Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/02—Inorganic compounds
  • C11D7/04—Water-soluble compounds
  • C11D7/10—Salts
  • C11D7/16—Phosphates including polyphosphates
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/0065—Solid detergents containing builders
  • C11D17/0073—Tablets
  • C11D17/0078—Multilayered tablets
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3707—Polyethers, e.g. polyalkyleneoxides

Definitions

• the present invention is in the field of detergent tablets. More specifically, the invention encompasses a process for preparing a multiphase tablet.
• Machine dishwashing tablets are popular with the consumer as they have several advantages over powdered products in that they do not require measuring and they are compact and so easy to store.
• the present invention provides multiphase tablets, which are easy to produce and yet do not exhibit separation of the layers.
• the present invention provides a A process for producing a multiphase detergent tablet comprising the steps of:
• the process of the invention relate to any tablet having 3 or more phases however it is preferable if the process is for a table having 3 layers.
• the force used for the initial compaction pressure, (step a) is 5 kN or greater, preferably 10 kN or greater.
• the force used for the middle layers, (step b), is preferably 10 kN or greater more preferably 15 kN or greater, most preferably 20kN or greater.
• the compaction pressure for the initial compaction step a) and the middle compaction step b) is 60 kN or less, more preferably 45 kN or less, most preferably 35 kN or less.
• the compaction step for the middle layer is between 20 kN and 35 kN.
• the compaction pressure of step c) is substantially the same as step a) and a further compaction step d) is undertaken proceedings step c).
• the force of compaction step d) is at least double the force used for compaction step a).
• the final compaction step of the tablet may be conducted after the addition of the addition of the final composition.
• a pre-compaction step may be undertaken followed by a final compaction step.
• the force used for the final compaction is 50kN or greater, preferably 75kN or greater.
• the final compaction force should 200 kN or less, preferably 150 kN or less.
• the final force for compacting the tablet is from 100 to 150 kN.
• the tablets of the invention may be in any form suitable for addition to a washing or dishwasher machine.
• compositions for use with the process can be formulated such that different phases have different colors and different textures.
• the tablet of the invention is a triple phase tablet the phases being in the form of layers.
• the center layer comprises differing compositions to the outer layers of the tablet.
• the process of this invention works particularly well if a hydratable salt is present in center layer. It is also particularly preferred if the center layer has a polyethylene glycol present.
• the tablet has a strength from 50 to 300 Newton's (N) as measured on a MTS Synergie 100 using a loadcell of 500 N maximum capacity.
• the initial -and secondary crosshead speeds being set at 25 mm/min, with a deformation limit of 200%.
• the tablets of the invention preferably have a mass of greater than 8g, more preferably from 12 to 30g, most preferably 15 to 27g. Tablet with a mass of 20, 22 or 25g are particularly useful.
• Polyethylene glycol if present in the tablet preferably has a molecular weight from 1500 to 10,000, more preferably 3000 to 8000.
• the total level of polyethylene glycol in the tablet is from 5-wt% to 20 wt %of the total weight of the tablet, more preferably from 7 wt% to 15 wt% of the total weight of the tablet.
• polyethylene glycol is present it is preferable if at least 60 wt% of the polyethylene glycol is in a single phase, more preferably 75 wt% of the hydrocarbon ether, most preferably at least 90wt% of the hydrocarbon ether. If the tablet is a triple layer tablet it is preferable if the ratios cited in the preceding sentence apply to the middle layer.
• hydratable salt it is meant that the salt is in a state in which it may absorb additional water by hydration. That is to say that the salt is present either in its anhydrous form, or in a partially hydrated form.
• the hydratable salt is preferably particulate in nature and may, for example be alkali metal carbonate, bicarbonate, (poly) phosphate, citrate (anhydrous) or sulfate. Mixtures of two or more hydratable compounds may also be used, but preferably, sodium tripolyphosphate is used.
