WO2000002994A1 - Detergent tablet with high mechanical and dissolution characteristics - Google Patents
Detergent tablet with high mechanical and dissolution characteristics Download PDFInfo
- Publication number
- WO2000002994A1 WO2000002994A1 PCT/US1999/015676 US9915676W WO0002994A1 WO 2000002994 A1 WO2000002994 A1 WO 2000002994A1 US 9915676 W US9915676 W US 9915676W WO 0002994 A1 WO0002994 A1 WO 0002994A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- tablet
- particulate material
- highly soluble
- acid
- soluble compound
- Prior art date
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 58
- 238000004090 dissolution Methods 0.000 title description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 74
- 239000011236 particulate material Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 37
- 230000000694 effects Effects 0.000 claims abstract description 27
- 239000004094 surface-active agent Substances 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims description 106
- -1 hydrotrope compound Chemical class 0.000 claims description 24
- 239000003752 hydrotrope Substances 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 claims description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 13
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- 239000003826 tablet Substances 0.000 description 155
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 41
- 239000007844 bleaching agent Substances 0.000 description 39
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- 125000000129 anionic group Chemical group 0.000 description 13
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- 125000003118 aryl group Chemical group 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
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- 239000001509 sodium citrate Substances 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 235000019351 sodium silicates Nutrition 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 229920005613 synthetic organic polymer Polymers 0.000 description 1
- 239000002700 tablet coating Substances 0.000 description 1
- 238000009492 tablet coating Methods 0.000 description 1
- 108010075550 termamyl Proteins 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- MSLRPWGRFCKNIZ-UHFFFAOYSA-J tetrasodium;hydrogen peroxide;dicarbonate Chemical compound [Na+].[Na+].[Na+].[Na+].OO.OO.OO.[O-]C([O-])=O.[O-]C([O-])=O MSLRPWGRFCKNIZ-UHFFFAOYSA-J 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
- 239000005019 zein Substances 0.000 description 1
- 229940093612 zein Drugs 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/3418—Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates
-
- 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
-
- 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
- C11D3/0005—Other compounding ingredients characterised by their effect
-
- C11D2111/12—
Definitions
- the present invention relates to detergent tablets, especially those adapted for use in washing.
- cleaning compositions in tablet form have often been proposed, these have not (with the exception of soap bars for personal washing) gained any substantial success, despite the several advantages of products in a unit dispensing form.
- One of the reasons for this may be that detergent tablets usually dissolve slower than the constituent powders from which they are made, simply because the constituent powders are forced close together in the tablet, with comparatively little opportunity for water to permeate between them. This gives rise to the problem that slow dissolving tablets cause residues which may for example be visible through the door of the washing machine during the wash cycle, or which stick to the fabrics at the end of the wash cycle, or both.
- EP-A-0 711 827 published on the 5 th of May 1996, discloses laundry detergent tablets containing a highly water-soluble material which improves disintegration of the whole tablet and dissolution of its soluble ingredients.
- the object of the present invention is to provide tablets formed by compressing a particulate material, the particulate material comprising a surfactant, the tablet being suitable for storing, shipping and handling without breakage while dissolving easily and rapidly in wash solution, releasing the active ingredients into the wash solution and completely disintegrating and dispersing in alkaline or surfactant-rich solutions such as the wash liquor.
- the object of the invention is achieved by providing a tablet of the above mentioned kind, whereby the particulate material further comprises a highly soluble compound, the highly soluble compound having a cohesive effect on the particulate material.
- a method is provided of preparing an aqueous solution of a laundry detergent for use in a washing machine, wherein the aqueous solution of laundry detergent is formed by dissolving in water a tablet formed by compressing a particulate material, the tablet comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesive effect on the particulate material.
- the invention relates to a highly soluble compound having a cohesive effect on the particulate material.
- the invention relates to a highly soluble compound.
- a highly soluble compound is defined as follow:
- a solution is prepared as follows comprising de-ionised water as well as 20 grams per litre of a specific compound: 1- 20 g of the specific compound is placed in a Sotax Beaker. This beaker is placed in a constant temperature bath set at 10°C. A stirrer with a marine propeller is placed in the beaker so that the bottom of the stirrer is at 5 mm above the bottom of the Sotax beaker. The mixer is set at a rotation speed of 200 turns per minute.
- Step 3 is repeated after 20, 30, 40, 50, 1 min, 2 min, 5 min and 10 min after step 2.
- the specific compound is highly soluble according to the invention when the conductivity of the solution reaches 80% of its maximum value in less than 10 seconds, starting from the complete addition of the de-ionised water to the compound. Indeed, when monitoring the conductivity in such a manner, the conductivity reaches a plateau after a certain period of time, this plateau being considered as the maximum value.
- a compound is preferably in the form of a flowable material constituted of solid particles at temperatures comprised between 10 and 80°Celsius for ease of handling, but other forms may be used such as a paste or a liquid.
- Example of highly soluble compounds include Sodium di isoalkylbenzene sulphonate or Sodium toluene sulphonate.
- the Cohesive Effect on the particulate material of a detergent matrix is characterised by the force required to break a tablet based on the examined detergent matrix pressed under controlled compression conditions. For a given compression force, a high tablet strength indicates that the granules stuck highly together when they were compressed, so that a strong cohesive effect is taking place.
- Means to assess tablet strength are given in Pharmaceutical dosage forms : tablets volume 1 Ed. H.A. Lieberman et al, published in 1989.
- the cohesive effect induced by the highly soluble compound is measured according to the invention by comparing the tablet strength of the original base powder without highly soluble compound with the tablet strength of a powder mix which comprises 97 parts of the original base powder and 3 parts of the highly soluble compound.
- the highly soluble compound is added to the matrix in a form in which it is substantially free of water (water content below 10% (pref. below 5%)).
- the temperature of the addition is between 10 and 80C, more pref. between 10 and 40C.
- a highly soluble compound is defined as having a cohesive effect on the particulate material according to the invention when at a given compacting force of 3000N, tablets with a weight of 50g of detergent particulate material and a diameter of 55mm have their tablet tensile strength increased by over 30% (preferably 60 and more preferably 100%) by means of the presence of 3% of the highly soluble compound having a cohesive effect in the base particulate material.
