2 , or typically less than 2GN·m ^-2 , even more preferably less than 1GN·m ^-2 , when measured with a Perkin-Elmer DMA 7e apparatus, but typically A modulus of elasticity or Young's modulus of even less than 0.5GN·m ^-2 , or even less than 0.1GN·m ^-2 , or even less than 0.01GN·m ^-2 . Especially when the matrix of the present invention contains bubbles formed, for example, by introducing a gas into the matrix, its modulus of elasticity is lower than 0.1GN·m ^-2 , or even 0.01GN·m ^-2 , or even lower than 0.005GN ·m ^-2 , or even lower than 0.0001GN·m ^-2 .

Preferably the matrix is flexible, having a relative yield strain of greater than 2%, preferably greater than 15% or even greater than 50% when measured with a Perkin-Elmer DMA 7e apparatus. (The yield strain in this test is the ultimate deformation at which a piece of substrate is subjected to irreversible deformation).

Specifically, this means that a matrix sample having a section of a certain length, say 1 cm, is compressed by a static force (which is variable but equal to at least two times the atmospheric pressure) applied along the axis of the section. times), after removal of the force, the length changes to at least 90% to 110% of the original length. Measurements can be made with, for example, a Perkin-Elmer DMA 7e device.

Similarly, the matrix preferably has a degree of flexibility that is variable when elongating a matrix sample of a section of a specified length (eg, 1 cm) by applying a static force along the axis of the section , but at least equal to twice the atmospheric pressure, the length changes to at least 90% to 110% of its original length after removal of the force. Measurements can be made with, for example, a Perkin-Elmer DMA 7e device.

Especially when using this device, the static force applied along the axis of the ¹ cm matrix sample section is gradually increased until the deformation of the component along the above section direction is 70%. Then, the force is removed and the resulting deformation of the matrix sample along the cross-sectional direction is measured. It is preferred that after the test the section length is preferably from 90% to 110%, preferably from 95% to 105%, or even 98% to 100% of the original section length.

The modulus of elasticity or Young's modulus is related to the relative density, i.e. $\frac{{\mathrm{E.}}^{*}}{{\mathrm{E.}}_{\mathrm{the\; s}}}\≈{\left(\frac{{\mathrm{\ρ}}^{*}}{{\mathrm{\ρ}}_{\mathrm{the\; s}}}\right)}^2,$

where ρ ^* is the relative density of the matrix or even the components, _ρs is the relative density of the matrix components or components as described in the present invention, E ^* is the Young's modulus of the matrix or even the components themselves, Es is the matrix group component or even component Young's modulus. This means that by adjusting the amount and/or type of plasticizer, and optionally changing the density (or, as described below, for example, by introducing air during the making of the foam component), it is possible to make even hard plastics with high The polymer material of ES becomes elastic and flexible matrix.

The matrix, or even the entire component, is in the form of a foam, which preferably forms a network of open and/or closed cells, especially a network of solid supports or plates forming the edges or faces of the open and/or closed cells . The space within the cell may contain part of the active ingredient and/or gas, such as air.

Preferably the ratio of closed cells to open cells in the component matrix, or the component ensemble, is greater than 1:1, preferably greater than 3:2, even greater than 2:1 or even greater than 3:1. The closed cell volume (V 0 ) can be obtained by calculating the total volume V _T of a matrix or component sample (assuming a spherical shape), then measuring the open cell volume (V ₀ ) using the Mercury Porosimetry Test method, and subtracting this open cell volume from the total volume. _C : V _T =V ₀ +V _C ), thereby determining the ratio.

polymer material

Any polymeric material may be used to form the matrix of the present invention, preferably the polymeric material itself has a Tg as described above, or more typically, the polymeric material may be formed into a matrix having a Tg as described above with a suitable amount of plasticizer.

Preferably the polymeric material comprises or consists of one (or more) amorphous polymers.

The polymeric material may consist of a single type of homopolymer, or be a mixture of polymers. Blends of various polymers are especially advantageous for controlling the mechanical and/or solubility properties of the components, depending on the application of the component and its requirements.

Preferably the polymeric material comprises a water dispersible or more preferably water soluble polymer. According to the method for determining the water solubility and water dispersibility of the components of the invention, water dispersible or water soluble is typically defined as described above. Preferably, the water-dispersible polymers of the present invention have a dispersibility of at least 50%, preferably at least 75%, or even at least 95%, when measured by the above-mentioned method using a glass filter with a maximum pore size of 50 microns; more Preferably the polymer of the present invention is a water soluble polymer having at least 50%, preferably at least 75%, or even at least 95% of the water soluble.

The polymer may have any average molecular weight, preferably from about 1,000 to 1,000,000, or even from 4,000 to 250,000, or even from 10,000 to 200,000, or even from 20,000 to 75,000. More preferred polymeric materials have a weight average molecular weight of 30,000 to 70,000.

Depending on the desired properties of the components of the invention, the polymeric material can be adjusted. For example, to reduce solubility properties, the polymers included in the material may have a high molecular weight, typically above 50,000 or even 100,000, and vice versa. For example, to vary the solubility properties, polymers with different degrees of hydrolysis can be used. For example to improve (reduce) the modulus of elasticity, the degree of crosslinking of the polymer can be increased and/or the molecular weight can be increased.

Preferably the polymers used in the components of the invention have a secondary function, for example as a function in the composition into which the component will be incorporated. Thus, for example, it is useful for cleaning products when the polymer in the polymeric material is a dye transfer inhibiting polymer, a dispersant, etc.

