ES2212513T3 - DETERGENT COATED PAD. - Google Patents

Abstract

A coated detergent tablet, characterized in that the coating comprises reinforcing fibers.

Description

Coated detergent tablet.

The present invention relates to tablets coated detergents, especially those intended for use in machine wash, and procedures to make the tablets coated detergents

Although they have frequently been proposed cleaning compositions in the form of pills, these (except for bars of soap for personal washing) have not achieved success substantial, despite the several advantages that the unitary use products. One of the reasons for this it may be that detergent tablets need a procedure of relatively complex manufacturing. In particular, it is often desirable to provide the tablet with a coating, which adds to The difficulties of manufacturing.

Although the uncoated tablets are completely effective in terms of use, usually they lack the surface hardness necessary to resist the friction that is part of the normal procedures of manufacturing, packaging and handling. The result is that uncoated tablets experience friction during these processes, which leads to the detachment of particles and the loss of active material.

Finally, it is often desired to coat the pills for aesthetic purposes, to improve the exterior image of the pills and produce some particular aesthetic effect. They have proposed numerous methods of coating pills and many of them have been suggested for detergent tablets. Nevertheless, All these methods have certain disadvantages, as will be explained later.

The GB patent document A-0.989.683, published April 22, 1965, describes a procedure for preparing a particulate detergent from surfactants and inorganic salts; spray it with water soluble silicate; and compress the detergent particles to form a solid pill that retains the shape. Finally, an organic film-forming polymer and easily soluble in water (for example polyvinyl alcohol) provides a coating to make the detergent tablet resistant to abrasion and accidental breakage.

The document EP-A-0.002.293, published on 13 June 1979, describes a coating of tablets, comprising a hydrated salt, such as acetate, metaborate, orthophosphate, Tartrate and sulfate.

The document EP-A-0.716.144, published on 12 June 1996, also describes detergent tablets to wash the clothing, which have water soluble coatings that can be organic polymers, including acrylic / maleic copolymer, polyethylene glycol, PVPVA and sugar.

Patent document W09518215, published on 6 July 1995, provides water insoluble coatings for solid cast pills. The tablets are provided with hydrophobic coatings, which include wax, fatty acids, amides of fatty acids and polyethylene glycol.

The document EP-A-0.846.754, published on 10 June 1998, provides a pill that has a coating comprising a dicarboxylic acid, the material having coating typically a melting point of 40 ° C to 200 ° C.

The document EP-A-0.846.755, published on 10 July 1998, provides a pill that has a coating comprising a water insoluble material at 25 ° C, such as acids C 12 -C 22 fatty acids, adipic acid or acids C 8 -C 13 dicarboxylic.

The document EP-A-0.846.756, published on 10 June 1998, provides a pill that has a coating comprising a disintegrating material and, preferably, a effervescent material.

The present invention provides a means by that tablets coated with a coating such that they can be stored, transported and handled without spoiling, easily breaking the coating when the tablet is in the automatic washing machine, releasing the active ingredients in the wash solution.

The object of the present invention is provide a pill that has a coating that is what hard enough to protect the tablet from forces mechanical when stored, transported and handled, and provides sufficient flexibility to the coating to avoid its chipping due to mechanical stress.

Summary of the invention

The object of the invention is obtained providing a coated detergent tablet, characterized because the coating comprises reinforcing fibers.

Detailed description of the invention Covering

The strength of a pill can be improved manufacturing a coated tablet and, in addition, by coating a Uncoated tablet improves the mechanical characteristics of the pill while maintaining or further improving its dissolution. This applies very advantageously to tablets multilayers, since through the coating can be transmitted the mechanical characteristics of a more elastic layer to the rest of the tablet, thus combining the advantage of the coating with the advantage of the more elastic layer. In fact, the limitations mechanics will be transmitted through the coating, improving thus the mechanical integrity of the tablet.

In an embodiment of the present invention, the tablets can then be coated so that the tablet does not absorb moisture or absorb it only at a very slow rate. The coating is also strong for moderate mechanical shocks to those who subject the pills during handling, packaging and transport they carry no more than very low levels of breakage or friction. Finally, the coating is preferably brittle so that the tablet quickly falls apart when it is subjected to a crash stronger mechanic. Moreover, it is advantageous that the material of coating dissolves under alkaline conditions, that is easily emulsified by surfactants. This helps to avoid the problem of visible waste in the window of a washing machine Automatic front loading during the wash cycle, and also prevents the deposit of particles or undissolved masses of the material of coating on the load of laundry that is washed. Solubility in Water is measured following the ASTM E1 test protocol 148-87 titled, Standardized Test Method for Perform water solubility measurements.

The coating material has a point of melting preferably 40 ° C to 100 ° C.

The coating can be applied in several ways. Two preferred methods of coating are a) the coating with a molten material, and b) coating with a material solution.

In a), the coating material is applied to a temperature above its melting point and solidifies on The pill. In b), the coating is applied as a solution, drying the solvent to form a coherent coating. The substantially insoluble material can be applied to the tablet, for example, by spraying or immersion. Normally when the molten material is sprayed on the tablet, it will solidify quickly to form a coherent coating. When the pills are dipped into the molten material and then removed, the rapid cooling again causes rapid solidification of the coating material. During the solidification phase, the coating undergoes some internal effort (eg, contraction on cooling) and external effort (eg, relaxation of the tablet). This will likely cause some cracks in the structure, such as edge chipping if the material of coating is too brittle to withstand these efforts mechanics The addition of reinforcing fibers allows strengthening the coating structure so you can better resist the mechanical effort Moreover, it is preferred that the coating comprise a component that is liquid at 25 ° C. It is believed that this liquid component will allow the coating to resist and absorb better mechanical effort by making the structure of the coating be more flexible. The component that is liquid at 25 ° C it is preferably added to the coating materials in proportions of less than 10% by weight of the coating, plus preferably less than 5% by weight, and most preferably less than 3% by weight. The component that is liquid at 25 ° C is added preferably to the coating materials in proportions of less than 0.1% by weight of the coating, more preferably less than 0.3% by weight, and most preferably less than 0.5% by weight. Preferably, the coating comprises a structure crystallized By crystallized, it will be understood that the coating it comprises a material that is solid at room temperature (25 ° C) and which has a structure that presents some order. This can be typically detected by classical crystallography techniques, e.g. X-ray analysis, on the material itself. In one embodiment more preferred, the material that forms the crystallized structure does not co-crystallizes with the optional component that is liquid at 25 ° C and has been mentioned before, or does it only partially,. In fact, it is preferred that the optional component remain in a liquid state at 25 ° C in the crystalline structure of the coating in order to provide flexibility to the structure and resistance to mechanical stress. In another embodiment, the component optional which is liquid at 25 ° C can advantageously have a functionality in washing clothes, for example, oil silicone, which provides the benefit of suppressing foam, or a essential oil.

The coating comprises different materials of the optional component that is liquid at 25 ° C. Suitable materials for the coating they are, for example, dicarboxylic acids. Particularly suitable dicarboxylic acids are selected. from the group consisting of oxalic acid, malonic acid, acid succinic, glutaric acid, adipic acid, pimelic acid, acid suberic, azelaic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid and mixtures thereof. The more preferred is adipic acid. Obviously the materials essentially insoluble that have a melting point below 40 ° C are not solid enough at room temperature and it has found that materials that have a melting point by above approximately 200 ° C it is not practical to use them. Preferably, it was found that a acid with a melting point of more than 90 ° C such as azelaic acid, sebacic acid, dodecanedioic acid and more preferably an acid with a melting point of more than 145 ° C such as adipic acid. "Melting point" means the temperature at which the material becomes a clear liquid when heated slowly, for example, in a capillary tube.

In accordance with the present invention, it can be apply a coating of any desired thickness. For the Most of the purposes, the coating represents 1% to 10%, preferably from 1.5% to 7% of the weight of the tablet.

The coatings of the pads are very hard and provide added resistance to the tablet.

