MXPA01000373A - Detergent tablet with high mechanical and dissolution characteristics - Google Patents

Detergent tablet with high mechanical and dissolution characteristics

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Publication number
MXPA01000373A
MXPA01000373A MXPA/A/2001/000373A MXPA01000373A MXPA01000373A MX PA01000373 A MXPA01000373 A MX PA01000373A MX PA01000373 A MXPA01000373 A MX PA01000373A MX PA01000373 A MXPA01000373 A MX PA01000373A
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MX
Mexico
Prior art keywords
tablet
acid
highly soluble
particles
soluble compound
Prior art date
Application number
MXPA/A/2001/000373A
Other languages
Spanish (es)
Inventor
Eric Tcheou
Jean Wevers
Jose Luis Vega
Original Assignee
The Procter & Gamble Company
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Filing date
Publication date
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Publication of MXPA01000373A publication Critical patent/MXPA01000373A/en

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Abstract

The present invention relates to a tablet formed by compressing a particulate material, the particulate material comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesive effect on the particulate material. In a further aspect of the invention there is provided a method 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.

Description

DETERGENT TABLET WITH MECHANICAL AND HIGH DISSOLUTION CHARACTERISTICS The present invention relates to detergent tablets, especially those adapted for use in washing. Although cleaning compositions in tablet form have often been proposed, they have not gained (with the exception of soap bars for personal washing) any substantial success, despite the various advantages of the products in a unit assortment form. . One of the reasons for this may be that detergent tablets usually dissolve slower than the constituent powders of which they are made, simply because the constituent powders are bound by force in the tablet, the water having a comparatively small opportunity to penetrate between the tablets. they. This gives rise to the problem that slowly dissolving tablets cause residues which may, for example, be visible through the washing machine door during the washing cycle, or which stick to the fabrics at the end of the washing cycle. , or both. EP-A-0 711 827, published May 5, 1996, discloses laundry detergent tablets containing a highly water-soluble material that improves the disintegration of the whole tablet and the dissolution of its soluble ingredients.
However, particularly in certain front-loading washing machines, tablet waste problems that appear visibly in the washing machine window have still been encountered. The object of the present invention is to provide tablets formed by compressing a material formed of particles, the material formed of particles comprising a surfactant, the tablet being suitable for storage, shipping and handling without breaking while dissolving easily and quickly in washing solution. , releasing the active ingredients in the washing solution and disintegrating and completely dispersing in alkaline solutions or solutions rich in surfactant such as the washing solution.
BRIEF DESCRIPTION OF THE INVENTION The object of the invention is achieved by providing a tablet of the aforementioned type, wherein the material formed from particles further comprises a highly soluble compound, the highly soluble compound having a cohesion effect on the material formed from particles. In another aspect of the invention there is provided a method for preparing an aqueous solution of a laundry detergent for use in a washing machine, wherein the aqueous laundry detergent solution is formed by dissolving in water a tablet formed by compressing a material formed of particles, the tablet comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesion effect on the material formed from particles.
DETAILED DESCRIPTION OF THE INVENTION The invention relates to a highly soluble compound having a cohesion effect on the material formed from particles.
Highly soluble compounds The invention relates to a highly soluble compound. Said compound could be formed from a mixture or from a single compound. Accog to the invention, a highly soluble compound is defined as follows: A solution is prepared in the following manner comprising deionized water as well as 20 grams per liter of a specific compound: 1- 20 g of the specific compound is placed in a Sotax beaker. This beaker is placed in a bath at a constant temperature set at 10 ° C. An agitator with a marine propellant is placed in the beaker so that the bottom of the agitator is 5 mm above the bottom of the Sotax beaker. The mixer is adjusted to a rotation speed of 200 revolutions per minute. 2- 980 g of the deionized water are introduced into the Sotax beaker. 3-10 s after the introduction of water, the conductivity of the solution is measured, using a conductivity meter. 4- Step 3 is repeated after 20, 30, 40, 50, 1 min, 2 min, 5 min and 10 min after step 2. 5- The measurement taken at 10 min is used as the plateau value or maximum value . 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 deionized water to the compound. In truth, by monitoring the conductivity in this way, the conductivity reaches a plateau after a certain time, this plateau being considered as the maximum value. Said compound is preferably in the form of a flowable material consisting of solid particles at temperatures between 10 and 80 ° Celsius for ease of handling, but other forms such as a paste or a liquid can be used. Examples of highly soluble compounds include sodium diisoalkylbenzene sulfonate or sodium toluene sulfonate.
Cohesion Effect For purposes of this invention, the cohesion effect on the material formed from particles of a detergent matrix is characterized by the force required to break a tablet based on the examined detergent matrix compressed under controlled compression conditions. For a given compression force, a high tablet strength indicates that the granules remained very tight when they were compressed, so that a strong cohesion effect is taking place. Means for evaluating tablet resistance (also called diametral fracture stress) are provided 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 mixture comprising 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% (preferably below 5%)). The temperature of the addition is between 10 and 80C, most preferably between 10 and 40C. A highly soluble compound is defined as having a cohesive effect on the material formed from particles according to the invention when at a given compaction force of 3000 N, tablets with a weight of 50 g of material formed of detergent particles and a 55 mm diameter have their tablet tensile strength increased by more than 30% (preferably 60 and most preferably 100%) by the presence of 3% of the highly soluble compound having a cohesion effect on the material formed from particles base. An example of a compound having a cohesive effect is sodium diisoalkylbenzenesulfonate. It was found that by integrating a highly soluble compound having a cohesion effect on the material formed from particles according to the invention to a tablet formed by compressing a material formed from particles comprising a surfactant, dissolving the tablet in a solution aqueous was significantly increased. In a preferred embodiment, at least 1% by weight of the tablet is formed of the highly soluble compound, preferably at least 2%, most preferably at least 3%, and most preferably at least 5% by weight of the tablet being formed from of the highly soluble compound having a cohesion effect on the material formed from particles. It should be mentioned that 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. In accordance with the present invention, it was found that the highly soluble compound having a cohesion effect on the material formed from particles allows to obtain a tablet having a higher tensile strength at a constant compaction force or a resistance to tension equal to a lower compaction force compared to traditional tablets. Typically, the tablet will have a tensile strength of more than 5kPa, preferably of more than 10kPa, preferably, in particular for use in laundry applications, of more than 15kPa, most preferably of more than 30kPa, and most preferably more than 50 kPa, in particular for use in dishwashing or automatic dishwashing applications; and a tensile strength of less than 300 kPa, preferably less than 200 kPa, preferably less than 100 kPa, most preferably less than 80 kPa, and most preferably less than 60 kPa. In truth, in case of application for laundry, the tablets should be less compressed than in the case of applications for automatic dishwashing, for example, wherein the dissolution is more easily achieved, so that in a laundry application, the tensile strength is preferably less than 30 kPa. This allows to produce tablets having a strength and mechanical strength comparable to the strength or mechanical strength of the traditional tablets while they have a less compact tablet thus dissolving more easily. In addition, since the compound is highly soluble, the solution of the tablet is further facilitated, resulting in a synergy which leads to easier dissolution for a tablet according to the invention.
