EP0933421B1 - Compact phosphate-free cleaning tablets - Google Patents

Compact phosphate-free cleaning tablets Download PDF

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Publication number
EP0933421B1
EP0933421B1 EP97811000A EP97811000A EP0933421B1 EP 0933421 B1 EP0933421 B1 EP 0933421B1 EP 97811000 A EP97811000 A EP 97811000A EP 97811000 A EP97811000 A EP 97811000A EP 0933421 B1 EP0933421 B1 EP 0933421B1
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EP
European Patent Office
Prior art keywords
tablet
carrier material
surfactants
cleaning agent
surfactant
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP97811000A
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German (de)
French (fr)
Other versions
EP0933421A1 (en
Inventor
Karin Kleeli
Hans Eggenschwiler
Rudolf Gitzi
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mifa AG Frenkedorf
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Mifa AG Frenkedorf
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Publication date
Application filed by Mifa AG Frenkedorf filed Critical Mifa AG Frenkedorf
Priority to DE59712770T priority Critical patent/DE59712770D1/en
Priority to EP97811000A priority patent/EP0933421B1/en
Priority to AT97811000T priority patent/ATE346133T1/en
Publication of EP0933421A1 publication Critical patent/EP0933421A1/en
Application granted granted Critical
Publication of EP0933421B1 publication Critical patent/EP0933421B1/en
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/08Silicates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0034Fixed on a solid conventional detergent ingredient
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047Detergents in the form of bars or tablets
    • C11D17/0065Solid detergents containing builders
    • C11D17/0073Tablets
    • C11D17/0082Coated tablets
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/046Salts
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246Silicates, e.g. diatomaceous earth
    • C11D3/128Aluminium silicates, e.g. zeolites