Preferred polymers are selected from polyvinyl alcohol and derivatives thereof, polyethylene glycol and derivatives thereof, polyvinylpyrrolidone and derivatives thereof, cellulose ethers and derivatives thereof, and these polymers with each other or with other monomers or copolymers of oligomers. Most preferred are PVP (and derivatives thereof) and/or PEG (and derivatives thereof), most preferred are PVA (and derivatives thereof) or a mixture of PVA and PEG and/or PVP (and derivatives thereof). The most preferred polymeric material may also comprise only PVA. Preferably these polymers have a degree of hydrolysis of at least 50%, more preferably at least 70%, or even 85% to 95%.

plasticizer

Any plasticizer suitable to aid in the formation of the matrix of the present invention may be used. Mixtures of plasticizers may also be used.

Preferably the plasticizer, or at least one plasticizer, has a boiling point above 40°C, preferably above 60°C, or even above 95°C, or even above 120°C, or even above 150°C.

Preferred plasticizers include trihydric alcohols or glycerol, diol derivatives including ethylene glycol, ethylene glycol oligomers such as diethylene glycol, triethylene glycol, tetraethylene glycol and weight average molecular weights below 1000 polyethylene glycols, paraffin and hydrocarbon waxes, ethanol acetamide, ethanol formamide, triethanolamine or its acetate and ethanolamine salts, sodium thiocyanate, ammonium thiocyanate, polyols such as 1,3-butanediol , sugars, sugar alcohols, urea, dibutyl or dimethyl phthalate, oxa monobasic acids, oxa dibasic acids, diglycolic acid and others with at least one ether group distributed along their chain segment Linear carboxylic acids, water or mixtures of these substances.

When water is used, an additional plasticizer is preferably present. If water is used, it is typically present in the foam component in an amount of at least 3%, more preferably more than 3%, preferably even at least 5%, or even at least 10% by weight.

The plasticizer is preferably present in an amount of at least 0.5% by weight of the article, preferably of the substrate, and whenever water is the sole plasticizer, it is present in an amount of at least 3% by weight of the component, or preferably of the substrate.

Preferably the plasticizer is present in an amount of 1% to 35% by weight of the article or substrate, more preferably 2% to 25%, or even to 15%, or even to 10% or even to 8% by weight of the article or substrate . The exact amount present depends on the polymeric material and plasticizer used, but is necessary to give the desired Tg to the substrate of the article. For example when urea is used it is preferably present in an amount of 1% to 10% by weight of the matrix and when glycerol or ethylene glycol or other glycol derivatives are used higher amounts are preferred e.g. as components or matrix 2% to 15% by weight.

active ingredient

The active ingredient may be any material that will be released into a liquid environment, or preferably an aqueous environment, and is preferably an ingredient that is active in an aqueous environment. For example, when used in a cleaning composition, the component may contain any active cleaning ingredients. The component may also include compositions such as cleaning compositions or personal care compositions.

It is especially advantageous to incorporate in the composition active ingredients which are sensitive to or react on contact with moisture, or solid ingredients which have limited strength against impact force and tend to form dust during handling.

The active ingredient is generally a moisture sensitive ingredient, a temperature sensitive ingredient, an oxidizable ingredient, a volatile ingredient or a combination of these substances. The active ingredient may be a biologically active material, a hazardous or toxic material, an agricultural ingredient such as an agricultural fertilizer, a medicinal ingredient such as a drug or medicament, or a cleaning ingredient.

Especially preferred active ingredients in this component are, for example, enzymes, fragrances, bleaching agents, bleach accelerators, fabric cationic and/or silicone softeners and/or conditioning agents, antibacterial agents, brighteners, photobleaches and these mixture of substances.

Other active ingredients are perhydrate bleaches, such as metal perborates, metal percarbonates, especially the sodium salts. Other preferred active ingredients are organic peroxyacid bleach precursors or accelerator compounds, preferably alkyl peroxyacid precursor compounds of the imide type, including N-, N, N ¹ N ¹ tetraacetylated imide Alkyl diamines, wherein the alkylene group contains 1 to 6 carbon atoms, specifically these compounds have the alkylene group containing 1, 2 and 6 carbon atoms, such as tetraacetylethylenediamine (TAED), 3, 5 , sodium 5-trimethylhexanoyloxybenzenesulfonate (iso-NOBS), sodium nonanoyloxybenzenesulfonate (NOBS), sodium acetoxybenzenesulfonate (ABS) and pentaacetylglucose, and amides Substituted alkyl peroxyacid precursor compounds.

More preferably the active ingredient used in the compositions of the present invention is one or more enzymes. Preferred enzymes include commercially available lipases, cutinases, amylases, neutral and alkaline proteases, cellulases, endolases, esterases, pectinases commonly incorporated into detergent compositions , lactase and peroxidase. Suitable enzymes are discussed in US3519570 and US3533139. Preferred commercially available proteases include those sold under the trade names Alcalase, Savinase, Primase, Durazym and Esperase by Novo Industries A/S (Denmark), those sold under the trade names Maxatase, Maxacal and Maxapem by Gist-Brocades, Genencor International and those sold under the trade names Opticlean and Optimase by Solvay Enzymes. Preferred amylases include, for example, alpha-amylases obtained from a special strain of Bacillus licheniformis, which are described in more detail in GB-1269839 (Novo). Preferred commercially available amylases include, for example, those sold under the trade name Rapidase by Gist-Brocades, and those sold under the trade name Termamyl, Duramyl and BAN by Novo Industries A/S. More preferred amylases may be those described in PCT/US9703635, WO95/26397 and WO96/23873. The starting material for the lipase may be a fungus or a bacterium such as fat obtained from strains of Humicola, Thermomyces sp. or Pseudomonas including Pseudomonas pseudoalcaligenes or Pseudomonas fluorescens enzyme. Lipases derived from chemically or genetically modified variants of these strains may also be used in the present invention. A preferred lipase is obtained from Pseudomonas pseudoalcaligenes, which is described in granted European patent EP-B-0218272.

