Dosage element and a method of manufacturing a dosage element

Abstract

A dosage element to be consumed in use in a ware washing machine, the dosage element including a container, whereby the container encloses a non-consolidated particulate composition and a gel in direct contact with one another.

Claims

1. A method of manufacturing a ware washing unit dosage element having one compartment comprising the steps of: (a) introducing a gel precursor composition into a water-soluble receptacle, wherein the gel precursor composition consists of 10-60 wt % of a non-ionic surfactant, and 10-60 wt % of a polyethylene glycol having a molecular weight in the range of 150-600 with the balance being a bleach activator, and optionally 0.1-8.0 wt % of polyethylene glycol having a molecular weight in the range of 1,000-35,000, water, a dye, and/or a builder; (b) converting the gel precursor composition, or allowing the gel precursor composition to convert, into a shape-stable gel; and (c) introducing a flowable particulate composition into the receptacle adjacent and in direct contact with the shape-stable gel such that the shape-stable gel and the flowable particulate composition do not substantially seep into each other; wherein the method does not comprise consolidating the flowable particulate composition.

2. The method of claim 1, wherein the water content of the shape-stable gel is less than 10 wt % water.

3. The method of claim 2, wherein the water content of the shape-stable gel is less than 5 wt % water.

4. The method of claim 3, wherein the water content of the shape-stable gel is less than 2 wt % water.

5. The method of claim 1, wherein the density of the shape-stable gel is between 0.7 g/cm.sup.3 and 2.0 g/cm.sup.3.

6. The method of claim 1, wherein the flowable particulate composition comprises a bleach and/or an enzyme.

7. The method of claim 1, wherein the gel precursor composition is introduced into the receptacle at an elevated temperature and cools to form the shape-stable gel.

8. The method of claim 1, which does not comprise compacting the flowable particulate composition.

9. The method of claim 1, wherein the shape-stable gel forms a layer at the bottom of the receptacle, and the flowable particulate composition forms a layer on top of the shape-stable gel.

10. The method of claim 1, wherein the ratio by weight of the flowable particulate composition to the shape-stable gel is in the range of 1:1 to 20:1.

11. The method of claim 1, further comprising introducing a pill or core of material into the receptacle.

12. The method of claim 11, wherein the introducing the pill or core of material into the receptacle occurs before, or at the same time as, the introducing the gel precursor composition into the receptacle.

13. The method of claim 11, wherein the introducing the pill or core of material into the receptacle locates the pill or core of material such that the gel precursor composition forms a barrier between the pill or core of material and the flowable particulate composition.

14. A dosage element manufactured by the method of claim 1.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) Various features and advantages of the present invention may be more readily understood with reference to the following detailed description taken in conjunction with the accompanying drawings, wherein like reference numerals designate like structural elements, and in which:

(2) FIGS. 1(a) to 1(h) illustrate a preferred process for forming a dosage element in accordance with an embodiment of the invention; and

(3) FIG. 2 is a perspective view of a dosage element in accordance with a preferred embodiment of the invention.

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS

(4) To facilitate an understanding of the principles and features of the various embodiments of the invention, various illustrative embodiments are explained below. Although exemplary embodiments of the invention are explained in detail, it is to be understood that other embodiments are contemplated. Accordingly, it is not intended that the invention is limited in its scope to the details of construction and arrangement of components set forth in the following description or examples. The invention is capable of other embodiments and of being practiced or carried out in various ways. Also, in describing the exemplary embodiments, specific terminology will be resorted to for the sake of clarity.

(5) It must also be noted that, as used in the specification and the appended claims, the singular forms a, an and the include plural references unless the context clearly dictates otherwise. For example, reference to a component is intended also to include composition of a plurality of components. References to a composition containing a constituent is intended to include other constituents in addition to the one named.

(6) Also, in describing the exemplary embodiments, terminology will be resorted to for the sake of clarity. It is intended that each term contemplates its broadest meaning as understood by those skilled in the art and includes all technical equivalents which operate in a similar manner to accomplish a similar purpose.

(7) Ranges may be expressed herein as from about or approximately or substantially one particular value and/or to about or approximately or substantially another particular value.

(8) When such a range is expressed, other exemplary embodiments include from the one particular value and/or to the other particular value.

(9) Similarly, as used herein, substantially free of something, or substantially pure, and like characterizations, can include both being at least substantially free of something, or at least substantially pure, and being completely free of something, or completely pure.

(10) By comprising or containing or including is meant that at least the named compound, element, particle, or method step is present in the composition or article or method, but does not exclude the presence of other compounds, materials, particles, method steps, even if the other such compounds, material, particles, method steps have the same function as what is named.

(11) It is also to be understood that the mention of one or more method steps does not preclude the presence of additional method steps or intervening method steps between those steps expressly identified. Similarly, it is also to be understood that the mention of one or more components in a composition does not preclude the presence of additional components than those expressly identified.

