EP0957159A1 - Detergent tablet and process thereof - Google Patents

Detergent tablet and process thereof Download PDF

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Publication number
EP0957159A1
EP0957159A1 EP99420117A EP99420117A EP0957159A1 EP 0957159 A1 EP0957159 A1 EP 0957159A1 EP 99420117 A EP99420117 A EP 99420117A EP 99420117 A EP99420117 A EP 99420117A EP 0957159 A1 EP0957159 A1 EP 0957159A1
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EP
European Patent Office
Prior art keywords
tablet
layer
outer layers
dissolution
layers
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EP99420117A
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German (de)
French (fr)
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EP0957159B1 (en
Inventor
Jean-Louis Maitre
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CHIMIOTECHNIC
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CHIMIOTECHNIC
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3942—Inorganic per-compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0078—Multilayered tablets

Definitions

  • the invention relates to a detergent tablet and to its method of manufacturing.
  • powders or gels for dishwashers have been proposed. whose quantity required is empirically measured by the consumer who place in the dispenser of said dishwasher. This type of packaging is not satisfactory since the consumer mostly uses too much too little or too much powder or gel, leading to either improper washing, or overconsumption of products.
  • a multilayer tablet made up of at least two layers, one of which includes a bleach and a bleach activator, while the other includes an anti-corrosion agent.
  • Document EP-A-0 481 547 describes a pellet comprising a core coated with two consecutive layers.
  • the core contains the bleaching agent, while the outer layer is made up of enzymes, the nucleus and the outer layer being separated by a layer polymer-based intermediate.
  • This type of tablet has the disadvantage to interrupt the activity of the various constituents between the moment when the layer external is completely dissolved and the moment when the nucleus begins to dissolve.
  • Document DE-A-4 404 279 describes a tablet comprising at least three layers, of which the central layer contains a bleaching agent. He is in additionally mentioned that the tablet can also contain activators of bleaching or enzymes. However, nothing is said about the exact location of these various constituents, as well as the sequence of dissolution of the tablet.
  • the problem which the invention proposes to solve is to provide a multi-layer detergent tablet for efficient washing while avoiding in particular the deposit of a white veil on the dishes.
  • Another problem which the invention proposes to solve is to provide a multilayer tablet, the dissolution sequence of which allows in particular to separate the activity of the bleaching agent from that of the anti-corrosion system.
  • Another problem which the invention proposes to solve is to provide a multi-layer tablet which remains stable during storage. We have indeed found that in the tablets proposed until then, the enzymatic system was degraded in particular by bleaching agents or blending agents bleaching / bleaching activators.
  • said anti-scale agent is hydrated, advantageously prehydrated.
  • the outer layers have a identical composition.
  • the dissolution of the outer layers is carried out in a time range between two and seven minutes, preferably three to five minutes.
  • the dissolution of the middle layer takes place in a range of time between 8 and 16 minutes, advantageously 10 minutes.
  • the dissolution time of each of the layers varies in depending on the hardness of the tablet.
  • the hardness of the tablet is chosen between 3 and 40 kilopascals (KP), advantageously at 10 to 25 KP.
  • the tablet of the invention is in the form of three flat layers superimposed on each other by compacting their most surface large. In this way, the dissolution of the apparent periphery of the layer intermediate during the first sequence is very limited.
  • the anti-scale agent is chosen from the group comprising the tripolyphosphate, soda, organic phosphonates, aminopolyalkylenephosphonates, aminopolycarboxylates, homo and / or acrylic and maleic copolymers, acidic or in neutralized form.
  • the two outer layers include an enzyme system made up of protease type enzymes, amylase and lipase.
  • these outer layers may include an alkaline agent, a surfactant, an anti-tarnishing agent in particular with regard to silverware.
  • bleaching agent in practice a bleaching agent is used. bleaching chosen from the group comprising mono soda perborate or tetrahydrate, sodium percarbonate and sodium monopersulfate.
  • the middle layer includes in addition to a bleach activator selected from the group comprising tetraacetylene diamine (TAED), pentaacetylglucose (PAG), tetraacetylglycoluryl (TAGU).
  • TAED tetraacetylene diamine
  • PAG pentaacetylglucose
  • TAGU tetraacetylglycoluryl
  • the middle layer further comprises a complexing agent chosen from the group comprising phosphonate or homopolymers of acrylic acid or copolymers of acrylic and maleic acid.
  • the middle layer includes also an alkaline agent.
  • the middle layer includes an agent surfactant with anti-foaming activity.
  • This optimized stability characteristic makes it possible to implement much more peroxidizing bleaches such as sodium persulfate or still chlorinated compound.
  • the invention also relates to the method of manufacturing the tablet. detergent for washing dishes.
  • the first outer layer and the central layer are packed to a precompression value of between 10 kg / cm 2 and 100 kg / cm 2 , while the complex obtained is pressed to a value of between 20 kg / cm 2 and 400 kg / cm 2 .
  • said tablet will be oval, parallelepipedic, prismatic truncated or not and pyramidal truncated or not so that it can be introduced into the door panel case.
  • Example 1 tablet with phosphate
  • composition of the outer layers is first prepared, each of the constituents of which is included in the composition of the outer layers.
  • composition of the outer layers as a percentage by weight of the final tablet tripolyphosphate 22 acrylic homopolymer (PM 4500) 1 protease 0.75 amylase 0.75 dye traces surfactant: non-ionic 0.5 silicate / carbonate granulate 5
  • the first half is placed on a support, then it is packed by subjecting it to a precompression force of 15 kg / cm 2 .
  • a second mixture is then prepared intended to form the central layer.
  • composition of the middle layer as a percentage by weight of the final tablet phosphonate 0.85 soda perborate 7.5 silicate / carbonate co-granulates 15.44 TAED 4 nonionic surfactant 1 soda disilicate 10 perfume 0.20 pastillage additive 1
  • the second mixture is deposited on the first external layer, then it is packed by subjecting it to a precompression force of 15 kg / cm 2 .
  • the mixture intended to form the second outer layer is deposited on the central layer, then the tablet obtained is subjected to a pressure of 60 kg / cm 2 .
  • the hardness of the tablets obtained measured using a SCHLEUNIGER is 14 KP.
  • Example 2 phosphate-free tablet
  • composition of each of the outer and middle layers is as follows: • composition of the outer layers as a percentage by weight of the final tablet acrylic homopolymer (PM 4500) 1.5 phosphonate 0.425 protease 0.85 amylase 0.85 dye traces nonionic surfactant 0.5 cogranulate carbonate silicate 10.875 trisodium citrate 15 • composition of the middle layer as a percentage by weight of the final tablet acrylic homopolymer (PM 4500) 3 soda perborate 12.5 TAED 4 nonionic surfactant 1 perfume 0.2 pastillage additive 1 soda 5 cogranulate carbonate / silicate 13.3
  • the weight of the outer layers is 6 grams.
  • the weight of the inner layer is 8 grams.
  • the hardness of the tablets obtained measured using a SCHLEUNIGER is 14 KP.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)