Other preferred lipases of the present invention are obtained by cloning the gene of Humicola lanuginosa and expressing it on the gene of Aspergillus oryzae, as described in European patent application EP-A-0258068, available from Novo Industri A/S, Bagsvaerd, Denmark commercially available under the trade name Lipolase. This lipase is also described in US Patent No. 4,810,414, issued March 7, 1989 to Huge-Jensen et al.

Dissolving aid

The compositions of the present invention include a dissolution aid.

The dissolution aid is complementary to the active ingredient of the composition of the invention. If the composition of the invention comprises more than one active ingredient, preferably one of the active ingredients is selected from or acts as a dissolution aid. For the purposes of the present invention, dissolution aids are always additional ingredients to the active ingredients of the components of the present invention.

Therefore, for the purposes of the present invention, for a composition defined by comprising a dissolution aid and an active ingredient, wherein said composition comprises a dual-functional ingredient capable of acting as an active ingredient or active ingredient as defined in the present invention role of dissolution aids, and in addition to this dual-functional ingredient, additional dissolution aids or active ingredients must be present in the articles of the invention in order to obtain the composition of the invention comprising active ingredients and dissolution aids .

The above statements regarding components with dual functionality also hold true when considering other embodiments of the invention. It is essential for the composition of the present invention to contain the active ingredient, the polymeric material and the plasticizer (forming the matrix), and the dissolution aid. In order to obtain the composition of the invention, therefore, at least four different constituents must be present in said composition. Essential ingredients may preferably be selected to have a dual function.

The above statements regarding ingredients having a dual function are also true when considering more preferred embodiments of the invention, eg preferred components comprising additional ingredients such as stabilizing aids.

The dissolution aid may preferably include sulfonated compounds such as C ₁ -C ₄ alkyl (alkenyl) sulfonates, C ₁ -C ₄ aryl sulfonates, diisobutylbenzene sulfonate, toluene sulfonic acid Salt, cumene sulfonate, xylene sulfonate, and salts of these substances such as sodium salt, and derivatives or combinations thereof, preferably diisobutylbenzene sulfonate, sodium toluene sulfonate , sodium cumene sulfonate, sodium xylene sulfonate and combinations of these substances.

The dissolution aid may include C ₁ -C ₄ alcohols, such as methanol, ethanol, propanol, such as isopropanol, and derivatives of these substances, and combinations of these substances, preferably ethanol and/or isopropanol .

The dissolution aid may comprise a C ₄ -C ₁₀ diol, such as hexanediol and/or cyclohexanediol, preferably 1,6-hexanediol and/or 1,4-cyclohexanedimethanol.

The dissolution aid may include compounds that can act as thickeners, such as cellulose-based compounds, especially modified cellulose.

The dissolution aid may contain bulking agents such as clay. Preferred clays are montmorillonite clays, especially dioctahedral or trioctahedral montmorillonite clays. More preferred clays are montmorillonite clays and hectorite clays, or other clays found in bentonite formations.

The dissolution aid preferably comprises a foaming system. Preferred foaming systems include an acid source capable of reacting with an alkali source in the presence of water to generate gas. Gases produced by this reaction include nitrogen, oxygen and carbon dioxide gas. The acid source can be any organic, mineral or inorganic acid, or derivatives or mixtures of these acids. Preferred acid sources include organic acids. Suitable acid sources include citric, malic, maleic, fumaric, aspartic, glutaric, tartaric, succinic or adipic acids, monosodium phosphate, boric acid or derivatives of these. Particularly preferred is citric acid, maleic acid or malic acid.

As previously stated, the foaming system preferably includes a source of alkalinity, but for the purposes of the present invention it is to be understood that the source of alkalinity may be part of the component, or part of the composition comprising the component, or may be present in the In the lotion of the component or a composition comprising the component. Any source of alkalinity that reacts with an acid source to produce a gas can be used in the present invention. Preferred sources of alkalinity are perhydrate bleaches, including perborate and silicate materials.

The preferred gas is carbon dioxide and thus the preferred source of alkalinity is a carbonate source, which may be any type of carbonate known in the art. In preferred embodiments, the carbonate source is a carbonate. Examples of preferred carbonates are alkaline earth and alkali metal carbonates, including sodium or potassium carbonate, bicarbonates and sesquicarbonates, and mixtures of these salts with ultrafine calcium carbonate, as described in 1973 11 Disclosed in German Patent Application 2321001 published on 15th. Alkali metal percarbonates may also be used as a source of suitable carbonates, which may be present in combination with one or more other carbonate sources.

The molar ratio of said acid source and alkali source present in the composition is preferably 50:1 to 1:50, more preferably 20:1 to 1:20, more preferably 10:1 to 1:10, more preferably 5: 1 to 1:3, more preferably 3:1 to 1:2, more preferably 2:1 to 1:2.

additional ingredients

The components of the invention preferably include additional ingredients which improve the stability of the active ingredients of the articles of the invention.

These additional ingredients generally stabilize the active ingredient(s) of the composition of the invention and are especially preferred when the active ingredient(s) include an oxidative or moisture sensitive active ingredient such as one or more enzymes. These additional ingredients also stabilize the matrix in the composition of the invention, thus indirectly stabilizing the active ingredient. These stabilizing components are defined as "stabilizers" in the present invention.

The stabilizer is preferably a compound which stabilizes the active ingredient or the matrix against degradation by oxidation and/or moisture during storage. The stabilizer may be or include a foam matrix stabilizer. The stabilizer may be or include an active ingredient stabilizer, especially an enzyme stabilizer. Stabilizers which indirectly stabilize the active ingredient by stabilizing the foam matrix of the article are referred to herein as "foam stabilizers".