Definitions

  • the present invention relates to a phosphate-free detergent tablet according to independent claim 1, and to a process for its preparation according to independent claim 9.
  • Detergents or cleaning agents in tablet form are enjoying increasing popularity, because they allow the required amount of detergent or detergent, in comparison to the addition of corresponding powdered agents to dose in a more defined unit quantity.
  • the use of a defined unit quantity of detergent or cleaning agent is also more convenient and safer, since spillage of the often aggressive substances is avoided.
  • a dishwashing detergent in the form of a multilayer tablet which contains a bleaching agent, a bleach activator, a silver / copper corrosion inhibitor and other conventional ingredients.
  • the silver / copper corrosion inhibitor is not contained together in a layer together with the bleaching agent and the bleach activator.
  • brittleness is essentially the surfactant or surfactants, which reduce the tablet hardness and thus prevent the sintering effect during pressing.
  • This brittleness and instability is further enhanced by the hygroscopicity of the substances contained in the tablets: hygroscopy causes more or less humidity to be absorbed by the tablet over time, significantly increasing the tablet's volume and further reducing tablet hardness.
  • the currently sold detergent tablets are offered in individualized packaging and must first be unpacked for their use by the user or user before they can be placed in the dispenser. Consequently, the currently marketed detergent tablets are ultimately unsatisfactory due to their brittleness and hygroscopicity, and thus their overall suppleness.
  • the object of the present invention was to provide a phosphate-free detergent for dishwashers in single-phase or multi-phase tablet form, which tablet contains one or more surfactants and which is so compact that it does not need to be packaged to prevent it with the time in the breaks goes.
  • Detergent tablet is generally to be understood as a tablet for cleaning purposes in machine-washing processes in dishwashers.
  • porous support material should be such that it is readily able to take up the surfactant or the surfactants.
  • Preferred porous support materials are disilicates, sulfates, zeolites or Mixtures thereof. These are present as salts, with their alkali metal salts, for example the sodium or potassium salts being particularly preferred.
  • the sodium disilicate (Na 6 Si 2 O 7 ), which belongs to the group of sorosilicates and is characterized by an excellent absorption capacity of surfactants.
  • Surfactants are the interfacial tension reducing substances because they have a hydrophilic and a hydrophobic part.
  • the use of surfactants in the detergent tablet according to the invention is on the one hand indispensable because they are responsible for the main wash action.
  • the surfactants cause the formation of interfaces on the individual surfaces of the grains, in which they are to be included and thus prevent a sintering effect during the pressing of tablets.
  • the surfactants have a fundamentally negative influence on the tablet hardness.
  • Nonionic low-foaming surfactants are used for the tablet according to the invention.
  • Very particularly preferred surfactants are ethylene oxide-propylene oxide (EO-PO) - adducts, such as surfactants under the trade name Plurafac ®.
  • the surfactant or the surfactants are incorporated or incorporated into the carrier material by means of a fluidizing mixer, for example a fluid bed mixer or an eddy current granulator.
  • a fluidizing mixer for example a fluid bed mixer or an eddy current granulator.
  • the level of surfactant should be at least 2.5% by weight, based on the total weight of the tablet.
  • inventive detergent or cleaning agent tablet is characterized by a Cover material off.
  • This coating material is applied to or around the powder grains consisting of carrier material / surfactant, thus causing a substantially complete, sealing of the powder grains and thus prevents the lowering of the tablet hardness by the surfactant or the surfactants.
  • the coating material (coating) must not displace the surfactant in the carrier material. It is quite desirable if the coating material (coating) has properties that are beneficial for the cleaning effect of the resulting tablet.
  • coating materials which are "co-builders” are used according to the invention.
  • the so-called “builders” themselves are builders that play a central role in the washing process. They not only contribute to the washing process themselves through specific effects, but also decisively influence the effect of other detergent components, for example the surfactants or bleaching agents. They do this, for example, by their possible binding capacity of polyvalent ions, or as ion transport agents or in textile washes by adsorption of molecularly disperse substances or heterocoagulation with pigments to prevent textile graying.
  • the coating materials used are water glass, soda or homopolymers and copolymers of polycarboxylic acids, in particular acrylic acid-maleic acid copolymers or a mixture thereof, these having the function of a co-builder.
  • the acrylic acid-maleic acid copolymer is a co-formable coating material.
  • the detergent tablet according to the invention contains 15-30% of the porous carrier material.
  • the content of surfactants is preferably between 2.5 to 5.0%.
  • the proportion of the coating material is preferably between 1-6%.
  • the surfactant content should have a value of at least 2.5% by weight, based on the total weight.
  • the inventive detergent or cleaning agent tablet may also contain other components, such as a silver or copper corrosion inhibitors, enzymes, perfume compounds, bleaching agents, stabilizers, activators, brighteners, foam inhibitors, corrosion inhibitors, dyes, adjusters and other auxiliary and fillers.
  • a silver or copper corrosion inhibitors such as a silver or copper corrosion inhibitors, enzymes, perfume compounds, bleaching agents, stabilizers, activators, brighteners, foam inhibitors, corrosion inhibitors, dyes, adjusters and other auxiliary and fillers.
  • a further aspect of the present invention is a process for making a detergent tablet.
  • incorporation of the surfactant (s) into the porous support material is carried out by spraying the surfactant or surfactants into the support material with or in a stream of air and at a temperature of about 15 to 45 ° C.
  • the incorporation of the surfactant or of the surfactants into the porous carrier material is preferably carried out by means of a fluidizing mixer, in particular by fluidized bed granulation or a fluidized bed mixer.
  • the resulting fully soaked powder is further mixed for between 20 and 50 minutes at a temperature of between 15 and 35 ° C, preferably about 30 ° C, so as to complete Diffusion of the surfactant or surfactants in the carrier material to effect.
  • the coating is applied by means of fluidized bed granulation on the powder grains.
  • the process is preferably carried out so that the coated powder grains are continuously dried at temperatures of between about 40-60 ° C, especially about 50-60 ° C.
  • this is preferably dried to a residual moisture content of ⁇ 5% by weight.
  • the sprayed granules are further vortexed for 30 minutes at 30 ° C, so as to give the surfactant mixture sufficient time to penetrate into the powder grains or to diffuse.
  • the coating is applied to the powder grains.
  • 70 kg of a 20% strength solution of an acrylic acid-maleic acid copolymer are sprayed in the eddy current granulator and dried continuously at a temperature of about 55 ° C during about 50 minutes. It is formed in this process, small coated powder grains having a mean grain size of about 0.5 mm. The resulting powder is essentially dust-free.
  • the product is dried at 50 ° C to a residual moisture of ⁇ 5% and discharged.
  • the powder is mixed by means of a mixer with other ingredients (trisodium citrate, sodium perborate, TAED, enzymes, soda) and the powder is poured into a press, where it is pressed into a tablet.
  • other ingredients trisodium citrate, sodium perborate, TAED, enzymes, soda
  • a two-phase detergent tablet two different powder granules are prepared in a first step.
  • a first component or powder mixture is prepared according to Example 1.
  • the second component or powder mixture corresponds with respect to the proportions of the first component, except that no benzotriazole is present, but 0.2 kg of a blue dye.
  • the finished and dried powder mixtures are ready mixed in a mixer and then the powder of the first layer is filled by means of a dosing aid, such as a Paddeldosierer, in the down-pulled lower punch.
  • a dosing aid such as a Paddeldosierer
  • the powder With the upper punch, the powder is then slightly compressed, so that there is still enough rough surface to sinter with the second component or powder mixture.
  • the lower punch moves back into the filling position, the second phase is filled and then pressed with high force.
  • the lower stamp is raised so that the scraper, the tablet can be guided by the turntable.

Abstract

A tablet containing washing or cleaning agent is prepared by compressing powder grains consisting of (i) a porous carrier (I); (ii) at least one surfactant, incorporated into (I); and (iii) a coating (III) that practically completely covers the grains. Independent claims are also included for the following: (a) a method for producing these tablets; and (b) tablets produced this way.

Description

Die vorliegende Erfindung betrifft eine phosphatfreie Reinigungsmitteltablette gemäss dem unabhängigen Anspruch 1, sowie ein Verfahren zu deren Herstellung gemäss dem unabhängigen Anspruch 9.The present invention relates to a phosphate-free detergent tablet according to independent claim 1, and to a process for its preparation according to independent claim 9.

Waschmittel bzw. Reinigungsmittel in Tablettenform erfreuen sich einer steigenden Beliebtheit, weil sie es erlauben die erforderliche Waschmittel- bzw. Reinigungsmittelmenge, im Vergleich zur Zugabe von entsprechend pulverförmigen Mitteln, in einer definierteren Einheitsmenge zu dosieren. Ausserdem ist die Verwendung einer definierten Einheitsmenge an Waschmittel- bzw. Reinigungsmittel auch handlicher und sicherer, da ein Verschütten der vielfach aggressiven Substanzen vermieden wird.Detergents or cleaning agents in tablet form are enjoying increasing popularity, because they allow the required amount of detergent or detergent, in comparison to the addition of corresponding powdered agents to dose in a more defined unit quantity. In addition, the use of a defined unit quantity of detergent or cleaning agent is also more convenient and safer, since spillage of the often aggressive substances is avoided.