Among the examples of optional components that they are liquids at 25º, polyethylene glycols, oil are included thermal, silicone oil, esters of dicarboxylic acids, acids monocarboxylic, paraffin, triacetin, perfumes or solutions alkaline It is preferred that the structure of the components that are liquids at 25 ° C are similar to that of the material that forms the crystallized structure, so that the structure does not break down from account. In a very preferred embodiment, the structure Crystallized is made of adipic acid, the component that is liquid at 25 ° C by the name Coasol ™ a from Chemoxy International, which is a mixture of esters diisobutyl of glutaric, succinic and adipic acids. The advantage of using this component is the good dispersion in the adipic acid to provide flexibility. It will be noted that the Adipic acid disintegration is further enhanced by the Adipate content of Coasol ™.

The fracture of the coating can be improved by washing by adding a disintegrant in the coating. East disintegrant will swell once it comes in contact with water and It 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 coating melt to a level of up to 30%, preferably between 5% and 20%, the most preferably between 5 and 10% by weight. Possible described disintegrants in Handbook of Pharmaceutical Excipients (1986). Examples of suitable disintegrants include starch: natural, modified or pregelatinized, sodium starch gluconate salt; rubber: agar rubber; guar gum, garrofín gum, karaya gum, pectin gum, tragacanth gum; croscarmellose sodium, crospovidone, cellulose, carboxymethyl cellulose, alginic acid and its salts, including sodium alginate, silicon dioxide, clay, polyvinylpyrrolidone, soy polysaccharides, exchange resins ionic, polymers containing cationic groups (eg, ammonium quaternary), amines substituted polyacrylates, amino acid polymerized cationics such as poly-L-lysine hydrochloride polyallylamine) and mixtures thereof.

Preferably, the coating comprises a acid having a melting temperature of at least 145 ° C, such as, for example, adipic acid, as well as a clay such as, for example, a bentonite clay, in which the clay is used as disintegrant and also to make adipic acid structure more favorable for water penetration, thus improving the dispersion of adipic acid in an aqueous medium. The ones are preferred clays with a particle size less than 75 µm, more preferably less than 53 µm, in order to obtain the effect desired on the acid structure. Clays are preferred Bentonites In fact, when the acid has such a melting point that traditional cellulosic disintegrants experience a thermal degradation during the coating process, it find that such clays will be more suitable since they are more heat stable. In addition, it has been found that disintegrants traditional cellulosics, such as, for example, the NymceI ™, turn brown at these temperatures.

According to the invention, the coating It also includes reinforcing fibers. It has been found that fibers improve the resistance of the coating to mechanical stress and minimize the incidence of the chipping defect. Preferably, such fibers have a length of at least 100 µm, more preferably at least 200 µm and most preferably at least 250 µm to allow reinforcement of the structure. Preferably said fibers have a length less than 500 µm, more preferably less than 400 µm and what more preferably less than 350 µm in order not to influence on the dispersion of the coating in an aqueous medium. The Materials that can be used for these fibers include viscose, rayon, natural nylon, synthetic nylon (polyamides types 6 and 6.6), acrylics, polyester, cotton and derivatives of cellulose such CMC. The most preferred is a cellulosic material available under the trademark Solka-FIoc ™ from Fibers Sales & Development It should be noted that such fibers normally do not need pre-compression to reinforce the structure of the coating. Preferably, such fibers are added to a level less than 5% by weight of the coating, more preferably less than 3% by weight. Preferably, such fibers are added to a level greater than 0.5% by weight of the coating, more preferably greater than 1% by weight.

A preferred procedure to produce a tablet according to the invention comprises the steps of:

(a) form a core by compressing a material in particles, comprising the surfactant particulate material and detergent builder;

(b) apply a coating material to the core, the coating material being in the form of dough cast

(c) let the material of solidify cast coating;

characterized in that the coating comprises reinforcing fibers

Another preferred method for producing a tablet according to the invention comprises the steps of:

(a) form a core by compressing a material in particles, comprising the surfactant particulate material and detergent builder;

(b) apply a coating material to the core, the coating material being dissolved in a solvent or in water;

(c) let the solvent or solvent evaporate Water;

characterized in that the coating comprises reinforcing fibers

The tablets may comprise such components. such as fragrances, surfactants, detergents, etc. The compositions Typical tablets for the preferred embodiment of the present invention are described in the application documents Europeans in process with this EP-A-846755, EP-A-846798, EP-A-846756 and EP-A-846754 for example. Typically, the elements that enter the tablet composition detergents or other forms of detergents such as liquids or granules are detailed in the following paragraphs.

Highly soluble compounds

The tablet may comprise a compound highly soluble Said compound could be formed from a Mix or single compound. A highly soluble compound is define as follows:

A solution comprising as follows is prepared deionized water as well as 20 grams per liter of a compound specific:

1- In a Sotax glass 20 g of the compound are put specific. This glass is put in a constant temperature bath set at 10 ° C. A marine propeller stirrer is introduced into the glass so that the bottom of the agitator is 5 mm above from the bottom of the Sotax glass. The mixer is set at a speed of rotation of 200 revolutions per minute.

2- 980 g of deionized water are put in the glass Sotax

3- 10 s after entering the water, the conductivity of the solution, using a meter conductivity.

4- Repeat stage 3 after 20 s, 30 s, 40 s, 50 s, 1 min, 2 min, 5 min and 10 min after the stage two.

5- The measurement taken at 10 min is used as plateau value or maximum value.

The specific compound is highly soluble. according to the invention when the conductivity of the solution reaches the 80% of its maximum value in less than 10 seconds, starting from the complete addition of deionized water to the compound. In fact when conductivity is monitored in this way, conductivity reaches a plateau after a certain period of time, considering this plateau as the maximum value. Preferably, said compound is in the form of a flowable material consisting of solid particles at temperatures between 10 and 80ºC for ease of handling, but other forms such as a paste can be used or a liquid

Examples of highly soluble compounds include sodium diisoalkylbenzenesulfonate (DIBS) or the sodium toluenesulfonate.

Cohesive effect

The tablet may comprise a compound of cohesive effect on the particulate material of a detergent matrix that forms the tablet. The cohesive effect on the particulate material of a detergent matrix that forms the tablet or a layer of the tablet is characterized by the force required to break a tablet or a layer when the examined detergent matrix is compressed under controlled compression conditions. For a given compression force, a high strength of a tablet or a layer indicates that the granules were strongly bonded together when compressed, so that a strong cohesive effect is taking place. The means to estimate the resistance of a pill or a layer (also called diametral fracture stress) are given in Pharmaceutical dosage forms: tablets , volume 1 compiled by HA Lieberman et al , published in 1989.

The cohesive effect is measured by comparing the resistance of the tablet or the original base powder layer without compound of cohesive effect with the strength of the tablet or the layer of a powder mixture comprising 97 parts of the base powder original and 3 parts of the compound with cohesive effect. The compound of cohesive effect is added to the matrix preferably in a way in which it is substantially free of water (content of water below 10% (preferably below 5%)). The Addition temperature is between 10 and 80 ° C, more preferably between 10 and 40 ° C.

A compound is said to have a cohesive effect. on the particulate material according to the invention when at a compaction force of 3000 N, the pads with a weight of 50 g of particulate detergent material and a diameter of 55 mm have increased the tensile strength of the tablet in more than 30% (preferably 60 and more preferably 100%) through the presence of 3% of the effect compound cohesive in the base material in the form of particles. An example of a compound that has a cohesive effect is a sodium diisoalkylbenzenesulfonate.

When a highly soluble compound is integrated which also has a cohesive effect on the particulate material used for a pill or a layer that is formed by compressing the particulate material comprising a surfactant, rises significantly dissolving the tablet or the layer in aqueous solution. In a preferred embodiment, at least 1% by weight of a pill or layer is formed by the compound highly soluble, and more preferably at least 2%, even more preferably at least 3% and most preferably at least 5% in weight of the tablet or the layer is formed by the compound highly soluble that has a cohesive effect on the material in particles

It should be noted that a composition comprising a highly soluble compound in addition to surfactant is described in EP-A-0 524 075, this composition being a liquid composition.