(12) The materials described as making up the various elements of the invention are intended to be illustrative and not restrictive. Many suitable materials that would perform the same or a similar function as the materials described herein are intended to be embraced within the scope of the invention. Such other materials not described herein can include, but are not limited to, for example, materials that are developed after the time of the development of the invention.

(13) Preferred components of a dishwashing tablet, in particular of the particulate portion of the dishwashing tablet of the invention, are as follows:

(14) Bleaching Compounds

(15) Any type of bleaching compound conventionally used in detergent compositions may be used according to the present invention. Preferably the bleaching compound is selected from inorganic peroxides or organic peracids, derivatives thereof (including their salts) and mixtures thereof. Especially preferred inorganic peroxides are percarbonates, perborates and persulphates with their sodium and potassium salts being most preferred. Sodium percarbonate and sodium perborate are most preferred, especially sodium percarbonate.

(16) Organic peracids include all organic peracids traditionally used as bleaches, including, for example, perbenzoic acid and peroxycarboxylic acids such as mono- or diperoxyphthalic acid, 2-octyldiperoxysuccinic acid, diperoxydodecanedicarboxylic acid, diperoxy-azelaic acid and imidoperoxycarboxylic acid and, optionally, the salts thereof. Especially preferred is phthalimidoperhexanoic acid (PAP).

(17) Desirably the bleaching compound is present in the compositions in an amount of from 1 to 60 wt %, especially 5 to 55 wt %, most preferably 10 to 50% wt, such as 10 to 20% wt. When the compositions of the invention comprise two or more distinct regions, the amount of bleaching compound typically present in each can be chosen as desired although the total amount of the bleaching compound will typically be within the amounts stated hereinabove.

(18) Builders

(19) The detergent compositions may also comprise conventional amounts of detergent builders which may be either phosphorous based or non-phosphorous based, or even a combination of both types. Suitable builders are well known in the art.

(20) If phosphorous builders are to be used then it is preferred that mono-phosphates, di-phosphates, tri-polyphosphates or oligomeric-polyphosphates are used. The alkali metal salts of these compounds are preferred, in particular the sodium salts. An especially preferred builder is sodium tripolyphosphate (STPP).

(21) The non-phosphorous based builder may be organic molecules with carboxylic group(s), amino acid based compound or a succinate based compound. The term succinate based compound and succinic acid based compound are used interchangeably herein.

(22) Builder compounds which are organic molecules containing carboxylic groups include citric acid, fumaric acid, tartaric acid, maleic acid, lactic acid and salts thereof. In particular the alkali or alkaline earth metal salts of these organic compounds may be used, and especially the sodium salts. An especially preferred builder is sodium citrate.

(23) Preferred examples of amino acid based compounds according to the invention are MGDA (methyl-glycine-diacetic acid, and salts and derivatives thereof) and GLDA (glutamic-N,N-diacetic acid and salts and derivatives thereof). GLDA (salts and derivatives thereof) is especially preferred according to the invention, with the tetrasodium salt thereof being especially preferred. Other suitable builders are described in U.S. Pat. No. 6,426,229 which is incorporated by reference herein. Particular suitable builders include; for example, aspartic acid-N-monoacetic acid (ASMA), aspartic acid-N,N-diacetic acid (ASDA), Aspartic acid-N-monopropionic acid (ASMP), iminodisuccinic acid (IDA), N-(2-sulfomethyl) aspartic acid (SMAS), N-(2-sulfoethyl)aspartic acid (SEAS), N-(2-sulfomethyl)glutamic acid (SMGL), N-(2-sulfoethyl)glutamic acid (SEGL), N-methyliminodiacetic acid (MIDA), -alanirie-N,N-diacetic acid (-ALDA), p-alanine-N,N-diacetic acid (-ALDA), serine-N,N-diacetic acid (SEDA), isoserine-N,N-diacetic acid (ISDA), phenylalanine-N,N-diacetic acid (PHDA), anthranilic acid-N,N-diacetic acid (ANDA), sulfanilic acid-N,N-diacetic acid (SLDA), taurine-N, N-diacetic acid (TUDA) and sulfomethyl-N,N-diacetic acid (SMDA) and alkali metal salts or ammonium salts thereof.

(24) Further preferred succinate compounds are described in U.S. Pat. No. 5,977,053 and have the formula;

(25) ##STR00001##
in which R, R.sup.1, independently of one another, denote H or OH, R.sup.2, R.sup.3, R.sup.4, R.sup.5, independently of one another, denote a cation, hydrogen, alkali metal ions and ammonium ions, ammonium ions having the general formula R.sup.6R.sup.7R.sup.8R.sup.9N+ and R.sup.6, R.sup.7, R.sup.8, R.sup.9, independently of one another, denoting hydrogen, alkyl radicals having 1 to 12 C atoms or having 2 to 3 C atoms. A preferred example is tetrasodium imminosuccinate.