Insbesondere bei Geschirrspülmitteln haben sich in den letzten Jahren eine Reihe von phosphatfreien Reinigungsmitteltabletten auf dem Markt etabliert, wobei sich ganz besonders diejenigen der sogenannten zweiten Generation besonders durchzusetzen scheinen. Diese werden nicht mehr in den Besteckkorb gelegt, sondern im Dosierfach deponiert und dort bei der Hauptwäsche freigesetzt. Das Dosierfach in modernen Spülmaschinen ist daher rechteckig (26 x 36 mm) ausgelegt, so dass eine Tablette bequem eingelegt werden kann.Particularly in the case of dishwashing detergents, a number of phosphate-free detergent tablets have become established on the market in recent years, with those of the so-called second generation in particular appear to be particularly successful. These are no longer placed in the cutlery basket, but deposited in the dispenser and released there in the main wash. The dispenser in modern dishwashers is therefore rectangular (26 x 36 mm) designed so that a tablet can be easily inserted.

In der internationalen Anmeldung WO 97/03177 wird beispielsweise ein Geschirrspülmittel in Form einer Mehrschichttablette beschrieben, welche ein Bleichmittel, einen Bleichaktivator, ein Silber/Kupferkorrosionsschutzmittel sowie andere übliche Bestandteile enthält. Dabei ist das Silber/Kupferkorrosionsschutzmittel nicht gemeinsam in einer Schicht zusammen mit dem Bleichmittel und dem Bleichaktivator enthalten.In the international application WO 97/03177, for example, a dishwashing detergent in the form of a multilayer tablet is described, which contains a bleaching agent, a bleach activator, a silver / copper corrosion inhibitor and other conventional ingredients. In this case, the silver / copper corrosion inhibitor is not contained together in a layer together with the bleaching agent and the bleach activator.

Die gegenwärtig auf dem Markt vertriebenen Tabletten sind in bezug auf ihre Dosierungshandlichkeit, insoweit die Tabletten tatsächlich formbeständig sind, durchaus befriedigend, aber sie sind eben auf der anderen Seite so brüchig und hygroskopisch, dass eine vollständige Einzelverpackung für jede Tablette unerlässlich ist. Verzichtet man auf eine Einzelverpackung tendieren die ungeschützten Tabletten durch Stösse untereinander langsam in die Brüche zu gehen, so dass letztendlich nur noch Bruchstücke in einem Pulversatz übrig bleiben.The currently marketed tablets are quite satisfactory in terms of their dosage handling, as far as the tablets are actually dimensionally stable, but on the other hand they are so brittle and hygroscopic that a complete single package is indispensable for each tablet. If one dispenses with individual packaging, the unprotected tablets tend to break slowly as a result of collisions with each other, so that ultimately only fragments remain in a powder set.

Verantwortlich für die Brüchigkeit ist im wesentlichen das Tensid bzw. die Tenside, welche die Tablettenhärte verringern und damit beim Pressen den Sintereffekt verhindern. Diese Brüchigkeit und Instabilität wird ausserdem noch durch die Hygroskopie der in den Tabletten enthaltenden Stoffen verstärkt : Die Hygroskopie bewirkt, dass mit der Zeit mehr oder weniger Luftfeuchtigkeit von der Tablette aufgenommen wird, die Tablette dadurch erheblich an Volumen gewinnt und so die Tablettenhärte weiter herabsetzt.Responsible for the brittleness is essentially the surfactant or surfactants, which reduce the tablet hardness and thus prevent the sintering effect during pressing. This brittleness and instability is further enhanced by the hygroscopicity of the substances contained in the tablets: hygroscopy causes more or less humidity to be absorbed by the tablet over time, significantly increasing the tablet's volume and further reducing tablet hardness.

Infolgedessen werden die gegenwärtig vertriebenen Waschmittel- bzw. Reinigungsmittel-Tabletten in individueller Verpackung angeboten und müssen zu deren Verwendung vom Benutzer bzw. Verwender zuerst wieder ausgepackt werden, bevor sie in das Dosierfach gelegt werden können. Folglich sind die gegenwärtig vertriebenen Waschmittel- bzw. Reinigungsmittel-Tabletten infolge ihrer Brüchigkeit und Hygroskopie und somit in bezug auf ihre Gesamthandlichkeit letztendlich nicht befriedigend.As a result, the currently sold detergent tablets are offered in individualized packaging and must first be unpacked for their use by the user or user before they can be placed in the dispenser. Consequently, the currently marketed detergent tablets are ultimately unsatisfactory due to their brittleness and hygroscopicity, and thus their overall suppleness.

Für Waschmitteltabletten wurde dieses Problem bereits angegangen (siehe EP 0 466 484 und EP 0 711 828); die dort offenbarten Lösungen sind aber für Geschirrspülmittel nicht geeignet.For detergent tablets, this problem has already been addressed (see EP 0 466 484 and EP 0 711 828); but the solutions disclosed there are not suitable for dishwashing detergents.

Die Aufgabe der vorliegenden Erfindung bestand darin ein phosphatfreies Reinigungsmittel für Geschirrspülmaschinen in einphasiger oder mehrphasiger Tablettenform bereitzustellen, wobei die Tablette ein Tensid oder mehrere Tenside enthält und die so kompakt bzw. fest ist, dass sie nicht verpackt werden muss, um zu verhindern, dass sie mit der Zeit in die Brüche geht.The object of the present invention was to provide a phosphate-free detergent for dishwashers in single-phase or multi-phase tablet form, which tablet contains one or more surfactants and which is so compact that it does not need to be packaged to prevent it with the time in the breaks goes.