A highly soluble compound with effect cohesive on the particulate material allows to obtain a pill that, compared to traditional pills, has greater tensile strength when a force is applied compaction constant, or that has equal resistance to traction when a smaller compaction force is applied. Typically, a whole pill will have a resistance to tensile greater than 5 kPa, preferably greater than 10 kPa, more preferably, in particular for use in washing applications of clothing, greater than 15 kPa, more preferably even greater than 30 kPa and most preferably greater than 50 kPa, in particular for use in dishwashing applications by hand or in a dishwasher automatic; and a tensile strength of less than 300 kPa, preferably less than 200 kPa, more preferably less than 100 kPa, more preferably even less than 80 kPa and most preferably less than 60 kPa. In fact, if they are going to go to laundry, the tablets should be less compressed than if they will be used, for example, for automatic dishwashing, so that dissolution is more easily achieved, so in a Clothes washing application tensile strength is preferably less than 30 kPa.

This allows to produce pills or layers that even having a strength and mechanical resistance comparable to the solidity or mechanical strength of traditional pads are less compact and, therefore, dissolve more easily. Even more, As the compound is highly soluble, the dissolution of the pill or layer leading to a synergism that leads to facilitate the dissolution of a tablet according to the invention.

Tablet manufacturing

The tablet can comprise several layers. For Single layer manufacturing purposes, the layer can considered properly as a pill.

You can prepare detergent tablets simply mixing the solid ingredients with each other and pressing mixing in a conventional tablet press, for example, as those used in the pharmaceutical industry. Preferably, the main ingredients, in particular surfactants gelling agents are used in the form of particles. In the ingredients in the form of solid particles can be incorporated, of conventional way, any liquid surfactants, by example, surfactants or foam suppressors.

As for the laundry tablets in particular ingredients such as the improver of the detergency and the surfactant, can be dried by spraying conventional way and then compact at a suitable pressure. Preferably, the tablets according to the invention will be compress using a force less than 100,000 N, more preferably less than 50,000 N, even more preferably less than 5,000 N and most preferably less than 3,000 N. In fact, the most preferred embodiment is a tablet suitable for wash clothes, compressed using a force less than 2500 N, but you can also consider, for example, pills for automatically wash the dishes, so these tablets for automatically wash dishes are usually more compressed than the laundry pills.

The particulate material used to making a pill can be produced by any procedure of production of particles or granules. An example of saying procedure is spray drying (in a drying tower by spray in isocurrent or countercurrent) which typically produces low apparent densities of 600 g / l or less. You can prepare particulate materials with greater density by granulation and densification in a mixer / granulator discontinuous high shear or by a continuous procedure of granulation and densification (for example, using mixers Lodige® CB and / or Lodige® KM). Other suitable procedures include the fluidized bed procedures, the procedures of compaction (eg, roller compaction), extrusion, as well as any chemical procedure to produce any material in particles, such as flocculation, crystallization, sintering, etc. The individual particles can also be any other particle, granule, sphere or grain.

The components of the material in the form of particles can be mixed together by any means conventional. For example, the batch mixture is suitable in a concrete mixer, a Nauta mixer, a tape mixer or any other. Alternatively, the mixing procedure is you can carry out continuously dosing each component in weight on a moving belt, and mixing them in one or more drums or mixers. The binder that does not gel can be spray on the mixture of some or all components of the particulate material. You can also spray others liquid ingredients on the mixture of components, either by separately or previously mixed. For example, they can be sprayed the perfume and suspensions of optical brighteners. It can add a finely divided auxiliary flow agent (an agent powder such as zeolites, carbonates, silicas) to the material in particle shape after spraying the binder, preferably towards the end of the procedure, to do the minor sticky mixture.

The tablets can be manufactured using any compaction procedure, such as pressing, agglomeration or extrusion, preferably pressed. The team suitable includes a classic single plunger or a rotary press (such as Courtoy®, Korch®, Manesty®, or Bonals®). Pills prepared according to this invention preferably have a diameter between 20 mm and 60 mm, preferably at least 35 mm and up to 55 mm, and a weight between 25 and 100 g. The height ratio to diameter (or width) of the pads is preferably larger than 1: 3, more preferably greater than 1: 2. Compaction pressure used to prepare these pills does not need to exceed 100,000 kN / m2, or preferably 30,000 kN / m2, more preferably it does not exceed 5,000 kN / m2, more preferably it still does not exceed 3,000 kN / m2 and most preferably does not exceed of 1,000 kN / m2. In a preferred embodiment according to the invention, the tablet has a density of at least 0.9 g / cm3, more preferably at least 1.0 g / cm3, and preferably less than 2.0 g / cm3, more preferably less than 1.5 g / cm3, even more preferably less than 1.25 g / cm3 and most preferably less than 1.1 g / cm3.

Multi-layer tablets are typically formed in rotary presses, putting the matrices of each layer, one behind of another in containers of forced feeding of the matrices. TO As the procedure continues, the layers of matrices are made then go through the precompression stations together and compression to form the multilayer tablet. With some rotary garments, it is also possible to compress the first layer fed before compressing the tablet as a whole.

Hydrotrope compound

A detergent tablet can integrate a highly soluble compound with cohesive effect, which is also a hydrotrope compound Such a hydrotrope compound can be used in general to favor the dissolution of surfactant avoiding the gelation A specific compound is defined as a hydrotrope of as follows (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% in weight of the specific compound and 75% by weight of water.

2. After this, octanoic acid is added to the solution in a proportion of 1.6 times the weight of the compound specific solution, the solution being at a temperature of 20ºCelsius. The solution is mixed in a Sotax glass with a stirrer of marine propeller, the propeller being located approximately 5 mm by on the bottom of the glass, adjusting the mixer at a speed of rotation 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, that phase being a phase liquid

It should be noted that, in a preferred embodiment of the invention, the hydrotrope compound is a flowable material made of solid particles in operating conditions between 15 and 60ºCelsius.

Hydrotropic compounds include those that are listed below.

A list of hydrotropes can be found comercials at McCutcheon's Emulsifiers and Detergents published by McCutcheon Division of Manufacturing Confectioners Company. Between Other compounds of interest also include:

1. Non-ionic hydrotropes with the following structure:

\delm{C}{\delm{\para}{CH _{3} }}

H --- CH_{2}O)_{y}HR --- O --- (CH 2 CH 2 O) x (

 \ delm {C} {\ delm {\ para} {CH3}} 

H --- CH 2 O) and H

in which R is an alkyl chain C_ {8} -C_ {10}, x varies from 1 to 15, and y from 3 to 10.

2. Anionic hydrotropes such as alkali metal arylsulfonates. This includes metal salts alkalines of benzoic acid, salicylic acid, acid benzenesulfonic acid and its many derivatives, naphthoic acid and various hydroxyaromatic acids Examples of these are salts acid-derived sodium, potassium and ammonium benzenesulfonate toluenesulfonic acid, xylenesulfonic acid, cumenesulfonic acid, tetralinsulfonic acid, naphthalenesulfonic acid, acid methylnaphthalenesulfonic acid, dimethylnaphthalenesulfonic acid, acid trimethylnaphthalenesulfonic.

Other examples include acid salts dialkylbenzenesulfonic acids, such as acid salts diisopropylbenzenesulfonic acid, ethylmethylbenzenesulfonic acid, 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 of 1 to 18 carbon atoms.

3. Hydrotropes solvents such as glycerins alkoxylated and alkoxylated glycerides, glycerol esters alkoxylated, alkoxylated fatty acids, glycerin esters, polyglycerol esters. Preferred alkoxylated glycerins They have the following structure:

one

where l, m and n are, in each case, a number of 0 to approximately 20, with l + m + n = approximately 2 a about 60, preferably about 10 to approximately 45 and R represents H, CH 3 or C 2 H 5.

Preferred alkoxylated glycerides have the following structure:

two

where R_ {1} and R2 are, in each case, C_ {n} COO or - (CH 2 CHR 3 -O) l -H wherein R 3 = H, CH 3 or C 2 H 5 and l is a number of 1 to about 60, n is a number from about 6 to approximately 24.