• compositions of the invention preferably comprise a water-soluble phosphate, typically contain this phosphate at a level of from 1 to 90% by weight, preferably from 10 to 80% by weight, most preferably from 20 to 80% by weight of the composition.
• water-soluble phosphates are the alkali metal tripolyphosphates, sodium, potassium and ammonium pyrophosphate, sodium and potassium orthophosphate, sodium polymeta/phosphate in which the degree of polymerization ranges from about 6 to 21, and salts of phytic acid. Sodium or potassium tripolyphosphate is most preferred.
• sodium tripolyphosphate with high Phase I Content is used.
• Sodium tripolyphosphate with high Phase I can be prepared by heating to above the transition temperature at which phase II anhydrous sodium polyphosphate is transformed into the phase I form.
• a process for the manufacture of particles containing a high proportion of the phase I form of sodium tripolyphosphate by spray drying below 420°C is given in US-A-4536377.
• Suitable material is commercially available. Suppliers include Rhodia, Courbevoie, France and Albright & Wilson, Warley, West Midlands, UK.
• the sodium tripolyphosphate should be partially hydrated, but the phase I anhydrous form should also be present.
• the sodium tripolyphosphate in the particles may incorporate up to 5% (by weight of the sodium tripolyphosphate in these particles) of water of hydration.
• the extent of hydration is desirably from 1% to 4% or 5% by weight. This degree of hydration in general means that the sodium tripolyphosphate is partially hydrated.
• the sodium tripolyphosphate in these particles is preferably hydrated by a process that leads to a homogeneous distribution of the water of hydration within the tripolyphosphate.
• the bulk density of the of sodium tripolyphosphate particles is preferably 0.75 Kg/M 3 or less, more preferably from 0.52 to 0.72 Kg/M 3 .
• the tablet has more than one phase that from 10 wt% to 30 wt% of the total level of phosphate present in the tablet is present in the phase comprising the higher level of polyethylene glycol.
• compositions of the invention may contain a non-hydratable builder in addition to the hydratable salt.
• a non-hydratable builder in addition to the hydratable salt.
• the ratio of hydratable salt to non-hydratable builder is at least 2:1, more preferably 3:1.
• the non-hydratable builder is present in a separate phase to the solid hydrocarbon poly ether, especially if the solid hydrocarbon polyether is a polethylene glycol.
• the non-hydratable builder is preferably present from 1 to 50% by weight, more preferably from 5 to 30% by weight of the composition.
• Suitable examples of non-phosphorus-containing inorganic builders include water-soluble alkali metal, borates, and silicates, including layered silicates such as SKS-6 ex. Hoechst, metasilicates, and crystalline and amorphous aluminosilicates, silicates including layered silicates and zeolites.
• Organic detergent builders can also be used as nonphosphate builders in the present invention.
• organic builders include alkali metal citrates, succinates, malonates, fatty acid sulfonates, fatty acid carboxylates, nitrilotriacetates, oxydisuccinates, alkyl and alkenyl disuccinates, oxydiacetates, carboxymethyloxy succinates, ethylenediamine tetraacetates, tartrate monosuccinates, tartrate disuccinates, tartrate monoacetates, tartrate diacetates, oxidized starches, oxidized heteropolymeric polysaccharides, polyhydroxysulfonates, polycarboxylates such as polyacrylates, polymaleates, polyacetates, polyhydroxyacrylates, polyacrylate/polymaleate and polyacrylate/ polymethacrylate copolymers, acrylate/maleate/vinyl alcohol terpolymers, aminopolycarboxylates and polyacetal carboxylate
• Such carboxylates are described in U.S. Patent Nos. 4,144,226, 4,146,495 and 4,686,062.
• Alkali metal citrates, nitrilotriacetates, oxydisuccinates, acrylate/maleate copolymers and acrylate/maleate/vinyl alcohol terpolymers are especially preferred nonphosphate builders.