(26) Preferably the total amount of builder present in the compositions of the invention is an amount of at least 5 wt %, preferably at least 10 wt %, more preferably at least 20 wt %, and most preferably at least 25 wt %, preferably in an amount of up to 70 wt %, preferably up to 60 wt %, more preferably up to 60 wt %, and most preferably up to 35 wt %. The actual amount used will depend upon the nature of the builder used.

(27) The detergent compositions of the invention may further comprise a secondary builder (or cobuilder). Preferred secondary builders include homopolymers and copolymers of polycarboxylic acids and their partially or completely neutralized salts, monomeric polycarboxylic acids and hydroxycarboxylic acids and their salts, phosphates and phosphonates, and mixtures of such substances. Preferred salts of the abovementioned compounds are the ammonium and/or alkali metal salts, i.e. the lithium, sodium, and potassium salts, and particularly preferred salts is the sodium salts.

(28) Secondary builders which are organic are preferred.

(29) Suitable polycarboxylic acids are acyclic, alicyclic, heterocyclic and aromatic carboxylic acids, in which case they contain at least two carboxyl groups which are in each case separated from one another by, preferably, no more than two carbon atoms.

(30) Polycarboxylates which comprise two carboxyl groups include, for example, water-soluble salts of, malonic acid, (ethylenedioxy)diacetic acid, maleic acid, diglycolic acid, tartaric acid, tartronic acid and fumaric acid. Polycarboxylates which contain three carboxyl groups include, for example, water-soluble citrate. Correspondingly, a suitable hydroxycarboxylic acid is, for example, citric acid.

(31) Another suitable polycarboxylic acid is the homopolymer of acrylic acid. Other suitable builders are disclosed in WO 95/01416, to the contents of which express reference is hereby made.

(32) Surfactants

(33) The detergent compositions of the invention may contain surface active agents, for example, anionic, cationic, amphoteric or zwitterionic surface active agents or mixtures thereof. Many such surfactants are described in Kirk Othmer's Encyclopedia of Chemical Technology, 3rd Ed., Vol. 22, pp. 360-379, Surfactants and Detersive Systems, incorporated by reference herein. In general, bleach-stable surfactants are preferred.

(34) A preferred class of nonionic surfactants is ethoxylated non-ionic surfactants prepared by the reaction of a monohydroxy alkanol or alkylphenol with 6 to 20 carbon atoms. Preferably the surfactants have at least 12 moles particularly preferred at least 16 moles, and still more preferred at least 20 moles of ethylene oxide per mole of alcohol or alkylphenol.

(35) Particularly preferred non-ionic surfactants are the non-ionics from a linear chain fatty alcohol with 16-20 carbon atoms and at least 12 moles particularly preferred at least 16 and still more preferred at least 20 moles of ethylene oxide per mole of alcohol.

(36) According to one embodiment of the invention, the non-ionic surfactants additionally may comprise propylene oxide units in the molecule. Preferably these PO units constitute up to 25% by weight, preferably up to 20% by weight and still more preferably up to 15% by weight of the overall molecular weight of the non-ionic surfactant.

(37) Surfactants which are ethoxylated mono-hydroxy alkanols or alkylphenols,which additionally comprises polyoxyethylene-polyoxypropylene block copolymer units may be used. The alcohol or alkylphenol portion of such surfactans constitutes more than 30%, preferably more than 50%, more preferably more than 70% by weight of the overall molecular weight of the non-ionic surfactant.

(38) Another class of suitable non-ionic surfactants includes reverse block copolymers of polyoxyethylene and, polyoxypropylene and block copolymers of polyoxyethylene and polyoxypropylene initiated with trimethylolpropane.

(39) Another preferred class of nonionic surfactant can be described by the formula:
R.sup.1O[CH.sub.2CH(CH.sub.3)O]x[CH.sub.2CH.sub.2O].sub.Y[CH.sub.2CH(OH)R.sup.2]

(40) where R.sup.1 represents a linear or branched chain aliphatic hydrocarbon group with 4-18 carbon atoms or mixtures thereof, R.sup.2 represents a linear or branched chain aliphatic hydrocarbon rest with 2-26 carbon atoms or mixtures thereof, x is a value between 0.5 and 1.5 and y is a value of at least 15.

(41) Another group of preferred nonionic surfactants are the end-capped polyoxyalkylated non-ionics of formula:
R.sup.1O[CH.sub.2CH(R.sup.3)0]x[CH.sub.2].sub.kCH(OH)[CH.sub.2].sub.jOR.sup.2

(42) where R.sup.1 and R.sup.2 represent linear or branched chain, saturated or unsaturated, aliphatic or aromatic hydrocarbon groups with 1-30 carbon atoms, R.sup.3 represents a hydrogen atom or a methyl, ethyl, n-propyl, iso-propyl, n-butyl, 2-butyl or 2-methyl-2-butyl group, x is a value between 1 and 30 and, k and j are values between 1 and 12, preferably between 1 and 5. When the value of x is >2 each R.sup.3 in the formula above can be different. R.sup.1 and R.sup.2 are preferably linear or branched chain, saturated or unsaturated, aliphatic or aromatic hydrocarbon groups with 6-22 carbon atoms, where group with 8 to 18 carbon atoms are particularly preferred. For the group R.sup.3H, methyl or ethyl are particularly preferred. Particularly preferred values for x are comprised between 1 and 20, preferably between 6 and 15.