4. Polymer hydrotropes such as those described in EP636687:

\melm{\delm{\para}{E}}{C}{\uelm{\para}{R}}

)_{x} --- (CH_{2} ---

\melm{\delm{\para}{R _{2} }}{C}{\uelm{\para}{R _{1} }}

)_{y} ------ (CH_ {2} ---

 \ melm {\ delm {\ para} {E}} {C} {\ uelm {\ para} {R}} 

) x --- (CH2 ---

 \ melm {\ delm {\ para} {R 2}} {C} {\ uelm {\ para} {R 1}}} 

)_{Y} ---

in which E is a functional group hydrophilic,

R is H or an alkyl group C_ {1} -C_ {or} is a functional group hydrophilic;

R1 is H, a lower alkyl group or a aromatic group,

R2 is H or a cyclic alkyl group or aromatic.

The polymer typically has a molecular weight between approximately 1,000 and 1,000,000.

5. Hydrotropes of unusual structure, such as acid 5-carboxy-4-hexyl-2-cyclohexene-1-yloctanoic acid (Diacid®)

The use of a compound of this class in the invention would further increase the dissolution rate of the tablet, since a hydrotrope compound facilitates, for example, the surfactant solution. Said compound could be formed at from a mixture or a single compound.

Tensile strength

For the purpose of measuring resistance to traction of a layer, the layer itself can be considered as a pill.

Depending on the composition of the material of heading, and the shape of the pads, the compaction force used can be adjusted so as not to affect the resistance to traction, or at the time of disintegration in the washing machine. The procedure can be used to prepare homogeneous tablets or with layers, of any shape or size.

For a cylindrical tablet, the resistance to traction corresponds to diametral fracture traction (DFS) which is a way to express the resistance of a pill or layer, and it determined by the following equation:

Tensile strength = 2 F/ \ piDt

in which F is the maximum force (Newtons) that cause failure (breakage) by traction measured by a hardness tester of pads, VK 200, supplied by Van Kell Industries, Inc. D is the diameter of the tablet or the layer, and t is the thickness of the pill or coat. For a non-round pill, \ piD it can simply be replaced by the perimeter of the tablet.

(Method Pharmaceutical Dosage Forms: Tablets Volume 2 Pages 213 to 217).

A tablet with a fractured traction diametral less than 20 kPa is considered to be fragile and it will probably result in some pills arriving broken to the consumer. Diametral fracture traction is preferred of at least 25 kPa.

This applies similarly to non-pads. cylindrical to define tensile strength, pads whose normal cross section at the height of the tablet is not round, and in which force is applied along one direction perpendicular to the direction of the height of the tablet and normal to side of the tablet, the side being perpendicular to the section non-round cross

Dosage of the pills

The dosage rate of a pill Detergent can be determined as follows:

Two pills weighing 50 grams nominal are weighed each one, and then they are put in the box of a washing machine Baucknecht® WA9850 automatic. The water supply is adjusted to the washing machine at a temperature of 20ºC and a hardness of 0.003 moles per liter (2.1 grains per gallon), the flow rate being adjusted of water inlet in the box at 8 I / min. The level of waste of the tablet remaining in the box after putting in operation of the washing machine in washing program No. 4 (clothes white / colored, short cycle). The percentage of waste after Dosage is determined as follows:

dosage = residual weight x 100 / original weight of the tablet

The level of waste is determined by repeating the procedure 10 times and the average value of the level of residue based on the ten individual measurements. In this forced test, a residue of 40% of the weight is considered acceptable initial of the pill. A residue less than 30% is preferred, and better still a residue less than 25%.

It will be noted that the measure of water hardness usually expressed in traditional units of "grains by gallon ", knowing that 0.001 moles per liter equals 7.0 grains per gallon, which represents the concentration of Ca 2+ ions in solution.

Effervescence agent

Detergent tablets can also comprise an effervescence agent.

Effervescence, as defined here, is defined like the release of gas bubbles by a liquid like result of a chemical reaction between a source of soluble acid and an alkali metal carbonate, to produce carbon dioxide gaseous.

that is, C 6 H 8 O 7 {3} + 3NaHCO 3 Na Na 3 C 6 H 5 O 7 {3} + 3CO 2 3H 2 O

Additional examples of sources of acid and carbonate and other effervescent systems can be found in: (Pharmaceutical Dosage Forms: Tablets Volume 1 Pages 287 a 291).

In addition to detergent ingredients, you can Add an effervescence agent to the tablet mixture. The adding this effervescence agent to the detergent tablet Improves the disintegration time of the tablet. Preferably the amount will be between 5 and 20% and most preferably between 10 and 20% by weight of the tablet. Preferably the agent of Effervescence will be added as an agglomerate of the different particles or as a compact, and not as separate particles.

Due to the gas generated by the effervescence in the tablet, this can have a D.F.S. taller and keep having the same disintegration time as a pill without effervescence. When the D.F.S. of the effervescent tablet stays the same as that of a non-effervescent tablet, the disintegration of the tablet Effervescent will be faster.

An auxiliary agent of solution using compounds such as sodium acetate or urea. You can also find a list of auxiliary agents for suitable solution in Pharmaceutical Dosage Forms: Tablets, Volume 1, second edition, compiled by H.A. Lieberman et l, ISBN 0-8247-8044-2.

Detergent Surfactants

A detergent composition typically comprises surfactants The dissolution of surfactants is favored by addition of highly soluble compound.

Non-limiting examples of useful surfactants here, typically at levels of about 1% to about 55%, by weight, include alkyl (C 11 -C 18) - benzenesulfonates ("LAS") and the (C 10 -C 20) alkyl sulfates ("AS") conventional primary chain, branched and random, the (2,3) -alkyl (C 10 -C 18) secondary sulfates of formula CH 3 (CH 2) x (CHOSO 3 M +) CH 3 Y CH 3 (CH 2) y (CHOSO 3 - M +) CH 2 CH 3 where x e (y + 1) are integers of at least approximately 7, preferably at least about 9, and M is a cation Water solubilizer, especially sodium, unsaturated sulfates such as oil sulfate, (C 10 -C 18) alkyl alkoxy sulfates ("AE_ {x} S"; especially ethoxy sulfates of 1-7 EO), (C 10 -C 18) alkyl alkoxy carboxylates (especially ethoxycarboxylates with 1-5 EO), glycerol ethers C 10-18, the alkyl ( C 10 -C 18 polyglycosides and their corresponding sulfated polyglycosides and acid esters alpha-borne fatty C_ {12} -C_ {18}. If desired, you can also include in the global compositions non-ionic surfactants and conventional amphoteric such as alkyl (C_ {12} -C_ {18}) ethoxylates ("AE") Including the so-called (narrow peak alkyl) ethoxylates and (C 6 -C 12) alkyl phenolalkoxylates (especially mixed ethoxylates and ethoxy / propoxy), betaines C 12 -C 18, and sulfobetains ("sultaines"), amine oxides C 10 -C 18, and the like. Can also be use the N-(C 10 -C 18) alkyl amides of polyhydroxy fatty acids. Typical examples include the C 12 -C 18 N-methylglylamides. See WO 9,206,154. Other sugar-derived surfactants include the N-alkoxy polyhydroxy acid amides fatty, such as N- (3-methoxypropyl) glucamide C_ {10} -C_ {18}. To make low foam you can use the N-propyl to N-hexyl C 12 -C 18 glucamides. Can also be used C 10 -C 20 conventional soaps. Whether you want a lot of foaming, soaps can be used C_ {10} -C_ {16} branched chain. They are especially useful mixtures of anionic and non-surfactants ionic Other conventional useful surfactants are those listed in classic texts. In a preferred embodiment, the tablet comprises at least 5% by weight of surfactant, plus preferably at least 15% by weight, even more preferably at minus 25% by weight and most preferably between 35% and 45% by weight of surfactant.

Non-gelling binders

In detergent compositions you can integrate non-gelling binders to further facilitate the dissolution.

