MXPA01000528A - Process for producing a powder from a tablet - Google Patents

Process for producing a powder from a tablet

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Publication number
MXPA01000528A
MXPA01000528A MXPA/A/2001/000528A MXPA01000528A MXPA01000528A MX PA01000528 A MXPA01000528 A MX PA01000528A MX PA01000528 A MXPA01000528 A MX PA01000528A MX PA01000528 A MXPA01000528 A MX PA01000528A
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MX
Mexico
Prior art keywords
tablet
powder
tablets
weight
acid
Prior art date
Application number
MXPA/A/2001/000528A
Other languages
Spanish (es)
Inventor
Jose Luis Vega
Novo Maria Del Mar Ollero
Dijk Paul Irma Albertus Van
Original Assignee
The Procter & Gamble Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by The Procter & Gamble Company filed Critical The Procter & Gamble Company
Publication of MXPA01000528A publication Critical patent/MXPA01000528A/en

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Abstract

The present invention relates to a process for producing a powder from a tablet, the tablet having a tensile strength of at least 5 kilo Pascal, the tablet comprising at least 2%by weight of surfactants, whereby the process is characterised in that it comprises a first step of submitting the tablet to mechanical degradation, and a second step of sifting to obtain the powder, whereby the powder obtained comprises less than 4%per weight of particles passing through a 150 micro meter sieve.