Abstract

A detergent tablet with a sandwich structure of at least three layers comprises: (1) two external layers comprising an antiscaling agent; and (2) an internal layer comprising a bleaching agent. The external layers dissolve faster than the internal layer and are retarding agents for the internal layer in order to pretreat the washing water against lime scale. The tablet dissolves in two steps: first the external layers, then the internal layer when the external layers are entirely dissolved. An Independent claim is also included for the manufacturing of the tablet.

Description

L'invention se rapporte à une tablette détergente ainsi qu'à son procédé de fabrication.The invention relates to a detergent tablet and to its method of manufacturing.

On connaít diverses sortes de compositions détergentes pour le lavage de la vaisselle en machine.We know various kinds of detergent compositions for washing washing up in the machine.

On a ainsi proposé notamment des poudres ou des gels pour lave-vaisselle dont la quantité nécessaire est mesurée empiriquement par le consommateur qui les place dans le doseur dudit lave-vaisselle. Ce type de conditionnement n'est pas satisfaisant dans la mesure où le consommateur utilise la plupart du temps une trop faible ou une trop forte quantité de poudre ou de gel, conduisant ainsi soit à un mauvais lavage, soit à une surconsommation de produits.In particular, powders or gels for dishwashers have been proposed. whose quantity required is empirically measured by the consumer who place in the dispenser of said dishwasher. This type of packaging is not satisfactory since the consumer mostly uses too much too little or too much powder or gel, leading to either improper washing, or overconsumption of products.

Pour résoudre ce problème, on a proposé des tablettes dites monocouche constituées d'un mélange de composants tels que agents anti-calcaire, système enzymatique, agents de blanchiment, etc... Toutefois, ce type de tablettes présente l'inconvénient de conduire à la dissolution plus ou moins rapide et aléatoire des composants en fonction du cycle et de la température de lavage. De plus, les effets techniques des composants sont combinés de façon non rationnelle. En outre et surtout, on peut être amené à constater le dépôt d'un voile blanc sur la vaisselle, particulièrement apparent sur les verres, ce qui suggère un mauvais lavage ou rinçage et conduit à une dégradation rapide et apparente de la qualité de la vaisselle et à la perte de l'effet de transparence des verres.To solve this problem, so-called monolayer tablets have been proposed. made up of a mixture of components such as anti-scale agents, system enzymatic, bleaching agents, etc ... However, this type of tablets has the disadvantage of leading to the more or less rapid and random dissolution of components depending on the wash cycle and temperature. In addition, the effects component techniques are combined in an irrational way. Furthermore and above all, we may have to note the deposit of a white veil on the dishes, particularly noticeable on glasses, which suggests improper washing or rinsing and leads to a rapid and apparent deterioration in the quality of the dishes and the loss of the transparency effect of the glasses.

Pour résoudre ce problème, on a proposé dans le document WO 97/03177 une tablette muticouches constituée d'au moins deux couches, dont une comprend un agent de blanchiment et un activateur de blanchiment, tandis que l'autre comprend un agent anti-corrosif.To solve this problem, the document WO 97/03177 has been proposed. a multilayer tablet made up of at least two layers, one of which includes a bleach and a bleach activator, while the other includes an anti-corrosion agent.

Même si ce concept permet de séparer les deux actions, respectivement blanchiment et anticorrosion, on peut être amené à constater encore l'apparition du voile blanc sur la vaisselle et les verres en particulier. En d'autres termes, le système anti-calcaire n'a pas joué son rôle immédiatement, ou tout au moins de façon insuffisante.Even if this concept allows to separate the two actions, respectively bleaching and anticorrosion, we may still notice the appearance of white veil on dishes and glasses in particular. In other words, the anti-lime system did not play its role immediately, or at least insufficiently.