Tablet manufacture The invention makes it possible to obtain a less compact and less dense tablet at a constant compaction force compared to a traditional detergent tablet. The detergent tablets of the present invention can be prepared by simply mixing the solid ingredients and compressing the mixture in a conventional tablet press as used, for example, in the pharmaceutical industry. Preferably, the main ingredients, in particular gelling surfactants, are used in the form of particles. Any liquid ingredients, for example, surfactant or foam suppressant, can be incorporated in a conventional manner into the ingredients formed of solid particles. In particular for laundry tablets, the ingredients such as builder and surfactant can be spray-dried in a conventional manner and then can be compacted at a suitable pressure. Preferably, the tablets according to the invention are compressed using a force of less than 100000N, preferably less than 50000N, preferably less than 5000N and most preferably less than 3000N. Indeed, the most preferred embodiment is a tablet suitable for washing compressed laundry using a force of less than 2500 N, but automatic table washing tablets can also be considered for example, wherein such tablets for automatic dishwashing usually They are more compressed than laundry tablets. The particulate material used to make the tablet of this invention can be made by any process of particle formation or granulation. An example of such a process is spray drying (in a co-current or countercurrent spray drying tower) which typically gives low bulk densities of 600 g / L or lower. The materials formed from higher density particles can be prepared by granulation and densification in a batch mixer by high shear / granulator or by a continuous granulation and densification process (for example, using Lodige® CB and / or Lodige® mixers). KM). Other suitable methods include fluidized bed processes, compaction methods (for example roll compaction), extrusion, as well as any material formed from particles made by any chemical method such as flocculation, crystallization, concretion, etc. The individual particles can also be any other particle, granule, sphere or grain. The components of the material formed of particles can be mixed together by any conventional means. The batch is suitable in, for example, a concrete mixer, Nauta mixer, ribbon mixer, or any other. Alternatively, the mixing process can be carried out continuously by measuring each component by weight in a moving band, and mixing them in one or more drum (s) or mixer (s). A non-gelling binder can be sprayed into the mixture of some or all of the components of the material formed of particles. Other liquid ingredients can also be sprayed into the mixture of components either separately or pre-mixed. For example, perfume and suspensions of optical brighteners can be sprayed. A finely divided flow aid (powdering agent such as zeolites, carbonates, silicas) can be added to the material formed from particles after spraying the binder, preferably towards the end of the process, to make the mixture less tacky. The tablets can be manufactured using any compaction process, such as tabletting, briquetting, or extrusion, preferably tabletting. Suitable equipment includes a standard single-stroke press or rotary press (such as Courtoy®, Korch®, Manesty®, or Bonals®). The tablets prepared according to this invention preferably have a diameter between 20 mm and 60 mm, preferably 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, most preferably greater than 1: 2. The compaction pressure used to prepare these tablets does not need to exceed! 00000 kN / m2, preferably not exceeding 30000 kN / m2, preferably not exceeding 5000 kN / m2, most preferably not exceeding 3000 kN / m2 and most preferably not exceeding 1000 kN / m2. In a preferred embodiment according to the invention, the tablet has a density of at least 0.9 g / cc, preferably of at least 1.0 g / cc, and preferably less than 2.0 g / cc, most preferably less than 1.5 g / cc , most preferably less than 1.25 g / cc and most preferably less than 1.1 g / cc.
Hydrotrope Compound In a preferred embodiment of the invention, the highly soluble compound having a cohesive effect is a hydrotrope compound, a specific compound being defined as a hydrotrope in the following manner (see S.E. Friberg and M. Chiu, J. Dispersion Science and Technology, 9 (5 &6), pages 443 to 457, (1988-1989)): 1. A solution comprising 25% by weight of the specific compound and 75% by weight of water is prepared. 2. Then octanoic acid is 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 ° Celcius. The solution is mixed in a Sotax beaker with a stirrer with a marine propellant, the impeller being positioned approximately 5 mm above the bottom of the beaker, the mixer being adjusted at a rotation speed of 200 revolutions per minute. 3. The specific compound is hydrotrope if the octanoic acid is completely solubilized, that is, if the solution comprises only one phase, the phase being a liquid phase.
It should be mentioned that in a preferred embodiment of the invention, the hydrotrope compound is a flowable material made of solid particles under operating conditions between 15 and 60 ° Celsius. Hydrotrope compounds include the following listed compounds: A list of commercial hydrotropes could be found in McCutcheon Emulsifiers and Detergents published by the McCutcheon Division of Manufacturing Confectioners Company. Compounds of interest also include: 1. Nonionic hydrotrope with the following structure: R - O - (CH2CH2O) x (CH-CH2O) and H CH3 wherein R is a C8-C10 alkyl chain, x ranges from 1 to 15, and from 3 to 10. 2. Anionic hydrotropes such as alkali metal arylsulfonates. This includes alkali metal salts of benzoic acid, salicylic acid, benzenesulfonic acid and its many derivatives, naphthoic acid and various hydro-aromatic acids. Examples of these are sodium, potassium and ammonium salts and benzenesulfonate salts derived from toluene sulfonic acid, xylene sulfonic acid, cumene sulphonic acid, tetralinsulphonic acid, naphthalenesulphonic acid, methylnaphthalenesulphonic acid, dimethylnaphthalenesulphonic acid, trimethylnaphthalenesulphonic acid.
Other examples include dialkylbenzenesulfonic acid salts such as salts of diisopropylbenzenesulfonic acid, ethylmethylbenzenesulfonic acid, alkylbenzenesulfonic acid with an alkyl chain length of 3 to 10, (preferably 4 to 9), linear or branched alkylsulfonates with an alkyl chain with 1 to 18 carbons. 3. Solvent hydrotropes such as alkoxylated glycerines and alkoxylated glycerides, alkoxylated glycerines of esters, alkoxylated fatty acids, glycerin esters, polyglycerol esters. The preferred alkoxylated glycerines have the following structure: where I, m, and n are each a number from 0 to about 20, with l + m + n = from about 2 to about 60, preferably from about 10 to about 45 and R represents H, CH3 or C2H5. Preferred alkoxylated glycerides have the following structure wherein R1 and R2 are each CnCOO or - (CH2CHR3-O) H where R3 = H, CH3 or C2H5 and I is a number from 1 to about 60, n is a number from about 6 to about 24. 4. Hydrotropes polymeric agents such as those described in wherein E is a hydrophilic functional group, R is H or a C1-C10 alkyl group or is a hydrophilic functional group; R1 is H or a lower alkyl group or an aromatic group, R2 is H or a cyclic alkyl group or aromatic group. The polymer typically has a molecular weight of between about 1000 and 1000000. 5. Hydrotropes of unusual structure such as 5-carboxy-4-hexyl-2-cyclohexane-1-yl octanoic acid (Diacid®). The use of said compounds in the invention would further increase the rate of dissolution of the tablet, since a hydrotrope compound facilitates the dissolution of surfactants, for example. Such a compound could be formed from a mixture or from a single compound.