Foam stabilizers preferably include surfactants such as fatty alcohols, fatty acids, alkanolamides, amine oxides or derivatives of these or combinations thereof. Foam stabilizers may include betaines, sultaines, phosphine oxides, alkyl sulfoxides or derivatives of these or combinations thereof.

Other preferred foam stabilizers include one or more anions or cations such as mono-, di-, trivalent or other multivalent metal ions, preferably sodium, calcium, magnesium, potassium, aluminum, zinc, copper, nickel, cobalt , iron, manganese and silver salts, preferably with anionic counterions as sulfate, carbonate, oxide, chloride, bromide, iodide, phosphate, borate, acetate, citrate and nitrate, or these combination of substances.

The foam stabilizer may comprise finely divided particles, preferably the finely divided particles have an average particle size of less than 10 microns, more preferably less than 1 micron, even more preferably less than 0.5 microns, or less than 0.1 microns. Preferred finely divided particles are aluminosilicates as described above, eg zeolites, silicas or electrolytes, and in finely divided particle form.

Foam stabilizers may include agar, sodium alginate, sodium lauryl sulfate, polyethylene oxide, guar gum, polyacrylates or derivatives of these or combinations thereof.

The foam stabilizer may be a coating separate from the matrix in the article. Foam stabilizers typically enclose the article or its active ingredient partially, preferably completely, within it.

Typically, the coating is contacted with the active ingredient, preferably thereby forming a coating thereon, before the active ingredient is contacted with the plasticizer of the polymeric material or matrix, and preferably incorporated into the article.

Typically, after the polymeric material and plasticizer form the matrix, preferably after the active ingredient has been contacted with said matrix or incorporated into the article, the coating is brought into contact with the article, preferably thereby forming the coating thereon.

Preferred coatings comprise polymers, typically selected from polyvinyl alcohol and its derivatives, polyethylene glycol and its derivatives, polyvinylpyrrolidone and its derivatives, cellulose ethers and their derivatives, and any of these polymers Copolymers between or with other monomers or oligomers. Most preferred are PVP (and derivatives thereof) and/or PEG (and derivatives thereof), most preferred are PVA (and derivatives thereof) or a mixture of PVA and PEG and/or PVP (and derivatives thereof). These polymers do not form the matrix of the articles of the invention and are therefore different from the polymeric material of the foam matrix.

Preferred coatings include compounds such as trihydric alcohols or glycerin, including diol derivatives of ethylene glycol, oligomers of polyethylene glycol, such as diethylene glycol, triethylene glycol, tetraethylene glycol Alcohols and polyethylene glycols with a weight-average molecular weight M.W. below 1000, waxes and polyethylene glycols, ethanol acetamide, ethanol formamide, triethanolamine or its acetate, ethanolamine salts, sodium thiocyanate, ammonium thiocyanate, Polyols such as 1,3-butanediol, sugars, sugar alcohols, urea, dibutyl or dimethyl phthalate, oxa monobasic acids, oxa dibasic acids, diglycolic acid and others with at least A linear carboxylic acid with ether groups distributed along its chain, water or a mixture of these substances. These compounds do not form the foam matrix of the compositions of the present invention. These compounds are therefore distinct from the plasticizers of the foam matrix.

Especially if the active ingredient comprises one or more enzymes, preferred stabilizers are those agents which directly stabilize the active ingredient, defined in the present invention as "active stabilizers" or "enzyme stabilizers". Typical active stabilizers act directly with and stabilize the active ingredient.

Typical active stabilizers for use in the present invention preferably include surfactants. Suitable surfactants for use in the present invention are those previously described herein as suitable as matrix stabilizers. In addition to these surfactants, other surfactants suitable for use in the present invention may include sodium alkyl (alkenyl) sulfonates, sodium alkoxy sulfonates, preferably sodium alkoxy sulfonates including any configuration of 10 Those of up to 18 carbon atoms are preferably linear and have an average degree of ethoxylation of 1 to 7, preferably 2 to 5.

Other preferred active stabilizers include boric acid, formic acid, acetic acid and salts thereof. The salts of these acids preferably contain counterions such as calcium and/or sodium.

Preferably the active stabilizer comprises cations such as calcium and/or sodium. Calcium chloride and/or sodium chloride are preferred.

Other preferred active stabilizers include small peptide chains averaging 3 to 20, preferably 3 to 10 amino acids, which interact with and stabilize the active ingredient, especially the enzyme(s).

Other active stabilizers include small nucleic acid molecules, and typically contain 3 to 300, preferably 10 to 100 nucleosides. Typical nucleic acid molecules are deoxyribonucleic acid and ribonucleic acid. The nucleic acid molecule may exist in a complex form with other molecules, such as proteins, or may form a complex with the active ingredient in the preparation of the present invention, especially with one (or more) enzymes.

Active stabilizers suitable for use in the present invention, especially when a bleaching agent is included in the article of the present invention, include antioxidants and/or reducing agents such as thiosulfates, methionine, urea, thiourea dioxide, Guanidine hydrochloride, guanidine carbonate, guanidine sulfamate, monoethanolamine, diethanolamine, triethanolamine, amino acids such as glycine, sodium glutamate, proteins such as bovine serum albumin and casein, tert-butylhydroxytoluene, 4,4-butylene Base bis(6-tert-butyl-3-methylphenol), 2,2'-butylene bis(6-tert-butyl-4-methylphenol), (monostyrenated cresol, distyrenated Cresol, monostyrenated phenol, distyrenated phenol, 1,1-bis(4-hydroxy-phenyl)cyclohexane and derivatives thereof, or combinations thereof.

Other active stabilizers may include reversible active ingredient inhibitors. Without wishing to be bound by theory, the researchers believe that reversible active ingredient inhibitors can form complexes with the active ingredient and improve the activity of the active ingredient, particularly if the active ingredient includes one or more enzymes. Stability, whereby the active ingredient is stabilized on storage. When the active ingredient is released, typically into a liquid environment, the reversible inhibitor dissociates from the active ingredient and the active ingredient can then perform the reaction for which it was assigned or intended.