Description

PROCEDURE TO PRODUCE A DUST FROM A TABLET The present invention relates to a process for producing a powder from detergent tablets, especially those adapted for use in washing. Detergent tablets are widely used in different types of washing or cleaning applications. In automatic dishwashing application, such tablets are produced from an original highly compressed powder having a given chemical composition, wherein the highly compressed tablet is not sensitive to mechanical stress because it is solid, and wherein the tablet dissolves easily in the dishwasher to produce the aqueous solution comprising surfactants. In the process of producing such tablets, it may happen that a low proportion of the tablet produced is not suitable for use, for example, due to an unsuitable chemical composition, or due to line breakage. In such a case, the tablets that are not suitable for use are typically recirculated by grinding and dissolving the unsuitable tablets to form a solution, so that a powder can be obtained from this solution, this powder being added in small proportion to the powder original that is going to be compressed again to make suitable tablets to be used.
The present invention relates to a process for producing a powder from a tablet, the tablet having a tensile strength of at least 5 kilo Pascal, the tablet comprising at least 2% by weight of surfactants. One of the advantages of said method is that it can be used to reduce waste in the environment while maintaining satisfactory quality for the tablets to be used. Although having these and other advantages, existing methods for producing a powder from a tablet, in particular the methods used to recirculate tablets for automatic dishwashing, have disadvantages. For example, the granular structure of the recirculated powder is different from the original powder due to the crushing and dissolution of the tablet made from the original powder. The invention seeks to provide a process of the aforementioned type that allows obtaining a recirculated powder while having a satisfactory control over the granulated structure of the recirculated powder.
BRIEF DESCRIPTION OF THE INVENTION According to the invention, this object is carried out in a method of the above type since it comprises a first step of subjecting the tablet to mechanical degradation, and a second step of sifting to obtain the powder, wherein the powder obtained comprises less of 4% by weight of particles passing through a 150 micron sieve. A method according to the invention has a number of advantages. Because the recirculation of the tablet is carried out using mechanical agitation and sieving, the recirculated powder can be obtained without going through a dissolution step, although it may be preferred to add said step under particular conditions. In addition, sieving taken in combination with mechanical agitation makes it possible to control the granular structure of the product, so that the level of fine particles passing through the 150 micron sieve is kept to a minimum. It should be mentioned that the 150 micron sieve is introduced to define the level of fine particles obtained in the recirculated powder obtained, and is usually different to the medium used in the second sieve step.
DETAILED DESCRIPTION OF THE INVENTION The invention relates to a process for producing a powder from a tablet, the tablet having a tensile strength of at least 5 kPa. In a preferred embodiment according to the invention, the tensile strength is at least 10 kPa, preferably at least 15 kPa and more preferably at least 20 kPa, so that the tablet is mechanically strong enough while dissolves easily The tablet also comprises 2% by weight surfactants. In a preferred embodiment according to the invention, the tablet comprises at least 5% by weight of surfactants, preferably 10% by weight of surfactants, preferably at least 15% and most preferably at least 20%. Indeed, the invention relates more particularly to laundry tablets, laundry tablets having a particularly high level of surfactant. The process according to the invention comprises a first step, wherein the tablet is subjected to mechanical degradation. Mechanical degradation can be obtained by different means, the preferred means for mechanical degradation being provided by centrifugation, preferably by use of a fine centrifugal screen, in particular a KEUTEC fine KEK centrifugal sieve, preferably a KEMUTEC K650. The second step of the procedure is to sift to obtain the powder. Indeed, after being subjected to mechanical degradation, the tablet is not a solid block but consists of a plurality of grains having a particular grained structure. Sifting allows selecting a part of this granulated structure. In a preferred embodiment according to the invention, the sieving is obtained by a mesh having a plurality of openings of 5 mm in diameter. The rest of the granulated structure is removed and does not form part of the obtained powder. Typically, the rest of the granulated structure that is not subjected to the second step represents less than 1% by weight of the total of the granulated structure. Preferably, the rest of the granulated structure is reinserted at the beginning of the procedure together with the tablets to be processed, in order to close the process cycle. According to the invention, the powder obtained is such that it comprises less than 4% by weight of particles that pass through a 150 micron sieve. In a preferred embodiment, the powder obtained is such that it comprises less than 3.5% by weight of particles passing through the 150 micron sieve. It should be mentioned that the 150 micrometer sieve referred to is usually different from the sieving means used in the second step according to the invention, and that it is mentioned in order to provide means to analyze the granular structure of the powder obtained. The reduction to the minimum of the level of fine particles allows to improve the sanitary and environmental characteristics of the obtained powder. This applies more particularly to a tablet comprising enzymes, wherein it is preferred that the enzyme components of the tablet do not decompose during the process. The decomposition of the percarbonate components should also be avoided, since the stability of the finished product could be affected. Indeed, in a preferred embodiment, the invention relates to a tablet comprising percarbonates. Likewise, limiting the level of fine particles allows a better solution for a tablet in a washing environment to be obtained if a tablet comprising the obtained powder is made. The invention particularly applies to remixing unsatisfactory tablets to an original powder, wherein the powder obtained is added to an original powder to form a mixture, the added powder constituting at least 1% and up to 20% by weight of the mixture, the mix being compressed to form a tablet. Preferably, in such a case, the powder obtained comprises a weight percentage of particles that pass through a 150 micron sieve that is less than twice the weight percentage of particles that pass through a 150 micron sieve and form part of the original powder. In fact, the closer the granulated structure of the powder obtained to the original powder, in particular with respect to fine particles, the more reliable the remixing process will be. In such a case, the original tablet that is subjected to the process according to the invention is as such manufactured typically by compressing the original powder, and adding or not a coating. Typically, the invention relates to tablets having a tensile strength of less than 100 kPa. More tablets having a tensile strength of less than 80 kPa are preferred, even more tablets having a tensile strength of less than 50 kPa are preferred, and tablets with a tensile strength of less than 50 kPa are preferred. of 30 kPa. Indeed, the tablets according to the invention must be easily dissolved in a washing environment, so that the tablets should not be compressed excessively. It should be mentioned that the process according to the invention could also be considered to produce a powder from a tablet typically used for automatic dishwashing, although the dissolution characteristics are not as demanding as for laundry laundry tablets, so that the invention is even more favorable when applied to laundry tablets. When applied industrially, the process according to the invention allows a plurality of tablets to be treated at a rate of at least 7.56 and up to 20.16 kilograms per second and by mechanical degradation and screening means. A speed between 17.64 and 20.16 kilograms per second is even more preferred.