If non-gelling binders are used, the suitable non-gelling binders include organic polymers such as polyethylene glycols, polyvinylpyrrolidones, polyacrylates and water soluble acrylate copolymers. The Handbook of Pharmaceutical Excipients, second edition, has the following Classification of binders: gum arabic, alginic acid, carbomer, sodium carboxymethyl cellulose, dextrin, ethyl cellulose, gelatin, guar gum, hydrogenated vegetable oil type 1, hydroxyethylcellulose, hydroxypropylmethylcellulose, liquid glucose, magnesium aluminum silicate, maltodextrin, methylcellulose, polymethacrylates, povidone, sodium alginate, starch and zein. The more preferable binders also have a cleaning function active in washing clothes, as with polymers cationic, that is, quaternary compounds of hexamethylenediamine ethoxylated, bishexamethylenetriamines, or others such as pentaamines, ethoxylated polyethyleneamines, maleic acrylic polymers.

Non-gelling binder materials preferably they are pulverized and therefore have a point of appropriate melting below 90 ° C, preferably below 70 ° C and even more preferably below 50 ° C, so that they do not damage nor do they degrade the other active ingredients in the matrix. The best Preferred are non-aqueous liquid binders (i.e. that are not in aqueous solution) that can be sprayed in the state molten. However, they can also be solid binders. incorporated in the matrix by dry addition but having binding properties inside the tablet.

Non-gelling binder materials are preferably used in an amount within the range of 0.1 at 15% of the composition, more preferably below 5% and especially if it is an active material that is not used for washing the clothes, below 2% by weight of the tablet.

It is preferred to avoid gelling binders, such as non-ionic surfactants in their liquid state or molten. Non-ionic surfactants and other binders that gels are not excluded from the compositions, but it is preferred that are processed in detergent tablets as components of particulate materials, and not as liquids.

Detergency builders

They can be optionally included in the compositions of this invention detergency builders for Help control mineral hardness. Improvers can be used inorganic as well as organic detergency. The improvers of the detergency are typically used in compositions for washing tissues to help remove dirt in the form of particles

The level of detergency builder can Vary widely according to the end use of the composition.

Inorganic detergency builders or that contain phosphorus include, but are not limited to, the alkali metal, ammonium and alkanolammonium salts of polyphosphates (exemplified by tripolyphosphates, pyrophosphates, and metaphosphates vitreous polymers), phosphonates, phytic acid, silicates, carbonates (including bicarbonates and sesquicarbonates), sulfates and aluminosilicates. However, salts are not always needed other than phosphates. It is important to note that the compositions of the present invention work surprisingly well even in presence of so-called "weak" breeders (compared with phosphates) such as citrate, or in the so-called "under-improved" situation that may occur with zeolite or Laminate silicate type improvers.

Examples of silicate type improvers are the alkali metal silicates, particularly those with a SiO 2 ratio: Na 2 O in the range 1.6: 1 to 3.2: 1 and laminar silicates, such as laminar sodium silicates described in US Pat. 4,664,839, issued May 12 from 1987 to H. Rieck. NaSKS-6 is the trademark for a crystalline laminar silicate marketed by Hoechst (represented here vulgarly by the abbreviation "SKS-6"). Unlike breeders Zeolite type, the Na silicate type improver SKS-6 does not contain aluminum. NaSKS-6 it has the morphological form Na2 SiO5 of a laminar silicate. I know can be prepared by methods such as those described in the German patent documents DE-A3.417.649 and DE-A-3,742,043. SKS-6 is a very preferred laminar silicate for use here, but other silicates can be used in this invention laminar, such as those with the general formula: NaMSi_ {O} {2x + 1} • H2O in which 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 various layered silicates of Hoechst include NaSKS-5, NaSKS-7 and NaSKS-11, such as alpha, beta and gamma forms. How indicated above, the form delta-Na2 {SiO_ {5} (form NaSKS-6) is the most preferred for use here. Other silicates may also be useful, such as magnesium silicate that can act as a cresting agent in granular formulations, as a bleaching stabilizing agent oxygenated and as a component of foam control systems.

Examples of carbonate salts as improvers are the alkali and alkaline earth metal carbonates that are described in German patent application No. 2,321,001, published November 15, 1973.

They are also useful in the present invention. aluminosilicate type detergency builders. The aluminosilicate type detergency builders have great importance in most detergent compositions high-performance granules currently marketed and they can also be a detergency builder ingredient significant in liquid detergent formulations. Breeders Aluminosilicate include those that have the empirical formula:

M_ {z} (zAlO2) y} \ cdotxH2 O

in which z and y are whole numbers that are worth minus 6, the molar ratio of z a y is in the range of 1.0 a approximately 0.5, and x is an integer in the range of about 15 to about 264

Ion exchange materials of the aluminosilicate type are available in the market. These aluminosilicates can have crystalline or amorphous structure and can be natural or synthetic aluminosilicates. A method for producing ion exchange materials of the aluminosilicate type is described in US Pat. 3,985,669, Krummel, et al , issued October 12, 1976. The ion exchange materials of the aluminosilicate, crystalline and synthetic type which are preferred and useful here 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 12 [(AlO 2) 12 (SiO 2) 12] \ x 2 O

where x is about 20 to approximately 30, especially around 27. This material is known as Zeolita A. In this invention can also be used dehydrated zeolites (x = 0-10). Preferably, the aluminosilicate has a particle size of approximately 0.1-10 micrometers diameter.

Organic detergent builders that are suitable for the purposes of the present invention include, but are not limited to, a wide range of polycarboxylate compounds. As used herein, "polycarboxylate" refers to compounds having a plurality of carboxylate groups, preferably at least 3 carboxylates. In general, a polycarboxylate enhancer can be added to the composition in acid form, but it can also be added in the form of a neutralized salt. When used as a salt, alkali metals, such as sodium, potassium and lithium, or alkanolammonium salts are preferred. Among the polycarboxylate type improvers, various categories of useful materials are included. An important category of polycarboxylate type enhancers encompasses ether polycarboxylates, including oxydisuccinate, as described in US Pat. 3,128,287, by Berg, issued April 7, 1964, and US Pat. 3,635,830, by Lamberti, issued on January 18, 1972. See also the "TMS / TDS" improvers of US Pat. 4,663,071, issued to Bush et al , on May 5, 1987. Suitable polycarboxylate ether also includes cyclic compounds, particularly alicyclic compounds, such as those described in US Pat. 3,923,679; 3,835,163; 4,158,635; 4,120,874 and 4,102,903.

Other useful detergency builders include ether-hydroxypolycarboxylates, copolymers of maleic anhydride with ethylene or vinyl methyl ether, acid 1,3,5-trihydroxybenzene-2,4,6-trisulfonic and carboxymethyloxysuccinic acid, the various metal salts alkali, ammonium and substituted ammonium of polyacetic acids such as ethylenediaminetetraacetic acid and nitrilotriacetic acid, as well as polycarboxylates such as melitic acid, succinic acid, oxidisuccinic acid, poly (maleic acid), acid benzene-1,3,5-tricarboxylic acid carboxymethyloxysuccinic, and its soluble salts.

Type Detergency Enhancers citrate, for example, citric acid and its soluble salts (particularly sodium salt), are detergency builders of polycarboxylate type of particular importance for formulations high performance liquid detergents due to its availability from renewable resources and their biodegradability Citrates can also be used in granular compositions, especially in combination with zeolite and / or laminar silicate detergency builders. The Oxydisuccinates are also especially useful in these Compositions and combinations

They are also suitable in the compositions detergents of the present invention the 3,3-dicarboxy-4-oxa-1,6-hexanedioates and related compounds described in US Pat. 4,566,984, Bush, issued on January 28, 1986. The breeders Useful succinic acid type include alkyl acids and C 5 -C 20 alkenyl succinic and salts thereof. A particularly preferred compound of this type is acid dodecenyls succinic.

Specific examples of type improvers succinate include: lauryl succinate, myristyl succinate, palmitylsuccinate, 2-dodecenylsuccinate (preferred),  2-pentadecenylsuccinate, and the like. The lauryl succinates are the preferred detergency builders of this group, and are described in the 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 US Pat. 1979, Diehl, issued March 3,308,067, 71967. See also US Pat. 3,723,322.