Active stabilizers suitable for use in the present invention may include sugars, typical sugars for use in the present invention include those selected from the group consisting of sucrose, glucose, fructose, raffinose, trehalose, lactose, maltose and derivatives thereof and combinations thereof.

The active stabilizer may also contain sugar alcohols, such as sorbitol, mannitol, cyclohexanol and derivatives thereof and combinations thereof.

It may be preferred that the active stabilizer is in the form of a coating or barrier layer, at least partially enclosing the article of the invention or its active ingredient, preferably completely enclosing the article of the invention or especially the active ingredient of the enzyme. Method for preparing foam components

The components of the invention may be prepared by any of the following methods: preparing a polymeric matrix having a defined Tg, the polymeric matrix being formed from a polymeric material and a plasticizer, and compounding this matrix with an active ingredient and a stabilizer. Preferred methods include chemically or physically introducing gases into the polymeric material and plasticizer, and optionally active ingredients. A preferred method of preparing the composition of the invention comprises the following steps:

a) obtaining a mixture of polymer material and plasticizer, preferably water and additional plasticizer;

b) chemically or physically introducing a gas into the mixture of said polymeric material and water;

c) adding the active ingredient to said mixture before step b) and/or simultaneously with step b) and/or after step b);

d) bringing said mixture into contact with a dissolution aid before and/or simultaneously with step c) and/or after step c);

e) shaping the resulting mixture product;

If water is present, part of the water is removed after or simultaneously with one or more steps a) to e).

The mixture in step a) is preferably an aqueous mixture or slurry and part of the water is removed after or during steps b), c) and/or d) such that the resulting composition comprises 3% by weight or more of free moisture.

Step c) preferably comprises the step of obtaining a body comprising the active ingredient or a part of the active ingredient, and closing the body with the mixture in step b).

Step d) preferably comprises the step of mixing the active ingredient with the stabilizer, more preferably mixing completely, or blocking the active ingredient with the stabilizer, before the stabilizer, preferably the active ingredient, is brought into contact with the mixture.

Preferably the composition comprises open cells and/or closed cells, the method comprising the steps of:

a) forming a mixture of polymer material, active material, dissolution aid, plasticizer and liquid, wherein the liquid and plasticizer may be the same compound;

b) forming the mixture of claim b) into a body, and

c) evaporating the liquid or a portion of the liquid to form a space in the mixture which forms the inner region of the cell in the above-mentioned components,

Wherein step c) is preferably carried out by freeze-drying or by heating the body, whereby the liquid or part of the liquid is evaporated.

Step b) can also be carried out with the mixture of a) under pressure, preferably with mixing and/or at increased temperature, followed by removal of the pressure or part of the pressure, whereby the liquid evaporates. For example, extrusion methods can be used. Wherein preferably a mixture of polymer material, plasticizer preferably comprising water, optionally active ingredients and/or dissolution aids is introduced into the extruder, where the mixture is further mixed due to mixing and due to the heat applied and heating, preferably where the mixture forms a melt, and then reducing the pressure at the exit of the extruder where the extruded mixture (which may be formed into a desired shape, such as pellets) leaves the extruder, whereby the liquid or part of the liquid evaporates, or preferably water Evaporates as steam from the extrusion mixture. This results in a cell as described above with a space which may contain a gas, preferably air, and optionally an active ingredient. These spaces form the inner regions of the cells in the matrix of components of the invention.

Step b) of the method can also be carried out by heating the mixture so that the liquid or part of the liquid evaporates, forming a space as described above. This step is preferably carried out by conveying the mixture to a spray drying tower, preferably by sending the mixture from nozzles which form droplets of the mixture, and spray drying the droplets at conventional temperatures, whereby the components are obtained.

The gas or foam can be introduced physically or chemically by any of the known methods mentioned above, preferably

- optionally physical foaming by injection of gas (dry or wet route) under conditions of mixing, high shear agitation (dry or wet route), gas dissolution including critical gas diffusion and relaxation (dry or wet route);

- chemical foaming by means of in situ formation of gas (by chemical reaction of one or more components, including formation of _CO2 with foaming systems);

- Steam foaming, UV radiation curing.

These foaming steps are preferably followed by a drying step or an additional drying step to remove excess liquid or a portion of liquid, eg water. In particular this drying step is carried out at least after formation of the polymer matrix and optionally after addition of the active ingredient, preferably as the last step in the process. This drying step is preferably carried out such that the final component volume after the drying step is about the same as the volume before drying. Furthermore, the drying step is preferably carried out by freeze-drying, whereby solvents such as water are removed under vacuum and reduced temperature. Also useful is slow fluid bed drying, or oven drying at moderately increased temperatures, eg, 40-80°C, or even 40-60°C.

Preferred methods comprise at least the steps of forming a mixture of polymeric material and liquid, preferably polymeric material and a solvent, preferably comprising water, and adding a plasticizer (or possibly additional plasticizer) thereto. If active ingredients and/or dissolution aids are required in the matrix, these substances can also be added to the mixture of polymeric material solvent and plasticizer. Alternatively, or in addition, it may be preferred to form the matrix around the active material, preferably around a core of active material and carrier material.

Preferred methods of incorporating dissolution aids into the compositions of the present invention include:

a) bringing the dissolution aid into contact with the dry foam component, preferably adding the dissolution aid to the dry foam component, to obtain the foam component of the present invention, for example by injecting, or sealing the component matrix; and/or

b) cooling the foam component to a temperature near, preferably just above, the freezing point of said foam component and then contacting or adding a dissolution aid to said foam component In, the foam component of the present invention is obtained; and/or

c) as in b), after which the foam components are frozen, for example before freeze drying; and/or

d) Partial coating with a material, such as cetyl alcohol, preferably the dissolution aid.