- An example of a compond having a cohesive effect is Sodium di isoalkylbenzene sulphonate.
- a highly soluble compound having a cohesive effect on the particulate material according to the invention to a tablet formed by compressing a particulate material comprising a surfactant, the dissolution of the tablet in an aqueous solution was significantly increased.
- at least 1 % per weight of the tablet is formed from the highly soluble compound, more preferably at least 2%, even more preferably at lest 3% and most preferably at least 5% per weight of the tablet being formed from the highly soluble compound having a cohesive effect on the particulate material.
- a composition comprising a highly soluble compound as well as a surfactant is disclosed in EP-A-0 524 075, this composition being a liquid composition.
- the highly soluble compound having a cohesive effect on the particulate material allows to obtain a tablet having a higher tensile strength at constant compacting force or an equal tensile strength at lower compacting force when compared to traditional tablets.
- the tablet will have a tensile strength of more than 5kPa, preferably of more than 10kPa, more preferably, in particular for use in laundry applications, of more than 15kPa, even more preferably of more than 30 kPa and most preferably of more than 50 kPa, in particular for use in dish washing or auto dish washing applications; and a tensile strength of less than 300 kPa, preferably of less than 200 kPa, more preferably of less than 100 kPa, even more preferably of less than 80 kPa and most preferably of less than 60 kPa.
- the tablets should be less compressed than in case of auto dish washing applications for example, whereby the dissolution is more readily achieved, so that in a laundry application, the tensile strength is preferably of less than 30 kPa.
- Detergent tablets of the present invention can be prepared simply by mixing the solid ingredients together and compressing the mixture in a conventional tablet press as used, for example, in the pharmaceutical industry.
- the principal ingredients in particular gelling surfactants, are used in particulate form.
- Any liquid ingredients, for example surfactant or suds suppressor, can be incorporated in a conventional manner into the solid particulate ingredients.
- the ingredients such as builder and surfactant can be spray-dried in a conventional manner and then compacted at a suitable pressure.
- the tablets according to the invention are compressed using a force of less than 100000N, more preferably of less than 50000N, even more preferably of less than 5000N and most preferably of less than 3000 N.
- the most preferred embodiment is a tablet suitable for laundry compressed using a force of less than 2500N, but tablets for auto dish washing may also be considered for example, whereby such auto dish washing tablets are usually more compressed than laundry tablets.
- the particulate material used for making the tablet of this invention can be made by any particulation or granulation process.
- An example of such a process is spray drying (in a co-current or counter current spray drying tower) which typically gives low bulk densities 600g/l or lower.
- Particulate materials of higher density can be prepared by granulation and densification in a high shear batch mixer/granulator or by a continuous granulation and densification process (e.g. using Lodige® CB and/or Lodige® KM mixers).
- Other suitable processes include fluid bed processes, compaction processes (e.g. roll compaction), extrusion, as well as any particulate material made by any chemical process like flocculation, crystallisation sentering, etc.
- Individual particles can also be any other particle, granule, sphere or grain.
- the components of the particulate material may be mixed together by any conventional means. Batch is suitable in, for example, a concrete mixer, Nauta mixer, ribbon mixer or any other. Alternatively the mixing process may be carried out continuously by metering each component by weight on to a moving belt, and blending them in one or more drum(s) or mixer(s).
- Non-gelling binder can be sprayed on to the mix of some, or all of, the components of the particulate material.
- Other liquid ingredients may also be sprayed on to the mix of components either separately or premixed. For example perfume and slurries of optical brighteners may be sprayed.
- a finely divided flow aid dustting agent such as zeolites, carbonates, silicas
- the tablets may be manufactured by using any compacting process, such as tabletting, briquetting, or extrusion, preferably tabletting.
- Suitable equipment includes a standard single stroke or a rotary press (such as Courtoy®, Korch®,
- the tablets prepared according to this invention preferably have a diameter of between 20mm and 60mm, preferably of at least 35 and up to 55 mm, and a weight between 25 and 100 g.
- the ratio of height to diameter (or width) of the tablets is preferably greater than 1 :3, more preferably greater than 1 :2.
- the compaction pressure used for preparing these tablets need not exceed 100000 kN/m 2 , preferably not exceed 30000 kN/m 2 , more preferably not exceed 5000 kN/m 2 , even more preferably not exceed 3000kN/m 2 and most preferably not exceed 1000kN/m 2 .
- the tablet has a density of at least 0.9 g/cc, more preferably of at least 1.0 g/cc, and preferably of less than 2.0 g/cc, more preferably of less than 1.5 g/cc, even more preferably of less than 1.25 g/cc and most preferably of less than 1.1 g/cc.
- the highly soluble compound having a cohesive effect is a hydrotrope compound, a specific compound being defined as being hydrotrope as follows (see S.E. Friberg and M. Chiu, J. Dispersion Science and Technology, 9(5&6), pages 443 to 457, (1988-1989)):
- a solution is prepared comprising 25% by weight of the specific compound and 75% by weight of water.
- Octanoic Acid is thereafter added to the solution in a proportion of 1.6 times the weight of the specific compound in solution, the solution being at a temperature of 20°Celsius.
- the solution is mixed in a Sotax beaker with a stirrer with a marine propeller, the propeller being situated at about 5mm above the bottom of the beaker, the mixer being set at a rotation speed of 200 rounds per minute.
- the specific compound is hydrotrope if the the Octanoic Acid is completely solubilised, i.e . if the solution comprises only one phase, the phase being a liquid phase.
- the hydrotrope compound is a flowable material made of solid particles at operating conditions between 15 and 60° Celsius.
- Hydrotrope compounds include the compounds listed thereafter:
- Compounds of interest also include:
- Anionic hydrotropes such as alkali metal aryl sulfonates. This includes alkali metal salts of benzoic acid, salicylic acid, bezenesulfonic acid and its many derivatives, naphthoic acid and various hydroaromatic acids.
- dialkyl benzene sulfonic acid such as salts of di- isopropyl benzene sulfonic acid, ethyl methyl benzene sulfonic acid, alkyl benzene sulfonic acid with an alkyl chain length with 3 to 10, (pref. 4 to 9), linear or branched alkyl sulfonates with an alkyl chain with 1 to 18 carbons.