In the compositions can also be incorporated fatty acids, eg monocarboxylic acids C_ {12} -C_ {18}, alone or in combination with improvers mentioned above, especially improvers citrate and / or succinate type, to provide activity Additional improver The use of such fatty acids generally will result in a decrease in foam, which should be taken into account by the formulator.

In situations where they can be used phosphorus-based detergency builders, and especially in the formulation of bars used for laundry operations to hand, the various alkali metal phosphates such can be used such as the well known sodium tripolyphosphates, sodium pyrophosphate and sodium orthophosphate. Breast enhancers can also be used. phosphonate type detergency such as ethane-1-hydroxy-1,1-diphosphonate and other known phosphonates (see, for example, the Patents of USA 3,159,581; 3,213,030; 3,422,021; 3,400,148 and 3,422,137).

Bleaching

Optionally the detergent compositions of the The present invention may contain bleaching agents or bleaching compositions containing a bleaching agent and one or more bleach activators. When they are present, the bleaching agents will typically be at levels of about 1% to about 30%, more typically of about 5% to about 20%, of the composition detergent, especially for washing fabrics. If they are present, the amount of bleach activators will typically be about 0.1% to about 60%, more typically of about 0.5% to about 40% of the composition bleach comprising the bleaching agent plus the activator of the bleaching

The bleaching agents used here may be any of the bleaching agents useful for detergent compositions in textile cleaning, cleaning rigid surfaces or other types of cleaning known now or that They will be known later. Among these, the Oxygenated bleaching agents as well as other bleaching agents. In this invention can be used perborate bleaching agents, e.g., sodium perborate (e.g., mono- or tetra-hydrated).

Another category of bleaching agent that can be used without restriction includes percarboxylic acid bleaching agents and their salts. Suitable examples of this class of agents include magnesium monoperoxyphthalate hexahydrate, the magnesium salt of metachloroperbenzoic acid, 4-nonylamino-4-oxoperoxybutyric acid and diperoxidedecanedioic acid. Such bleaching agents are described in US Pat. No. 4,483,781, Hartman, issued on November 20, 1984, No. 740,446, Bums et al ., filed on June 3, 1985, in European patent application 0.133,354, Banks et al . published on February 20, 1985, and US Pat. No. 4,412,934, Chung et al . Issued November 1, 1983. Very preferred bleaching agents also include 6-nonylamino-6-oxoperoxicaproic acid as described in US Pat. 4,634,551, issued January 6, 1987, Burns et al .

Bleaching agents can also be used peroxygenated Suitable peroxygen bleaching compounds include sodium carbonate peroxyhydrate and bleaches equivalents of the type "percarbonate", sodium pyrophosphate peroxyhydrate, urea peroxyhydrate and sodium peroxide. Too a persulfate type bleach can be used (eg OXONE, commercially manufactured by DuPont).

A preferred percabonate type bleach it comprises dry particles with an average particle size in the range from about 500 micrometers to about 1,000 micrometers, and not less than about 10% by weight of said particles are less than about 200 micrometers and no more about 10% by weight of said particles are greater than approximately 1,250 micrometers. Optionally, the percarbonate is it can be coated with a silicate, borate or soluble surfactants in Water. Percarbonate is available from various sources commercials such as FMC, Solvay and Tokai Denka.

You can also use mixtures of these bleaching agents

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 bleach activator . In U.S. Patent Nos. 4,915,854, issued April 10, 1990 to Mao et al . and No. 4,412,934 various non-limiting examples of activators are described. Nonanoyloxybenzenesulfonate (NOBS) and tetraacetylethylenediamine (TAED) activators are typical, and mixtures thereof can also be used. See also US 4,634,551 for other typical bleach and activators useful in this invention.

Bleach activators derived from groups Most preferred amido are those of formulas:

\hskip0,5cm

o

\hskip0,5cm

R^{1}C(O)N(R^{5})R^{2}C(O)LR 1 N (R 5) C (O) R 2 C (O) L

 \ hskip0,5cm 

or

 \ hskip0,5cm 

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, R2 it is an alkylene group containing from 1 to about 6 atoms carbon, and R 5 is H or an alkyl, aryl or alkylaryl group containing from about 1 to about 10 atoms of carbon, and L is any leaving group. An outgoing group is any group that is displaced from the bleach activator as consequence of the nucleophilic attack on the activator of bleaching by perhydrolysis anion. An outgoing group preferred is phenyl.

Preferred examples of activators of bleaches of the above formulas include (6-octanamido-caproyl) oxybenzenesulfonate, (6-nonanamidocaproyl) -oxybenzenesulfonate, (6-decanamido-caproyl) oxybenzenesulfonate and mixtures thereof, as described in US Pat. 4,634,551 incorporated into this memory as a reference.

Other class of bleach activators comprises the benzoxazine type activators described by Hodge and cabbage. in US Patent 4,966,723, issued October 30, 1990, incorporated herein by reference. An activator Most preferred of the type of benzoxazine is:

3

Another class of bleach activators Preferred includes acyl lactam activators, especially acyl-caprolactams and Acyl-Valerolactams of formulas:

4

in which R 6 is H or an alkyl group, aryl, alkoxyaryl or alkaryl containing from one to about 12 carbon atoms Extremely Lactam Activators Preferred include benzoyl-caprolactam, octanoyl-caprolactam, 3,5,5-trimethylhexanoyl-caprolactam,  nonanoil-caprolactam, decanoyl-caprolactam, undecenoyl-caprolactam, benzoil-valerolactam, octanoil-valerolactam, decanoil-valerolactam, undecenoil-valerolactam, nonanoil-valerolactam, 3,5,5-trimethylhexanoyl-valerolactam and their mixtures. See also U.S. Patent 4,545,784, issued to Sanderson, on October 8, 1985, incorporated herein as a reference, which describes acyl-caprolactams, including benzoyl-caprolactam, adsorbed on perborate sodium

Bleaching agents other than peroxygenated bleaching agents can also be used herein. One type of non-oxygenated bleaching agent of particular interest includes photoactivated bleaching agents such as sulfonated zinc and / or aluminum phthalocyanine. See, US Pat. 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 means of a manganese compound. Such compounds are well known in the art and include, for example, the manganese based catalysts described in US Patent 5,246,621, in US Patent 5,244,594; in US Patent 5,194,416; in US Patent 5,114,606; and in the publications of European patent applications Nos. 549.271A1, 549.272A1, 544.440A2 and 544.490A1. Preferred examples of these catalysts include Mn IV 2 (uO) 3 (1,4,7-trimethyl-1,4,7-triazacyclononane) 2 (PF 6) 2, Mn III 2 (uO) 1 (u-OAc) 2 (1,4,7-trimethyl-1,4,7-triazacyclononane) _ {2 - (ClO 4) 2, Mn IV 4 (uO) 6 (1.4,
7-triazacyclononane) 4 (ClO 4) 4, Mn III Mn IV 4 (uO) 1 (u-OAc) 2 - (1,4,7-trimethyl-1,4,7-triazacyclononane) 2 (ClO 4) 3, Mn IV (1,4,
7-trimethyl-1,4,7-triazacyclononane) - (OCH 3) 3 (PF 6) and mixtures thereof. Other types of metal-based bleach catalysts include those described in US Pat. 4,430,243 and 5,114,611. The use of manganese with various complex ligands to increase bleaching is also published in the following US 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.

For practical reasons, and not by way of limitation, the compositions and methods of the present invention can be adjust to provide on the order of at least one part by ten million of the active species as a bleach catalyst in the aqueous washing medium, and preferably will provide about 0.1 ppm to about 700 ppm, more preferably from about 1 ppm to about 500 ppm, of the bleach catalyst species in the wash water.