Le document EP-A-0 481 547 décrit une pastille comprenant un noyau enrobé de deux couches consécutives. Dans un mode de réalisation préféré, le noyau contient l'agent de blanchiment, tandis que la couche externe est composée d'enzymes, le noyau et la couche externe étant séparés par une couche intermédiaire à base de polymère. Ce type de pastille présente dont l'inconvénient d'interrompre l'activité des différents constituants entre le moment où la couche externe est totalement dissoute et le moment où le noyau commence à se dissoudre.Document EP-A-0 481 547 describes a pellet comprising a core coated with two consecutive layers. In a preferred embodiment, the core contains the bleaching agent, while the outer layer is made up of enzymes, the nucleus and the outer layer being separated by a layer polymer-based intermediate. This type of tablet has the disadvantage to interrupt the activity of the various constituents between the moment when the layer external is completely dissolved and the moment when the nucleus begins to dissolve.

Le document DE-A-4 404 279 décrit une tablette comprenant au moins trois couches, dont la couche centrale contient un agent de blanchiment. Il est en outre mentionné que la tablette peut contenir également des activateurs de blanchiment ou encore des enzymes. Cependant, rien n'est indiqué concernant la localisation exacte de ces différents constituants, de même que la séquence de dissolution de la tablette.Document DE-A-4 404 279 describes a tablet comprising at least three layers, of which the central layer contains a bleaching agent. He is in additionally mentioned that the tablet can also contain activators of bleaching or enzymes. However, nothing is said about the exact location of these various constituents, as well as the sequence of dissolution of the tablet.

Le problème que se propose de résoudre l'invention est de fournir une tablette détergente multicouches permettant un lavage efficace en évitant notamment le dépôt d'un voile blanc sur la vaisselle.The problem which the invention proposes to solve is to provide a multi-layer detergent tablet for efficient washing while avoiding in particular the deposit of a white veil on the dishes.

Un autre problème que se propose de résoudre l'invention est de fournir une tablette multicouches, dont la séquence de dissolution permette notamment de séparer l'activité de l'agent de blanchiment de celle du système anti-corrosif.Another problem which the invention proposes to solve is to provide a multilayer tablet, the dissolution sequence of which allows in particular to separate the activity of the bleaching agent from that of the anti-corrosion system.

Un autre problème que se propose de résoudre l'invention est de fournir une tablette multicouches qui reste stable lors du stockage. On a en effet constaté que dans les tablettes proposées jusqu'alors, le système enzymatique était dégradé en particulier par les agents de blanchiment ou le mélange agents de blanchiment/activateurs de blanchiment.Another problem which the invention proposes to solve is to provide a multi-layer tablet which remains stable during storage. We have indeed found that in the tablets proposed until then, the enzymatic system was degraded in particular by bleaching agents or blending agents bleaching / bleaching activators.

Pour résoudre l'ensemble de ces problèmes, l'invention propose une tablette détergente constituée d'une structure sandwich en au moins trois couches superposées, respectivement :

  • deux couches externes ;
  • une couche médiane ;
caractérisée en ce que :
  • les couches externes comprennent un agent anti-calcaire ;
  • la couche médiane comprend un agent de blanchiment ;
  • les couches externes présentent un temps de dissolution plus rapide que celui de la couche médiane et ont pour fonction de constituer des agents retardateurs à la dissolution de la couche médiane et donc de ses effets, en vue de permettre un prétraitement anti-calcaire de l'eau de lavage et donc l'obtention d'une eau pure pour le lavage ultérieur ;
la structure sandwich tricouches permettant d'obtenir une séquence de dissolution de la tablette en deux temps à savoir :
  • tout d'abord, la dissolution des deux couches externes,
  • puis, lorsque les couches externes sont complètement dissoutes, la dissolution de la couche médiane.
To solve all of these problems, the invention proposes a detergent tablet consisting of a sandwich structure in at least three superimposed layers, respectively:
  • two outer layers;
  • a middle layer;
characterized in that:
  • the outer layers include an anti-scale agent;
  • the middle layer includes a bleaching agent;
  • the outer layers have a faster dissolution time than that of the middle layer and have the function of constituting agents delaying the dissolution of the middle layer and therefore of its effects, with a view to allowing an anti-lime pretreatment of the washing water and therefore obtaining pure water for subsequent washing;
the three-layer sandwich structure making it possible to obtain a sequence for dissolving the tablet in two stages, namely:
  • first, the dissolution of the two outer layers,
  • then, when the outer layers are completely dissolved, the middle layer dissolves.

Afin de permettre la dissolution rapide de l'agent anti-calcaire, et donc des couches externes, ledit agent anti-calcaire est hydraté, avantageusement préhydraté.In order to allow the rapid dissolution of the anti-scale agent, and therefore outer layers, said anti-scale agent is hydrated, advantageously prehydrated.

On pourra par exemple utiliser du tripolyphosphate préhydraté commercialisé par RHONE-POULENC sous la marque "RHODIAPHOS HPA 3,5".We can for example use prehydrated tripolyphosphate marketed by RHONE-POULENC under the brand "RHODIAPHOS HPA 3.5 ".

