EP1179042B1 - Method of producing a multi-layer tablet - Google Patents
Method of producing a multi-layer tablet Download PDFInfo
- Publication number
- EP1179042B1 EP1179042B1 EP00929538A EP00929538A EP1179042B1 EP 1179042 B1 EP1179042 B1 EP 1179042B1 EP 00929538 A EP00929538 A EP 00929538A EP 00929538 A EP00929538 A EP 00929538A EP 1179042 B1 EP1179042 B1 EP 1179042B1
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- EP
- European Patent Office
- Prior art keywords
- tablet
- layer
- hollow
- filled
- introducing
- 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.)
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B11/00—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
- B30B11/02—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space
- B30B11/08—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space co-operating with moulds carried by a turntable
- B30B11/085—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space co-operating with moulds carried by a turntable for multi-layer articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
- B30B15/06—Platens or press rams
- B30B15/065—Press rams
Definitions
- the invention relates to a method for producing a tablet. especially a detergent tablet, with at least a first and a second layer, and one after producible product.
- Two-layer tablets with different ones, are also increasingly to be found Distribution of ingredients in the two layers is present, on the one hand separate incompatible ingredients from each other until the tablet is used, on the other hand to realize different release profiles of ingredients.
- the problem with tablets with at least two layers is that the compound between the individual layers must be sufficiently stable to dissolve the layers prevent each other during storage and transportation of the multilayer tablets.
- the development and manufacture of stable multilayer tablets is therefore time and cost consuming and sensitive to the change of internal and external parameters in the process.
- the invention is therefore based on the object of developing the known method in that that the production of more stable multilayer tablets is made possible. at them to a much lesser extent a solution of the individual layers from one another occurs.
- the invention relates to a method for producing a tablet. especially a detergent tablet, with at least a first and a second layer comprising the following steps a) introducing a first measured amount of a first particulate Composition in a mold cavity of a tablet press; b) pressing the first measured quantity with a first pressing pressure by means of a press ram that is on its Pressing surface has at least one protrusion to produce a first pressed layer, in its upper surface one corresponding to the protrusion (s) on the press ram Has recess (s); c) introducing a second measured quantity of one second particulate composition onto the first pressed layer in the mold cavity the tablet press; and d) pressing the second measured quantity with a second Press pressure by means of the press ram to form a second pressed layer with a corresponding one To produce recess (es) in their upper surface, as well as product that can be produced thereafter.
- steps (c) and (d) are repeated in each case.
- the invention further relates to a multilayer Tablet, in particular a detergent tablet, that using the by the invention proposed method can be produced.
- one tablet with at least one first pressed Layer and a second arranged above pressed layer provided, thereby characterized in that the first layer in the area the second layer is attached, a recess having, the second layer one to the Depression has complementary protrusion, which in the recess engages, the top of the second layer is complementary to the protrusion Includes deepening.
- the lower layer 10 of the method Tablet 1 prepared in that a first measured amount of a first particulate Composition in a mold Given tablet press and there with a first Press pressure is pressed by means of a ram, which has a bulge on its pressing surface, which too thereby in the uppermost surface 11 of the lower Layer 10 of tablet 1 produced depression 12 is essentially complementary.
- a second is pressed onto the first pressed layer 10 measured amount of a second particulate Composition (which is usually from the first particulate composition is different) in given the shape of the tablet press and with a second pressure (usually higher than the first pressure is) by means of the press die second layer of tablet 20 pressed. Consequently, be the two tablet layers 10 and 20 not only against each other along the horizontal boundary layer pressed, but especially in the ...
- the molded body 30 has the embodiment shown a core 31 and an additional protective sheath 32. around him e.g. Protect during storage and release of ingredients during use to control the core 31.
- compositions of the tablet or shaped body can vary widely depending on the use Vary scope. Different possibilities in the preferred area of application are in the following examples.
- compositions of the tablets in Examples 1 to 7 represent dishwashing detergent compositions the depressions in the tablets of Examples 2 to 7 are filled with various shaped bodies in the top of the top layer.
- example 8 describes a detergent tablet and a detergent tablet.