• the composition optionally comprises alkali metal silicates.
• the SiO 2 level should be from 1% to 25%, preferably from 2% to 20%, more preferably from 3% to 10%, based on the weight of the ADD.
• the alkali metal silicate is hydrous, having from 15% to 25% water, more preferably, from 17% to 20%.
• the highly alkali metasilicates can in general be employed, although the less alkaline hydrous alkali metal silicates having a SiO 2 :M 2 O ratio of from 2.0 to 2.4 are, as noted, greatly preferred.
• Anhydrous forms of the alkali metal silicates with a SiO 2 :M 2 O ratio of 2.0 or more are also less preferred because they tend to be significantly less soluble than the hydrous alkali metal silicates having the same ratio.
• Sodium and potassium, and especially sodium, silicates are preferred.
• Enzymes may be present in the compositions of the invention.
• Examples of enzymes suitable for use in the cleaning compositions of this invention include lipases, peptidases, amylases (amylolytic enzymes) and others which degrade, alter or facilitate the degradation or alteration of biochemical soils and stains encountered in cleansing situations so as to remove more easily the soil or stain from the object being washed to make the soil or stain more removable in a subsequent cleansing step. Both degradation and alteration can improve soil removal.
• the enzymes most commonly used in machine dishwashing compositions are amylolytic enzymes.
• the composition of the invention also contains a proteolytic enzyme. Enzymes may be present in a weight percentage amount of from 0.2 to 5% by weight.
• amylolytic enzymes the final composition will have amylolytic activity of from 10 2 to 10 6 Maltose units/kg.
• proteolytic enzymes the final composition will have proteolytic enzyme activity of from 10 6 to 10 9 Glycine Units/kg.
• Bleach material may optionally and preferably be incorporated in composition for use in processes according to the present invention. These materials may be incorporated in solid form or in the form of encapsulates and less preferably in dissolved form.
• the level of bleach material is preferably greater than 0.5 wt% of a bleaching material.
• the bleach material may be a chlorine- or bromine-releasing agent or a peroxygen compound. Peroxygen based bleach materials are however preferred.
• the peroxyacids usable in the present invention are solid and, preferably, substantially water-insoluble compounds.
• substantially water-insoluble is meant herein a water-solubility of less than about 1% by weight at ambient temperature.
• peroxyacids containing at least about 7 carbon atoms are sufficiently insoluble in water for use herein.
• Inorganic peroxygen-generating compounds are also typically used as the bleaching material of the present invention.
• these materials are salts of monopersulphate, perborate monohydrate, perborate tetrahydrate, and percarbonate.
• Monoperoxy acids useful herein include alkyl peroxy acids and aryl peroxyacids such as peroxybenzoic acid and ring-substituted peroxybenzoic acids (e.g. peroxy-alphanaphthoic acid); aliphatic and substituted aliphatic monoperoxy acids (e.g. peroxylauric acid and peroxystearic acid) and phthaloyl amido peroxy caproic acid (PAP).
• alkyl peroxy acids and aryl peroxyacids such as peroxybenzoic acid and ring-substituted peroxybenzoic acids (e.g. peroxy-alphanaphthoic acid); aliphatic and substituted aliphatic monoperoxy acids (e.g. peroxylauric acid and peroxystearic acid) and phthaloyl amido peroxy caproic acid (PAP).
• diperoxy acids useful herein include alkyl diperoxy acids and aryldiperoxy acids, such as 1,12-di-peroxydodecanedioic acid (DPDA); 1,9-diperoxyazelaic acid, diperoxybrassylic acid, diperoxysebacic acid and diperoxyisophthalic acid; and 2-decyldiperoxybutane-1,4-dioic acid.
• DPDA 1,12-di-peroxydodecanedioic acid
• 1,9-diperoxyazelaic acid diperoxybrassylic acid, diperoxysebacic acid and diperoxyisophthalic acid
• 2-decyldiperoxybutane-1,4-dioic acid 2-decyldiperoxybutane-1,4-dioic acid.