Coating The strength of the tablet according to the invention can be further improved by making a coated tablet, the coating covering an uncoated tablet according to the invention, thereby further improving the mechanical characteristics of the tablet while maintaining or improving yet plus the dissolution. In one embodiment of the present invention, the tablets may be coated such that the tablet does not absorb moisture, or absorb moisture only at a very slow rate. The coating is also strong to moderate mechanical shocks to which the tablets are subjected during handling, packing and shipping resulting in very low breaking or friction levels. Finally, the coating is preferably brittle so that the tablet decomposes when subjected to stronger mechanical shock. Furthermore, it is favorable if the coating material dissolves under alkaline conditions, or is easily emulsified by surfactants. This helps to avoid the problem of visible residues in the window of a front loading washing machine during the washing cycle, and also avoids the deposit of undissolved particles or lumps of coating material in the laundry load.
The solubility in water is measured following the test protocol of E1148-87 of ASTM entitled, "Standard test method for aqueous solubility measurements".
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. same. The coating material preferably has a melting point of 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. In a), the coating material is applied at a temperature above its melting point, and solidifies in the tablet. In b), the coating is applied as a solution, the solvent being dried to leave a consistent coating. The substantially insoluble material can be applied to the tablet by, for example, spraying or immersion. Normally when the molten material is sprayed onto the tablet, it will solidify rapidly to form a consistent coating. When the tablets are immersed in the molten material and then removed, rapid cooling again causes rapid solidification of the coating material. Clearly 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 viable to be used. Preferably, the materials are melted on the scale of 60 ° C to 160 ° C, more preferably 70 ° C to 120 ° C. By "melting point" is meant the temperature at which the material to be heated slowly in, for example, a capillary tube becomes a transparent liquid. A coating of any desired thickness can be applied in accordance with the present invention. For most purposes, the coating forms from 1% to 10%, preferably from 1.5% to 5%, of the weight of the tablet. The tablet coatings of the present invention are very hard and provide extra resistance to the tablet. In a preferred embodiment of the present invention, the fracture of the coating in the wash is improved by adding a disintegrant to the coating. This disintegrant will swell once it is in contact with water and will break the coating into small pieces. This will improve the dissolution of the coating in the wash solution. The disintegrant is suspended in the molten coating 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 the Pharmaceutical Excipients Manual (1986). Examples of suitable disintegrants include starch: natural, modified or pregelatinized starch, sodium starch gluconate; gum: gum agar, guar gum, locust bean gum, karaya gum, pectin gum, gum tragacanth; croscarmilose-sodium, crospovidone, cellulose, carboxymethyl cellulose, algenic acid and its salts including sodium alginate, silicon dioxide, clay, polyvinyl pyrrolidone, soy polysaccharides, ion exchange resins and mixtures thereof.
Stress Resistance Depending on the composition of the starting material, and the shape of the tablets, the compaction force used can be adjusted so as not to affect the tensile strength, and the decay time in the washing machine. This procedure can be used to prepare homogenous or layered tablets of any size or shape. For a cylindrical tablet, the tensile strength corresponds to the diametral fracture stress (DFS) which is a way to express the strength of a tablet, and is determined by the following equation: = 2F μDt Where F is the maximum force (Newton) to cause voltage failure (fracture) measured by a tablet hardness tester VK 200 supplied by Van Kell Industries, Inc. D is the diameter of the tablet, and t the thickness of the tablet. (Method Pharmaceutical Dosage Forms: Tablets Volume 2 page 213 to 217).
A tablet that has a diametral fracture stress less than 20 kPa is considered fragile and is likely to result in some tablets being delivered broken 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, where the normal cross section at the height of the tablet is not round, and where the force is applied along a direction perpendicular to the direction of the height of the tablet and normal next to the tablet, the side being perpendicular to the non-round cross section.
Tablet Assortment The assortment speed of a detergent tablet can be determined as follows: Two tablets, nominally 50 grams each, are weighed, and then placed in the dispenser of a Baucknecht® WA9850 washer. The water supply to the washing machine is adjusted to a temperature of 20 ° C and a hardness of 3.57 g / l, the inlet water flow velocity of the spout being adjusted to 8 l / min. The level of tablet residues remaining in the dispenser is verified by changing the wash ignition and the wash cycle setting to wash program 4 (white / colors, short cycle). The assortment percentage residue is determined as follows:% of assortment = weight of waste x 100 / weight of the original tablet The residue level is determined by repeating the procedure 10 times and an average residue level is calculated based on ten individual measurements. In this stress test, a residual of 40% of the starting tablet weight is considered acceptable. A residue of less than 30% is preferred, and less than 25% is more preferred. It is worth mentioning that the measure of water hardness is given in the traditional "grain per gallon" unit, where 0.001 mol per liter = 7.0 grains per gallon, representing the concentration of Ca2 + ions in solution.
Effervescent In another preferred embodiment of the present invention, the tablets further comprise an effervescent. "Effervescence" as defined herein means the formation of gas bubbles from a liquid, as a result of a chemical reaction between a soluble acid source and an alkali metal carbonate, to produce gaseous carbon dioxide, ie, C6H8O7 + 3NaHCO3? Na3C6H5O7 + 3CO2 t + 3H2O Additional examples of acid and carbonate sources and other effervescent systems can be found in: (Pharmaceutical Dosage Forms: Tablets Volume 1 page 287 to 291). An effervescent can 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. Preferably the effervescent should be added as an agglomerate of different particles or as a compact product, and not as separate particles. Due to the gas created by the effervescence in the tablet, the tablet may have a D.F.S. higher and still have the same disintegration time as a tablet without effervescence. When the D.F.S. of the tablet with effervescence remains the same as a tablet without effervescence, the disintegration of the tablet with effervescence will be faster. An additional dissolution aid could be provided using compounds such as sodium acetate or urea. A list of suitable dissolving aids can be found in Pharmaceutical Dosage Forms: Tablets, Volume 1, Second Edition, Edited by H.A. Lieberman et al, ISBN 0-8247-8044-2.
Detersive Surfactants The tablet according to the invention comprises surfactants. The dissolution of surfactants is favored by the addition of the highly soluble compound. Non-limiting examples of surfactants useful herein typically at levels of about 1% to about 55%, by weight, include the conventional CM-CIS alkylbenzene sulphonates ("LAS") and C?-C20 alkyl sulfates ("AS") ) branched and random chain, the secondary C10-C18 alkyl sulfates (2,3) of formula CH3 (CH2)? (CHOSO3-M +) CH3 and CH3 (CH2) and (CHOSO3, M +) CH2CH3 where xy (y +1 ) are integers of at least about 7, preferably at least about 9, and M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, C?-C18 alkylalkoxy sulfates ("AEXS"; ethoxysulfates EO 1-7), alkylalkoxycarboxylates of C10-C18 (especially the ethoxycarboxylates EO 1-5), the glycerol ethers of C10-18. C10-C18 alkyl polyglycosides and their corresponding sulphated polyglycosides, and alpha-sulfonated fatty acid esters of C? 2-C-? s- If desired, conventional nonionic and amphoteric surfactants such as C? 2 alkyl ethoxylates. -C? S ("AE") including the so-called narrow peak alkyl ethoxylates and C6-C-? 2 alkylphenolalkoxylates (especially mixed ethoxylates and ethoxy / propoxy), C? 2-C? S betaines and sulfobetaines ("sultaines") "), C10-C18 amine oxides, and the like, can also be included in the general compositions. The C10-C18 polyhydroxy fatty acid N-alkylamides can also be used. Typical examples include the C12-C18 N-methylglucamides. See WO 9,206,154. Other surfactants derived from sugar include the polyhydroxy fatty acid N-alkoxyamides, such as C10-C18 N- (3-methoxypropyl) glucamide. The N-propyl to N-hexyl glucamides of C12-C-is can be used for low foam production. Conventional C? 0-C20 soaps can also be used. If high foam production is desired, the branched-chain C-io-C-iß soaps can be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts. In a preferred embodiment, the tablet comprises at least 5% by weight of surfactant, preferably at least 15% by weight, most preferably at least 25% by weight, and most preferably between 35% and 45% by weight of surfactant.