- the following table relates to the composition of the two layers of a two-layer dishwasher tablet (weight ratio approx. 50:50), layer 1 being the first (lower) layer, which is only slightly compressed in step (b) (without actual compression), but this is sufficient to form a smooth surface with the corresponding recess in the top.
- the final tablet is pressed at a pressure of approximately 100 kN / cm 2 .
- Examples 2 to 7 also relate to two-layer dishwasher tablets, the composition on individual layers of the tablet compared to those of Example 1 are only slightly changed (if at all).
- the individual examples concrete examples of use of various moldings are described for illustration.
- the in the resulting in the process according to the invention in the Top of the top (second) layer can be used and can be fixed with glue, for example.
- the actual manufacturing process of the tablet, especially those described in Example 1 Press pressures remain unchanged.
- the protease contained therein becomes Released faster than that contained in the tablet and may already have its effect unfold directly at the beginning of the main wash cycle.
- fresh enzymes protease and amylase
- composition of the tablet essentially corresponds to that of Examples 1 and 2, with the difference that protease or amylase which is stable in hot water is used in layer 2 of the tablet.
- composition of the shaped body corresponds to that of the shaped body from Example 2.
- the Shaped body sets cold water-active protease and amylase at the beginning of the main wash cycle free. By dissolving the tablet during the warm-up process, it becomes bleach-stable enzymes stable in hot water are released into the rinsing solution.
- This embodiment enables a time-delayed dissolution of in solution with bleaching agents incompatible enzymes possible.
- the following table shows an exemplary formulation for a two-layer washing intensifier tablet.
- the weight of the first (lower) layer is approximately 74% of the total tablet. while the second (upper) layer makes up about 26%.
- the following table shows an exemplary formulation for a detergent tablet, in which case the two layers are in a weight ratio of 70 (lower (1st) layer) to 30 (upper (2nd) layer).
- the manufacturing process is as follows:
- a mixture of 1.05 g of amidosulfonic acid and 0.45 maleic acid is formed in a rotary press under a pressure of 890 kg / cm 2 to give a shaped body.
- 0.1975 g of fragrance is absorbed onto 0.0525 g of finely divided silica to give a free-flowing granular material.
- the resulting 0.25 g is mixed with 0.6 g of microcrystalline cellulose and 0.15 g of cross-linked polyvinylpyrrolidone.
- the mixture is tableted in a round press with an inner diameter of 10 mm under a pressure of 2900 kg / cm 2 to give an elliptical shaped body with a height of 13.1 mm and a weight of approx. 1 g.
- such Shaped bodies can be produced as follows:
- chlorine bleach e.g. pure sodium dichloroisocyanurate.
- a suitable press under a pressure of 5,600 kg / cm 2 .
- the shaped body comprises several substances in the rinse cycle a washing machine should have their respective effects.
- Act in the specific case it is the combination of a fabric softener. a means of reducing the Build-up of static electricity in the tissue and a means to improve the renewed Moisture absorption through the fabric.
- a slurry of 58% urea, 18% dimethyldistearylammonium chloride (DMDSAC) (90%), 8% of a C 9-11 alcohol, ethoxylated with 9 moles of ethylene oxide, and 16% water was prepared.
- the slurry was spray dried to obtain a granular material with a density of 580 g / l and the following composition: 68.8% by weight urea, 19.2% by weight DMDSAC, 9.5% by weight not -ionic surfactant and 2.5% by weight water.
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Herstellung einer Tablette. insbesondere einer Reinigungsmitteltablette, mit wenigstens einer ersten und einer zweiten Schicht, sowie ein danach herstellbares Produkt.The invention relates to a method for producing a tablet. especially a detergent tablet, with at least a first and a second layer, and one after producible product.
Im Bereich der Wasch- und Reinigungsmittel, Wasserenthärter, Waschverstärker, Geschirrspülmittel, Desinfektionsmittel, Entkalker, etc. haben sich in den letzten Jahren Tabletten als eine einfach zu dosierende und einfach zu handhabende Darreichungsform im Markt etabliert.In the field of detergents and cleaning agents, water softeners, washing boosters, dishwashing detergents, Disinfectants, decalcifiers, etc. have become tablets in recent years an easy-to-dose and easy-to-use dosage form established on the market.