Es war ausserdem ein Ziel der vorliegenden Erfindung ein Verfahren zur Herstellung von kompakten und stabilen Reinigungsmittel-Tabletten für Geschirrspülmaschinen bereitzustellen, welche nicht einzeln verpackt werden müssen, um zu verhindern, dass sie mit der Zeit in die Brüche geht.It has also been an object of the present invention to provide a method for making compact and stable detergent tablets for dishwashers which need not be individually packaged to prevent them from failing over time.

Die oben genannten Ziele werden gemäss den unabhängigen Ansprüchen gelöst.The above objects are achieved according to the independent claims.

Die erfindungsgemässe Reinigungsmittel-Tablette für Geschirrspülmaschinen wird aus Pulverkörnern durch Zusammenpressen erhalten, wobei die Pulverkörner der Reinigungsmittel-Tablette

  • a) ein poröses Trägermaterial,
  • b) ein oder mehrere im Trägermaterial eingearbeitete Tenside, und
  • c) ein Überzugsmaterial zum, im wesentlichen vollständigen, Versiegeln der Pulverkörner.
umfasst.The inventive detergent tablet for dishwashers is obtained from powder grains by compression, wherein the powder grains of the detergent tablet
  • a) a porous carrier material,
  • b) one or more incorporated in the carrier material surfactants, and
  • c) a coating material for, substantially complete, sealing the powder grains.
includes.

Unter Reinigungsmittel-Tablette ist generell eine Tablette für Reinigungszwecke in maschinell durchgeführten Reinigungsvorgängen in Geschirrspülmaschinen zu vestehen.Detergent tablet is generally to be understood as a tablet for cleaning purposes in machine-washing processes in dishwashers.

Das poröse Trägermaterial sollte dabei so beschaffen sein, dass es ohne weiteres in der Lage ist das Tensid bzw. die Tenside aufzunehmen. Bevorzugte poröse Trägermaterialien sind Disilikate, Sulfate, Zeolithe oder Mischungen derselben. Diese liegen als Salze vor, wobei deren Alkalimetallsalze, z.B. die Natrium oder Kaliumsalze besonders bevorzugt sind.The porous support material should be such that it is readily able to take up the surfactant or the surfactants. Preferred porous support materials are disilicates, sulfates, zeolites or Mixtures thereof. These are present as salts, with their alkali metal salts, for example the sodium or potassium salts being particularly preferred.

Ganz besonders bevorzugt ist das Natriumdisilikat (Na6Si2O7), welches zu der Gruppe der Sorosilikate gehört und sich durch eine hervorragende Aufnahmefähigkeit von Tensiden auszeichnet.Most preferably, the sodium disilicate (Na 6 Si 2 O 7 ), which belongs to the group of sorosilicates and is characterized by an excellent absorption capacity of surfactants.

Tenside sind die Grenzflächenspannung herabsetzende Substanzen, weil sie einen hydrophilen und einen hydrophoben Anteil aufweisen. Die Verwendung von Tensiden in der erfindungsgemässen Reinigungsmittel-Tablette ist einerseits unabdingbar, weil diese für die Hauptwaschwirkung verantwortlich sind. Andererseits bewirken die Tenside die Bildung von Trennflächen auf den einzelnen Flächen der Körner, in welche diese aufgenommen werden sollen und verhindern damit einen Sintereffekt beim Pressen von Tabletten. Damit haben die Tenside grundsätzlich einen ausgesprochen negativen Einfluss auf die Tablettenhärte.Surfactants are the interfacial tension reducing substances because they have a hydrophilic and a hydrophobic part. The use of surfactants in the detergent tablet according to the invention is on the one hand indispensable because they are responsible for the main wash action. On the other hand, the surfactants cause the formation of interfaces on the individual surfaces of the grains, in which they are to be included and thus prevent a sintering effect during the pressing of tablets. Thus, the surfactants have a fundamentally negative influence on the tablet hardness.

Für die erfindungsgemässe Tablette werden nicht-ionogene, schaumarme Tenside verwendet. Ganz besonders bevorzugte Tenside sind Ethylenoxid-Propylenoxid (EO-PO)- Addukte, wie beispielsweise die Tenside mit der Handelsbezeichnung Plurafac®.Nonionic low-foaming surfactants are used for the tablet according to the invention. Very particularly preferred surfactants are ethylene oxide-propylene oxide (EO-PO) - adducts, such as surfactants under the trade name Plurafac ®.

In einer bevorzugten Ausführungsform werden das Tensid bzw. die Tenside mittels eines fluidisierenden Mischers, beispielsweise einem Fliessbettmischer oder einem Wirbelstromgranulator, in das Trägermaterial eingearbeitet, bzw. aufgenommen. Dabei sollte zur Sicherstellung einer optimalen "Performance" (d.h. Leistungsfähigkeit) der Waschmittel- bzw. Reinigungsmittel-Tablette der Tensidanteil einen Wert von mindestens 2,5 Gew.-% bezogen auf das Gesamtgewicht der Tablette aufweisen.In a preferred embodiment, the surfactant or the surfactants are incorporated or incorporated into the carrier material by means of a fluidizing mixer, for example a fluid bed mixer or an eddy current granulator. In doing so, to ensure optimum "performance" (i.e., performance) of the detergent tablet, the level of surfactant should be at least 2.5% by weight, based on the total weight of the tablet.