Further processing is eg shaping of the final component into bodies such as granules or beads, which are generally dried to obtain components. Gas is preferably added prior to the shaping step. Shaping steps include granulation steps, such as atomization or spray drying, extrusion, microtablet making. Freeze drying is the preferred method of drying the bulk to form components.

The following is the preferred method, which results in less dusty or even dust-free granules with a substrate Tg below 10°C, elastic modulus, as measured by the prestressed Heubach test as described below. The amount is lower than 0.5GN·m ^-2 , which will be further described in the following specific examples. The first preferred method is as follows:

The desired amount of polymer material solution (or mixture of polymer and liquid) is obtained and eg (introduced) into a mixing tank. The desired amount of active material (solution), such as an enzyme solution, and dissolution aid is then added, and the desired amount of plasticizer, and optionally other additional ingredients, such as fillers, thickeners, etc. are added. Stir these materials to form a homogeneous mixture. A gas such as air is preferably introduced into the solution by high shear mixing by any of the methods described above, preferably physically.

The mixture is then granulated by atomization, preferably using a positive displacement pump to transfer the mixture solution into a nozzle(s), preferably using single or multiple liquid nozzles to generate droplets. These droplets are then preferably frozen by a freezing medium (which may include liquid nitrogen, freon, cryogenic oil). These frozen particles are then transferred to a vacuum chamber, preferably at a temperature (as measured at the surface of the particles) below 0°C.

The frozen particles are preferably collected from the spray tower and transferred without increasing the temperature. The side walls and contact pans of the lyophilizer are preferably kept below 0°C to keep the particles frozen. When a vacuum is applied, the frozen ice crystals will sublime into a gaseous form, causing cells to form within the particle. The overall degree of drying can be controlled by the degree of vacuum, the contact temperature of the side wall of the chamber and the plate.

When the granules have dried to the desired moisture content, they will flow freely. The particles are then preferably classified by passing through various sieves and/or processing equipment.

It has been found that the optional introduction of gas (bubbles) into the polymer solution mixture described above results in a better impact resistance of the particles and this is reflected by its electrical model. Bubbles can be introduced in various ways.

During the atomization step, the atomizing nozzle should preferably be located in the spray column and be of sufficient height to allow the particles to freeze as they fall with gravity. Nozzles can be designed in various ways - single hydraulic nozzles, rotary inserts, sonic or multi-fluid nozzles. The important aspect is to interrupt the flow of liquid to form individual droplets. As these droplets fall with gravity, they must be cooled so that they freeze. The freezing medium is preferably a non-aqueous gas or liquid which enables rapid freezing of liquid droplets. The actual temperature at which these droplets are cooled to form particles is preferably below 0°C, preferably below -20°C.

It is also preferred to modify the above method in the following way:

A gas, preferably _CO2 gas, is introduced into the mixture and this mixture is introduced into the spray drying tower as described above, whereby spray dried effervescent particles are formed, which can be classified if desired. Preferably the tower has an inlet temperature of about 130°C, an outlet temperature of about 75°C, and a spray rate of 12.5 g/min. For example, a Niro Mobil Minor with two fluid nozzles can thus be used. The resulting particles may already be in the desired form, or may be further freeze-dried under vacuum. Another preferred method is as follows:

The desired amount of polymer material solution (or alternatively powdered polymer may be used if a liquid is added) is obtained and introduced, for example, into a mixing tank. The desired amount of plasticizer is then added, and optionally other additional ingredients such as fillers, thickeners and the like. Stir these materials to form a homogeneous mixture. A gas such as air is preferably introduced into the solution by any of the methods described above, preferably by physical high shear mixing methods.

Granules comprising active ingredients such as enzymes, and dissolution aids, and optionally other ingredients such as fillers or carriers are also prepared, for example by fluid bed coating by applying a first 'core' (typically when these active substances are enzymes When these core particles are sugar or starch particles) are loaded onto a fluidized bed, and the active material or a solution of the active material is sprayed onto these core materials, the solvent such as water is then transferred from the active material with hot fluidizing air. The solution was dried and removed.

The above polymer mixture is then introduced onto these actives/cores, for example by positive displacement pumps onto atomizing nozzles in the fluidized bed as described above. It is possible to use more than one nozzle and it may be preferable to add different ingredients to the core through different nozzles.

The required fluidizing gas is preferably below 0°C, preferably around -20°C. The fluidizing gas then freezes the polymer mixture/solution to the outside of the active core. This is a critical parameter to be controlled, generally the air temperature must be below 0°C to allow rapid freezing of the polymer mixture/solution onto the core particles.

The frozen particles thus obtained are then preferably transferred to a vacuum chamber as described above, or otherwise sorted.

The granules of the invention obtained by this technique comprise a matrix surrounded by the active ingredient.

It has been found that the above step of optional introduction of gas (bubbles) into the polymer solution mixture results in better impact resistance of the particles, as reflected by their Young's modulus. Another preferred method is as follows:

The desired amount of polymer material solution (or solid polymer and appropriate amount of liquid) is obtained and introduced, for example, into a mixing tank. The desired amount of active material (solution), such as enzyme solution and dissolution aid (solution), is then added (to the mixing tank), and the desired amount of plasticizer, and optionally other additional ingredients such as fillers, Thickener. Stir these materials to form a homogeneous mixture. A gas such as air is preferably introduced into the solution by any of the methods described above, preferably by physical high shear mixing methods.

The polymer solution is then pumped from the mixing tank into an extruder, or into a cavity terminated by a forming plate. Gases may be injected into the mixture, eg, dispersed, by mechanical shear mixers or static mixers before entering the extruder or cavity.