• Peroxyacid bleach precursors are well known in the art. As non-limiting examples can be named N,N,N',N'-tetraacetyl ethylene diamine (TAED), sodium nonanoyloxybenzene sulphonate (SNOBS), sodium benzoyloxybenzene sulphonate (SBOBS) and the cationic peroxyacid precursor (SPCC) as described in US-A-4,751,015.
• TAED N,N,N',N'-tetraacetyl ethylene diamine
• SNOBS sodium nonanoyloxybenzene sulphonate
• SBOBS sodium benzoyloxybenzene sulphonate
• SPCC cationic peroxyacid precursor
• a bleach catalyst such as the manganese complex, e.g. Mn-Me TACN, as described in EP-A-0458397, or the sulphonimines of US-A-5,041,232 and US-A-5,047,163, is to be incorporated, this may be presented in the form of a second encapsulate separately from the bleach capsule or granule. Cobalt catalysts can also be used.
• suitable reactive chlorine- or bromine-oxidizing materials are heterocyclic N-bromo and N-chloro imides such as trichloroisocyanuric, tribromoisocyanuric, dibromoisocyanuric and dichloroisocyanuric acids, and salts thereof with water-solubilizing cations such as potassium and sodium.
• Hydantoin compounds such as 1,3-dichloro-5,5-dimethyl-hydantoin are also quite suitable.
• Particulate, water-soluble anhydrous inorganic salts are likewise suitable for use herein such as lithium, sodium or calcium hypochlorite and hypobromite.
• Chlorinated trisodium phosphate and chloroisocyanurates are also suitable bleaching materials.
• Encapsulation techniques are known for both peroxygen and chlorine bleaches, e.g. as described in US-A-4,126,573, US-A-4,327,151, US-A-3,983,254, US-A-4,279,764, US-A-3,036,013 and EP-A-0,436,971 and EP-A-0,510,761.
• encapsulation techniques are particularly useful when using halogen based bleaching systems.
• the tablet has more than one phase it is highly desirable if the bleach and the bleach catalyst is in a separate phase to the colouring agent.
• a surfactant system comprising a surfactant selected from nonionic, anionic, cationic, ampholytic and zwitterionic surfactants and mixtures thereof is preferably present in the composition.
• the surfactant is a low to non foaming nonionic surfactant, which includes any alkoxylated nonionic surface-active agent wherein the alkoxy moiety is selected from the group consisting of ethylene oxide, propylene oxide and mixtures thereof, is preferably used to improve the detergency without excessive foaming.
• an excessive proportion of nonionic surfactant should be avoided.
• nonionic surfactants for use in the invention are the low- to non-foaming ethoxylated straight-chain alcohols of the Plurafac® RA series, supplied by the Eurane Company; of the Lutensol® LF series, supplied by the BasF Company and of the Triton® DF series, supplied by the Rohm & Haas Company.
• anionic surfactant may be used but may require the additional presence of antifoam to surpress foaming. If an anionic surfactant is used it is advantageously present at levels of 2 wt% or below.
• a water-soluble polymeric polycarboxylic compound is advantageously present in the dish wash composition.
• these compounds are homo- or co-polymers of polycarboxylic compounds, especially co-polymeric compounds in which the acid monomer comprises two or more carboxyl groups separated by not more than two carbon atoms. Salts of these materials can also be used.
• Particularly preferred polymeric polycarboxylates are co-polymers derived from monomers of acrylic acid and maleic acid.
• the average molecular weight of these polymers in the acid form preferably ranges from 4,000 to 70,000.
• polymeric polycarboxylic compounds suitable for use in the composition of the invention are homopolymeric polycarboxylic acid compounds with acrylic acid as the monomeric unit.