(43) As described above, in case x>2, each R.sup.3 in the formula can be different. For instance, when x=3, the group R.sup.3 10 could be chosen to build ethylene oxide (R.sup.3H) or propylene oxide (R.sup.3=methyl) units which can be used in every single order for instance (PO)(EO)(EO), (EO)(PO)(EO), (EO)(EO)(PO), (EO)(EO)(EO), (PO)(EO)(PO), (PO) (PO) (EO) and (PO)(PO)(PO). The value 3 for x is only an example and bigger values can be chosen whereby a higher number of variations of (HO) or (PO) units would arise.

(44) Particularly preferred end-capped polyoxyalkylated alcohols of the above formula are those where k=1 and j=1 originating molecules of simplified formula:
R.sup.1O[CH.sub.2CH(R.sup.3)O].sub.xCH.sub.2CH(OH)CH.sub.2OR.sup.2

(45) The use of mixtures of different nonionic surfactants is suitable in the context of the present invention, for instance, mixtures of alkoxylated-alcohols and hydroxy group containing alkoxylated alcohols.

(46) Preferably the non-ionic surfactants are present in the compositions of the invention in an amount of from 0.1% wt to 5% wt, more preferably 0.5% wt to 3% wt, such as 0.5 to 3% wt.

(47) The surfactants are typically included in amounts of up to 15% wt, preferably of from 0.5% wt to 10% wt, such as 1% wt to 5% wt in total.

(48) Anti-Foam Agents

(49) The detergent composition according to the invention may comprise one or more foam control agents. Suitable foam control agents for this purpose are all those conventionally used in this field, such as, for example, silicones and paraffin oil. If present, the foam control agents are preferably present in the, composition in amounts of 5% by weight or less of the total weight of the composition.

(50) Anti-Corrosion Agents

(51) It is known to include a source of multivalent ions in cleaning compositions, and in particular in automatic dishwashing compositions, for technical and/or performance reasons. For example, multivalent ions and especially zinc and/or manganese ions have been included for their ability to inhibit corrosion on metal and/or glass. Bismuth ions may also have benefits when included in such compositions.

(52) For example, organic and inorganic redox-active substances which are known as suitable for use as silver/copper corrosion inhibitors are mentioned in WO 94/26860 and WO 94/26859. Suitable inorganic redox-active substances are, for example, metal salts and/or metal complexes chosen from the group consisting of zinc, manganese, titanium, zirconium, hafnium, vanadium, cobalt and cerium salts and/or complexes, the metals being in one of the oxidation states II, III, IV, V or VI. Particularly suitable metal salts and/or metal complexes are chosen from the group consisting of MnSO.sub.4, Mn(II) citrate, Mn(II) stearate, Mn(II) acetylacetonate, Mn(II) [1-hydroxyethane-1,1-diphosphonate], V.sub.2O.sub.5, V.sub.2O.sub.4, VO.sub.2, TiOSO.sub.4, K.sub.2ZrF.sub.6, K.sub.2ZrF.sub.6, CoSO.sub.4, Co(NO.sub.3).sub.2 and Ce(NO.sub.3).sub.3. Zinc salts are specially preferred corrosion inhibitors.

(53) Therefore, an especially preferred optional ingredient according to the present invention is a source of multivalent ions such as those mentioned in the immediately preceding paragraph and in particular zinc, bismuth and/or manganese ions. In particular a source of zinc ions is preferred. Any suitable source of multivalent ions may be used, with the source preferably being chosen from sulphates, carbonates, acetates, gluconates and metal-protein compounds and those mentioned in the immediately preceding paragraph.

(54) Any conventional amount of multivalent ions/multivalent ions source may be included in the compositions of the invention. However, it is preferred that the multivalent ions are present in an amount of from 0.01% wt to 5% wt, preferably 0.1% wt to 3% wt, amount of multivalent ion the invention will thus be such as 0.5% wt to 2.5% wt. The source in the compositions of correspondingly higher.

(55) The detergent composition may also comprise a silver/copper corrosion inhibitor in conventional amounts. This term encompasses agents that are intended to prevent or reduce the tarnishing of non-ferrous metals, in particular of silver and copper. Preferred silver/copper corrosion inhibitors are benzotriazole or bis-benzotriazole and substituted derivatives thereof. Other suitable agents are organic and/or inorganic redox-active substances and paraffin oil. Benzotriazole derivatives are those compounds in which the available substitution sites on the aromatic ring are partially or completely substituted. Suitable substituents are linear or branch-chain C.sub.1.sub._.sub.20 alkyl group's and hydroxyl, thio, phenyl or halogen such as fluorine, chlorine, bromine and iodine. A preferred substituted benzotriazole is tolyltriazole.