Selon un mode de réalisation avantageux de l'invention, et pour permettre une séquence de dissolution homogène de la tablette, les couches externes ont une composition identique.According to an advantageous embodiment of the invention, and to allow a homogeneous dissolution sequence of the tablet, the outer layers have a identical composition.

En pratique, la dissolution des couches externes est réalisée dans une gamme de temps comprise entre deux et sept minutes, avantageusement trois à cinq minutes.In practice, the dissolution of the outer layers is carried out in a time range between two and seven minutes, preferably three to five minutes.

De même, la dissolution de la couche médiane s'effectue dans une gamme de temps comprise entre 8 et 16 minutes, avantageusement 10 minutes.Similarly, the dissolution of the middle layer takes place in a range of time between 8 and 16 minutes, advantageously 10 minutes.

Par ailleurs, le temps de dissolution de chacune des couches varie en fonction de la dureté de la pastille. En pratique, la dureté de la pastille est choisie entre 3 et 40 kilopascals (KP), avantageusement à 10 à 25 KP. Furthermore, the dissolution time of each of the layers varies in depending on the hardness of the tablet. In practice, the hardness of the tablet is chosen between 3 and 40 kilopascals (KP), advantageously at 10 to 25 KP.

Comme déjà dit, la tablette de l'invention se présente sous forme de trois couches planes superposées l'une à l'autre par tassement de leur surface la plus large. De la sorte, la dissolution de la périphérie apparente de la couche intermédiaire lors de la première séquence est très limitée.As already said, the tablet of the invention is in the form of three flat layers superimposed on each other by compacting their most surface large. In this way, the dissolution of the apparent periphery of the layer intermediate during the first sequence is very limited.

En pratique, le poids de la tablette de l'invention est d'environ 20 grammes, le poids de chacune des couches se répartissant comme suit :

  • couches externes de 5 à 7 g
  • couche médiane de 6 à 10 g.
In practice, the weight of the tablet of the invention is approximately 20 grams, the weight of each of the layers distributed as follows:
  • outer layers of 5 to 7 g
  • middle layer from 6 to 10 g.

De préférence, l'agent anti-calcaire est choisi dans le groupe comprenant le tripolyphosphate, le citrate de soude, les phosphonates organiques, les aminopolyalkylènephosphonates, les aminopolycarboxylates, les homo et/ou copolymères acryliques et maleiques acides ou sous forme neutralisées.Preferably, the anti-scale agent is chosen from the group comprising the tripolyphosphate, soda, organic phosphonates, aminopolyalkylenephosphonates, aminopolycarboxylates, homo and / or acrylic and maleic copolymers, acidic or in neutralized form.

Pour permettre l'attaque des salissures, les deux couches externes comprennent un système enzymatique constitué d'enzymes du type protéase, amylase et lipase.To allow dirt attack, the two outer layers include an enzyme system made up of protease type enzymes, amylase and lipase.

En outre, ces couches externes peuvent comprendre un agent alcalin, un agent tensioactif, un agent anti-ternissant notamment à l'égard de l'argenterie.In addition, these outer layers may include an alkaline agent, a surfactant, an anti-tarnishing agent in particular with regard to silverware.

Comme déjà dit, c'est seulement lorsque les deux couches externes sont dissoutes, que débute l'action de la couche médiane.As already said, it is only when the two outer layers are dissolved, that the action of the middle layer begins.

En tant qu'agent de blanchiment, on utilise en pratique un agent de blanchiment choisi dans le groupe comprenant le perborate de soude mono ou tétrahydraté, le percarbonate de soude et le monopersulfate de soude. As a bleaching agent, in practice a bleaching agent is used. bleaching chosen from the group comprising mono soda perborate or tetrahydrate, sodium percarbonate and sodium monopersulfate.

Néanmoins, pour permettre un blanchiment de la vaisselle plus efficace après élimination du calcaire et des salissures, la couche médiane comprend en outre un activateur de blanchiment choisi dans le groupe comprenant le tétraacétylène diamine (TAED), le pentaacétylglucose (PAG), le tétraacétylglycoluryl (TAGU).However, to allow more effective dishwashing after removal of lime and dirt, the middle layer includes in addition to a bleach activator selected from the group comprising tetraacetylene diamine (TAED), pentaacetylglucose (PAG), tetraacetylglycoluryl (TAGU).

Pour permettre la complexation des ions métalliques et amener des effets dispersants, la couche médiane comprend en outre un agent complexant choisi dans le groupe comprenant le phosphonate ou les homopolymères d'acide acrylique ou copolymères d'acide acrylique et maléique.To allow complexing of metal ions and bring effects dispersants, the middle layer further comprises a complexing agent chosen from the group comprising phosphonate or homopolymers of acrylic acid or copolymers of acrylic and maleic acid.

Pour renforcer l'activité de lavage, la couche médiane comprend également un agent alcalin.To strengthen the washing activity, the middle layer includes also an alkaline agent.

Pour éviter l'apparition de mousse, la couche médiane comprend un agent tensioactif à activité anti-mousse.To avoid the appearance of foam, the middle layer includes an agent surfactant with anti-foaming activity.