Ausserdem zeichnet sich die erfindungsgemässe Waschmittel- bzw. Reinigungsmittel-Tablette durch ein Überzugsmaterial aus. Dieses Überzugsmaterial wird auf bzw. um die Pulverkörner bestehend aus Trägermaterial/Tensid aufgebracht, bewirkt so eine, im wesentlichen vollständige, Versiegelung der Pulverkörner und verhindert somit die Herabsetzung der Tablettenhärte durch das Tensid bzw. die Tenside.In addition, the inventive detergent or cleaning agent tablet is characterized by a Cover material off. This coating material is applied to or around the powder grains consisting of carrier material / surfactant, thus causing a substantially complete, sealing of the powder grains and thus prevents the lowering of the tablet hardness by the surfactant or the surfactants.

Das Überzugsmaterial (coating) darf dabei nicht das Tensid im Trägermaterial verdrängen. Es ist dabei durchaus erwünscht, wenn das Überzugsmaterial (coating) über Eigenschaften verfügt, welche für die Reinigungswirkung der resultierende Tablette zuträglich sind.The coating material (coating) must not displace the surfactant in the carrier material. It is quite desirable if the coating material (coating) has properties that are beneficial for the cleaning effect of the resulting tablet.

Erfindungsgemäss verwendet werden daher Überzugsmaterialen, welche "Co-Builder" sind. Die sogenannten "Builder" selbst sind Gerüststoffe, welche beim Waschprozess eine zentrale Rolle übernehmen. Sie tragen nicht nur durch spezifische Effekte selbst zum Waschgeschehen bei, sondern beeinflussen auch in entscheidender Weise die Wirkung anderer Waschmittelkomponenten, beispielsweise der Tenside oder Bleichmittel. Sie tun dies beispielsweise durch ihr allfälliges Bindevermögen von mehrwertigen Ionen, oder als Ionentransportmittel oder bei Textilwaschvorgängen durch Adsorption von molekulardispersen Substanzen bzw. Heterokoagulation mit Pigmenten zur Verhinderung von Textilvergrauung.Therefore, coating materials which are "co-builders" are used according to the invention. The so-called "builders" themselves are builders that play a central role in the washing process. They not only contribute to the washing process themselves through specific effects, but also decisively influence the effect of other detergent components, for example the surfactants or bleaching agents. They do this, for example, by their possible binding capacity of polyvalent ions, or as ion transport agents or in textile washes by adsorption of molecularly disperse substances or heterocoagulation with pigments to prevent textile graying.

Als Überzugsmaterialien werden Wasserglas, Soda oder Homo- und Copolymere von Polycarbonsäuren, insbesondere Acrylsäure-Maleinsäure-Copolymere oder eine Mischung derselben verwendet, wobei diese die Funktion eines Co-Builders ausüben. Ganz besonders bevorzugt ist das Acrylsäure-Maleinsäure-Copolymer als Co-Büilderfähiges Überzugsmaterial.The coating materials used are water glass, soda or homopolymers and copolymers of polycarboxylic acids, in particular acrylic acid-maleic acid copolymers or a mixture thereof, these having the function of a co-builder. Most preferably, the acrylic acid-maleic acid copolymer is a co-formable coating material.

In der erfindungsgemässen Reinigungsmittel-Tablette sind 15-30 % des porösen Trägermaterials enthalten.The detergent tablet according to the invention contains 15-30% of the porous carrier material.

Der Gehalt an Tensiden liegt bevorzugt bei zwischen 2,5 bis 5,0 %.The content of surfactants is preferably between 2.5 to 5.0%.

Der Anteil des Überzugsmaterials liegt vorzugsweise zwischen 1-6 %.The proportion of the coating material is preferably between 1-6%.

Wie bereits oben erwähnt, sollte zur Sicherstellung einer optimalen "Performance" (Leistungsfähigkeit) der Waschmittel- bzw. Reinigungsmittel-Tablette der Tensidanteil einen Wert von mindestens 2,5 Gew.-% bezogen auf das Gesamtgewicht aufweisen.As already mentioned above, in order to ensure optimum "performance" of the detergent or cleaning agent tablet, the surfactant content should have a value of at least 2.5% by weight, based on the total weight.

Die erfindungsgemässe Waschmittel- bzw. Reinigungsmittel-Tablette kann ausserdem noch weitere Komponenten enthalten, wie beispielsweise einen Silber bzw. Kupfer-Korrosionsschutz, Enzyme, Parfumverbindungen, Bleichmittel, Stabilisatoren, Aktivatoren, Aufheller, Schauminhibitoren, Korrosionsinhibitoren, Farbstoffe, Stellmittel und weitere Hilfs- und Füllstoffe.The inventive detergent or cleaning agent tablet may also contain other components, such as a silver or copper corrosion inhibitors, enzymes, perfume compounds, bleaching agents, stabilizers, activators, brighteners, foam inhibitors, corrosion inhibitors, dyes, adjusters and other auxiliary and fillers.

Ein weiter Aspekt der vorliegenden Erfindung besteht in einem Verfahren zur Herstellung einer Reinigungsmittel-Tablette.A further aspect of the present invention is a process for making a detergent tablet.