Dabei sind zunehmend auch zweischichtige Tabletten anzutreffen, bei denen eine unterschiedliche Verteilung von Inhaltsstoffen in den beiden Schichten vorliegt, zum einen um miteinander nicht-kompatible Inhaltsstoffe bis zum Einsatz der Tablette voneinander zu trennen, zum anderen um unterschiedliche Freisetzungsprofile von Inhaltsstoffen zu realisieren.Two-layer tablets, with different ones, are also increasingly to be found Distribution of ingredients in the two layers is present, on the one hand separate incompatible ingredients from each other until the tablet is used, on the other hand to realize different release profiles of ingredients.
Diese Tabletten werden in ähnlichen Pressen hergestellt wie einschichtige Tabletten, wobei allerdings Modifikationen vorgenommen werden müssen. Im Falle einer zweischichtigen Tablette wird üblicherweise zunächst ein erstes Gemisch mit einer ersten Zusammensetzung in eine Form gefüllt und mit einem ersten Druck vorgepreßt. Anschließend wird ein zweites Gemisch mit einer zweiten, unterschiedlichen Zusammensetzung auf die vorgepreßte erste Schicht in der Form gefüllt und die abschließende Pressung bei einem zweiten, üblicherweise höheren Druck durchgeführt.These tablets are manufactured in presses similar to single-layer tablets, whereby however, modifications must be made. In the case of a two-layer tablet is usually first a first mixture with a first composition in filled a mold and pre-pressed with a first pressure. Then a second Mix with a second, different composition on the pre-pressed first Layer filled in the mold and the final pressing on a second one, usually carried out higher pressure.
Bei Tabletten mit wenigstens zwei Schichten stellt sich das Problem, daß die Verbindung zwischen den einzelnen Schichten ausreichend stabil sein muß, um eine Lösung der Schichten voneinander bei Lagerung und Transport der mehrschichtigen Tabletten zu verhindern. Die Ursachen für das Lösen der Schichten voneinander können vielfältig sein, z.B. unterschiedliche Volumenausdehnungen der einzelnen Schichten. Reaktionen an der Grenzfläche zwischen den Schichten, etc. Es ist daher von essentieller Bedeutung, die Zusammensetzungen der einzelnen Schichten genau aufeinander abzustimmen und die Drücke beim Pressen der einzelnen Schichten genau einzustellen. Die Entwicklung und Herstellung stabiler mehrschichtiger Tabletten ist daher zeit- und kostenaufwendig sowie empfindlich gegenüber der Veränderung von internen und externen Parametern im Prozeß.The problem with tablets with at least two layers is that the compound between the individual layers must be sufficiently stable to dissolve the layers prevent each other during storage and transportation of the multilayer tablets. The There may be many reasons for the layers coming apart, e.g. different Volume expansion of the individual layers. Reactions at the interface between the layers, etc. It is therefore essential to the compositions of each Coordinate layers exactly to each other and the pressures when pressing the individual Adjust layers precisely. The development and manufacture of stable multilayer tablets is therefore time and cost consuming and sensitive to the change of internal and external parameters in the process.
Der Erfindung liegt daher die Aufgabe zugrunde, das bekannte Verfahren dahingehend weiterzubilden, daß die Herstellung stabilerer mehrschichtige Tabletten ermöglicht wird. bei denen in weit geringerem Umfang eine Lösung der einzelnen Schichten voneinander auftritt.The invention is therefore based on the object of developing the known method in that that the production of more stable multilayer tablets is made possible. at them to a much lesser extent a solution of the individual layers from one another occurs.