Highly soluble compounds The tablet according to the invention may further comprise a highly soluble compound to further facilitate dissolution.
Said compound could be formed from a mixture or from a single compound. 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 are 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 beaker Sotax 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 The tablet according to the invention could also comprise a compound or a mixture of compounds having a cohesion effect, so that the tablet could be mechanically even more resistant to a constant compression force. 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 pressed 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. It is worth mentioning that in particular, by integrating a highly soluble compound having a cohesion effect on a tablet formed by compressing a material formed of particles comprising a surfactant, the dissolution of the tablet in an aqueous solution was significantly increased. In a preferred embodiment, at least 1% by weight of the tablet is formed from 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 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. A 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 tensile strength equal to a lower compaction force at Comparison with traditional tablets. Typically, the tablet will have a tensile strength of more than 5kPa, preferably more than 10kPa, preferably, in particular for use in laundry applications, of more than 15kPa, most preferably of more than 30 kPa; and a tensile strength of less than 100 kPa, preferably less than 80 kPa and most preferably less than 60 kPa. Indeed, in case of application for laundry, the tablets should be less compressed than in the case of applications for automatic dishwashing, for example, where the dissolution is more easily achieved, so that in a wash application of clothes, the tensile strength is preferably less than 30 kPa. This allows to produce tablets having a strength and mechanical strength comparable with 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 together 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, compacting methods (e.g., 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 needs not to exceed 00000 kN / m2, preferably not to exceed 30000 kN / m2, preferably not to exceed 5000 kN / m2, most preferably not to exceed 3000 kN / m2 and most preferably not to exceed 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 and most preferably less than 1.1 g / cc.Hydrotrope Compound In a preferred embodiment of the invention, the tablet also comprises a hydrotrope compound that further favors the dissolution of the tablet in an aqueous solution, a specific compound being defined as hydrotrope in the following manner (see SE 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 salts and ammonium benzenesulfonate salts derived from toluenesulfonic acid, xylenesulfonic acid, cumenesulfonic acid, tetralinsulfonic acid, naphthalenesulfonic acid, methylnaphthalenesulfonic acid, dimethylnaphthalenesulfonic acid, trimethylnaphthalenesulfonic acid.
Other examples include salts of dialkylbenzenesulfonic acid such as salts of diisopropylbenzenesulfonic acid, ethyl methyl benzenesulfonic acid, alkylbenzenesulfonic acid with an alkyl chain length of 3 to 10, (preferably 4 to 9), linear or branched alkyl sulfonates 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) 1-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 Polymer hydrotropes such as those described in EP636687: 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 compound 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 can then be coated so that the tablet does not absorb moisture, or absorb moisture only at a very slow rate. The coating is also resistant so that moderate mechanical shocks to which the tablets are subjected during handling, packing and shipping result in very low breaking or friction levels. Finally, the coating is preferably brittle so that the tablet decomposes when subjected to stronger mechanical shock. In addition, it is favorable if the coating material is dissolved 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, carboxymethylcellulose, algenic acid and its salts including sodium alginate, silicon dioxide, clay, polyvinylpyrrolidone, 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 pDt 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. (Pharmaceutical Dosage Forms Method: 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. Typically, the tablet according to the invention will have a tensile strength in a direction normal to the main axis of more than 5kPa, preferably of more than 10kPa, preferably, particularly for use in laundry applications, of more than 15kPa, most preferably more than 20kPa. The tablet according to that invention should also be easily dissolved so that it has a tensile strength of preferably less than 75kPa, and most preferably less than 50kPa. 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 original tablet The residue level is determined by repeating the procedure 10 times and an average residue level is calculated based on the 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 which is a compound that favors further dissolution of the tablet in an aqueous solution. "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 must 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 from about 1% to about 55%, by weight, include conventional C-β-C? 8 alkylbenzene sulfonates ("LAS") and C 10 -C 20 alkyl sulfates ( "AS") of branched and random chain, the secondary Cι-C.β alkyl sulphates (2,3) of the formula CH 3 (CH 2) ((CHOS 3 3-M +) CH 3 and CH 3 (CH 2) and (CHOSO 3-M +) CH2CH3 where xy (and +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 olenylsulfate, C-? Or C alkylalkoxy sulfates, 8 ("AEXS", especially ethoxysulfates EO 1-7), alkylalkoxycarboxylates of C 0 -C 8 (especially the ethoxycarboxylates EO 1-5), the glycerol ethers of C 10 -? S, the alkyl polyglucosides of C 10 -C 18 and their corresponding sulphated polyglycosides, and alpha-sulfonated fatty acid esters of C? 2-C-? 8. If desired, conventional non-ionic and amphoteric surfactants such as C- | 2-C? 8 alkyl ethoxylates ("AE") including so-called narrow peak alkyl ethoxylates and C6-Cl2 alkylphenol alcoxylates (especially ethoxylates and ethoxy / mixed propoxy), C12-C18 betaines and sulfobetaines ("sultaines"), C-IO-C-IS amine oxides, and the like can also be included in the general compositions. The N-alkylamides of polyhydroxy fatty acids of C? O-C- | 8 can also be used. Typical examples include the N-methylglucamides of C? 2-C? 8. See WO 9,206,154. Other surfactants derived from sugar include polyhydroxy fatty acid N-alkoxyamides, such as C 0 -C 8 N- (3-methoxypropyl) glucamide. The N-propyl N-hexyl glucamides of C, 2-C-? S can be used for low foam production. Conventional C? 0-C2o soaps can also be used - If high foam production is desired, the branched-chain C10-Ci6 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-gelling binders Non-gelling binders can be integrated into the particles forming the tablet to facilitate further dissolution. Such compounds further promote the dissolution of the tablet in an aqueous solution. If non-gelling binders are used, 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, sodium 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 liquid non-aqueous binders (ie, not in aqueous solution) are preferred 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. The 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 the 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 or P-containing detergent builders 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 an SiO2: NaO ratio in the 1.6: 1 to 3.2: 1 scale and layered silicates, such as the layered sodium silicates described in US Pat. 