Das erfindungsgemässe Verfahren umfasst dabei die folgenden Schritte:

  • a) Ein nicht-ionogenes, schaumarmes Tensid oder mehrere nicht-ionogene, schaumarme Tenside werden in ein poröses Trägermaterial eingearbeitet bzw. von diesem aufgenommen.
  • b) Die so enstandenen Tensid-Trägermaterial-Pulverkörner werden mit einem Überzug versehen, so dass eine im wesentlichen vollständige Versiegelung der Pulverkörner erreicht wird.
  • c) Schliesslich werden die im Schritt b) erhaltenen Pulverkörner gegebenfalls mit anderen Inhaltsstoffen gemischt und zu einer Tablette gepresst.
The method according to the invention comprises the following steps:
  • a) A non-ionic, low-foaming surfactant or more non-ionic, low-foaming surfactants are incorporated or absorbed in a porous support material.
  • b) The thus-formed surfactant-carrier powder grains are coated so that substantially complete sealing of the powder grains is achieved.
  • c) Finally, the powder grains obtained in step b) are optionally mixed with other ingredients and pressed into a tablet.

In einer bevorzugten Ausführungsform wird das Einarbeiten des Tensids bzw. der Tenside in das poröse Trägermaterial durch Einsprühen des Tensids bzw. der Tenside in das Trägermaterial mit bzw. in einem Luftstrom und bei einer Temperatur von etwa 15 bis 45°C durchgeführt. Vorzugsweise wird das Einarbeiten des Tensids bzw. der Tenside in das poröse Trägermaterial mittels eines fluidisierenden Mischers, insbesondere mittels Wirbelschichtgranulation oder einem Fliessbettmischer, durchgeführt.In a preferred embodiment, incorporation of the surfactant (s) into the porous support material is carried out by spraying the surfactant or surfactants into the support material with or in a stream of air and at a temperature of about 15 to 45 ° C. The incorporation of the surfactant or of the surfactants into the porous carrier material is preferably carried out by means of a fluidizing mixer, in particular by fluidized bed granulation or a fluidized bed mixer.

Nach dem Einsprühen des Tensids bzw. der Tenside auf das Trägermaterial wird das entstandene vollgesogene Pulver in einer anderen bevorzugten Ausführungsform während zwischen 20 und 50 Minuten bei einer Temperatur von zwischen 15 und 35°C, vorzugsweise etwa 30°C weitergemischt, um so eine vollständige Diffusion des Tensids bzw. der Tenside in das Trägermaterial zu bewirken. Vorzugsweise wird der Überzug mittels Wirbelschichtgranulation auf die Pulverkörner appliziert.After spraying the surfactant (s) onto the support material, in another preferred embodiment, the resulting fully soaked powder is further mixed for between 20 and 50 minutes at a temperature of between 15 and 35 ° C, preferably about 30 ° C, so as to complete Diffusion of the surfactant or surfactants in the carrier material to effect. Preferably, the coating is applied by means of fluidized bed granulation on the powder grains.

Ausserdem ist es in der Regel erwünscht, dass in den Rohmaterialien vorhandene und im Verfahren freigesetzte Feuchtigkeit entfernt wird. Daher wird das Verfahren bevorzugt so durchgeführt, dass die beschichteten Pulverkörner fortlaufend bei Temperaturen von zwischen etwa 40-60°C, insbesondere etwa 50-60°C, getrocknet werden.Moreover, it is usually desirable that moisture present in the raw materials and released in the process be removed. Therefore, the process is preferably carried out so that the coated powder grains are continuously dried at temperatures of between about 40-60 ° C, especially about 50-60 ° C.

Wenn schlussendlich das erhaltene Granulat mit dem fertigen Überzug erhalten wird, wird dieses vorzugsweise auf einen Restfeuchtigkeitsgehalt von <5 Gew.-% getrocknet.When finally the obtained granules are obtained with the finished coating, this is preferably dried to a residual moisture content of <5% by weight.

Ein letzter Aspekt der vorliegenden Erfindung besteht in einer Reinigungsmittel-Tablette, welche nach dem oben beschriebenen Verfahren erhältlich ist, d.h. welches durch die folgenden Verfahrensschritte erhältlich ist :

  • a) Ein nicht-ionogenes, schaumarmes Tensid oder mehrere nicht-ionogene, schaumarme Tenside werden vorzugsweise mittels eines fluidisierenden Mischers in ein poröses Trägermaterial eingearbeitet bzw. von diesem aufgenommen.
  • b) Die so enstandenen Tensid-Trägermaterial-Pulverkörner werden mit einem Überzug versehen, so dass eine im wesentlichen vollständige Versiegelung der Pulverkörner erreicht wird.
  • c) Schliesslich werden die im Schritt b) erhaltenen Pulverkörner gegebenenfalls mit anderen Inhaltsstoffen gemischt und zu einer Tablette gepresst.
A final aspect of the present invention is a detergent tablet obtainable by the method described above, ie which is obtainable by the following process steps:
  • a) Be a non-ionic, low-foaming surfactant or several non-ionic, low-foaming surfactants Preferably incorporated by means of a fluidizing mixer in a porous carrier material or received by this.
  • b) The thus-formed surfactant-carrier powder grains are coated so that substantially complete sealing of the powder grains is achieved.
  • c) Finally, the powder grains obtained in step b) are optionally mixed with other ingredients and pressed into a tablet.

Im folgenden soll nun die vorliegende Erfindung anhand von zwei Beispielen verdeutlicht werden, wobei die Beispiele nicht als beschränkend auf den Schutzbereich anzusehen sind.In the following, the present invention will now be illustrated with reference to two examples, the examples are not to be regarded as limiting the scope.