Du fait de la séparation de l'activité enzymatique de celle de blanchiment, on observe une très bonne stabilité au stockage de la tablette de l'invention. De plus, compte tenu du fait que le milieu peroxydant est sans eau libre, il n'y a que très peu de risque de perte d'oxygène actif. En d'autres termes, le système enzymatique n'est pas perturbé par le système peroxydant.Due to the separation of the enzymatic activity from that of bleaching, very good storage stability of the tablet of the invention is observed. Of more, taking into account the fact that the peroxidizing medium is without free water, there is only very little risk of loss of active oxygen. In other words, the system enzymatic is not disturbed by the peroxidizing system.

Cette caractéristique de stabilité optimisée permet de mettre en oeuvre des agents de blanchiment beaucoup plus peroxydant du type persulfate de soude ou encore composé chloré.This optimized stability characteristic makes it possible to implement much more peroxidizing bleaches such as sodium persulfate or still chlorinated compound.

L'invention concerne également le procédé de fabrication de la tablette détergente pour le lavage de la vaisselle. The invention also relates to the method of manufacturing the tablet. detergent for washing dishes.

Selon ce procédé :

  • on mélange tout d'abord les différents constituants destinés à former les couches externes ;
  • parallèlement, on mélange les différents constituants destinés à former la couche centrale ;
  • on dépose sur un support, puis on tasse partie du mélange destiné à former la première couche externe ;
  • on dépose ensuite sur ladite première couche externe le mélange destiné à former la couche centrale, puis on tasse le complexe obtenu ;
  • puis, on dépose sur la couche centrale la partie restante du mélange formant la seconde couche externe ;
  • enfin, on presse la tablette obtenue.
According to this process:
  • firstly the various constituents intended to form the outer layers are mixed;
  • in parallel, the various constituents intended to form the central layer are mixed;
  • it is deposited on a support, then cup part of the mixture intended to form the first outer layer;
  • the mixture intended to form the central layer is then deposited on said first external layer, then the complex obtained is packed;
  • then, the remaining part of the mixture forming the second outer layer is deposited on the central layer;
  • finally, the tablet obtained is pressed.

Selon une caractéristique du procédé, on tasse la première couche externe et la couche centrale à une valeur de précompression comprise entre 10 kg/cm2 et 100 kg/cm2, tandis que le complexe obtenu est pressé à une valeur comprise entre 20 kg/cm2 et 400 kg/cm2.According to one characteristic of the process, the first outer layer and the central layer are packed to a precompression value of between 10 kg / cm 2 and 100 kg / cm 2 , while the complex obtained is pressed to a value of between 20 kg / cm 2 and 400 kg / cm 2 .

En pratique, ladite tablette sera de forme ovale, parallélépipédique, prismatique tronquée ou non et pyramidale tronquée ou non de sorte à pouvoir être introduite dans le boitier de la contre porte.In practice, said tablet will be oval, parallelepipedic, prismatic truncated or not and pyramidal truncated or not so that it can be introduced into the door panel case.

En effet, compte tenu du fait que la tablette ne doit agir que pendant le lavage, il est recommandé d'introduire ladite tablette dans le doseur de la contre-porte du lave-vaisselle.In fact, given the fact that the tablet should only act during the washing, it is recommended to insert the said shelf in the countermeter of the door of dishwasher.

Les caractéristiques de l'invention et les avantages qui en découlent ressortiront mieux des exemples de réalisation suivants.The characteristics of the invention and the advantages which flow therefrom The following exemplary embodiments will better emerge.

Dans les deux exemples de réalisation suivants, on propose deux formulations différentes de la tablette de l'invention avec ou sans la présence de phosphate dans les couches externes (respectivement exemple 1 et exemple 2) In the following two exemplary embodiments, two are proposed different formulations of the tablet of the invention with or without the presence of phosphate in the outer layers (respectively example 1 and example 2)

Exemple 1 : tablette avec phosphate Example 1 : tablet with phosphate

On prépare tout d'abord un mélange dont chacun des constituants entre dans la composition des couches externes. • composition des couches externes en pourcentage en poids de la tablette finale : tripolyphosphate 22 homopolymère acrylique (PM 4500) 1 protéase 0,75 amylase 0,75 colorant traces tensioactif: non ionique 0,5 granulé silicate/carbonate 5 A mixture is first prepared, each of the constituents of which is included in the composition of the outer layers. • composition of the outer layers as a percentage by weight of the final tablet: tripolyphosphate 22 acrylic homopolymer (PM 4500) 1 protease 0.75 amylase 0.75 dye traces surfactant: non-ionic 0.5 silicate / carbonate granulate 5

On dépose la première moitié sur un support, puis on la tasse en la soumettant à une force de précompression de 15 kg/cm2.The first half is placed on a support, then it is packed by subjecting it to a precompression force of 15 kg / cm 2 .

On prépare ensuite un second mélange destiné à former la couche centrale. • composition de la couche médiane en pourcentage en poids de la tablette finale phosphonate 0,85 perborate de soude 7,5 cogranulés silicate/carbonate 15,44 TAED 4 tensio actif non ionique 1 disilicate de soude 10 parfum 0,20 additif de pastillage 1 A second mixture is then prepared intended to form the central layer. • composition of the middle layer as a percentage by weight of the final tablet phosphonate 0.85 soda perborate 7.5 silicate / carbonate co-granulates 15.44 TAED 4 nonionic surfactant 1 soda disilicate 10 perfume 0.20 pastillage additive 1

On dépose le deuxième mélange sur la première couche externe, puis on le tasse en le soumettant à une force de précompression de 15 kg/cm2.The second mixture is deposited on the first external layer, then it is packed by subjecting it to a precompression force of 15 kg / cm 2 .