- Solvent hydrotropes such as alkoxylated glycerines and alkoxylated glycerides, esters slakoxylated glycerines, alkoxylated fatty acids, esters of glycerin, polyglycerol esters.
- Preferred alkoxylated glycerines have the following structure:
- R represents H, CH 3 or
- Preferred alkoxylated glycerides have the following struture
- C2H 5 and I is a number from 1 to about 60, n is a number from about 6 to about
- E is a hydrophilic functional group
- R is H or a C1-C10 alkyl group or is a hydrophilic functional group
- R1 is H a lower alkyl group or an aromatic group
- R2 is H or a cyclic alkyl or aromatic group.
- the polymer typically has a molecular weight of between about 1000 and
- Such compound would further increase the dissolution rate of the tablet, as a hydrotrope compound facilitates dissolution of surfactants, for example.
- a hydrotrope compound facilitates dissolution of surfactants, for example.
- Such a compound could be formed from a mixture or from a single compound.
- Solidity of the tablet according to the invention may be further improved by making a coated tablet, the coating covering a non-coated tablet according to the invention, thereby further improving the mechanical characteristics of the tablet while maintaining or further improving dissolution.
- the tablets may then be coated so that the tablet does not absorb moisture, or absorbs moisture at only a very slow rate.
- the coating is also strong so that moderate mechanical shocks to which the tablets are subjected during handling, packing and shipping result in no more than very low levels of breakage or attrition.
- the coating is preferably brittle so that the tablet breaks up when subjected to stronger mechanical shock.
- the coating material is dissolved under alkaline conditions, or is readily emulsified by surfactants.
- Water solubility is measured following the test protocol of ASTM E1148-87 entitled, "Standard Test Method for Measurements of Aqueous Solubility".
- Suitable coating materials are dicarboxylic acids.
- Particularly suitable dicarboxylic acids are selected from the group consisting of oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and mixtures thereof.
- the coating material has a melting point preferably of from 40 °C to 200 °C.
- the coating can be applied in a number of ways. Two preferred coating methods are a) coating with a molten material and b) coating with a solution of the material.
- the coating material is applied at a temperature above its melting point, and solidifies on the tablet.
- the coating is applied as a solution, the solvent being dried to leave a coherent coating.
- the substantially insoluble material can be applied to the tablet by, for example, spraying or dipping. Normally when the molten material is sprayed on to the tablet, it will rapidly solidify to form a coherent coating. When tablets are dipped into the molten material and then removed, the rapid cooling again causes rapid solidification of the coating material.
- substantially insoluble materials having a melting point below 40 °C are not sufficiently solid at ambient temperatures and it has been found that materials having a melting point above about 200 °C are not practicable to use.
- the materials melt in the range from 60 °C to 160 °C, more preferably from 70 °C to 120 °C.
- melting point is meant the temperature at which the material when heated slowly in, for example, a capillary tube becomes a clear liquid.
- a coating of any desired thickness can be applied according to the present invention. For most purposes, the coating forms from 1 % to 10%, preferably from 1.5% to 5%, of the tablet weight.
- the tablet coatings of the present invention are very hard and provide extra strength to the tablet.
- the fracture of the coating in the wash is improved by adding a disintegrant in the coating.
- This disintegrant will swell once in contact with water and break the coating in small pieces. This will improve the dissolution of the coating in the wash solution.
- the disintegrant is suspended in the coating melt at a level of up to 30%, preferably between 5% and 20%, most preferably between 5 and 10% by weight. Possible disintegrants are described in Handbook of Pharmaceutical Excipients (1986).
- Suitable disintegrants include starch: natural, modified or pregelatinized starch, sodium starch gluconate; gum: agar gum, guar gum, locust bean gum, karaya gum, pectin gum, tragacanth gum; croscarmylose Sodium, crospovidone, cellulose, carboxymethyl cellulose, algenic acid and its salts including sodium alginate, silicone dioxide, clay, polyvinylpyrrolidone, soy polysacharides, ion exchange resins and mixtures thereof.
- the used compacting force may be adjusted to not affect the tensile strength, and the disintegration time in the washing machine.
- This process may be used to prepare homogenous or layered tablets of any size or shape.
- F is the maximum force (Newton) to cause tensile failure (fracture) measured by a VK 200 tablet hardness tester supplied by Van Kell industries, Inc.
- D is the diameter of the tablet, and t the thickness of the tablet.
- a tablet having a diametral fracture stress of less than 20 kPa is considered to be fragile and is likely to result in some broken tablets being delivered to the consumer.
- a diametral fracture stress of at least 25 kPa is preferred. This applies similarly to non cylindrical tablets, to define the tensile strength, whereby the cross section normal to the height of the tablet is non round, and whereby the force is applied along a direction perpendicular to the direction of the height of the tablet and normal to the side of the tablet, the side being perpendicular to the non round cross section.
- the rate of dispensing of a detergent tablet can be determined in the following way:
- the water supply to the washing machine is set to a temperature of 20 °C and a hardness of 21 grains per gallon, the dispenser water inlet flow-rate being set to 8 l/min.
- the level of tablet residues left in the dispenser is checked by switching the washing on and the wash cycle set to wash program 4 (white/colors, short cycle).
- the dispensing percentage residue is determined as follows:
- % dispensing residue weight x 100 / original tablet weight
- the level of residues is determined by repeating the procedure 10 times and an average residue level is calculated based on the ten individual measurements.
- the tablets further comprises an effervescent.
- Effervescency as defined herein means the evolution of bubbles of gas from a liquid, as the result of a chemical reaction between a soluble acid source and an alkali metal carbonate, to produce carbon dioxide gas, i.e. C6H 8 O 7 + 3NaHCO 3 ⁇ * • Na 3 C 6 H 5 O 7 + 3C02 + 3H 2 O
- An effervescent may be added to the tablet mix in addition to the detergent ingredients.
- the addition of this effervescent to the detergent tablet improves the disintegration time of the tablet.
- the amount will preferably be between 5 and 20 % and most preferably between 10 and 20% by weight of the tablet.
- the effervescent should be added as an agglomerate of the different particles or as a compact, and not as separated particles. Due to the gas created by the effervescency in the tablet, the tablet can have a higher D.F.S. and still have the same disintegration time as a tablet without effervescency. When the D.F.S. of the tablet with effervescency is kept the same as a tablet without, the disintegration of the tablet with effervescency will be faster.