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-Na2S¡Os silicate morphology in layers. 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? 2? +? - 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, as the forms alpha, beta and gamma. As mentioned above, delta-Na2SiO5 (NaSKS-6 form) is more preferred for use herein. Other silicates can also be useful, for example, magnesium silicate, which can 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 most heavy duty granular detergent compositions marketed today, and can also be a significant detergency enhancing ingredient in liquid detergent formulations. Aluminosilicate detergency builders include those having the empirical formula: where z and y are integers of at least 6, the molar ratio of zay is in the range of 1.0 to about 0.5, and x is an integer of 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: Na12 [(AI02) 12 (S? O2) i2] -xH2? 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 ether polycarboxylates, including oxydisuccinate, as described in Berg, U.S. 3,128,287, issued April 7, 1964, and Lamberti et al, US Patent 3,635,830, issued January 18, 1972. See also detergency 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 mellitic acid, succinic acid, oxydisuccinic acid, polymaleic acid, benzene-1, 3,5-tricarboxylic acid, carboxymethyloxysuccinic acid, and soluble salts of the same. Citrate detergent 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 due to 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-i2-C? 8 monocarboxylic acids, can also be incorporated into the compositions alone, or in combination with the aforementioned builders, especially citrate and / or succinate builders. , to provide additional detergency 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, US 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 agents include magnesium monoperoxyphthalate hexahydrate, the magnesium salt of metachloroperbenzoic 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, Bums et al., Filed June 3, 1985, European patent application 0,133,354, Banks et al., Published February 20, 1985, and US patent. 4,412,934, Chung et al., Issued November 1, 1983. Most preferred bleaching agents also include 6-nonyl-6-yl-6-oxoperoxycaproic acid as described in the U.S.A. 4,634,551, issued on January 6, 1987 to Bums 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 suitable leaving 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 perhydrotic 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. 549.271 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) 2 (PF6) 2, Mnlll2 (u-0) 1 (u- OAc) 2 (1, 4,7-trimethyI-1, 4,7-triazacyclononane) 2- (CIO 4) 2; Mnlv4 (uO) 6 (1, 4,7-triazacyclononane) 4 (CIO4) 4, Mn ^ Mn ^ u-OJ ^ u-OAcHI, 4,7-trimethyl-1, 4,7-triazaciclonane) 2 (CIO) 3, Mn? V (1, 4,7-trimethyl-1, 4,7-triazacyclononane) - (OCH) 3 (PF6), and mixtures thereof. Other metal-based bleach catalysts include those described in the U.S.A. 4,430,243 and patent of E.U.A. 5,114,611. The use of manganese with various complex ligands to improve bleaching is also reported in the following U.S. 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. As a practical matter, and not by way of limitation, the compositions and methods herein can be adjusted to provide in order of at least one part per ten million active bleach catalyst species 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. 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 Humicola or a fungus that produces cellulase 212 belonging to the genus Aeromonas, and cellulase extracted from the hepatopancreas of a marine mollusk (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 lipases 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 Ll POLAS E 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 described 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, foam suppressants, fabric softeners, dye transfer inhibiting agents and perfumes.
EXAMPLES The following procedure was carried out according to the invention: the tablets are fed into a feedworm by means of a fine sieve inlet at a speed of 17.64 kg / s. The feeding worm carries the tablets inside a cylindrical sieving chamber. The tablets are collected by a rotating vane assembly and are launched centrifugally against a sieve of a size that has a mesh size of 5mm. The blades in the blade assembly are placed in a helix configuration to carry the material over the entire length of the sieve. The obtained powder passes through the sieve and is collected in the main fine sieve outlet. The rest of the material is taken to the end of the sieving chamber and is discharged through a separate outlet. Equipment specifications: the fine screen cover is manufactured from carbon steel coated with epoxy resin. The motor, couplings and bearings are located outside the processing area so as not to come into contact with the product. The impulse arrow is made of stainless steel and carries both the feeding worm and the paddle assembly. The design of the frame of sieve is a construction of 3 armours of 3 rings all welded or construction with bolts in carbon steel or stainless steel.
The fine centrifugal sieve has been used for circular tablets. The dimensions are: weight: 53 + 1-2 g diameter: 54 mm, height 21.5 +/- 0.25 mm, tensile strength of the tablets: 35 +/- 4 Kpa. The chemical composition A of the tablets without coating is as follows: 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. t The bleach activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (acid form) and 2% water. The sodium salt particle of ethylene-amino-N, N-disuccinic acid / sulfate comprises 58% sodium salt of ethylene diamine-10 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. 15 The binder sprinkler system comprises 50% Lutensit K-HD 96 and 50% PEG (polyethylene glycol).
Production of the tablet i) Detergent base powder of composition A (see table) above) was prepared as follows: all were made for the material formed from particles of composition A based on a spray drum, before being mixed together in a mixing drum to form a homogeneous formed particle mixture. ii) The tablets were then manufactured in the following manner: 53 g of the mixture were introduced into a mold of the appropriate circular or rectangular shape and compressed. iii) The tablets were immersed in a bath comprising 80 parts of sebacic acid mixed with 20 parts of Nymcel zsb16. He 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. The powder obtained had a granulated structure in comparison with the granular structure of the original matrix A as follows: I fifteen The above table should read as follows: The powder obtained has 18.6% by weight of material remaining in the sieve of 1180 micrometers, which is compared with 9.66% by weight of the original mixture obtained after step i) above which it remains in the sieve of 1180 micrometers. The 6 sieves (1180, 850, 450, 250 and 150 micrometers) are placed one on top of the other, the larger mesh size in the upper part and the smaller mesh size in the lower part, so that the granulated structure can be analyzed The percentage by weight of the particles that pass through all the sieves, that is, the "through 150", represents the percentage by weight of fine particles. The above table also indicates the average particle size for the material considered. The most relevant measure to the invention is that the level of fine particles passing through the 150 micron sieve is below 4% by weight for the powder obtained, and is less than twice the percentage by weight of the particles that pass through the 150 micron sieve and forms part of the original powder or original mixture. It should be mentioned that the tablet subjected to the process according to the invention and described in this example has a coating, the powder obtained compared to the original powder or mixture used to make the tablet without coating. The procedure also applies to uncoated tablets.