Beipiel 1Example 1 Herstellung einer Einphasen-SpülmitteltablettePreparation of a single phase detergent tablet

200 kg Natriumdisilikat und 2,5 kg Benzotriazol als Silberschutz sowie 20 kg Natriumsulfat werden vorgelegt und fluidisierend gemischt. Ausserdem wird das Gemisch für die Tensidaufnahme auf 30°C Produkttemperatur vorgewärmt. Danach wird das Pulver mit 24 kg der zuvor gemischten Tensid/Parfüm-Lösung während etwa 20 Minuten besprüht.200 kg of sodium disilicate and 2.5 kg of benzotriazole as silver protection and 20 kg of sodium sulfate are initially charged and mixed in a fluidizing manner. In addition, the mixture for the surfactant absorption is preheated to 30 ° C product temperature. Thereafter, the powder is sprayed with 24 kg of the previously mixed surfactant / perfume solution for about 20 minutes.

Anschliessend wird das besprühte Granulat noch während 30 Minuten bei 30°C weitergewirbelt, um so der Tensidmischung genügend Zeit zu geben ins Innere der Pulverkörner einzudringen bzw. zu diffundieren.Subsequently, the sprayed granules are further vortexed for 30 minutes at 30 ° C, so as to give the surfactant mixture sufficient time to penetrate into the powder grains or to diffuse.

Nach der vollständigen Diffusion der Tensidmischung in die porösen Pulverpartikel, wird der Überzug auf die Pulverkörner appliziert. Dabei werden während etwa 50 Minuten 70 kg einer 20%-igen Lösung eines Acrylsäure-Maleinsäure-Copolymers im Wirbelstromgranulator besprüht und dabei fortlaufend bei einer Temperatur von etwa 55°C getrocknet. Es bilden sich bei diesem Vorgang kleine beschichtete Pulverkörner, welche eine mittlere Korngrösse von etwa 0,5 mm aufweisen. Das resultierende Pulver ist im wesentlichen staubfrei.After complete diffusion of the surfactant mixture into the porous powder particles, the coating is applied to the powder grains. 70 kg of a 20% strength solution of an acrylic acid-maleic acid copolymer are sprayed in the eddy current granulator and dried continuously at a temperature of about 55 ° C during about 50 minutes. It is formed in this process, small coated powder grains having a mean grain size of about 0.5 mm. The resulting powder is essentially dust-free.

Schliesslich wird das Produkt bei 50°C auf eine Restfeuchtigkeit von <5% getrocknet und ausgetragen.Finally, the product is dried at 50 ° C to a residual moisture of <5% and discharged.

Im nächsten Schritt wird das Pulver mittels eines Mischers mit weiteren Inhaltsstoffen gemischt (Trinatriumcitrat, Natriumperborat, TAED, Enzyme, Soda) und das Pulver in eine Presse eingefüllt, wo es zu einer Tablette gepresst wird.In the next step, the powder is mixed by means of a mixer with other ingredients (trisodium citrate, sodium perborate, TAED, enzymes, soda) and the powder is poured into a press, where it is pressed into a tablet.

Beipiel 2Example 2 Herstellung einer Zweiphasen-SpülmitteltablettePreparation of a two-phase detergent tablet

Für die Herstellung einer Zweiphasen-Spülmitteltablette werden in einem ersten Schritt zwei verschiedene Pulvergranulate zubereitet. Dabei wird eine erste Komponente bzw. Pulvermischung gemäss dem Beispiel 1 hergestellt. Die zweite Komponente bzw. Pulvermischung entspricht in bezug auf die Mengenverhältnisse der ersten Komponente, mit Ausnahme, dass kein Benzotriazol vorhanden ist, dafür aber 0,2 kg eines blauen Farbstoffs.For the preparation of a two-phase detergent tablet, two different powder granules are prepared in a first step. In this case, a first component or powder mixture is prepared according to Example 1. The second component or powder mixture corresponds with respect to the proportions of the first component, except that no benzotriazole is present, but 0.2 kg of a blue dye.

Die fertig erhaltenen und getrockneten Pulver-Mischungen werden in einem Mischer fertig gemischt und anschliessend wird das Pulver der ersten Schicht mittels einer Dosierhilfe, z.B. einem Paddeldosierer, in den nach unten gezogenen Unterstempel gefüllt. Mit dem Oberstempel wird das Pulver dann leicht komprimiert, so dass noch genügend rauhe Oberfläche vorhanden ist, um mit der zweiten Komponente bzw. Pulvermischung zu versintern. Danach fährt der Unterstempel wieder in die Füllposition, die zweite Phase wird gefüllt und anschliessend mit hoher Kraft verpresst. Der Unterstempel wird hochgefahren, damit beim Abstreifer die Tablette vom Drehteller geführt werden kann.The finished and dried powder mixtures are ready mixed in a mixer and then the powder of the first layer is filled by means of a dosing aid, such as a Paddeldosierer, in the down-pulled lower punch. With the upper punch, the powder is then slightly compressed, so that there is still enough rough surface to sinter with the second component or powder mixture. Thereafter, the lower punch moves back into the filling position, the second phase is filled and then pressed with high force. The lower stamp is raised so that the scraper, the tablet can be guided by the turntable.