Die Erfindung betrifft ein Verfahren zur Herstellung einer Tablette. insbesondere einer Reinigungsmitteltablette, mit wenigstens einer ersten und einer zweiten Schicht, umfassend die folgenden Schritte a) Einbringen einer ersten abgemessenen Menge einer ersten teilchenförmigen Zusammensetzung in eine Formvertiefung einer Tablettenpresse; b) Pressen der ersten abgemessenen Menge mit einem ersten Preßdruck mittels eines Preßstempels, der auf seiner Preßfläche mindestens eine Vorwölbung aufweist, um eine erste gepreßte Schicht herzustellen, die in ihrer oberen Fläche eine der (den) Vorwölbung(en) auf dem Preßstempel entsprechende Vertiefung(en) aufweist; c) Einbringen einer zweiten abgemessenen Menge einer zweiten teilchenförmigen Zusammensetzung auf die erste gepreßte Schicht in der Formvertiefung der Tablettenpresse; und d) Pressen der zweiten abgemessenen Menge mit einem zweiten Preßdruck mittels des Preßstempel, um eine zweite gepreßte Schicht mit einer entsprechenden Vertiefung(en) in ihrer oberen Fläche herzustellen, sowie danach herstellbare Produkt.The invention relates to a method for producing a tablet. especially a detergent tablet, with at least a first and a second layer comprising the following steps a) introducing a first measured amount of a first particulate Composition in a mold cavity of a tablet press; b) pressing the first measured quantity with a first pressing pressure by means of a press ram that is on its Pressing surface has at least one protrusion to produce a first pressed layer, in its upper surface one corresponding to the protrusion (s) on the press ram Has recess (s); c) introducing a second measured quantity of one second particulate composition onto the first pressed layer in the mold cavity the tablet press; and d) pressing the second measured quantity with a second Press pressure by means of the press ram to form a second pressed layer with a corresponding one To produce recess (es) in their upper surface, as well as product that can be produced thereafter.
In einer besonderen Ausführungsform des erfindungsgemäßen Verfahrens werden für die Herstellung einer dritten und ggf. weiterer Schichten die Schritte (c) und (d) jeweils wiederholt.In a special embodiment of the method according to the invention, the Production of a third and possibly further layers, steps (c) and (d) are repeated in each case.
Die beim erfindungsgemäßen Verfahren in der obersten Schicht der Tablette entstehende(n) Vertiefung(en) wird (werden) bevorzugt verfüllt. The resultant (s) in the top layer of the tablet in the method according to the invention Well (s) are (are) preferably filled.
Des weiteren betrifft die Erfindung eine mehrschichtige Tablette, insbesondere eine Reinigungsmitteltablette, die unter Verwendung des durch die Erfindung vorgeschlagenen Verfahrens hergestellt werden kann.The invention further relates to a multilayer Tablet, in particular a detergent tablet, that using the by the invention proposed method can be produced.
Somit wird gemäß einem zweiten Aspekt der Erfindung eine Tablette mit mindestens einer ersten verpreßten Schicht und einer darüber angeordneten zweiten verpreßten Schicht bereitgestellt, dadurch gekennzeichnet, daß die erste Schicht in der Fläche, an der die zweite Schicht befestigt ist, eine Vertiefung aufweist, wobei die zweite Schicht eine zu der Vertiefung komplementäre Vorwölbung aufweist, die in die Vertiefung eingreift, wobei die Oberseite der zweiten Schicht eine zu der Vorwölbung komplementäre Vertiefung umfasst.Thus, according to a second aspect of the invention one tablet with at least one first pressed Layer and a second arranged above pressed layer provided, thereby characterized in that the first layer in the area the second layer is attached, a recess having, the second layer one to the Depression has complementary protrusion, which in the recess engages, the top of the second layer is complementary to the protrusion Includes deepening.