Enzymes

Enzymes can be included in the formulations of this memory for a wide variety of purposes in washing fabrics, which include, for example, the removal of stains based of proteins, based on carbohydrates, or based on triglycerides, and to prevent the transfer of dyes housed, and for fabric restoration. Enzymes to be incorporated here include proteases, amylases, lipases, cellulases and peroxidases, as well as mixtures thereof. Can also be Include other types of enzymes. They can be of any origin suitable, as plant, animal, bacterial, fungal and yeasts However, your choice is determined by several factors, such as optimal pH activity and / or stability, thermostability, stability against detergency builders assets, additives, etc. In this regard, enzymes are preferred bacterial or fungal, such as amylases and bacterial proteases and fungal cellulases

Normally enzymes are incorporated into sufficient amounts to provide up to about 5 mg by weight, more typically about 0.01 mg at approximately 3 mg of active enzyme per gram of the composition. In other words, the compositions of the present invention typically comprise from about 0.001% to about 5%, preferably 0.01-1% by weight of a commercial enzyme preparation. Usually protease enzymes are present in such commercial preparations at levels sufficient to provide 0.005 to 0.1 Anson (UA) units of activity per gram of composition.

Suitable examples of proteases within the scope of the present invention are subtilisins, which are obtained from particular strains of B. subtilis and B. licheniformis . Another suitable protease is obtained from a Bacillus strain, which exhibits its maximum activity over the pH range of 8-12, developed and sold by Novo Industries A / S under the trade name ESPERASE. The preparation of this enzyme and analogous enzymes is described in British patent GB 1,243,784 to Novo. Proteolytic enzymes suitable for removing commercially available protein-based stains include those marketed under the trade names 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 Serial No. 87303761.8, filed April 28, 1987, and Patent Application European 130,756, by Bott et al , published on January 9, 1985).

Amylases include, for example, alpha-amylases described in the specification of English patent 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 cellulases. Preferably, they will have an optimum pH between 5 and 9.5. U.S. Pat. 4,435,307, Barbesgoard et al , issued on March 6, 1984, describes suitable fungal cellulases obtained from Humicola in solens or Humicola strain DSM1800 or a cellulase 212 producing fungus belonging to the genus Aeromonas , and cellulase extracted from the hepatopancreas of a marine mollusk, (Dolabella Auricle Solander). Suitable cellulases are also described in GB-A-2,075,028; GB-A-2,095,275 and DE-OS-2,247,832. CAREZYME de Novo is especially useful.

Lipase enzymes suitable for use in detergents 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 for public inspection on Feb. 24, 1978. This lipase is available from Amano Pharmaceutical Co., Nagoya, Japan, under the trade name Lipase P "Amano", hereinafter referred to as forward "Amano-P". Other suitable commercial lipases include Amano-CES, Chromobacter viscosum lipases, for example, Chromobacter viscosum var. NRRLB 3673 lipolyticum from Toyo Jozo Co., Tagata, Japan; lipases produced by Chromobacter viscosum , from US Biochemical Corp. USA. and from Disoynth Co., the Netherlands; and lipases produced by Pseudomonas gladioli . The LIPOLASE® enzyme derived from Humicola lanuginosa and commercially available from Novo, see also EP 341,947, is a preferred lipase for use herein.

Peroxidases enzymes are used in combination with oxygen sources, eg a percarbonate, perborate, persulfate, hydrogen peroxide, etc. These are used for "bleaching in solution", that is, to prevent transfer of dyes or pigments that have been removed since substrates during washing operations to other substrates in The washing solution. Peroxidases enzymes are known in the technique and include, for example, horseradish peroxidase, ligninase and a halo-peroxidase such as chloro- and bromine peroxidase Compositions described detergents containing peroxidase, for example, in the Application PCT International WO 89/099813, published October 19, 1989, by O. Kirk, assigned to Novo Industries A / S.

A wide range of enzymatic materials and means for incorporation into synthetic detergent compositions are also described in US Pat. 3,553,139, issued on January 5, 1971 to McCarty et al . Enzymes are further described in US Pat. 4,101,457, of Place et al ., Issued July 18, 1978, and 4,507,219 Hughes, issued March 26, 1985. In US Pat. 4,261,868, Hora et al ., April 14, 1981, describe enzymatic materials useful for liquid detergent formulations and their incorporation into such formulations. Enzymes for use in detergents can be stabilized by various techniques. In U.S. Patent 3,600,319, issued on August 17, 1971, to Gedge et al., And in European Patent Application Publication No. 0 199,405, application number 86200586.5 published October 29, 1986, Venegas, enzyme stabilization techniques are described and exemplified. Enzyme stabilization systems are also described, for example, in US Pat. 3,519,570.

Other components that are currently used in detergent compositions and which can be incorporated into tablets detergents include chelating agents, release agents of dirt, anti-redeposition agents of the dirt, dispersing agents, foam suppressants, fabric softeners tissues, color transfer inhibitors and perfumes.

Advantageously, the compounds described previously for a product they are packed in a system of packing.

A packaging system can be formed from of a sheet of flexible material. The right materials for use As flexible sheet include monolayer films, co-extruded or stratified. Such movies they can comprise several components, such as polyethylene, polypropylene, polystyrene and poly (ethylene terephthalate). Preferably the packaging system is composed of a coextruded polyethylene and oriented polypropylene film biaxially with an MVTR value of less than 5 / g / day / m2. The MVTR value of the packaging system is preferably less than 10 g / day / m2, more preferably less than 5 g / day / m2. The Film (2) can have several thicknesses. Typically the thickness will be between 10 and 150 µm, preferably between 15 and 120 µm, more preferably between 20 and 100 µm, even more preferably between 25 and 80 µm and most preferably between 30 and 40 µm.

A packaging material preferably comprises a barrier layer that is typically found in the materials of packaging that have a low oxygen transmission rate, typically less than 300 cm3 / m2 / day, preferably less than 150 cm3 / m2 / day, more preferably less than 100 cm3 / m2 / day, even more preferably less than 50 cm3 / m2 / day and most preferably less than 10 cm3 / m2 / day. Typical materials that have these Barrier properties include bioriented polypropylene, poly (ethylene terephthalate), nylon, poly (ethylene-vinyl alcohol), or materials in sheets comprising one of these, as well as SiOx (oxides of silicon), or metallic paper, such as aluminum foil. A packaging material of this class may have an influence beneficial on product stability, for example, during the storage. Among the methods used to package, typically find the wrapping methods described in W092 / 20593, including flow wrap or total wrap. When such procedures are used, a joint is provided longitudinal, which can be a fin type joint or a joint overlap, after which a first end of the packaging system with a first end seal, followed by Close the second end with a second end gasket. The packaging system may comprise additional means of closure as described in W092120593. In particular it is appropriate to use torsion, a cold seal or an adhesive. In fact, it can be applied a cold seal band or a band of adhesive to the surface of the packaging system in a position adjacent to the second end of the packaging system, so that this band can provide both the initial closing and the additional closing of the system packing. In such a case, the cold seal or adhesive strip can correspond to a region that has a cohesive surface, is that is, a surface that will adhere only to another surface cohesive Such means of re-closing can also comprise spacers that will prevent unwanted adhesion. Sayings spacers are described in WO 95/13225, published on May 18, 1995. There may also be a plurality of spacers and a plurality of strips of adhesive material. The main requirement is that communication between the outside and the inside the package has to be minimal, even after the First opening of the packaging system. A closure can be used cold, and in particular a cold closure of reticular structure that is adapted to facilitate the opening of the system packing.

Examples Example 1

(Comparative)

i)

A powder is prepared detergent base of composition A as follows: all material in particles of the base composition was mixed in a mixing drum or spray drum to form a homogeneous particulate mixture, Apart from the binder spray system, the agent fluorescent or brightener, and the photobleaching zinc phthalocyanine sulphonate. Then the mixture in the form of particles was divided into two equal parts, one part to prepare a white layer and the other to prepare a green layer. The white layer material is obtained by spraying the brightener or fluorescent agent together with half the binder. The green layer material is obtained by spraying the phthalocyanine sulphonate of zinc bleacher together with the rest of the binder. Then the layers were independently processed in a KM Loedige 600®.

ii)

Using a Bonals® rotary press both matrices were filled in two independent forced feeding containers. Both layers are compress against each other at the precompression stations and compression to form a two layer pill.

iii)

In this example in particular, the pads have a square cross section of 45 mm side, a height of 24 mm and a weight of 45 g. The height of the green bottom layer corresponded to 50% of the total height of the tablet. The tensile strength of the pads does not coated was 13 kpa.

iv)

Then the tablet was coated with 2.5 g of coating formed by 90% in weight of sebacic acid and 10% by weight of Nymcel-ZSB 16? By Metsa Seria.