As the extrudate exits the forming plate, the pressure change causes the extrudate to swell or expand slightly. The extrudate is then cut to the correct length with a die end mill or some other device (eg heated wire, rotating knife, etc.). The extrudate can optionally be made more round by an additional rounding step. The processing equipment to realize this function may include (rotary disk, accumulating disk, pill making machine, rotating drum, mixing drum, etc.).

For example, a paste is prepared by mixing 75g PVOH, 15g citric acid, 2g PEO and 22.5g glycerol in a Braum mixer at high shear, i.e. set to full speed, for 40 seconds: then add 80g _H2O and 80 g enzyme and mix at high shear, ie at speed set to full, until a smooth foam forms, within about 2 minutes. The foam was extruded from a 10ml syringe onto a plastic plate. Let it sit for 24 hours to dry. Once dry, the foam strips were cut into approximately 1-2 mm long sections to form a formula of 63.2% polyvinyl alcohol, 19% glycerin, 12.7% citric acid, 1.6% PEO, 4% water, 3.2% enzyme (dry ) particles.

The modulus of elasticity of the obtained particles was 0.00016 GN·m ^-2 .

The resulting granules produced 0% dust when tested with the prestressed Heubach measurement, which indicates that the granules have very good impact resistance. (prestressed Heutach measuring method is known in the art, use the equipment provided by Heubach Engineering GmbH of Germany, the stress deformation (stressed modification) of the rotational speed of its rotor is 75 ± 1rpm, bead is tungsten carbide, and each bead weighs 82 grams). Preferred molding/tabletting method

The most preferred method involves forming pellets of the mixture described above using a mould; thereby introducing the mixture according to the invention into the mould, followed by drying (freeze drying). Also preferred is a method using ingot-making equipment in which the mixture as described above, preferably also containing the introduced gas, is forced through a rotating perforated drum onto a moving discharge belt and shaped into Lozenges (droplets or granules). When dry or hardened, the particles or beads thus formed are removed from the release tape with a scraper.

Preferably the first step prepares the mixture of polymeric material and plasticizer, liquid components, and optionally active ingredients and dissolution aids. Gases are preferably introduced into the mixtures according to the invention. Preferably the mixture must be free of large undissolved particles which would clog the perforations in the drum. The mixture is preferably in the temperature range of 0-50°C. The mixture is pumped into a splitter that enters the rotating perforated drum parallel to the long axis of the drum. The mixture is drawn into the interior of the drum and as the drum rotates, the mixture is brought into contact with an internal scraper blade mounted on and in contact with the inner surface of the drum along the length of the perforated drum and parallel to the feed splitter. The distance from the outer surface of the perforated drum is within the range of the desired particle height (which is smaller than the diameter of the perforated holes), but there is no contact with the moving release belt or the rotating smooth-surfaced drum, at which point the internal scraper meets the inner surface of the perforated drum In contact, the tangential velocity of the perforated drum matches the velocity of the release belt or the tangential velocity of the smooth-surfaced drum. When the mixture is driven through perforations with a pore size typically between 300-2000 microns (but can be smaller or larger), the mixture is deposited on the underlying surface. The rotational shear of the perforated drum draws the feedstock away from the material on the smooth surface, thereby leaving droplets or pastilles that will form the desired particles. These lozenges can be fixed by condensation or evaporation of some or all of the solvent liquid. If condensation is desired, the temperature of the release belt or smooth-surfaced drum can range from ambient to -20°C. If evaporation of the solvent is required, it can be accomplished by thermal conduction of the release band at a temperature ranging from ambient to 70°C, by passing dry air (which can be heated up to 200°C to reduce drying time) across the surface of the tablet, or by both . The resulting particles are then removed from the drum or release belt with a scraper. The removal method can be improved by using a suitable lubricant (release agent) such as silicone oil on the drum. Such lubricants or release agents give the granules the additional advantage of being able to increase tablet height by reducing the bonding properties between the polymerization mixture and the belt/drum if tablet height is a desired characteristic.

Example

Example 1

PROCESS FOR MAKING THE FOAM COMPONENTS OF THE INVENTION

4700g of 33% w/w polyvinyl alcohol solution (weight average molecular weight M.W. between 30000 and 70000) was mixed with 3360g of enzyme solution (containing 5% by weight of active enzyme and 85% by weight of water), 159.3g of glycerol and 155g of cyclic The hexanedimethanol was mixed in a high shear mixer until a smooth foam formed. This mixture was transferred to a feed tank and pumped with a gear pump into a micropellet making apparatus such as that supplied by Sandvik ProcessSystem of Totowa New York with a perforated drum with 1 mm diameter perforations at 2.5 mm intervals. The device deposits the pastilles on a smooth-surfaced drum coated with a layer of silicone oil and heated to about 30°C. When 1/4 of the drum is covered with pastilles, the drum stops rotating. The lozenges were dried with a hot air heater until the surface of the lozenges was dry to the touch. These resulting particles were then scraped off and collected.

Example 2

Process for preparing foam components of the present invention in tablet, bead or granule form Apparatus : microbalance, graduated 100 ml flask, Kenwood "Chef" food processor with stirrer and mixing tank, glass or Plastic abrasives, scrapers.

Chemicals : poly(vinyl alcohol) (Aldrich Chemicals, molecular weight Mw=30-70k), glycerin (99%, Aldrich Chemicals), citric acid (Aldrich, citric acid, anhydrous USP), distilled water, dry ice (or solid phase CO ₂ ), thermally insulated box.

step

1 Weigh 50±0.2g of PVA, 30±0.2g of glycerin, and 50±0.2g of cyclohexanedimethanol.

2 Mix the PVA, glycerin and citric acid with a mixer at the low speed setting (labeled 2, low shear).

3 Gradually add 50±1ml of water to the dry mixer and maintain the mechanical mixing for 2 minutes. A smooth colloid was obtained.