(56) Performance Polymers

(57) Polymers intended to improve the cleaning performance of the detergent compositions may also be included therein. For example sulphonated polymers may be used. Preferred examples include copolymers of CH.sub.2CR.sup.1CR.sup.2R.sup.3OC.sub.4H.sub.3R.sup.4S0.sub.3X wherein R.sup.1, R.sup.2, R.sup.3, R.sup.4 are independently 1 to 6 carbon alkyl or hydrogen, and X is hydrogen or alkali with any suitable other monomer units including modified acrylic, fumaric, maleic, itaconic, aconitic, mesaconic, citraconic and methylenemalonic acid or their salts, maleic anhydride, acrylamide, alkylene, vinylmethyl ether, styrene and any mixtures thereof. Other suitable sulfonated monomers for incorporation in sulfonated (co)polymers are 2-acrylamido-2-methyl-1-propanesulfonic methacrylamido-2-hydroxy-propanesulfonic acid, allysulfonic acid, methallysulfonic acid, 2-hydroxy-3-(2-propenyloxy) propanesulfonic acid, 2-methyl-2-propenen-1-sulfonic acid, styrenesulfonic acid, vinylsulfonic acid, 3-sulfopropyl acrylate, 3-sulfopropylmethacrylate, sulfomethylacrylamide, sulfomethylmethacrylamide and water soluble salts thereof. Suitable sulfonated polymers are also described in U.S. Pat. No. 5,308,532 and in WO 2005/090541.

(58) When a sulfonated polymer is present, it is preferably present in the composition in an amount of at least 0.1 wt %, preferably at least 0.5 wt %, more preferably at least 1 wt %, and most preferably at least 3 wt %, up to 40 wt %, preferably up to 25 wt %, more preferably up to 15 wt %, and most preferably up to 10 wt %.

(59) Enzymes

(60) The detergent composition of the invention may comprise one or more enzymes. It is preferred that the enzyme is selected from protease, lipase, amylase, cellulase and peroxidase enzymes. Such enzymes are commercially available and sold, for example, under the registered trademarks Esperase, Alcalase and Savinase by Nova Industries A/S and Maxatase by International Biosynthetics, Inc. It is most preferred that protease enzymes are included in the compositions according to the invention; such enzymes are effective for example in dishwashing detergent compositions.

(61) Desirably enzyme(s) is/are present in the composition in an amount of from 0.01 to 3 wt %, especially 0.1 to 2.5 wt %, such as 0.2 to 2 wt %.

(62) Buffering Systems

(63) The detergent composition according to the invention may comprise a buffering system to maintain the pH of the composition at a desired pH on dissolution and this may comprise a source of acidity or a source of alkalinity as necessary.

(64) A source of acidity may suitably be any components which are acidic; for example polycarboxylic acids. Citric acid is especially preferred. Salts of these acids may also be used. A source of alkalinity may suitably be any suitable compound which is basic; for example any salt of a strong base and a weak acid such as soda. However additional acids or bases may be present. In the case of alkaline compositions silicates, phosphates or hydrogen phosphates may suitably be used. Preferred silicates are sodium silicates such as sodium disilicate, sodium metasilicate and crystalline phyllosilicates.

(65) Perfume, Colors, Preservatives

(66) The detergent compositions of the invention may also comprise minor, conventional-amounts of perfumes, preservatives and/or colorants. Such ingredients are typically present in amounts of up to 2% wt.

(67) Contrasting Parts

(68) Preferred dosage forms have first and second parts which contrast with each other. They may contrast in the chemical nature of their components. Components may have different functions in a ware washing environment. They may be incompatible with each other. For example one component may interact adversely with another component to cause instability in storage or to reduce effective cleaning action, and such components may be segregated, one in the first part and one in the second part.

(69) Alternatively or additionally the first and second parts may be arranged to release their components at different times in the washing process. This may be achieved by use of different coverings or skins for the components; for example by use of different wall materials for the first and second parts, with different rates of dissolution in the wash water and/or by use of walls of different thicknesses for the first and second parts.

(70) Alternatively or additionally it may facilitate manufacture to separate certain components, and thereby create a contrast between the first and second parts.

(71) Alternatively or additionally the first and second parts may contrast in their properties for aesthetic reasons.

(72) The following are examples of contrasting first and second parts: an enzyme in one part and a bleach in another part; a corrosion inhibitor in one part and a bleach in another part; a corrosion inhibitor in one part and an enzyme in another part; an acid or a hydrolysable agent in one part and an alkalinity agent in another part; a solid (including a powder or a gel) in one part and a liquid in another part; a solid (including a powder or a gel) in one part and another solid (including a powder or a gel) in another part, to be kept apart, whether for chemical/functional reasons or aesthetic reasons; a liquid in one part and another liquid in another part, to be kept apart, whether for chemical/functional reasons or aesthetic reasons; a pre-wash formulation (including a ware washing machine cleaner, for example machine sanitizer and/or descaler), in one part and a main wash formulation in another part; a main wash formulation in one part and a rinse aid formulation in another part.