On dépose enfin sur la couche centrale le mélange destiné à former la seconde couche externe, puis on soumet la tablette obtenue à une pression de 60 kg/cm2.Finally, the mixture intended to form the second outer layer is deposited on the central layer, then the tablet obtained is subjected to a pressure of 60 kg / cm 2 .

La masse de la tablette obtenue est de 20 grammes, la masse de chaque couche se répartissant comme suit :

  • couche supérieure et couche inférieure : 6 grammes
  • couche médiane : 8 grammes
The mass of the tablet obtained is 20 grams, the mass of each layer distributed as follows:
  • upper layer and lower layer: 6 grams
  • middle layer: 8 grams

La dureté des tablettes obtenues mesurée à l'aide d'un appareil de SCHLEUNIGER est de 14 KP.The hardness of the tablets obtained measured using a SCHLEUNIGER is 14 KP.

On procède ensuite à des tests de dissolution dans un lave vaisselle de marque MIELE ® dans les conditions suivantes: programme sans prélavage à 45°C, temps de lavage 18 minutes. We then proceed to dissolution tests in a dishwasher of MIELE ® brand under the following conditions: program without prewash at 45 ° C, washing time 18 minutes.

Les temps de dissolution (en minute) de chacune des couches sont représentés dans le tableau ci-après. ESSAI 1 ESSAI 2 ESSAI 3 Temps de dissolution de la couche médiane 12 11 12 temps de dissolution de la couche supérieure 4 5 4 temps de dissolution de la couche inférieure 5 4 4 The dissolution times (in minutes) for each of the layers are shown in the table below. TEST 1 TEST 2 TEST 3 Dissolution time of the middle layer 12 11 12 dissolution time of the upper layer 4 5 4 dissolution time of the lower layer 5 4 4

Exemple 2 : tablette sans phosphate Example 2 : phosphate-free tablet

La composition de chacune des couches externes et médiane est la suivante: • composition des couches externes en pourcentage en poids de la tablette finale homopolymère acrylique (PM 4500) 1,5 phosphonate 0, 425 protéase 0,85 amylase 0,85 colorant traces tensio-actif non ionique 0,5 cogranulé carbonate silicate 10,875 citrate trisodique 15 • composition de la couche médiane en pourcentage en poids de la tablette finale homopolymère acrylique (PM 4500) 3 perborate de soude 12,5 TAED 4 tensio actif non ionique 1 parfum 0,2 additif de pastillage 1 citrate de soude 5 cogranulé carbonate/ silicate 13,3 The composition of each of the outer and middle layers is as follows: • composition of the outer layers as a percentage by weight of the final tablet acrylic homopolymer (PM 4500) 1.5 phosphonate 0.425 protease 0.85 amylase 0.85 dye traces nonionic surfactant 0.5 cogranulate carbonate silicate 10.875 trisodium citrate 15 • composition of the middle layer as a percentage by weight of the final tablet acrylic homopolymer (PM 4500) 3 soda perborate 12.5 TAED 4 nonionic surfactant 1 perfume 0.2 pastillage additive 1 soda 5 cogranulate carbonate / silicate 13.3

Le poids des couches externes est de 6 grammes.The weight of the outer layers is 6 grams.

Le poids de la couche interne est égale à 8 grammes.The weight of the inner layer is 8 grams.

La dureté des tablettes obtenues mesurée à l'aide d'un appareil de SCHLEUNIGER est de 14 KP.The hardness of the tablets obtained measured using a SCHLEUNIGER is 14 KP.

On procède ensuite à des tests de dissolution dans un lave vaisselle de marque MIELE ® dans les conditions suivantes: programme sans prélavage à 45°C, temps de lavage 18 minutes. We then proceed to dissolution tests in a dishwasher of MIELE ® brand under the following conditions: program without prewash at 45 ° C, washing time 18 minutes.

Les temps de dissolution (en minute) de chacune des couches sont représentés dans le tableau ci-après. ESSAI 1 ESSAI 2 ESSAI 3 Temps de dissolution de la couche médiane 14 15 15 temps de dissolution de la couche supérieure 5 6 5 temps de dissolution de la couche inférieure 6 5 6 The dissolution times (in minutes) for each of the layers are shown in the table below. TEST 1 TEST 2 TEST 3 Dissolution time of the middle layer 14 15 15 dissolution time of the upper layer 5 6 5 dissolution time of the lower layer 6 5 6

Les avantages de l'invention ressortent bien de la description.The advantages of the invention appear clearly from the description.

On notera notamment le séquencage des dissolutions des couches externes et de la couche médiane permettant d'épurer l'eau de lavage avant le lavage proprement dit et ainsi de ne pas obtenir de voile blanc sur la vaisselle et notamment sur les verres.Note in particular the sequencing of the dissolution of the outer layers and the middle layer to purify the wash water before washing proper and so not to get a white veil on the dishes and especially on glasses.