- dissolution aid could be provided by using compounds such as sodium acetate or urea.
- suitable dissolution aid may also be found in Pharmaceutical Dosage Forms: Tablets, Volume 1 , Second edition, Edited by H.A. Lieberman et all, ISBN 0-8247-8044-2.
- Surfactant are comprised in the tablet according to the invention.
- the dissolution of surfactants is favoured by the addition of the highly soluble compound.
- Nonlimiting examples of surfactants useful herein typically at levels from about
- LAS C-j -j_C-
- AS primary, branched-chain and random C10- 20 alkyl sulfates
- M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, the C10-C18 al M alkoxy sulfates ("AE X S"; especially EO 1-7 ethoxy sulfates), C10-C18 a, kyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C-
- AE X S especially EO 1-7 ethoxy sulfates
- C10-C18 a kyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates)
- Q-18 glycerol ethers the C-10-
- the conventional nonionic and amphoteric surfactants such as the C- ⁇ 2 _C-
- 8 N-alkyl polyhydroxy fatty acid amides can also be used.
- Typical examples include the C 12-Cl8 N-methylglucamides. See WO 9,206,154.
- Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C-
- rj-C 2 o conventional soaps may also be used. If high sudsing is desired, the branched-chain C ⁇
- the tablet comprises at least 5% per weight of surfactant, more preferably at least 15% per weight, even more preferably at least 25% per weight, and most preferably between 35% and 45% per weight of surfactant.
- Non gelling binders can be integrated to the particles forming the tablet in order to further facilitate dissolution.
- suitable non-gelling binders include synthetic organic polymers such as polyethylene glycols, polyvinylpyrrolidones, polyacrylates and water-soluble acrylate copolymers.
- binders classification Acacia, Alginic Acid, Carbomer, Carboxymethylcellulose sodium, Dextrin, Ethylcellulose, Gelatin, Guar gum, Hydrogenated vegetable oil type I, Hydroxyethyl cellulose, Hydroxypropyl methylcellulose, Liquid glucose, Magnesium aluminum silicate, Maltodextrin, Methylcellulose, polymethacrylates, povidone, sodium alginate, starch and zein.
- binders also have an active cleaning function in the laundry wash such as cationic polymers, i.e. ethoxylated hexamethylene diamine quaternary compounds, bishexamethylene triamines, or others such as pentaamines, ethoxylated polyethylene amines, maleic acrylic polymers.
- Non-gelling binder materials are preferably sprayed on and hence have an appropriate melting point temperature below 90°C, preferably below 70°C and even more preferably below 50°C so as not to damage or degrade the other active ingredients in the matrix.
- non-aqueous liquid binders i.e. not in aqueous solution
- they may also be solid binders incorporated into the matrix by dry addition but which have binding properties within the tablet.
- Non-gelling binder materials are preferably used in an amount within the range from 0.1 to 15% of the composition, more preferably below 5% and especially if it is a non laundry active material below 2% by weight of the tablet. It is preferred that gelling binders, such as nonionic surfactants are avoided in their liquid or molten form. Nonionic surfactants and other gelling binders are not excluded from the compositions, but it is preferred that they be processed into the detergent tablets as components of particulate materials, and not as liquids.
- Detergent builders can optionally be included in the compositions herein to assist in controlling mineral hardness. Inorganic as well as organic builders can be used. Builders are typically used in fabric laundering compositions to assist in the removal of particulate soils.
- the level of builder can vary widely depending upon the end use of the composition.
- Inorganic or P-containing detergent builders include, but are not limited to, the alkali metal, ammonium and alkanolammonium salts of polyphosphates
- compositions herein function surprisingly well even in the presence of the so-called “weak” builders (as compared with phosphates) such as citrate, or in the so-called "underbuilt” situation that may occur with zeolite or layered silicate builders.
- silicate builders are the alkali metal silicates, particularly those having a SiO 2 :Na 2 O ratio in the range 1.6:1 to 3.2:1 and layered silicates, such as the layered sodium silicates described in U.S. Patent 4,664,839, issued May 12, 1987 to H. P. Rieck.
- NaSKS-6 is the trademark for a crystalline layered silicate marketed by Hoechst (commonly abbreviated herein as "SKS-6").
- Hoechst commonly abbreviated herein as "SKS-6”
- the Na SKS-6 silicate builder does not contain aluminum.
- NaSKS-6 has the delta-Na 2 Si ⁇ 5 morphology form of layered silicate.
- SKS-6 is a highly preferred layered silicate for use herein, but other such layered silicates, such as those having the general formula NaMSi x 0 2x+ -
- Various other layered silicates from Hoechst include NaSKS-5, NaSKS-7 and NaSKS-11 , as the alpha, beta and gamma forms.
- delta-Na 2 Si ⁇ 5 (NaSKS-6 form) is most preferred for use herein.
- Other silicates may also be useful such as for example magnesium silicate, which can serve as a crispening agent in granular formulations, as a stabilizing agent for oxygen bleaches, and as a component of suds control systems.
- carbonate builders are the alkaline earth and alkali metal carbonates as disclosed in German Patent Application No. 2,321 ,001 published on November 15, 1973.
- Aluminosilicate builders are useful in the present invention. Aluminosilicate builders are of great importance in most currently marketed heavy duty granular detergent compositions, and can also be a significant builder ingredient in liquid detergent formulations. Aluminosilicate builders include those having the empirical formula:
- aluminosilicate ion exchange materials are commercially available. These aluminosilicates can be crystalline or amorphous in structure and can be naturally-occurring aluminosilicates or synthetically derived. A method for producing aluminosilicate ion exchange materials is disclosed in U.S. Patent 3,985,669, Krummel, et al, issued October 12, 1976.
- Preferred synthetic crystalline aluminosilicate ion exchange materials useful herein are available under the designations Zeolite A, Zeolite P (B), Zeolite MAP and Zeolite X.
- the crystalline aluminosilicate ion exchange material has the formula:
- x Na-
- This material is known as Zeolite A.
- the aluminosilicate has a particle size of about 0.1-10 microns in diameter.
- Organic detergent builders suitable for the purposes of the present invention include, but are not restricted to, a wide variety of polycarboxylate compounds.