Beispiel 3Example 3 Typische Zusammensetzung einer ReinigungstabletteTypical composition of a cleaning tablet

vorgefertigtes Granulat, wie in Beispiel 1 und 2 beschriebenprefabricated granules as described in Example 1 and 2 15-40%15-40% Trinatriumcitrattrisodium citrate 30-50%30-50% Natriumperboratsodium 5-15%5-15% Acrylsäure-MaleinsäureAcrylic acid-maleic CopolymersisatCopolymersisat 1-5%1-5% TAEDTAED 2-7%2-7% Enzymeenzymes 1-3%1-3% Sodasoda 2-7%2-7%

Claims (15)

  1. A cleaning agent tablet for dishwashers compressed from powder grains that contains one or more surfactants, characterised in that the powder grains comprise
    a) a porous carrier material,
    b) the one or more surfactants, incorporated into the carrier material, and
    c) a coating material for, essentially completely, sealing the powder grains,
    wherein the surfactants are non-ionogenic, low-foaming surfactants, the portion of surfactant in the tablet amounts to at least 2.5 % by weight referred to the total weight of the tablet, the coating material is a co-builder selected from the group consisting of water glass, soda (sodium carbonate) or a homo- or copolymer of a polycarboxylic acid, or a mixture thereof, and wherein the tablet contains 15 to 30 % by weight of the porous carrier material.
  2. Cleaning agent tablet according to claim 1, characterised in that the porous carrier material contains or consists of disilicates, sulfates, zeolites or mixtures thereof, in particular their alkaline metal salts.
  3. Cleaning agent tablet according to claim 2, characterised in that the porous carrier material contains or consists of sodium disilicate.
  4. Cleaning agent tablet according to anyone of claims 1 to 3, characterised in that the non-ionogenic, low-foaming surfactants contain or consist of surfactants on the basis of ethyleneoxide-propyleneoxide adducts.
  5. Cleaning agent tablet according to anyone of claims 1 to 4, characterised in that the copolymer of a polycarboxylic acid is an acrylic acid-maleic acid copolymer.
  6. Cleaning agent tablet according to anyone of claims 1 to 5, characterised in that the tablet contains 2.5 to 5 % by weight of one or more surfactants.
  7. Cleaning agent tablet according to anyone of claims 1 to 6, characterised in that the tablet contains 1-6 % by weight of the coating material.
  8. Cleaning agent tablet according to anyone of claims 1 to 7, characterised in that the tablet further contains a silver corrosion protecting agent or a copper corrosion protecting agent, respectively, enzymes, fragrances, bleaching agents, stabilizers, activators, brighteners, foam inhibitors, corrosion inhibitors, dyestuffs, suspending agents and/or further additives and fillers.
  9. Method for the production of a cleaning agent tablet according to anyone of claims 1 to 8, characterised in that
    a) one or more non-ionogenic, low-foaming surfactants are incorporated into a porous carrier material,
    b) the such generated surfactant-carrier material-powder grains are provided with a coating such that an essentially complete sealing of the powder grains is acchieved, and
    c) the such generated powder grains are compressed into a tablet.
  10. Method according to claim 9, characterised in that the incorporating of the surfactant(s) into the porous carrier material is made with a fluidising mixer, in particular by fluidised bed granulation or with a fluidised bed mixer.
  11. Method according to claim 9 or 10, characterised in that the incorporation of the surfactant(s) into the porous carrier material takes place by spraying the surfactant(s) into the carrier material in a stream of air and at a temperature of about 15 to 45°C.
  12. Method according to claim 11, characterised in that after the spraying of the surfactant(s) into the carrier material the generated adduct is further swirled for between about 20 and 50 minutes at a temperature of between 15 and 35°C, preferably about 30°C.
  13. Method according to anyone of claims 9 to 12, characterised in that the coating is applied to the powder grains by means of a fluidised bed granulation.
  14. Method according to claim 13, characterised in that the coated powder grains are continuously dried at temperatures of between about 50 - 60°C.
  15. Method according to anyone of claims 9 to 14, characterised in that the obtained granules are dried to a residual humidity content of <5 % by weight.
EP97811000A 1997-12-18 1997-12-18 Compact phosphate-free cleaning tablets Expired - Lifetime EP0933421B1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE59712770T DE59712770D1 (en) 1997-12-18 1997-12-18 Compact, phosphate-free detergent tablet
EP97811000A EP0933421B1 (en) 1997-12-18 1997-12-18 Compact phosphate-free cleaning tablets
AT97811000T ATE346133T1 (en) 1997-12-18 1997-12-18 COMPACT, PHOSPHATE-FREE CLEANING TABLET

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP97811000A EP0933421B1 (en) 1997-12-18 1997-12-18 Compact phosphate-free cleaning tablets

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EP0933421A1 EP0933421A1 (en) 1999-08-04
EP0933421B1 true EP0933421B1 (en) 2006-11-22

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Publication number Priority date Publication date Assignee Title
US6521581B1 (en) 2001-12-14 2003-02-18 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Water-soluble package with multiple distinctly colored layers of liquid laundry detergent
DE102004016497B4 (en) * 2004-04-03 2007-04-26 Henkel Kgaa Process for the production of granules and their use in detergents and / or cleaning agents

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9015503D0 (en) * 1990-07-13 1990-08-29 Unilever Plc Detergent composition
GB9422925D0 (en) * 1994-11-14 1995-01-04 Unilever Plc Detergent compositions
GB9526097D0 (en) * 1995-12-20 1996-02-21 Unilever Plc Process
DE19601841A1 (en) * 1996-01-19 1997-07-24 Henkel Kgaa Nonionic surfactant rich granulate containing oil absorption agent, useful for detergents
DE19606765A1 (en) * 1996-02-23 1997-08-28 Henkel Kgaa Process for the production of dishwasher tablets

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EP0933421A1 (en) 1999-08-04
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