4 Increase mixing speed and increase shear to maximum setting (labeled 8). Add 10-20ml of water until a PVA foam forms. This high shear mixing was maintained for 3 minutes.

5. Under the condition of maintaining mechanical mixing, gradually add the active ingredient, such as 2-10g of enzyme, into the foam to obtain a uniform active foam.

6 Stop mixing. Disperse the PVA foam in the mold and avoid any structural collapse.

7 Place the filled mold in an insulated box filled 1/3 with dry ice. Let stand in the freezer for 5 hours.

8 Quickly place the frozen sample in a vacuum freeze dryer (Edward XX) for 24 hours.

9 Remove the dried specimen from the mold.

Any active ingredient can be added in step 5 in any amount, generally up to about 50 g, eg fabric softener, bleach, nonionic surfactants.

Any dissolution aid can be added in step 5 in any amount, typically up to about 50 g, such as cyclohexanedimethanol or sodium toluenesulfonate.

Example 3

Process for preparing foam components of the present invention in tablet, bead or granule form

Device: as described in the previous embodiment

Chemicals: poly(vinyl alcohol) (Aldrich Chemicals, molecular weight Mw=30-70k), glycerin (99%, Aldrich Chemicals), sodium carbonate (Aldrich, anhydrous), lauryl sulfate surfactant (Aldrich) , distilled water, Petri dish (diameter 90mm), oven (set at 45°C±2°C).

step

1 Weigh 50±0.2g of PVA, 30±0.2g of glycerin, 20±0.2g of cyclohexanedimethanol, 20±0.2g of sodium carbonate and 2±0.2g of lauryl sulfate.

2 Mix the PVA, glycerin, citric acid and lauryl sulfate with the mixer at the low speed setting (labeled 2).

3 Gradually add 50±1 ml of water to the dry mixer and maintain the mechanical mixing for 2 minutes. A smooth colloid was obtained.

4 Add eg 5 g enzyme active ingredient, and sodium carbonate and stir vigorously for 30 seconds until a well expanded foam is obtained.

5 Disperse the foam in a Petri dish in a uniform 1 cm thick layer.

6 Place the Petri dish in an oven at 40°C for 24 hours.

7 Remove the dried foam film from the mold.

Any active ingredient can be added in step 4 in any amount, typically up to about 50 g, eg fabric softener, bleach, nonionic surfactants.

Any dissolution aid can be added in step 1 in any amount, typically up to about 50 g, eg SDS, STS, SXS, SCS, CHDM.

Available 55wt% polycarboxylate polymer, 20wt% anhydrous sodium carbonate and 25wt% enzyme, softening clay etc. repeat the above steps; Sodium and 20wt% enzyme, soften clay etc. Repeat above steps.

Claims (14)

1. A foam component comprising a matrix formed from a polymeric material and a plasticizer, a dissolution aid and preferably an active ingredient active in an aqueous environment, the foam component being stable in contact with air, It is unstable when in contact with water. 2. Foam component according to claim 1, which releases the active ingredient or part of the active ingredient on contact with water, preferably the component partially or completely decomposes, disperses, denatures and/or dissolves on contact with water. 3. A foam component as claimed in any preceding claim, having a modulus of elasticity of less than 10 GN·m ^-2 , preferably less than 1 GN·m ^-2 . 4. Foam component according to any one of the preceding claims, wherein the active ingredient is a cleaning product ingredient, a fabric care ingredient, a pharmaceutical ingredient or a cosmetic ingredient, preferably selected from enzymes, surfactants, brighteners, dyes, foams Inhibitors, bleaches, bleach boosters, fabric softeners, fabric conditioners, antimicrobials and mixtures of these substances. 5. The foam component of any preceding claim, wherein the dissolution aid comprises a foaming system, a hydrotrope, a cellulosic material, a water soluble salt or a combination of these. 6. A foam component according to any preceding claim, wherein the polymeric material has a glass transition temperature of less than 50°C, preferably less than 40°C. 7. A foam component according to any preceding claim, wherein said polymeric material comprises a water soluble polymer, preferably a water soluble polyvinyl alcohol. 8. A foam component as claimed in any preceding claim which is in particulate form and has an average particle size of from 50 to 4000 microns, preferably from 100 to 150 microns. 9. A foam component as claimed in any preceding claim having a relative density of from 0.05 to 0.9, preferably from 0.3 to 0.7. 10. A foam component according to any preceding claim, wherein said component comprises a series of open and closed cells, wherein the number ratio of open and closed cells is preferably at least 1:1. 11. A foam component according to any one of the preceding claims obtainable by a process comprising the steps of: a) obtaining a mixture of polymeric materials; b) chemically or physically introducing a gas into said mixture; c) bringing said mixture into contact with the active ingredient before and/or simultaneously with step b) and/or after step b); d) contacting said mixture with a dissolution aid before and/or simultaneously with step b) and/or after step b); and e) forming the resulting mixture into an article; Where water, if present, is preferably partially removed after or simultaneously with one or more steps a) to e). 12. The foam component of claim 11, wherein said dissolution aid is contacted with said mixture of polymeric material and plasticizer prior to step b). 13. Use of a foam component according to any one of claims 1 to 12 for the release of an active ingredient, preferably a detergent active ingredient, preferably an enzyme, into an aqueous environment, the aqueous environment being wash water. 14. Use of the foam component according to any one of claims 1 to 12 in a cleaning composition, a fabric care composition, a personal care composition, a cosmetic composition or a pharmaceutical composition, preferably to incorporate in these compositions selected from Active ingredients of enzymes, fragrances, surfactants, brighteners, dyes, suds suppressors, bleaches, bleach boosters, fabric softeners, antimicrobials, foaming systems and mixtures of these substances.