- polycarboxylate refers to compounds having a plurality of carboxylate groups, preferably at least 3 carboxylates.
- Polycarboxylate builder can generally be added to the composition in acid form, but can also be added in the form of a neutralized salt. When utilized in salt form, alkali metals, such as sodium, potassium, and lithium, or alkanolammonium salts are preferred. Included among the polycarboxylate builders are a variety of categories of useful materials.
- polycarboxylate builders encompasses the ether polycarboxylates, including oxydisuccinate, as disclosed in Berg, U.S. Patent 3,128,287, issued April 7, 1964, and Lamberti et al, U.S. Patent 3,635,830, issued January 18, 1972. See also "TMS/TDS" builders of U.S. Patent 4,663,071 , issued to Bush et al, on May 5, 1987.
- Suitable ether polycarboxylates also include cyclic compounds, particularly alicyclic compounds, such as those described in U.S. Patents 3,923,679; 3,835,163; 4,158,635; 4,120,874 and 4,102,903.
- ether hydroxypoiycarboxylates copolymers of maleic anhydride with ethylene or vinyl methyl ether, 1 , 3, 5- trihydroxy benzene-2, 4, 6-trisulphonic acid, and carboxymethyloxysuccinic acid
- various alkali metal, ammonium and substituted ammonium salts of polyacetic acids such as ethylenediamine tetraacetic acid and nitrilotriacetic acid
- polycarboxylates such as mellitic acid, succinic acid, oxy- disuccinic acid, polymaleic acid, benzene 1 ,3,5-tricarboxylic acid, carboxymethyloxysuccinic acid, and soluble salts thereof.
- Citrate builders e.g., citric acid and soluble salts thereof (particularly sodium salt), are polycarboxylate builders of particular importance for heavy duty liquid detergent formulations due to their availability from renewable resources and their biodegradability. Citrates can also be used in granular compositions, especially in combination with zeolite and/or layered silicate builders. Oxydisuccinates are also especially useful in such compositions and combinations.
- Also suitable in the detergent compositions of the present invention are the 3,3- dicarboxy-4-oxa-1 ,6-hexanedioates and the related compounds disclosed in U.S. Patent 4,566,984, Bush, issued January 28, 1986.
- Useful succinic acid builders include the C5-C 2 rj alkyl and alkenyl succinic acids and salts thereof.
- a particularly preferred compound of this type is dodecenylsuccinic acid.
- succinate builders include: laurylsuccinate, myristylsuccinate, palmitylsuccinate, 2-dodecenylsuccinate (preferred), 2- pentadecenylsuccinate, and the like. Laurylsuccinates are the preferred builders of this group, and are described in European Patent Application 86200690.5/0,200,263, published November 5, 1986. Other suitable polycarboxylates are disclosed in U.S. Patent 4,144,226, Crutchfield et al, issued March 13, 1979 and in U.S. Patent 3,308,067, Diehl, issued March 7, 1967. See also Diehl U.S. Patent 3,723,322.
- Fatty acids e.g., C ⁇
- Such use of fatty acids will generally result in a diminution of sudsing, which should be taken into account by the formulator.
- the various alkali metal phosphates such as the well-known sodium tripolyphosphates, sodium pyrophosphate and sodium orthophosphate can be used.
- Phosphonate builders such as ethane-1-hydroxy-1 ,1-diphosphonate and other known phosphonates (see, for example, U.S. Patents 3,159,581 ; 3,213,030; 3,422,021 ; 3,400,148 and 3,422,137) can also be used.
- the detergent compositions herein may optionally contain bleaching agents or bleaching compositions containing a bleaching agent and one or more bleach activators.
- bleaching agents will typically be at levels of from about 1 % to about 30%, more typically from about 5% to about 20%, of the detergent composition, especially for fabric laundering.
- the amount of bleach activators will typically be from about 0.1 % to about 60%, more typically from about 0.5% to about 40% of the bleaching composition comprising the bleaching agent-plus-bleach activator.
- the bleaching agents used herein can be any of the bleaching agents useful for detergent compositions in textile cleaning, hard surface cleaning, or other cleaning purposes that are now known or become known. These include oxygen bleaches as well as other bleaching agents.
- Perborate bleaches e.g., sodium perborate (e.g., mono- or tetra-hydrate) can be used herein.
- Another category of bleaching agent that can be used without restriction encompasses percarboxylic acid bleaching agents and salts thereof. Suitable examples of this class of agents include magnesium monoperoxyphthalate hexahydrate, the magnesium salt of metachloro perbenzoic acid, 4-nonylamino- 4-oxoperoxybutyric acid and diperoxydodecanedioic acid.
- Such bleaching agents are disclosed in U.S. Patent 4,483,781 , Hartman, issued November 20,
- Highly preferred bleaching agents also include 6-nonylamino-6- oxoperoxycaproic acid as described in U.S. Patent 4,634,551 , issued January 6, 1987 to Burns et al.
- Peroxygen bleaching agents can also be used. Suitable peroxygen bleaching compounds include sodium carbonate peroxyhydrate and equivalent "percarbonate" bleaches, sodium pyrophosphate peroxyhydrate, urea peroxyhydrate, and sodium peroxide. Persulfate bleach (e.g., OXONE, manufactured commercially by DuPont) can also be used. A preferred percarbonate bleach comprises dry particles having an average particle size in the range from about 500 micrometers to about 1 ,000 micrometers, not more than about 10% by weight of said particles being smaller than about 200 micrometers and not more than about 10% by weight of said particles being larger than about 1 ,250 micrometers. Optionally, the percarbonate can be coated with silicate, borate or water-soluble surfactants. Percarbonate is available from various commercial sources such as FMC, Solvay and Tokai Denka. Mixtures of bleaching agents can also be used.
- Peroxygen bleaching agents, the perborates, the percarbonates, etc. are preferably combined with bleach activators, which lead to the in situ production in aqueous solution (i.e., during the washing process) of the peroxy acid corresponding to the bleach activator.
- bleach activators Various nonlimiting examples of activators are disclosed in U.S. Patent 4,915,854, issued April 10, 1990 to Mao et al, and U.S. Patent 4,412,934.