Non-quenching binders Non-gelling binders can be integrated into the particles forming the tablet to facilitate further dissolution. If binders are used. non-gelling, suitable non-gelling binders include synthetic organic polymers such as polyethylene glycols, polyvinyl pyrrolidones, polyacrylates and water-soluble acrylate copolymers. The Pharmaceutical Excipients Second Edition manual has the following classification of binders: acacia, alginic acid, carbomer, carboxymethylcellulose-sodium, dextrin, ethylcellulose, gelatin, guar gum, hydrogenated vegetable oil type I, hydroxyethylcellulose, hydroxypropylmethylcellulose, liquid glucose, silicate magnesium-aluminum, maltodextrin, methylcellulose, polymethacrylates, povidone, sodium alginate, starch and zein. The most preferred binders also have an active cleaning function in the laundry of clothes such as cationic polymers, ie ethoxylated hexamethylenediamine quaternary compounds, bishexamethylene triamias, or others such as pentaamines, ethoxylated polyethylene amines, maleic acrylic polymers. The non-gelling binder materials are preferably sprayed and therefore have an appropriate melting point temperature below 90 ° C, preferably below 70 ° C and most preferably below 50 ° C in order not to damage or Degrade the other active ingredients in the matrix. More non-aqueous liquid binders are preferred (i.e., not in aqueous solution) which can be sprayed in molten form. However, they can also be solid binders incorporated in the matrix by dry addition but which have agglutination properties within the tablet. Non-gelling binder materials are preferably used in an amount within the range of 0.1 to 15% of the composition, most preferably below 5% and especially if it is an active material that is not for laundry below 2%. % by weight of the tablet. It is preferred to avoid gelling binders, such as nonionic surfactants, in their liquid form or molten form. Nonionic surfactants and other gelling binders are not excluded from the compositions, but it is preferred that they be processed into detergent tablets as components of materials formed from particles, and not as liquids.
Detergency builders Detergency builders may optionally be included in the compositions herein to help control mineral hardness. Inorganic as well as organic builders can be used. Builders are typically used in fabric washing compositions to aid in the removal of dirt formed from particles. The level of builder can vary widely depending on the final use of the composition. Inorganic detergents or P-containing detergents include, but are not limited to, the alkali metal, ammonium and alkanolammonium salts of polyphosphates (exemplified by tripolyphosphates, pyrophosphates, and vitreous polymeric metaphosphates), phosphonates, phytic acid, silicates, carbonates ( including bicarbonates and sesquicarbonates), sulphates, and aluminosilicates. However, non-phosphate builders are required in some places. Importantly, the compositions herein work surprisingly well even in the presence of so-called "weak" builders (as compared to phosphates) such as citrate, or in the so-called "poor builder condition" condition. which can occur with zeolite builders or layered silicate builders.
Examples of silicate builders are alkali metal silicates, in particular those having a Si? 2: Na2O ratio in the 1.6: 1 to 3.2: 1 scale and layered silicates, such as the layered sodium silicates described in US Patent 4,664,839, issued May 12, 1987 to HP Rieck NaSKS-6 is the trademark of a crystalline layered silicate marketed by Hoechst (commonly abbreviated herein as "SKS-6"). Unlike zeolite builders, the Na SKS-6 silicate builder does not contain aluminum. NaSKS-6 has the shape of laye-Na2S05 morphology of layered silicate. It can be prepared by methods such as those described in German DE-A-3,417,649 and DE-A-3,742,043. SKS-6 is a highly preferred layered silicate for use herein, but other layered silicates can be used herein, such as those having the general formula NaMSix? 2x +? - and H 2 O wherein M is sodium or hydrogen, x is a number from 1.9 to 4, preferably 2, and y is a number from 0 to 20, preferably 0. Other layered silicates from Hoechst include NaSKS-5, NaSKS-7 and NaSKS-11, such as alpha forms, beta and gamma. As mentioned above, delta-Na2S¡O5 (NaSKS-6 form) is more preferred for use herein. Other silicates may also be useful, for example, magnesium silicate, which may serve as a tightening agent in granulated formulations, as a stabilizing agent for oxygen bleaches, and as a component of foam control systems.
Examples of carbonate builders are alkaline earth metal and alkali metal carbonates which are described in German Patent Application No. 2,321,001 published November 15, 1973. Aluminosilicate builders are useful in the present invention. Aluminosilicate builders are of great importance in the heavy duty granular detergent compositions marketed today, and can also be a significant detergency builder ingredient in liquid detergent formulations. The aluminosilicate builders include those that have the empirical formula: Mz (zAIO2) and] -xH2O where z and y are integers of at least 6, the molar ratio of zay is on the scale of 1.0 to about 0.5, and x is a whole from about 15 to about 264. Useful aluminosilicate ion exchange materials are commercially available. These aluminosilicates may be of crystalline or amorphous structure and may be natural aluminosilicates or derivatives in a synthetic manner. A method for producing aluminosilicate ion exchange materials is described in the U.S.A. 3 patent., 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. In an especially preferred embodiment, the crystalline aluminosilicate ion exchange material has the formula: Na? 2 [(AIO2) i2 (SiO2) 12] -xH20 wherein x is from about 20 to about 30, especially about 27 This material is known as Zeolite A. Dehydrated zeolites (x = 0-10) can also be used herein. Preferably, the aluminosilicate has a particle size of about 0.1-10 microns in diameter. Organic detergency builders suitable for the purposes of the present invention include, but are not limited to, a wide variety of polycarboxylate compounds. As used herein, "polycarboxylate" refers to compounds having a plurality of carboxylate groups, preferably at least 3 carboxylates. The polycarboxylate builder in general can be added to the composition in acid form, but can also be added in the form of a neutralized salt. When used in salt form, alkali metal salts, such as sodium, potassium, and lithium, or alkanolammonium salts, are preferred. Polycarboxylate builders include a variety of categories of useful materials. An important category of polycarboxylate builders includes the ether polycarboxylates, including oxydisuccinate, as described in Berg, US Patent 3,128,287, issued April 7, 1964, and Lamberti et al, US Patent 3,635,830, issued January 18. 1972. See also detergent builders "TMS / TDS" of US Patent 4,663,071, issued to Bush et al, May 5, 1987. Suitable ether polycarboxylates also include cyclic compounds, particularly alicyclic compounds, such as those described in US Patents 3,923,679; 3,835,163; 4,158,635; 4,120,874 and 4,102,903. Other useful builders include ether hydroxypolycarboxylates, maleic anhydride copolymers with ethylene or vinyl methyl ether, 1,3,5-trihydroxybenzene-2,6,6-trisulfonic acid, and carboxymethyloxysuccinic acid, the different alkali metal salts, ammonium, and substituted ammonium salts of polyacetic acids such as ethylenediaminetetraacetic acid and nitrilotriacetic acid as well as polycarboxylates such as melific acid, succinic acid, oxydisuccinic acid, polymaleic acid, benzene-1, 3,5-tricarboxylic acid, carboxymethyloxysuccinic acid, and soluble salts of the same. Citrate detergency builders, for example, citric acid and soluble salts thereof (in particular sodium salt), are polycarboxylate builders of particular importance for heavy-duty liquid detergent formulations because of their availability of renewable resources and their biodegradability . The citrates can also be used in granular compositions, especially in combination with zeolite builders and / or layered silicate builders. Oxydisuccinates are also especially useful in said compositions and combinations.