(73) It is an important advantage of the invention that different portions may be combined without the need for separation walls.

(74) According to a second aspect of the invention, there is provided a method of manufacturing a dosage element for a ware washing machine, the method comprising the steps of: (a) forming a sheet or film into a receptacle; (b) introducing a flowable particulate composition into the receptacle; (c) locally displacing the particulate composition inside the receptacle to form a hollow therein; (d) introducing a gel or gel precursor into the hollow formed in the particulate composition; and (e) closing the receptacle with a lid.

(75) Preferably step (c) is accomplished without compaction of the particulate material, i.e. it remains a non-consolidated particulate material which when not constrained by the receptacle is capable of flowing.

(76) Preferably, prior to step (d) or (e) there is carried out a step (d1) or (e1) respectively in which a further component is introduced into the container. The further component may lie in or on the gel or gel precursor. Preferably, the further component is a solid form such as a pill. The further component may comprise a water-soluble or water-dispersible article. It may have a water-soluble polymeric skin containing active agents within.

(77) In one embodiment step (d) comprises pouring a gel precursor into the hollow formed in step (c), at which location gelation occurs.

(78) In another embodiment step (d) comprises locating a preformed gel in the hollow or forming the hollow with the preformed gel.

(79) A said further component may be located in the hollow before or after the gel or gel precursor is itself introduced into the hollow.

(80) Preferably, in step (e) the container and lid are sealed to each other, for example by adhesive (including water) or by heat sealing.

(81) According to a third aspect of the invention, there is provided a method of manufacturing a dosage element for a ware washing machine, the method comprising the steps of: (a) forming a sheet or film into a receptacle; (b) introducing a gel or gel precursor into the receptacle; (c) introducing a flowable particulate composition into the receptacle on top of the gel or gel precursor; and (e) closing the receptacle with a lid.

(82) Preferably step (c) is accomplished without compaction of the particulate material. That is, it remains a flowable particulate material i.e. it remains a non-consolidated particulate material which when not constrained by the receptacle is capable of flowing.

(83) Preferably, prior to step (b) or (c) there is carried out a step (b1) or (c1) respectively in which a further component is introduced into the container. The further component may lie under, on or wholly or partly within or on the gel or gel precursor as described further hereinabove. Preferably, the further component is a solid form such as a pill. The further component may comprise a water-soluble or water-dispersible article. It may have a water-soluble polymeric skin containing active agents within.

(84) Preferably, the receptacle is formed by thermoforming or injection molding.

(85) Preferably, in the second aspect the particulate composition is locally displaced by advancement and retraction of a probe or dibber. A suitable advancing pressure is 50 to 100 kPa. However use of a suitable preformed gel itself to locally displace the particulate composition is not excluded.

(86) Preferably, a mould comprises a plurality of cavities for forming a plurality of first parts at one time.

(87) Preferably, a second mould comprises a plurality of cavities for forming a plurality of second parts at one time.

(88) The methods preferably comprise the step of separating the completed dosage elements into individual dosage elements or into groups of dosage elements, for example 4-16 in number, which are packaged in such groups and are intended to be separated into individual dosage elements by the user.

(89) After the steps described above the dosage elements may be packaged.

(90) Preferably the steps described above define the manufacturing method fully; that is, there is preferably no further substantive manufacturing step. In particular there is for example preferably no step of setting the dosage elements face-to-face, for example by folding.

(91) The dosage element of the first aspect need not be made by the method of the second or third aspect. Nevertheless preferred aspects defined with reference to the second or third aspects may (unless not possible) be regarded as preferred aspects of the first aspect whether or not made by the method of the second/third aspects and vice-versa.

(92) However, the dosage element of the first aspect is preferably made by the method of the second or third aspect. In a fourth aspect of the invention there is provided a dosage element made by a method of the second or third aspect.

(93) According to a fifth aspect there is provided a method of ware washing in a machine, preferably a method of washing kitchenware in a dishwashing machine, using a dosage element of the first aspect. In this method the dosage element is wholly consumed in one wash cycle.

(94) All wall materials are water-soluble PVOH.

(95) Referring to FIGS. 1(a) through (h) there will now be described a dosage element in accordance with a first embodiment of the invention and a method of manufacture thereof.

(96) In FIG. 1(a) there is shown a casing 10 which forms an open pocket and sits within a thermoforming mould. It is filled with a first substance A which is a particulate composition, in which a depression may be formed, and remain.

(97) In FIG. 1(b) there is shown a next stage in the process of forming a dosage element. Here, a dibber 30 is used to approach the powder filled casing 10 and in step 1(c) to compact the powder and form a depression therein corresponding to the shape of the dibbing head 30. When the dibbing head 30 is removed in step 1(d), it can be seen that a hollow formation H is left.