- NOBS nonanoyloxybenzene sulfonate
- TAED tetraacetyl ethylene diamine
- Highly preferred amido-derived bleach activators are those of the formulae:
- R2 is an alkylene containing from 1 to about 6 carbon atoms
- R ⁇ is H or alkyl, aryl, or alkaryl containing from about 1 to about 10 carbon atoms
- L is any suitable leaving group.
- a leaving group is any group that is displaced from the bleach activator as a consequence of the nucleophilic attack on the bleach activator by the perhydrolysis anion.
- a preferred leaving group is phenyl sulfonate.
- bleach activators of the above formulae include (6- octanamido-caproyl)oxybenzenesulfonate, (6-nonanamidocaproyl)oxybenzene- sulfonate, ( ⁇ -decanamido-caproyl)oxybenzenesulfonate, and mixtures thereof as described in U.S. Patent 4,634,551 , incorporated herein by reference.
- Another class of bleach activators comprises the benzoxazin-type activators disclosed by Hodge et al in U.S. Patent 4,966,723, issued October 30, 1990, incorporated herein by reference.
- a highly preferred activator of the benzoxazin-type is:
- Still another class of preferred bleach activators includes the acyl lactam activators, especially acyl caprolactams and acyl valerolactams of the formulae:
- R 6 is H or an alkyl, aryl, alkoxyaryl, or alkaryl group containing from 1 to about 12 carbon atoms.
- Highly preferred lactam activators include benzoyl caprolactam, octanoyl caprolactam, 3,5,5-trimethylhexanoyl caprolactam, nonanoyl caprolactam, decanoyl caprolactam, undecenoyl caprolactam, benzoyl valerolactam, octanoyl valerolactam, decanoyl valerolactam, undecenoyl valerolactam, nonanoyl valerolactam, 3,5,5-trimethylhexanoyl valerolactam and mixtures thereof.
- the bleaching compounds can be catalyzed by means of a manganese compound.
- a manganese compound Such compounds are well known in the art and include, for example, the manganese-based catalysts disclosed in U.S. Pat. 5,246,621 , U.S. Pat. 5,244,594; U.S. Pat. 5,194,416; U.S. Pat. 5,114,606; and European Pat. App. Pub. Nos. 549,271 A1 , 549.272A1 , 544.440A2, and 544.490A1 ;
- Preferred examples of these catalysts include Mn ,v 2 (u-0) 3 (1 ,4,7-trimethyl- 1 ,4,7-triazacyclononane) (PF6) 2 , Mn"l 2 (u-0) ⁇ (u-OAc) 2 (1 ,4,7-trimethyM ,4,7- triazacyclononane) 2 .(Cl ⁇ 4) 2 , Mn IV 4(u-0)6(1 ,4,7-triazacyclononane)4(CI04)4, Mn Mn IV 4(u-0) ⁇ (u-OAc) 2 .(1 ,4,7-trimethyM ,4,7-triazacyclononane) (Cl ⁇ 4) 3 , Mn'V(l ,4,7-trimethyM ,4,7-triazacyclononane)- (OCH 3 ) 3 (PF6), and mixtures thereof.
- metal-based bleach catalysts include those disclosed in U.S. Pat. 4,430,243 and U.S. Pat. 5,114,611.
- the use of manganese with various complex ligands to enhance bleaching is also reported in the following United States Patents: 4,728,455; 5,284,944; 5,246,612; 5,256,779; 5,280,117; 5,274,147; 5,153,161 ; and 5,227,084.
- compositions and processes herein can be adjusted to provide on the order of at least one part per ten million of the active bleach catalyst species in the aqueous washing liquor, and will preferably provide from about 0.1 ppm to about 700 ppm, more preferably from about 1 ppm to about 500 ppm, of the catalyst species in the laundry liquor.
- Enzymes can be included in the formulations herein for a wide variety of fabric laundering purposes, including removal of protein-based, carbohydrate-based, or triglyceride-based stains, for example, and for the prevention of refugee dye transfer, and for fabric restoration.
- the enzymes to be incorporated include proteases, amylases, lipases, cellulases, and peroxidases, as well as mixtures thereof.
- Other types of enzymes may also be included. They may be of any suitable origin, such as vegetable, animal, bacterial, fungal and yeast origin. However, their choice is governed by several factors such as pH-activity and/or stability optima, thermostability, stability versus active detergents, builders and so on.
- bacterial or fungal enzymes are preferred, such as bacterial amylases and proteases, and fungal cellulases.
- Enzymes are normally incorporated at levels sufficient to provide up to about 5 mg by weight, more typically about 0.01 mg to about 3 mg, of active enzyme per gram of the composition.
- the compositions herein will typically comprise from about 0.001 % to about 5%, preferably 0.01 %-1 % by weight of a commercial enzyme preparation.
- Protease enzymes are usually present in such commercial preparations at levels sufficient to provide from 0.005 to 0.1 Anson units (AU) of activity per gram of composition.
- AU Anson units
- proteases are the subtilisins which are obtained from particular strains of B. subtilis and B. licheniforms. Another suitable protease is obtained from a strain of Bacillus, having maximum activity throughout the pH range of 8-12, developed and sold by Novo Industries A/S under the registered trade name ESPERASE. The preparation of this enzyme and analogous enzymes is described in British Patent Specification No. 1 ,243,784 of Novo.
- protealytic enzymes suitable for removing protein-based stains that are commercially available include those sold under the tradenames ALCALASE and SAVINASE by Novo Industries A/S (Denmark) and MAXATASE by International Bio-Synthetics, Inc. (The Netherlands).
- proteases include Protease A (see European Patent Application 130,756, published January 9, 1985) and Protease B (see European Patent Application Serial No. 87303761.8, filed April 28, 1987, and European Patent Application 130,756, Bott et al, published January 9, 1985).
- Amylases include, for example, ⁇ -amylases described in British Patent Specification No. 1 ,296,839 (Novo), RAPIDASE, International Bio-Synthetics, Inc. and TERMAMYL, Novo Industries.
- the cellulase usable in the present invention include both bacterial or fungal cellulase. Preferably, they will have a pH optimum of between 5 and 9.5.