Also suitable in the detergent compositions of the present invention are 3,3-dicarboxy-4-oxa-1,6-hexanedioates and the related compounds described in US Pat. No. 4,566,984, Bush, issued January 28, 1986. Improvers of useful succinic acid detergency include C5-C20 alkylsuccinic and alkenyl succinic acids and salts thereof. A particularly preferred compound of this type is dodecenylsuccinic acid. Specific examples of succinate builders include: laurylsuccinate, myristylsuccinate, palmitylsuccinate, 2-dodecenylsuccinate (preferred), 2-pentadecenylsuccinate, and the like. Lauryl succinates are the preferred builders of this group, and are described in European patent application 86200690.5 / 0,200,263, published on November 5, 1986. Other suitable polycarboxylates are described in US Pat. 4,144,226, Crutchfield et al., Issued March 13, 1979 and in the U.S. patent. 3,308,067, Diehl, issued March 7, 1967. See also Diehl patent of E.U.A. 3,723,322. Fatty acids, for example, C 12 -C 8 monocarboxylic acids > they may also be incorporated into the compositions alone, or in combination with the aforementioned builders, especially citrate and / or succinate builders, to provide additional builder activity. Said use of fatty acids will generally result in a decrease in foam production, which can be taken into account by the formulator.
In situations where phosphorus-based detergency builders can be used, and especially the formulation of bars used for manual washing operations, the various alkali metal phosphates such as the well-known sodium tripolyphosphates, sodium pyrophosphate and the like can be used. sodium orthophosphate. Phosphonate detergency 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.
Bleach The detergent compositions herein may optionally contain bleaching agents or bleaching compositions containing a bleaching agent and one or more bleach activators. When present, 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 washing. If present, 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 bleach-plus-bleach activator. The bleaching agents used herein may be any of the bleaching agents useful for detergent compositions in textile cleaning, hard surface cleaning, or other cleaning purposes that are known or are now disclosed. These include oxygen bleaches as well as other bleaching agents. Perborate whiteners, for example, sodium perborate (eg, mono- or tetrahydrate) can be used herein. Another category of bleaching agent that can be used without restriction includes percarboxylic acid bleaching agents and salts thereof. Suitable examples of this class of agent include magnesium monoperoxyphthalate hexahydrate, the magnesium salt of metachlorophenobenzoic acid, 4-nonylamino-4-oxoperoxybutyric acid and diperoxydecanedioic acid. Such bleaching agents are described in the patent of E.U.A. 4,483,781, Hartman, issued November 20, 1984, patent application of E.U.A. 740,446, Burns et al., Filed June 3, 1985, European patent application 0,133,354, Banks et al., Published February 20, 1985, and patent of E.U.A. 4,412,934, Chung et al., Issued November 1, 1983. Most preferred bleaching agents also include 6-nonylamino-6-oxoperoxycaproic acid as described in the U.S. patent. 4,634,551, issued on January 6, 1987 to Burns et al. Peroxygen bleach agents can also be used. Suitable peroxygen bleach compounds include sodium carbonate peroxyhydrate and equivalent "percarbonate" bleaches, sodium pyrophosphate peroxyhydrate, urea peroxyhydrate, and sodium peroxide. Persulfate bleach can also be used (for example, OXONE, manufactured commercially by DuPont). A preferred percarbonate bleach comprises dry particles having an average particle size in the range of about 500 microns to about 1,000 microns, no more than about 10% by weight of said particles being less than about 200 microns and not more than about 200 microns. about 10% by weight of said particles being greater than about 1.250 microns. Optionally, the percarbonate can be coated with silicate, borate or water soluble surfactants. Percarbonate is available from several commercial sources such as FMC, Sovay and Tokai Denka. Mixtures of bleaching agents can also be used. Peroxygen bleaching agents, perborates, percarbonates, etc., are preferably combined with bleach activators, which leads to in situ production in aqueous solution (i.e., during the washing process) of the peroxyacid corresponding to the activator of bleach. Several non-limiting examples of activators are described in the U.S. patent. 4,915,854, issued April 10, 1990 to Mao et al., And the US patent. 4,412,934. The activators of nonanoyloxybenzenesulfonate (NOBS) and tetraacetylethylenediamine (TAED) are typical, and mixtures thereof can also be used. See also patent of E.U.A. 4,634,551 for other typical bleaches and activators useful herein. Most preferred amido-derived bleach activators are those of the formulas: R 1 N (R 5) C (O) R 2 C (O) L or R 1 C (O) N (R 5) R 2 C (O) L wherein R 1 is an alkyl group containing from about 6 to about 12 carbon atoms, R 2 is an alkylene containing from 1 to about 6 carbon atoms, R 5 is H or alkyl, aryl, or alkaryl containing from about 1 to about 10 carbon atoms, and L is any appropriate outgoing group. A leaving group is any group that is displaced from the bleach activator as a consequence of the nucleophilic attack in the bleach activator by the perhydrolysis anion. A preferred leaving group is phenylsulfonate. Preferred examples of bleach activators of the above formulas include (6-ocatanamido-caproyl) oxybenzenesulfonate, (6-nonanamidocaproyl) oxybenzenesulfonate, (6-decanamido-caproyl) oxybenzenesulfonate, and mixtures thereof as described in the patent of E.U.A. 4,634,551, which is incorporated herein by reference. Another class of bleach activators comprises the benzoxaine activators described by Hodge et al., In the U.S. patent. 4,966,723, issued October 30, 1990, which is incorporated herein by reference. A highly preferred benzoxaine type activator is: Another class of preferred bleach activators includes acyl-lactam activators, especially acylcaprolactams and acylvalerolactams of the formulas: wherein R6 is H or an alkyl, aryl, alkoxyaryl, or alkaryl group containing 1 to about 12 carbon atoms. Most preferred lactam activators include benzoylcaprolactam, octanoylcaprolactam, 3,5,5-trimethylhexanoylcaprolactam, nonanoylcaprolactam, decanoylcaprolactam, undecenoylcaprolactam, benzoylvalerolactam, octanoylvalerolactam, decanoylvalerolactam, undecenoylvalerolactam, nonanoylvalerolactam, 3,5,5-trimethylhexanoylvalerolactam and mixtures thereof. See also patent of E.U.A. 4,545,784, issued to Sanderson, October 8, 1985, which is incorporated herein by reference, which discloses acylcaprolactams, including benzoylcaprolactam, adsorbed on sodium perborate.