On notera en outre l'intérêt de séparer les couches externes à base d'agents anti-calcaires et d'agents enzymatiques de la couche médiane à base d'agents de blanchiment en vue d'optimiser la stabilité de la tablette lors de son stockage.Note also the advantage of separating the outer layers based on agents anti-limescale and enzymatic agents of the middle layer based on bleaching to optimize the stability of the tablet during storage.

Claims (11)

Tablette détergente constituée d'une structure sandwich en au moins trois couches superposées, respectivement : deux couches externes ; une couche médiane ; caractérisée en ce que : les couches externes comprennent un agent anti-calcaire ; la couche médiane comprend un agent de blanchiment ; les couches externes présentent un temps de dissolution plus rapide que celui de la couche médiane et ont pour fonction de constituer des agents retardateurs à la dissolution de la couche médiane et donc de ses effets, en vue de permettre un prétraitement anti-calcaire de l'eau de lavage et donc l'obtention d'une eau pure pour le lavage ultérieur ; la structure sandwich tricouches permettant d'obtenir une séquence de dissolution de la tablette en deux temps à savoir : tout d'abord, la dissolution des deux couches externes, puis, lorsque les couches externes sont complètement dissoutes, la dissolution de la couche médiane. Detergent tablet consisting of a sandwich structure in at least three superimposed layers, respectively: two outer layers; a middle layer; characterized in that: the outer layers include an anti-scale agent; the middle layer includes a bleaching agent; the outer layers have a faster dissolution time than that of the middle layer and have the function of constituting agents delaying the dissolution of the middle layer and therefore of its effects, with a view to allowing an anti-lime pretreatment of the washing water and therefore obtaining pure water for subsequent washing; the three-layer sandwich structure making it possible to obtain a sequence for dissolving the tablet in two stages, namely: first, the dissolution of the two outer layers, then, when the outer layers are completely dissolved, the middle layer dissolves. Tablette selon la revendication 1, caractérisée en ce que les deux couches externes on une composition identique.Tablet according to claim 1, characterized in that the two outer layers have an identical composition. Tablette selon la revendication 2, caractérisée en ce que les deux couches externes comprennent en outre un système enzymatique.Tablet according to claim 2, characterized in that the two outer layers further comprise an enzymatic system. Tablette selon l'une des revendications 1 à 3, caractérisée en ce que l'agent anti-calcaire est préhydraté et choisi dans le groupe comprenant le tripolyphosphate, le citrate de soude,les phosphonates organiques, les aminopolyalkylènephosphonates, les aminopolycarboxylates, les homo et/ou copolymères acryliques et maleiques acides ou sous forme neutralisées. Tablet according to one of claims 1 to 3, characterized in that the anti-scale agent is prehydrated and chosen from the group comprising tripolyphosphate, sodium citrate, organic phosphonates, aminopolyalkylenephosphonates, aminopolycarboxylates, homo and / or acidic and neutralized acrylic and maleic copolymers. Tablette selon l'une des revendications 1 à 4, caractérisée en ce que l'agent de blanchiment est choisi dans le groupe comprenant le perborate de soude mono ou tétrahydraté, le percarbonate de soude et le monopersulfate de soude.Tablet according to one of claims 1 to 4, characterized in that the bleaching agent is chosen from the group comprising sodium perborate mono or tetrahydrate, sodium percarbonate and sodium monopersulfate. Tablette selon l'une des revendications 1 à 5, caractérisée en ce que la dissolution des couches externes est réalisée dans une gamme de temps comprise entre deux et sept minutes, avantageusement entre trois minutes et cinq.Tablet according to one of claims 1 to 5, characterized in that the dissolution of the external layers is carried out in a time range between two and seven minutes, advantageously between three minutes and five. Tablette selon l'une des revendications 1 à 6, caractérisée en ce que la dissolution de la couche médiane s'effectue dans une gamme de temps comprise entre huit et seize minutes, avantageusement dix minutes.Tablet according to one of claims 1 to 6, characterized in that the dissolution of the middle layer takes place in a time range between eight and sixteen minutes, advantageously ten minutes. Tablette selon l'une des revendications 1 à 7, caractérisée en ce que le poids de chacune des couches est réparti comme suit : couches externes : 5 à 7 g couche médiane : 6 à 10 g Tablet according to one of Claims 1 to 7, characterized in that the weight of each of the layers is distributed as follows: outer layers: 5 to 7 g middle layer: 6 to 10 g Tablette selon l'une des revendications 1 à 8, caractérisée en ce que la dureté de ladite tablette est choisie entre 3 et 40 kilopascals.Tablet according to one of claims 1 to 8, characterized in that the hardness of said tablet is chosen between 3 and 40 kilopascals. Procédé de fabrication de la tablette objet de l'une des revendications 1 à 9 selon lequel : on mélange tout d'abord les différents constituants destinés à former les couches externes ; parallèlement, on mélange les différents constituants destinés à former la couche centrale ; on dépose sur un support, puis on tasse partie du mélange destiné à former la première couche externe ; on dépose ensuite sur ladite première couche externe le mélange destiné à former la couche centrale, puis on tasse le complexe obtenu ; puis, on dépose sur la couche centrale la partie restante du mélange formant la seconde couche externe ; enfin, on presse la tablette obtenue. Method of manufacturing the tablet which is the subject of one of claims 1 to 9, according to which: firstly the various constituents intended to form the outer layers are mixed; in parallel, the various constituents intended to form the central layer are mixed; it is deposited on a support, then cup part of the mixture intended to form the first outer layer; the mixture intended to form the central layer is then deposited on said first external layer, then the complex obtained is packed; then, the remaining part of the mixture forming the second outer layer is deposited on the central layer; finally, the tablet obtained is pressed. Procédé selon la revendication 10, caractérisé en ce que l'on tasse la première couche externe et la couche centrale à une valeur de précompression comprise entre 10 kg/cm2 et 100 kg/cm2, tandis que le complexe obtenu est pressé à une valeur comprise entre 20 kg/cm2 et 400 kg/cm2.Method according to claim 10, characterized in that the first outer layer and the central layer are packed to a precompression value of between 10 kg / cm 2 and 100 kg / cm 2 , while the complex obtained is pressed to a value between 20 kg / cm 2 and 400 kg / cm 2 .
EP99420117A 1998-05-14 1999-05-12 Detergent tablet and process thereof Expired - Lifetime EP0957159B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9806338 1998-05-14
FR9806338A FR2778666B1 (en) 1998-05-14 1998-05-14 THREE-LAYERED DETERGENT TABLET