- Suitable cellulases are disclosed in U.S. Patent 4,435,307, Barbesgoard et al, issued March 6, 1984, which discloses fungal cellulase produced from Humicola insolens and Humicola strain DSM1800 or a cellulase 212-producing fungus belonging to the genus Aeromonas, and cellulase extracted from the hepatopancreas of a marine mollusk (Dolabella Auricula Solander).
- suitable cellulases are also disclosed in GB-A-2.075.028; GB-A-2.095.275 and DE-OS- 2.247.832. CAREZYME (Novo) is especially useful.
- Suitable lipase enzymes for detergent usage include those produced by microorganisms of the Pseudomonas group, such as Pseudomonas stutzeri ATCC 19.154, as disclosed in British Patent 1 ,372,034. See also lipases in Japanese Patent Application 53,20487, laid open to public inspection on February 24, 1978. This lipase is available from Amano Pharmaceutical Co.
- Lipase P Lipase P
- Other commercial lipases include Amano-CES, lipases ex Chromobacter viscosum, e.g. Chromobacter viscosum var. lipolyticum NRRLB 3673, commercially available from Toyo Jozo Co., Tagata, Japan; and further Chromobacter viscosum lipases from U.S. Biochemical Corp., U.S.A. and Disoynth Co., The Netherlands, and lipases ex Pseudomonas gladioli.
- the LIPOLASE enzyme derived from Humicola lanuginosa and commercially available from Novo is a preferred lipase for use herein.
- Peroxidase enzymes are used in combination with oxygen sources, e.g., percarbonate, perborate, persulfate, hydrogen peroxide, etc. They are used for "solution bleaching," i.e. to prevent transfer of dyes or pigments removed from substrates during wash operations to other substrates in the wash solution.
- Peroxidase enzymes are known in the art, and include, for example, horseradish peroxidase, ligninase, and haloperoxidase such as chloro- and bromo- peroxidase.
- Peroxidase-containing detergent compositions are disclosed, for example, in PCT International Application WO 89/099813, published October 19, 1989, by O. Kirk, assigned to Novo Industries A/S.
- Patent 3,600,319 issued August 17, 1971 to Gedge, et al, and European Patent Application Publication No. 0 199 405, Application No. 86200586.5, published October 29, 1986, Venegas. Enzyme stabilization systems are also described, for example, in U.S. Patent 3,519,570.
- compositions which are commonly used in detergent compositions and which may be incorporated into the detergent tablets of the present invention include chelating agents, soil release agents, soil antiredeposition agents, dispersing agents, brighteners, suds suppressors, fabric softeners, dye transfer inhibition agents and perfumes.
- the present invention also relates to a method of washing which significantly avoids this problem.
- the new method comprises preparing an aqueous solution of a laundry detergent for use in a washing machine, wherein the aqueous solution of laundry detergent is formed by dissolving in water a tablet formed by compressing a particulate material, the tablet comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesive effect on the particulate material
- the method more specifically relates to the preparation of an aqueous solution of a laundry detergent for use in a front-loading washing machine, the front-loading washing machine having a dispensing drawer and a washing drum, wherein the aqueous solution of laundry detergent is formed by dissolving a detergent tablet in water, characterised in that the detergent tablet is placed in the dispensing drawer and water is passed through the dispensing drawer so that the tablet is dispensed as an aqueous solution of a laudry detergent, the aqueous solution subsequently being
- Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and 33% carbonate.
- Anionic agglomerates 2 comprise of 40% anionic surfactant, 28% zeolite and
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate.
- Bleach activator agglomerates comprise of 81 % TAED, 17% acrylic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Binder spray-on system comprises of 50% Lutensit K-HD 96 and 50% PEG
- Example 1 (Comprising a highly soluble compound having a cohesive effect on the particulate material)
- a detergent base powder of composition A (see table above) was prepared as follows: all the particulate material of base composition A were mixed together in a mixing drum to form a homogenous particulate mixture. During this mixing the spray-ons were carried out.
- Example 4 (compound having a cohesive effect on the particulate material)
- Tablets were then made following the same way as described in Example 1.
- the force required to obtain a tablet tensile strength of 15 kPa was 3200 N.
- the tablet height was 1.82 cm.
- Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and
- Anionic agglomerates 2 comprise of 40% anionic surfactant, 28% zeolite and
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate.
- Bleach activator agglomerates comprise of 81 % TAED, 17% acrylic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Binder spray-on system comprises of 50% Lutensit K-HD 96 and 50% PEG
- composition B was prepared following the same process as in Example 1.
- Example 7 (PEG) i) The same composition B was prepared following the same process as in Example 1.
- Example 9 of a tablet according to the invention is a tablet according to the invention.
- DIBS sodium di isoalkylbenzene sulphonate
- the dispensing percentage residue of the 43g tablet was of less than 15%.
- Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and 33% carbonate
- Anionic agglomerates 2 comprise of 40% anionic surfactant, 28% zeolite and
- Nonionic agglomerate comprise 26% nonionic surfactant, 6% Lutensit K-HD 96,
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate
- Bleach activator agglomerates comprise of 81 % TAED, 17% acrylic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Binder spray-on system comp ⁇ ses of 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEGs
- Detergent of composition D was prepared as follows: all the particulate materials except for the dried zeolite were mixed together in a mixing drum to form a homogeneous particulate mixture. During this mixing the spray-ons were carried out. After the spray-ons the dusting was carried out with the dried zeolite.
- Detergent base powder composition Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate
- Bleach activator agglomerates comprise of 81 % TAED, 17% acryiic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Perfume encapsulates comprise 50% perfume and 50% starch.
- Polymer particle comprises 36%, 54% zeolite and 10% water
- the Nonionic spray-on system comprises of 67% C12-C15 AE5 (alcohol with an average of 5 ethoxy groups per molecule), 24% N-methyl glucose amide and
- a detergent base powder of composition E (see below) was prepared as follows: all the particulate materials of base composition E were mixed together in a mixing drum to form a homogenous particulate mixture. During this mixing the spray-ons were carried out. After the spray-on the sodium di isoalkylbenzene sulphonate (sticky hydrotrope) was added to the rest of the matrix.
- the level of residue in the dispenser of a washing machine was assed by means of a "stress tablet dispesing test": two laundry tablets are placed in to a Bauknecht WA9850 dispenser. The water supply to the washing machine is set to a temperature of 8C and a hardness of 21 grains per gal, the dispenser water inlet flowrate is set to 4!/min. The level of tablet residues left in the dispenser is checked by letting water flow through the dispenser for 78sec. The dispensing percentage residue is determined as follows:
- the % dispensing is shown in the tables below.