Bleaching agents other than oxygen bleaching agents are also known in the art and can be used herein. One type of non-oxygen bleaching agent of particular interest includes photoactivated bleaching agents such as sulfonated zinc and / or aluminum phthalocyanines. See patent of E.U.A. 4,033,718, issued July 5, 1977 to Holcombe et al. If used, the detergent compositions will typically contain from about 0.025% to about 1.25% by weight of such bleaches, especially sulfonated zinc phthalocyanine. If desired, the bleaching compounds can be catalyzed by a manganese compound. Such compounds are well known in the art and include, for example, the manganese-based catalysts described in the U.S.A. 5,246,621, patent of E.U.A. 5,244,594; patent of E.U.A. 5,194,416; patent of E.U.A. 5,114,606; and the publication of European patent application nos. 549.271A1, 549.272A1, 544.440A2, and 544.490A1. Preferred examples of these catalysts include Mnlv2 (uO) 3 (1, 4,7-trimethyl-1, 4,7-triazacyclononane) 2 (PF6) 2, Mn 'u-OJi (u- OAc) 2 (1, 4, 7-trimethyl-l, 4,7-triazacyclononane) 2- (CIO 4) 2; Mnlv4 (uO) 6 (1, 4,7-triazacyclononane) 4 (CIO4) 4, Mn '"Mnlv4 (uO)? (U-OAc) 2- (1, 4,7-trimethyl-1, 4,7- triazacyclononane) 2 (CIO 4) 3, Mn v (1, 4,7-trimethyl-1,4,7-triazacyclononane) - (OCH 3) 3 (PF 6), and mixtures thereof. metal-based bleaching include those described in US Patent 4,430,243 and US Patent 5,114,611 The use of manganese with various complex ligands to improve bleaching is also reported in the following US Patents 4,728,455, 5,284,944, 5,246,612, 5,256,770; 5,280,117; 5,274,147; 5,153,161; and 5,227,084 As a practical matter, and not by way of limitation, the compositions and methods herein can be adjusted to provide in the order of at least one part per ten million catalyst species. active bleaching in the aqueous wash solution, and preferably will provide from about 0.1 ppm to about 700 ppm, most preferably from about 1 ppm to about 500 ppm, of the catalyst species in the wash solution.
Enzymes Enzymes may be included in the formulations herein for a wide variety of fabric washing purposes, including removal of protein-based, carbohydrate-based, or triglyceride-based stains, for example, and to avoid dye transfer migratory, and for fabric restoration. Enzymes to be incorporated include proteases, amylases, lipases, cellulases, and peroxidases, as well as mixtures thereof. Other types of enzymes can also be included. They can be of any suitable origin, such as vegetable, animal, bacterial, fungal and yeast. However, its choice is governed by several factors such as pH activity and / or optimum stability, thermostability, stability against active detergents, builders, etc. In this regard, 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. In other words, the compositions herein will typically contain 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 0.005 to 0.1 Anson units (AU) of activity per gram of composition. Suitable examples of protease are the subtilisins which are obtained from particular strains of B. subtilis and B. licheniformis. Another suitable protease is obtained from a strain of Bacillus, which has a maximum activity in 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 by Novo. Suitable proteolytic enzymes for removing stains based on proteins 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). Other proteases include Protease A (see European patent application 130,756, published January 9, 1985) and Protease B (see European patent application series No. 87303761.8, filed on April 28, 1987, and European patent application 130,756 , Bott et al, published on January 9, 1985). Amylases include, for example, α-amylases described in British Patent Specification No. 1, 296,839 (Novo), RAPIDASE, International Bio-Synthetics, Inc. and TERMAMYL, Novo Industries. The cellulases that can be used in the present invention include both bacterial and fungal cellulose. Preferably, they will have an optimum pH between 5 and 9.5. Suitable cellulases are described in the US patent. 4,435,307, Barbesgoard et al, issued March 6, 1984, which describes fungal cellulose produced from Humicola insolens and strain DSM 1800 from Humicola or a fungus that produces cellulase 212 belonging to the genus Aeromonas, and cellulase extracted from the hepatopancreas from mollusc marine (Dolabella auricle Solander). Suitable cellulase 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 use include those produced by microorganisms of the Pseudomonas group, such as Pseudomonas stutzeri ATCC 19,154, as described in British Patent 1, 372,034. See also liasses in Japanese Patent Application 53,20487, open to public inspection on February 24, 1978. This lipase is available from Amano Pharmaceutical Co. Ltd., Nagoya, Japan, under the trade name Lipase P "Amano", that in the future will be called "Amano-P". Other commercial lipases include Amano-CES, lipases ex Choromobacter viscosum, e.g., Chromobacter viscosum var. lipolyticum NRRLB 3673, commercially available from Toyo Jozo Co., Tagata, Japan; and other Chromobacter viscosum lipases from U.S. Biochemical Corp., E.U.A. and Disoynth Co., The Netherlands, and lipases ex Pseudomonas gladioli. The LIPOLASE enzyme derived from Humicola lanuginosa and commercially available from Novo (see also EPO 341, 947) is a preferred lipase for use herein. Peroxidase enzymes are used in combination with oxygen sources, for example, percarbonate, perborate, persulfate, hydrogen peroxide, etc. They are used for "bleaching solutions" that is, to avoid transfer of dyes or pigments removed from substrates during washing operations to other substrates in the washing 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 described, for example, in PCT International Application WO 89/099813, published October 19, 1989, by O. Kirk, assigned to Novo Industries A / S. A wide range of enzyme materials and means for their incorporation into synthetic detergent compositions are also disclosed in U.S. Patent 3,553,139, issued January 5, 1971 to McCarty et al. In the patent of E.U.A. 4,101, 457, Place et al, issued July 18, 1978, and in the patent of E.U.A. 4,507,219, Hughes, issued March 26, 1985 also describes enzymes. Useful enzyme materials for liquid detergent formulations, and their incorporation into such formulations, are described in the US patent. 4,261, 868, Hora et al, issued April 14, 1981. Enzymes for use in detergents can be stabilized by various techniques. Enzyme stabilization techniques are described and exemplified in the US 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 the U.S. patent. 3,519,570. Other components that are commonly used in detergent compositions and that can be incorporated into the detergent tablets of the present invention include chelating agents, soil removal agents, soil anti-redeposition agents, dispersing agents, brighteners, suds suppressors, fabric softeners, agents for inhibiting the transfer of dyes and perfumes.
Washing method It is known to place traditional laundry detergent tablets in the wash tub together with laundry. However, this method tends to result in unpleasant-looking residues that appear visibly in the window, especially in certain types of washing machines that have been designed to operate with low water consumption. In extreme cases, visible residues may also be left on clothes at the end of the wash cycle due to incomplete dissolution. The present invention relates to a washing method that 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 laundry detergent solution is formed by dissolving in water a tablet formed by compressing material formed from particles, the tablet comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesion effect on the material formed from particles. In a preferred embodiment according to the invention, the method relates more specifically 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 an assortment compartment and a washing tub, wherein the aqueous laundry detergent solution is formed by dissolving a detergent tablet in water, characterized in that the detergent tablet is placed in the assortment compartment and water is passed through the assortment compartment in a manner that the tablet be stocked as an aqueous solution of a laundry detergent, the aqueous solution being subsequently passed in the wash tub.