(98) FIG. 1(e) shows the next step in the process, where a viscous gel precursor forming a substance B is poured or injected into the hollow H to form gel layer 40.

(99) FIGS. 1(f) and 1(g) show an optional procedure in which a pill 50 of a substance C is pressed into the gel layer 40 so as to sit in and on top of this gel layer.

(100) Finally, in FIG. 1(h) there is shown the procedure in which a lid 20, in the form of a top film, is added, following a cooling period, to cap and seal the casing 10.

(101) FIG. 2 shows a completed dosage element in accordance with the above construction.

(102) The preferred process, in detail, for forming a dosage element in accordance with the above construction is as described below in steps (A) through (G). (A) Forming the lower casing 10 as a primary component (bottom film) into a pocket, by thermoforming in the cavity of a thermoforming mould. A suitable forming temperature for the PVOH used is, for example, 120 C. The thickness of the film used to produce the pocket is preferably 90 to 120 m in this embodiment. A suitable forming vacuum is 0 to 2 kPa. (B) Introducing particulate composition A into the chamber formed by the lower casing 10. (C) Locally displacing particulate composition A with a dibber 20 in order to form depression H for a gel B. A suitable stamping pressure is especially 50 to 100 kPa depending on the particulate composition A used. (D) Pouring a precursor for gel B, preferably a gel/liquid, into the depression formed in step (c) to form a layer 40 and placing the further composition C preferably as a solid form such as a tablet 50, optionally PVOH coated, into the lower casing 10, preferably to be disposed in or on gel B. (E) Applying a film lid 20 over the casing, whilst still in the mould. The thickness of the PVOH film is 60 to 75 m in this embodiment. (F) Sealing the casing 10 and the top film 20 together. The films may be sealed together by any suitable means, for example by means of an adhesive or by heat sealing. Other methods of sealing include infra-red, radio frequency, ultrasonic, laser, solvent (such as water), vibration and spin welding. An adhesive such as an aqueous solution of PVOH may also be used. The seal desirably is water-soluble if the containers are water-soluble. If heat sealing is used, a suitable sealing temperature is for example 125 C. A suitable sealing pressure is especially 500 to 700 kPa depending on the heat sealing machine used. (G) Cutting the water-soluble article from neighbors with which it has been co-formed. Cutting may be effected by, for example, by HF or by mechanical punching).

(103) Whilst only the formation of a single dosage element has been discussed, it will be appreciated that the manufacturing process utilized will form tens or hundreds of such elements at a time using thermoforming moulds having a large plurality of pockets for forming multiple dosage elements and using continuous large thermoforming sheet materials which, only during the cutting step G, divide up the individual elements.

(104) Suitable chemical compositions are as follows. In these examples the powder is loaded into the receptacle. Next, the gel is loaded into the depression formed therein. Then, the pill is laid on top of the gel (see FIGS. 1 and 2).

Example 1

(105) Phosphate-containing composition and gel in one compartment having sodium percarbonate in a separate pill (Table 1 below) for use in an automatic dishwashing machine.

(106) TABLE-US-00001 TABLE 1 Powder Gel Pill Walls Raw Material (16.0 g) (2.5 g) (1.3 g) (0.4 g) Sodium tripolyphosphate 48.70 Sodium carbonate 16.00 Tri-sodium citrate 22.00 Phosphate speckles 4.00 Benzotriazol 0.40 HEDP 4 Na (88.5%) 0.30 Protease.sup.1 1.50 Amylase.sup.1- 1.00 1,2-Propylenediglycol 1.00 Perfume 0.10 Sulfonated polymer.sup.2 5.00 Glycerin 46.95 Gelatin 3.00 TAED 50.00 Dye 0.051 Percarbonate 100 PVOH (bottom film).sup.7 75 PVOH (top film).sup.8 25 100 100 100 100

Example 2

(107) Phosphate-containing composition and gel in one compartment having sodium percarbonate in a separate pill (Table 2 below) for use in an automatic dishwashing machine.

(108) TABLE-US-00002 TABLE 2 Powder Gel Pill Walls Raw Material (16.0 g) (2.5 g) (1.3 g) (0.4 g) Sodium tripolyphosphate 48.70 Sodium carbonate 16.00 Tri-sodium citrate 22.00 Phosphate speckles 4.00 Benzotriazol 0.40 HEDP 4 Na (88.5%) 0.30 Protease.sup.1 1.50 Amylase.sup.1- 1.00 1,2-Propylenediglycol 1.00 Perfume 0.10 Sulfonated polymer.sup.2 5.00 Solid surfactant 46.95 Polyglycol 10.00 TAED 43.00 Dye 0.05 Percarbonate 100 PVOH (bottom film).sup.7 67 PVOH (top film).sup.8 33 100 100 100 100

Example 3

(109) Phosphate-containing composition and gel in one compartment having a pressed pill adhered to the gel (Table 3 below) for use in an automatic dishwashing machine.