Publications (2)

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EP0957159A1 true EP0957159A1 (en) 1999-11-17
EP0957159B1 EP0957159B1 (en) 2002-10-09

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EP (1) EP0957159B1 (en)
AT (1) ATE225846T1 (en)
DE (1) DE69903371T2 (en)
ES (1) ES2182469T3 (en)
FR (1) FR2778666B1 (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001038478A1 (en) * 1999-11-26 2001-05-31 Unilever N.V. Detergent compositions
GB2358405A (en) * 1999-12-17 2001-07-25 Unilever Plc Use of dish-washing compositions
EP1239028A1 (en) * 2001-03-05 2002-09-11 Unilever Plc Detergent tablets
FR2926088A1 (en) * 2008-01-03 2009-07-10 Eurotab Sa Detergent tablet, useful e.g. in dishwasher devices, comprises five superimposed layers with three layers having different compositions, phosphate, active enzymes, detergent additives, surfactants and bleaching agents
WO2012069895A1 (en) 2010-11-12 2012-05-31 Dental Care Innovation Gmbh Soluble tablet, containing abrasive media
US10959931B2 (en) 2017-02-02 2021-03-30 Water Pik, Inc. Tablet including abrasive for dental cleaning

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0224128A2 (en) * 1985-11-21 1987-06-03 Henkel Kommanditgesellschaft auf Aktien Multilayered detergent tablets for mechanical dish-washing
EP0481547A1 (en) * 1990-10-17 1992-04-22 Unilever N.V. Machine dishwashing detergent tablets
DE4404279A1 (en) * 1994-02-10 1995-08-17 Henkel Kgaa Tablet with builder substances
WO1997003177A1 (en) * 1995-07-13 1997-01-30 Joh. A. Benckiser Gmbh Dish washer product in tablet form

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0224128A2 (en) * 1985-11-21 1987-06-03 Henkel Kommanditgesellschaft auf Aktien Multilayered detergent tablets for mechanical dish-washing
EP0481547A1 (en) * 1990-10-17 1992-04-22 Unilever N.V. Machine dishwashing detergent tablets
DE4404279A1 (en) * 1994-02-10 1995-08-17 Henkel Kgaa Tablet with builder substances
WO1997003177A1 (en) * 1995-07-13 1997-01-30 Joh. A. Benckiser Gmbh Dish washer product in tablet form

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001038478A1 (en) * 1999-11-26 2001-05-31 Unilever N.V. Detergent compositions
WO2001038479A1 (en) * 1999-11-26 2001-05-31 Unilever N.V. Detergent compositions
GB2358405A (en) * 1999-12-17 2001-07-25 Unilever Plc Use of dish-washing compositions
GB2358405B (en) * 1999-12-17 2004-10-20 Unilever Plc Use of dish-washing compositions
EP1239028A1 (en) * 2001-03-05 2002-09-11 Unilever Plc Detergent tablets
FR2926088A1 (en) * 2008-01-03 2009-07-10 Eurotab Sa Detergent tablet, useful e.g. in dishwasher devices, comprises five superimposed layers with three layers having different compositions, phosphate, active enzymes, detergent additives, surfactants and bleaching agents
WO2012069895A1 (en) 2010-11-12 2012-05-31 Dental Care Innovation Gmbh Soluble tablet, containing abrasive media
DE102010051226A1 (en) 2010-11-12 2012-05-31 Dental Care Innovation Gmbh Rinse-off tray with abrasive components
US10959931B2 (en) 2017-02-02 2021-03-30 Water Pik, Inc. Tablet including abrasive for dental cleaning
US11596587B2 (en) 2017-02-02 2023-03-07 Water Pik, Inc. Tablet including abrasive for dental cleaning

Also Published As

Publication number Publication date
ES2182469T3 (en) 2003-03-01
FR2778666A1 (en) 1999-11-19
FR2778666B1 (en) 2003-01-17
EP0957159B1 (en) 2002-10-09
ATE225846T1 (en) 2002-10-15
DE69903371T2 (en) 2003-06-18
DE69903371D1 (en) 2002-11-14

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