EXAMPLES The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The anionic agglomerates 2 comprise 40% anionic surfactant, 28% zeolite and 32% carbonate.
The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate. The layered silicate comprises 95% SKS 6 and 5% silicate. The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylenediamine-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylene diamine-N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The binder sprinkler system comprises 50% Lutensit K-HD 96 and 50% PEG (polyethylene glycol).
EXAMPLE 1 (It comprises a highly soluble compound that has a cohesion effect on the material formed of particles) i) A detergent base powder of composition A (see the table above) was prepared as follows: all material formed from particles of composition A base was mixed in a mixing drum to form a homogeneous particulate formed mixture. During this mixing, the sprays were carried out. ii) 97 parts of the base powder of composition A were mixed in a mixing drum with 3 parts of sodium diisoalkylbenzenesulfonate (highly soluble compound having a cohesion effect on the material formed from particles). Ii) The tablets were then manufactured in the following manner: 50 g of the mixture was introduced into a circular mold with a diameter of 5.5 cm and compressed to give a tablet tensile strength (or diametral fracture stress) ) of 15 kPa. The force required to obtain a tablet tensile strength of 15 kPa was 2400 N. The height of the tablet was 1.94 cm. V) The level of waste in a washing machine dispenser was evaluated by the "Tablet assortment test": two laundry tablets are placed in a Baucknecht WA9850 dispenser. The water supply to the washing machine is adjusted to a temperature of 20 ° C and a hardness of 3.57 g / l, the spout water inlet flow rate is adjusted to 8 l / min. The level of tablet residues remaining in the dispenser is verified by changing the wash ignition and the wash cycle setting to wash program 4 (color / blanks, short cycle). The assortment percentage residue is determined as follows:% of assortment = [(weight of waste) x 100] / (weight of original tablet) The assortment% is shown in the "Assortment waste" box.
EXAMPLE 2 (Highly soluble compound) i) The same composition A was prepared following the same procedure as in example 1. ii) 97 parts of base powder of composition A were mixed in a mixing drum with 3 parts of sodium toluenesulfonate (highly soluble compound). iii) The tablets were then manufactured in the same manner as described in Example 1. The force required to obtain a tablet tensile strength of 15 kPa was 3100 N. The height of the tablet was 1.88 cm. iv) The level of waste in a washing machine dispenser was evaluated following the same procedure as described in example 1. The assortment% is shown in the "Assortment waste" box.
EXAMPLE 3 (Highly soluble compound) i) The same composition A was prepared following the same procedure as in example 1. ii) 97 parts of base powder of composition A were mixed in a mixing drum with 3 parts of Sorbitol (highly soluble compound). iii) The tablets were then manufactured in the same manner as described in Example 1. The force required to obtain a tablet tensile strength of 15 kPa was 3500 N. The tablet height was 1.83 cm. iv) The level of waste in the spout of a washing machine was evaluated following the same procedure as described in example 1. The assortment% is shown in table 3.
EXAMPLE 4 (Compound having a cohesion effect on the material formed from particles) i) The same composition A was prepared following the same procedure as in example 1. ii) 97 parts of base powder of composition A were mixed in a mixing drum with 3 parts of sodium dodecylbenzenesulfonate (compound having an effect of cohesion on the material formed of particles). iii) The tablets were then manufactured in the same manner as described in Example 1. The force required to obtain a tablet tensile strength of 15 kPa was 2600 N. The tablet height was 1.95 cm. iv) The level of waste in the spout of a washing machine was evaluated following the same procedure as described in example 1. The assortment% is shown in table 3.
EXAMPLE 5 (Composition of material formed from base particles) i) The same composition A was prepared following the same procedure as in example 1. i) The tablets were then manufactured in the same manner 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. iii) The level of waste in the spout of a washing machine was evaluated following the same procedure as described in example 1. The assortment% is shown in table 3.
Results: Assortment Waste Chart: Conductivity chart for the compounds added to composition A to obtain the tablets of examples 1 to 4: Another composition of material formed of base particles: The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The anionic agglomerates 2 comprise 40% anionic surfactant, 28% zeolite and 32% carbonate. The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate.
The layered silicate comprises 95% SKS 6 and 5% silicate. The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylenediamine-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylene diamine-N, N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The binder sprinkler system comprises 50% Lutensit K-HD 96 and 50% PEG (polyethylene glycol).
EXAMPLE 6 (Composition of material formed from base particles) i) Composition B was prepared following the same procedure as in example 1. ii) The tablets were then manufactured in the same manner as described in example 1. The applied force was 2000N. The tablet tensile strength was 10.9 kPa.
EXAMPLE 7 (PEG) i) The same composition B was prepared following the same procedure as in example 1. ii) 97 parts of base powder of composition A were mixed in a mixing drum with 3 parts of PEG (binding compound). iii) The tablets were then manufactured in the same manner as described in Example 1. The force applied was 2000N. The tablet tensile strength was 12.8 kPa.
EXAMPLE 8 (Sodium diisoalkylbenzenesulfonate) i) The same composition B was prepared following the same procedure as in example 1. ii) 97 parts of base powder of composition A were mixed in a mixing drum with 3 parts of sodium diisoalkylbenzenesulfonate, ii) After the tablets were added. manufactured in the same way as described in Example 1. The applied force was 2000N. The tablet tensile strength was 17.8 kPa.
EXAMPLE 9 OF A TABLET ACCORDING TO THE INVENTION i) A detergent base powder of composition C was prepared in the following manner: all the particulate formed materials of base composition C were mixed in a mixing drum to form a homogeneous particulate formed mixture. During this mixing, the sprays were performed. After the spraying the sodium diisoalkylbenzenesulfonate (= DIBS) was added to the rest of the matrix. ii) The tablets were then manufactured in the following manner: 43 g of the mixture were introduced into a circular mold with a diameter of 5.5 cm and compressed to give a tablet tensile strength (or diametral fracture stress) of 15 kPa. (Ii) The assortment percentage residue of the 43g tablet was less than 15%.
The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The anionic agglomerates 2 comprise 40% anionic surfactant, 28% zeolite and 32% carbonate. The nonionic agglomerates comprise 26% nonionic surfactant, 6% Lutensit K-HD 96, 40% anhydrous sodium acetate, 20% carbonate and 8% zeolite. The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate.
The layered silicate comprises 95% SKS 6 and 5% silicate. The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylenediamine-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylenediamine-N, N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The binder sprinkler system comprises 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEG. Also, the following experiment was carried out, wherein the dissolution of a non-tableted granulated material was tested with and without a highly soluble compound, ie, DIBS: Detergent of composition D was prepared as follows: all materials formed from particles except the dried zeolite were mixed together in a mixing drum to form a homogeneous particulate formed mixture. During this mixing, the sprays were performed. After the spraying, the dust formation was carried out with the dry zeolite.