• the average weight of such homopolymers in the acid form preferably ranges from 1,000 to 100,000 particularly from 3,000 to 10,000.
• Acrylic sulphonated polymers as described in EP 851 022 (Unilever) are also suitable.
• this polymeric material is present at a level of at least 0.1%, more preferably at levels from 1 wt% to 7 wt% of the total composition.
• a chelating agent may be present in the composition. If present it is preferable if the level of chelating agent is from 0.5 to 3-wt% of the total composition.
• Preferred chelating agents include organic phosphonates, amino carboxylates, polyfunctionally-substituted compounds, and mixtures thereof.
• Particularly preferred chelating agents are organic phosphonates such as ⁇ -hydroxy-2 phenyl ethyl diphosphonate, ethylene diphosphonate, hydroxy 1,1-hexylidene, vinylidene 1,1 diphosphonate, 1,2 dihydroxyethane 1,1 diphosphonate and hydroxy-ethylene 1,1 diphosphonate. Most preferred is hydroxy-ethylene 1,1 diphosphonate (EHDP).
• Anti-tarnishing agents such as benzotriazole and those described in EP 723 577 (Unilever) may also be included.
• Optional ingredients are, for example, buffering agents, reducing agents, e.g., borates, alkali metal hydroxide and the well-known enzyme stabilisers such as the polyalcohols, e.g. glycerol and borax; anti-scaling agents; crystal-growth inhibitors, threshold agents; thickening agents and perfumes and the like.
• buffering agents reducing agents, e.g., borates, alkali metal hydroxide and the well-known enzyme stabilisers such as the polyalcohols, e.g. glycerol and borax; anti-scaling agents; crystal-growth inhibitors, threshold agents; thickening agents and perfumes and the like.
• reducing agents e.g., borates, alkali metal hydroxide
• the well-known enzyme stabilisers such as the polyalcohols, e.g. glycerol and borax
• anti-scaling agents e.g. glycerol and borax
• Reducing agents may e.g. be used to prevent the appearance of an enzyme-deactivating concentration of oxidant bleach compound.
• Suitable agents include reducing sulphur-oxy acids and salts thereof.
• Most preferred for reasons of availability, low cost, and high performance are the alkali metal and ammonium salts of sulphuroxy acids including ammonium sulphite ((NH 4 ) 2 SO 3 ), sodium sulphite (Na 2 SO 3 ), sodium bisulphite (NaHSO 3 ), sodium metabisulphite (Na 2 S 2 O 3 ), potassium metabisulphite (K 2 S 2 O 5 ), lithium hydrosulphite (Li 2 S 2 O 4 ), etc., sodium sulphite being particularly preferred.
• Another useful reducing agent is ascorbic acid.
• the amount of reducing agents to be used may vary from case to case depending on the type of bleach and the form it is in, but normally a range of about 0.01% to about 1.0% by weight, preferably from about 0.02% to about 0.5% by weight, will be sufficient.
• the pH of the wash liquor at ambient temperature is higher than 6.5, more preferably 7.5 or higher, most preferably 8.5 or higher.
• the pH is lower than 12, more preferably lower than 11.
• Example 1 (wt%) Sodium tripolyphosphate (partially hydrated) 56 Sodium citrate - Hydrated - Na disilicate 9 Na carbonate 16 Nonionic detergent 6 Na perborate 17 TAED 3 Manganese Catalyst 1.1 Sodium polyacrylate 3.7 Enzyme 4.5 Minors to 100%
• a particulate composition for making the middle layer was made by mixing the following ingredients
• the tablet had identical top and bottom layer of the first composition. Sandwiched between them was a thin middle layer of the second composition.
• step iii) above was replaced by the following process iv):
• the tablets were easy to manufacture and handled well without separation of the layers.

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Cited By (4)

Citations (4)

• 2001
  • 2001-03-05 EP EP01301981A patent/EP1239028A1/de not_active Withdrawn

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