- composition F The procedure to prepare tablets of example A was repeated for powder of composition F.
- the polymer sprayed-on the matrix comprised 0.67 parts of PEG4000 and 0.33 parts of PEG1000.
- Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and
- Anionic agglomerates 2 comprise of 40% anionic surfactant, 28% zeolite and
- Nonionic agglomerate comprise 26% nonionic surfactant, 6% Lutensit K-HD 96,
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate
- Bleach activator agglomerates comprise of 81% TAED, 17% acrylic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Binder spray-on system comprises of 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEGs
- Anionic agglomerates 1 comprise of 40% anionic surfactant, 27% zeolite and
- Anionic agglomerates 2 comprise of 40% anionic surfactant, 28% zeolite and
- Nonionic agglomerate comprise 26% nonionic surfactant, 6% Lutensit K-HD 96,
- Cationic agglomerates comprise of 20% cationic surfactant, 56% zeolite and
- Layered silicate comprises of 95% SKS 6 and 5% silicate
- Bleach activator agglomerates comprise of 81 % TAED, 17% acrylic/maleic copolymer (acid form) and 2% water.
- Ethylene diamine N,N-disuccinic acid sodium salt/Sulphate particle comprise of
- Zinc phthalocyanine sulphonate encapsulates are 10% active.
- Suds suppressor comprises of 11.5% silicone oil (ex Dow Corning); 59% of zeolite and 29.5% of water.
- Binder spray-on system comprises of 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEGs.
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/720,406 US6559115B1 (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
CA002336623A CA2336623C (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
BR9911986-2A BR9911986A (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
AU50961/99A AU5096199A (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
KR1020017000377A KR20010053468A (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
JP2000559216A JP2002520446A (en) | 1998-07-10 | 1999-07-12 | Detergent tablets with high mechanical and dissolution properties |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP98870151.2 | 1998-07-10 | ||
EP98870151 | 1998-07-10 | ||
EP98870181.9 | 1998-08-24 | ||
EP98870181A EP0971029B1 (en) | 1998-07-10 | 1998-08-24 | Detergent tablet with high mechanical and dissolution characteristics |
Publications (1)
Publication Number | Publication Date |
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WO2000002994A1 true WO2000002994A1 (en) | 2000-01-20 |
Family
ID=26152274
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/015676 WO2000002994A1 (en) | 1998-07-10 | 1999-07-12 | Detergent tablet with high mechanical and dissolution characteristics |
Country Status (14)
Country | Link |
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EP (1) | EP0971029B1 (en) |
JP (1) | JP2002520446A (en) |
KR (1) | KR20010053468A (en) |
CN (1) | CN1309691A (en) |
AR (1) | AR019366A1 (en) |
AT (1) | ATE289347T1 (en) |
AU (1) | AU5096199A (en) |
BR (1) | BR9911986A (en) |
CA (1) | CA2336623C (en) |
CZ (1) | CZ20004657A3 (en) |
DE (1) | DE69829044T2 (en) |
ES (1) | ES2238754T3 (en) |
MA (1) | MA24924A1 (en) |
WO (1) | WO2000002994A1 (en) |
Families Citing this family (4)
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JP2003506560A (en) * | 1999-08-10 | 2003-02-18 | ザ、プロクター、エンド、ギャンブル、カンパニー | Detergent compositions containing hydrotropes |
AU6288999A (en) * | 1999-10-06 | 2001-05-10 | Procter & Gamble Company, The | Detergent tablet with high dissolution and mechanical characteristics |
GB2367830A (en) | 2000-10-12 | 2002-04-17 | Procter & Gamble | Process for preparing tablets |
DE102009057222A1 (en) * | 2009-12-05 | 2011-06-09 | Clariant International Ltd. | Bleach catalyst compounds, process for their preparation and their use |
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-
1998
- 1998-08-24 EP EP98870181A patent/EP0971029B1/en not_active Expired - Lifetime
- 1998-08-24 AT AT98870181T patent/ATE289347T1/en not_active IP Right Cessation
- 1998-08-24 DE DE69829044T patent/DE69829044T2/en not_active Expired - Fee Related
- 1998-08-24 ES ES98870181T patent/ES2238754T3/en not_active Expired - Lifetime
-
1999
- 1999-07-12 WO PCT/US1999/015676 patent/WO2000002994A1/en not_active Application Discontinuation
- 1999-07-12 CA CA002336623A patent/CA2336623C/en not_active Expired - Fee Related
- 1999-07-12 CN CN99808500A patent/CN1309691A/en active Pending
- 1999-07-12 KR KR1020017000377A patent/KR20010053468A/en not_active Application Discontinuation
- 1999-07-12 JP JP2000559216A patent/JP2002520446A/en not_active Withdrawn
- 1999-07-12 MA MA25673A patent/MA24924A1/en unknown
- 1999-07-12 AU AU50961/99A patent/AU5096199A/en not_active Abandoned
- 1999-07-12 BR BR9911986-2A patent/BR9911986A/en not_active Application Discontinuation
- 1999-07-12 AR ARP990103367A patent/AR019366A1/en unknown
- 1999-07-12 CZ CZ20004657A patent/CZ20004657A3/en unknown
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Also Published As
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JP2002520446A (en) | 2002-07-09 |
KR20010053468A (en) | 2001-06-25 |
ATE289347T1 (en) | 2005-03-15 |
MA24924A1 (en) | 2000-04-01 |
AR019366A1 (en) | 2002-02-13 |
CZ20004657A3 (en) | 2001-09-12 |
AU5096199A (en) | 2000-02-01 |
CA2336623C (en) | 2005-03-22 |
CN1309691A (en) | 2001-08-22 |
DE69829044D1 (en) | 2005-03-24 |
EP0971029A1 (en) | 2000-01-12 |
ES2238754T3 (en) | 2005-09-01 |
BR9911986A (en) | 2001-03-27 |
CA2336623A1 (en) | 2000-01-20 |
EP0971029B1 (en) | 2005-02-16 |
DE69829044T2 (en) | 2006-02-09 |
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