       \ vskip1.000000 \ baselineskip
    

       \ vskip1.000000 \ baselineskip
    

       \ vskip1.000000 \ baselineskip
    

(Table goes to page next)

5

Anionic agglomerates 1 comprise 40% of anionic surfactant, 27% zeolite and 33% carbonate

Anionic agglomerates 2 comprise 40% of anionic surfactant, 28% zeolite and 32% carbonate

The non-ionic agglomerate comprises 26% of non-ionic surfactant, 6% Lutensit K-HD 96, 40% of anhydrous sodium acetate, 20% carbonate and 8% zeolite.

Cationic agglomerates comprise 20% of cationic surfactant, 56% zeolite and 24% sulfate

The laminar silicate comprises 95% of SKS 6 and 5% silicate

Bleacher activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (form acid) and 2% water.

Acid Sodium Salt Particles ethylenediamine-N, N-disuccinic / sulfate comprise 58% acidic sodium salt ethylenediamine-N, N-disuccinic, 23% sulfate and 19% water.

The foam suppressor comprises 11.5% oil silicone (ex Dow Corning); 59% of zeolite and 29.5% of water.

The binder spray system comprises 16% by weight polymer of the following class:

6

68% by weight of: PEG4000 and 16% by weight of: DIBS (Sodium diisoalkylbenzenesulfonate or toluenesulfonate of sodium).

Another example of a composition that can be use is as follows:

7

Anionic agglomerates 1 comprise 40% of anionic surfactant, 27% zeolite and 33% carbonate

Anionic agglomerates 2 comprise 40% of anionic surfactant, 28% zeolite and 32% carbonate

The non-ionic agglomerate comprises 26% of non-ionic surfactant, 6% Lutensit K-HD 96, 40% of anhydrous sodium acetate, 20% carbonate and 8% zeolite.

Cationic agglomerates comprise 20% of cationic surfactant, 56% zeolite and 24% sulfate

The laminar silicate comprises 95% of SKS 6 and 5% silicate

Bleacher activator agglomerates comprise 81% TAED, 17% acrylic / maleic copolymer (form acid) and 2% water.

Acid Sodium Salt Particles ethylenediamine-N, N-disuccinic / sulfate comprise 58% acidic sodium salt ethylenediamine-N, N-disuccinic, 23% sulfate and 19% water.

The foam suppressor comprises 11.5% oil silicone (ex Dow Corning); 59% of zeolite and 29.5% of water.

The binder spray system comprises 16% by weight polymer of the following class:

8

68% by weight of: PEG4000 and 16% by weight of: DIBS (Sodium diisoalkylbenzenesulfonate or toluenesulfonate of sodium).

Example 2

i)

A powder is prepared detergent base of composition A as follows: all material in particles of the base composition was mixed in a mixing drum or spray drum to form a homogeneous particulate mixture, Apart from the binder spray system, the agent fluorescent or brightener, and the photobleaching zinc phthalocyanine sulphonate. Then the mixture in the form of particles was divided into two equal parts, one part to prepare a white layer and the other to prepare a green layer. The white layer material is obtained by spraying the brightener or fluorescent agent together with half the binder. The green layer material is obtained by spraying the phthalocyanine sulphonate of zinc bleacher together with the rest of the binder. Then the layers were independently processed in a KM Loedige 600®.

ii)

Using a Bonals® rotary press both matrices were filled in two independent forced feeding containers. Both layers are compress against each other at the precompression stations and compression to form a two layer pill.

iii)

In this example in particular, the pads have a square cross section of 45 mm side, a height of 24 mm and a weight of 45 g. The height of the green bottom layer corresponded to 50% of the total height of the tablet. The tensile strength of the pads does not coated was 13 kpa.

iv)

Then the tablet was coated with 2.5 g of coating formed from 90% by weight of sebacic acid and 8% by weight of Nymcel-ZSB 16? By Metsa Seria and 2% by weight of Solka-Flok? 1016.

Example 3

(Comparative)

i)

A powder is prepared detergent base of composition A as follows: all material in particles of the base composition was mixed in a mixing drum or spray drum to form a homogeneous mixture in particles. The binder system was sprayed on top. Then the powder in a Loedige KM 600®.

ii)

Using a press from Instron® laboratory bench, detergent powder was introduced on the die The powder had been compressed with such force that The tensile strength of the tablet was 10 kpa.

iii)

In this example In particular, the pads have a diameter of 54 mm, a height of 24 mm and a weight of 45 g.

iv)

Then the tablet was coated with 2.5 g of coating formed from 90% by weight of adipic acid and 10% by weight of bentonite clay CSM

Example 4

(Comparative)

i)

A powder is prepared detergent base of composition A as follows: all material in particles of the base composition was mixed in a mixing drum or spray drum to form a homogeneous mixture in particles. The binder system was sprayed on top. Then the powder in a Loedige KM 600®.

ii)

Using a press from Instron® laboratory bench, detergent powder was introduced on the die The powder had been compressed with such force that The tensile strength of the tablet was 10 kpa.

iii)

In this example In particular, the pads have a diameter of 54 mm, a height of 24 mm and a weight of 45 g.

The tablet was then coated with 2.5 g of coating formed from 89% by weight of adipic acid, 10% by weight of bentonite clay and 1% Coasol ™.

Example 5

i)

A powder is prepared detergent base of composition A as follows: all material in particles of the base composition was mixed in a mixing drum or spray drum to form a homogeneous mixture in particles. The binder system was sprayed on top. Then the powder in a Loedige KM 600®.

ii)

Using a press from Instron® laboratory bench, detergent powder was introduced on the die The powder had been compressed with such force that The tensile strength of the tablet was 10 kpa.

iii)

In this example In particular, the pads have a diameter of 54 mm, a height of 24 mm and a weight of 45 g.

The tablet was then coated with 2.5 g of coating formed from 87% by weight of adipic acid, 10% by weight of bentonite clay and 1% Coasol ™ and 2% by weight of Solka-Flok? 1016.

Results

It was observed that:

For approximately 500 pills made of according to examples 1 and 2, the pads manufactured according to the example 1 have an incidence of chipping more than 5 times greater than the tablets manufactured according to example 2 once the coating has crystallized.

When comparing 10 tablets made according with examples 3, 4 and 5, the following incidence of chipping:

Example 3 Example 4 Example 5 Incidence of chipping 100% twenty% 0% (Pills 10 kpa when they are without coat)

Claims (9)

1. A coated detergent tablet, characterized in that the coating comprises reinforcing fibers. 2. A coated detergent tablet according to the claim 1, wherein the coating comprises a component which is liquid at 25 ° C. 3. A tablet according to claim 2, in the that the coating further comprises a structure crystallized 4. A tablet according to claims 2 or 3, in which the material that forms the crystallized structure is a dicarboxylic acid. 5. A tablet according to claims 1 or 4, in which the coating consists essentially of acid adipic 6. The coated detergent tablet according to the claim 5, wherein the coating comprises a clay. 7. A tablet according to claim 1, in the that the fibers have a length of at least 100 µm and less than 500 µm. 8. A procedure to prepare a pill according to any of the preceding claims, which It comprises the stages of: (a) form a core by compressing a material in particles, comprising the surfactant particulate material and detergent builder; (b) apply a coating material to the core, the coating material being in the form of dough cast (c) let the material of solidify cast coating; characterized in that the coating comprises reinforcing fibers. 9. A procedure to prepare a pill according to any one of claims 1 to 7, which It comprises the stages of: (a) form a core by compressing a material in particles, comprising the surfactant particulate material and detergent builder; (b) apply a coating material to the core, the coating material being dissolved in a solvent or in water; (c) let the solvent or solvent evaporate Water; characterized in that the coating comprises reinforcing fibers.