(110) TABLE-US-00003 TABLE 3 Powder Gel Pill Walls Raw Material (16.0 g) (2.5 g) (1.4 g) (0.3 g) Sodium tripolyphosphate 48.70 Sodium carbonate 16.00 Tri-sodium citrate 22.00 Phosphate speckles 4.00 Benzotriazol 0.40 HEDP 4 Na (88.5%) 0.30 Protease.sup.1 1.50 Amylase.sup.1- 1.00 1,2-Propylenediglycol 1.00 Perfume 0.10 Sulfonated polymer.sup.2 5.00 Solid Surfactant 46.95 Polyglycol 10.00 TAED 43.00 Dye 0.05 Lactose 20.00 Sodium CMC 18.00 Sodium bicarbonate 31.00 Citric acid 16.00 Protease.sup.1 8.00 HEDP 4 Na (88.5%) 2.00 Polyglycol 4.00 Mg-stearate 0.50 Dye 0.50 PVOH (bottom film).sup.7 67 PVOH (top film).sup.8 33 100 100 100 100

(111) A pill is manufactured by compressing the above pill formula with a compression of 1200 kg/cm.sup.2 (diameter 13.0 mm; height 8 mm; weight 1.4 g):

Example 4

(112) Zeolite-containing composition and gel in one compartment having pressed pill adhered to the gel (Table 4 below) for use in a laundry machine.

(113) TABLE-US-00004 TABLE 4 Powder Gel Pill Walls Raw Material (16.0 g) (2.5 g) (1.4 g) (0.3 g) LAS 12.58 Soap 1.24 Alkylsulfate 2.27 Phosphonate 0.58 Polymer 2.79 Zeolite 10.46 Sodium carbonate 26.81 Sodium sulfate 2.96 Sodium silicate 1.85 Amorphous silicate 8.75 Antifoam substance 0.47 Polyethyleneglycol 0.15 Amylase 0.26 Percarbonate 25.50 Optical brightener 0.29 Fragrance 0.26 Water 2.80 Solid surfactant 46.95 Polyglycol 10.00 TAED 43.00 Dye 0.05 Lactose 20.00 Sodium CMC 18.00 Sodium bicarbonate 31.00 Citric acid 16.00 Protease.sup.1 8.00 HEDP 4 Na (88.5%) 2.00 Polyglycol 4.00 Mg-stearate 0.50 Dye 0.50 PVOH (bottom film).sup.7 75 PVOH (top film).sup.8 25 100 100 100 100

(114) A pill is manufactured by compressing the above pill formula with a compression of 1200 kg/cm.sup.2 (diameter 13.0 mm; height 8 mm; weight 1.4 g):

Example 5

(115) Phosphate-containing composition and gel in one compartment having PAP in a separate compartment (Table 5 below) for use in an automatic dishwashing machine.

(116) TABLE-US-00005 TABLE 5 Powder Gel Pill Walls Raw Material (16.0 g) (2.5 g) (1.3 g) (0.4 g) Sodium tripolyphosphate 48.70 Sodium carbonate 16.00 Tri-sodium citrate 22.00 Phosphate speckles 4.00 Benzotriazol 0.40 HEDP 4 Na (88.5%) 0.30 Protease.sup.1 1.50 Amylase.sup.1- 1.00 1,2-Propylenediglycol 1.00 Perfume 0.10 Sulfonated polymer.sup.2 5.00 Glycerin 46.95 Gelatine 3.00 Sulfonated polymer.sup.2 50.00 Dye 0.05 PAP.sup.6 100 PVOH (bottom film).sup.7 75 PVOH (top film).sup.8 25 100 100 100 100 .sup.1Granules which contain approx. 3-10% active enzyme .sup.2AMPS co-polymer .sup.3Non-ionic low foaming surfactant .sup.4Mixed poly alkoxylate grade, P 41/12000, Clariant .sup.5Silicon oil .sup.6PAP with particle size (Q50% <15 pm) .sup.7PVOH foil, 90 pm, PT grade from Aicello .sup.8PVOH foil, 60 m, PT grade from Aicello .sup.9Sodium salt of methyl-glycine-diacetic acid

(117) The container used in this example has one compartment. The powder is delivered into the powder compartment. The gel mixture is heated to 65 C. and stirred for 20 min. Then the gel is mounted on top of the powder, a pill is positioned on the gel and the gel is allowed to chill. The insert in the examples is either a water soluble capsule comprising a PAP composition or percarbonate or could be a compressed pill. Finally the caps are sealed with PVOH film.

(118) In the PAP example the particle size of the PAP is suitably 0.01-100 pm (Q50%<15 pm).

(119) The dosage element as described above provides a very convenient and arrangement that is easy to manufacture and results in the production of different portions within a dosage element without there .being the need for extra separating walls or members to keep the integrity of the different components.