Claims (10)

  1. NOVELTY OF THE INVENTION CLAIMS r 5 1. A process for producing a powder from a tablet, the tablet having a tensile strength of at least 5 kilo Pascal, the tablet comprising at least 2% by weight of surfactants, characterized in that the process it comprises a first step of subjecting the tablet to mechanical degradation, and a second step of sifting to obtain the powder, characterized in that the powder obtained comprises less than 4% by weight of particles passing through a 150 micron sieve.
  2. 2. The method according to claim 1, further characterized in that the tablet is obtained by compressing an original powder.
  3. 3. The method according to claim 2, further characterized in that the powder obtained comprises a weight percentage of particles that pass through a 150 micron sieve that is less than twice the percentage by weight of particles passing through. of a 20 sieve 150 micrometers and is part of the original powder.
  4. 4. The process according to claim 1, further characterized in that the powder obtained is added to an original powder to form a mixture, the added powder constituting at least 1% and up to 20% by weight of the mixture, the mixture being compressed to form a tablet.
  5. 5. The method according to claim 1, further characterized in that the tablet has a tensile strength of less than 100 kilograms Pascal.
  6. 6. The method according to claim 1, further characterized in that the tablet comprises a coating.
  7. 7. The method according to claim 1, further characterized in that the tablet comprises enzymes.
  8. 8. The method according to claim 1, further characterized in that the mechanical degradation is provided by centrifugation.
  9. 9. The method according to claim 1, further characterized in that the screening is obtained by a mesh having a plurality of openings of 5 mm in diameter.
  10. 10. The method according to claim 1, further characterized in that the method applies a plurality of tablets at a speed of at least 7.56 and up to 20.16 kilograms per second.
MXPA/A/2001/000528A 1998-07-16 2001-01-15 Process for producing a powder from a tablet MXPA01000528A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP98202401 1998-07-16

Publications (1)

Publication Number Publication Date
MXPA01000528A true MXPA01000528A (en) 2001-09-07

Family

ID=

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