TABLE 1 Composition of detergent base powder The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate. The layered silicate comprises 95% SKS 6 and 5% silicate.
The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylenediamine-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylenediamine-N, N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The perfume encapsulates comprise 50% perfume and 50% starch. The polymer particle comprises 36%, 54% zeolite and 10% water. The non-ionic spray system comprises 67% C12-C15 AE5 (alcohol with an average of 5 ethoxy groups per molecule), 24% N-methylglucosamide and 9% water. 150 grams of this granular detergent of composition D were introduced into the assortment compartment of a "Hotpoint" washing machine. The water supply of the washing machine was adjusted to a temperature of 20 ° Celsius and a hardness of 3.57 g / l, at a flow rate of 2 liters per minute. After two minutes, 38 grams of the detergent composition D remained undissolved in the assortment compartment. 145 grams of this granular detergent of composition D were mixed with 5 grams of DIBS. This granulated mixture was introduced into the dispensing compartment of a "Hotpoint" washing machine. The water supply of the washing machine was adjusted to a temperature of 20 ° Celsius, at a hardness of 3.57 g / l, at a flow rate of 2 liters per minute. After two minutes, 30 grams of the detergent composition D remained undissolved in the assortment compartment. In another preferred embodiment according to the examples below, it was found that the addition in the formed material of particles of a highly soluble compound, the highly soluble compound being preferably a hydrotrope compound, together with a mixture of at least two polymers , further favored dissolution, this synergistic effect taking place in particular with a mixture of polymers such as PEG (polyethylene glycol), more in particular PEG having a molecular weight between 200 and 9000, preferably a mixture of PEG having a molecular weight of 1000 and 4000 was found convenient. Such PEGs are described, for example, in EP-A-0 522 766. Other polymers include cationic polymers such as Lutensit KHD96. The molecular weight is considered herein as an average molecular weight for a given molecular weight distribution.
EXAMPLE A (Formulation used for modified National Wave 1) i) A detergent base powder of the composition E (see below) was prepared in the following manner: all the particulate formed materials of the base composition E were mixed in a mixing drum to form a homogeneous particulate formed mixture. During this mixing, the sprays were carried out. After the spray, the sodium diisoalkylbenzenesulfonate (sticky hydrotrope) was added to the rest of the matrix. ii) The tablets were then manufactured in the following manner: 43 g of the mixture were introduced into a circular mold with a diameter of 5.5 cm and compressed to give a tablet tensile strength (or diametral fracture stress) of 15 kPa. i) The tablets were then immersed in a bath comprising 80 parts of sebacic acid mixed with 20 parts of Nymcel zsb16 to 140C. The time that the tablet was submerged in the heated bath was adjusted to allow the application of 3g of the mixture described therein. Then the tablet was allowed to cool to room temperature of 25C for 24 hours. iv) the level of waste in a washing machine spout was evaluated by means of a "low effort tablet assortment test": two wash tablets are placed in a Bauknecht WA9850 spout. The water supply to the washing machine is adjusted to a temperature of 8C and a hardness of 3.57 g / l, the spout water inlet flow rate is adjusted to 41 / min. The level of tablet waste remaining in the dispenser is checked by allowing water to flow through the dispenser for 78 sec. The assortment percentage residue is determined as follows: Assortment waste% = waste weight "100 original tablet weight The assortment% is shown in the tables below.
EXAMPLE B The procedure for preparing tablets of Example A was repeated for powder of composition F. The polymer sprayed on the matrix contained 0.67 parts of PEG4000 and 0.33 parts of PEG 1000. The use of a mixture of two PEG polymers led to better results of Assortment than the use of a PEG.
Detergent base powder compositions E and F The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The anionic agglomerates 2 comprise 40% anionic surfactant, 28% zeolite and 32% carbonate.
The non-ionic agglomerates comprise 26% nonionic surfactant, 6% Lutensit K-HD 96, 40% anhydrous sodium acetate, 20% carbonate and 8% zeolite. The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate. The layered silicate comprises 95% SKS 6 and 5% silicate. The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of etiiendiamino-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylenediamine-N, N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The binder sprinkler system comprises 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEG.
EXAMPLE C-D The procedure for preparing tablets of Example A was repeated for powder of composition G-H. The tensile strength of the tablet before its coating with the mixture of sebacic acid and Nymcel was 12 kPa.
The use of a mixture of three polymers led to better assortment results than the use of two polymers.
Detergent base powder compositions G and H The anionic agglomerates 1 comprise 40% anionic surfactant, 27% zeolite and 33% carbonate. The anionic agglomerates 2 comprise 40% anionic surfactant, 28% zeolite and 32% carbonate.
The nonionic agglomerates comprise 26% nonionic surfactant, 6% Lutensit K-HD 96, 40% anhydrous sodium acetate, 20% carbonate and 8% zeolite. The cationic agglomerates comprise 20% cationic surfactant, 56% zeolite and 24% sulfate. The layered silicate comprises 95% SKS 6 and 5% silicate. The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylenediamine-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylenediamine-N, N-disuccinic acid, 23% sulfate and 19% water. Sulfonated zinc phthalocyanine encapsulates are 10% active. The foam suppressor comprises 11.5% silicone oil (ex Dow Corning); 59% zeolite and 29.5% water. The binder sprinkler system comprises 0.5 parts of Lutensit K-HD 96 and 2.5 parts of PEG.

Claims (11)

NOVELTY OF THE INVENTION * * CLAIMS
1. A tablet formed by compressing a material formed of particles, the material formed of particles comprising a surfactant and a highly soluble compound, the highly soluble compound having a cohesion effect on the material formed of particles.
2. The tablet according to claim 1, further characterized in that at least 1% by weight of the tablet is formed from the highly soluble compound, preferably at least 2% by weight.
3. The tablet according to claim 1, further characterized in that the highly soluble compound comprises sodium diisolakylbenzenesulfonate.
4. The tablet according to claim 1, further characterized in that the tablet has a tensile strength of more than 5 kPa, and preferably of less than 300 kPa.
5. The tablet according to claim 1, characterized in that the tablet is compressed using a force of less than 100000 N.
6. - The tablet according to claim 1, further characterized in that the tablet contains at least 5% by weight of ! _ Surfactant.
7. The tablet according to claim 1, further characterized in that the highly soluble compound is a hydrophotic compound.
8. A coated tablet, characterized in that the uncoated tablet is in accordance with any of the preceding claims.
9. The tablet according to any of the preceding claims, further characterized in that the material formed of particles comprises a mixture of at least two polymers.
10. A method for preparing an aqueous solution of a "Laundry detergent for use in a washing machine, characterized in that the aqueous laundry detergent solution 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 cohesion effect on the material formed of particles.
11. The method according to claim 10, the tablet 20 having a density of at least 0.9 g / cc, preferably less than 2 g / cc.
MXPA/A/2001/000373A 1998-07-10 2001-01-10 Detergent tablet with high mechanical and dissolution characteristics MXPA01000373A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP98870151.2 1998-08-24
EP98870181 1998-08-24

Publications (1)

Publication Number Publication Date
MXPA01000373A true MXPA01000373A (en) 2001-09-07

Family

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