Überraschenderweise hat sich herausgestellt, daß das durch die Erfindung vorgeschlagene Verfahren ein einfaches Mittel zur Verstärkung der Verbindung zwischen den einzelnen Schichten einer mehrschichtigen Tablette bietet, so daß ein Lösen der Schichten voneinander bei Lagerung und Transport deutlich seltener auftritt und die Tablette in dieser Hinsicht unempfindlicher gegenüber Schwankungen interner (zum Beispiel Zusammensetzung der einzelnen Schichten) und externer (zum Beispiel Preßdrücke, Temperaturen, Luftfeuchte) Parameter beim Herstellungsprozeß ist. Ohne hier an eine bestimmte Theorie zur Erklärung dieses Phänomens gebunden sein zu wollen, wird vermutet, daß diese festeren Verbindungen zwischen den einzelnen Schichten der Tablette zumindest teilweise in einer stärkeren "Verzahnung" der Schichten begründet sind, wie dies durch die nachfolgende Beschreibung der Zeichnung noch deutlicher werden wird. Demgemäß ist es bei Verwendung des durch die Erfindung vorgeschlagenen Verfahrens möglich, bisher verwendete Preßdrücke zu verringern und gleichzeitig eine ebenso gute Verbindung zwischen den einzelnen Schichten zu erzielen wie bisher.Surprisingly, it has been found that the method proposed by the invention simple means of strengthening the connection between the individual layers of a multilayer Tablet offers so that a loosening of the layers from each other clearly in storage and transport occurs less often and the tablet in this regard less sensitive to fluctuations internal (for Example composition of the individual layers) and external (e.g. pressures, temperatures, Humidity) is a parameter in the manufacturing process. Without going into a particular theory to explain it wanting to be bound by this phenomenon suspects that these stronger connections between the individual layers of the tablet at least partially in justified a stronger "interlocking" of the layers are, as indicated by the following description of the Drawing will become even clearer. Accordingly, it is using what is proposed by the invention Process possible, previously used pressures reduce and at the same time an equally good connection to achieve between layers like so far.
Weitere Vorteile und Merkmale der Erfindung ergeben sich aus der nachfolgenden Beschreibung der Zeichnung. Die einzige Zeichnung zeigt eine Ausführungsform der Erfindung im Querschnitt als zweischichtige Tablette mit einem in einer Vertiefung in der obersten Schicht fixierten Formkörper.Further advantages and features of the invention result itself from the following description of the drawing. The only drawing shows an embodiment of the Invention in cross section as a two-layer tablet with one in a recess in the top layer fixed molded body.
Für die Zwecke des durch die Erfindung vorgeschlagenen
Verfahrens wird zunächst die untere Schicht 10 der
Tablette 1 dadurch hergestellt, daß eine erste
abgemessene Menge einer ersten teilchenförmigen
Zusammensetzung in eine Formvertiefung einer
Tablettenpresse gegeben und dort mit einem ersten
Preßdruck mittels eines Preßstempels gepreßt wird, der
auf seiner Preßfläche eine Ausbauchung aufweist, die zu
der dadurch in der obersten Fläche 11 der unteren
Schicht 10 der Tablette 1 hergestellten Vertiefung 12
im wesentlichen komplementär ausgebildet ist.For the purposes of what is proposed by the invention
First, the
Dann wird auf die erste gepreßte Schicht 10 eine zweite
abgemessene Menge einer zweiten teilchenförmigen
Zusammensetzung (die üblicherweise von der ersten
teilchenförmigen Zusammensetzung verschieden ist) in
die Formvertiefung der Tablettenpresse gegeben und mit
einem zweiten Preßdruck (der üblicherweise höher als
der erste Preßdruck ist) mittels des Preßstempels die
zweite Schicht der Tablette 20 gepreßt. Folglich werden
die beiden Tablettenschichten 10 und 20 nicht nur
entlang der horizontalen Grenzschicht gegeneinander
gepreßt, sondern insbesondere auch in der... Then a second is pressed onto the first pressed
Vertiefung 12 der unteren Schicht 10, wodurch
auch seitlich gerichtete Preßkräfte entstehen, die zweite Zusammensetzung also besonders
stark und fest in die Vertiefung 12 der unteren Schicht 10 hineingedrückt wird.
Ein merkbarer Effekt der Verstärkung der Verbindung zwischen den beiden Schichten durch
die Verzahnung zwischen der Vertiefung 12 der unteren Schicht 10 und der Vorwölbung 22
der oberen Schicht 20 und die stärkere Verbindung der Schichten in diesem Bereich ist bereits
bei Verwendung eines Preßstempels mit nur einer Vorwölbung deutlich feststellbar. Selbstverständlich
ist es möglich, diesen Effekt durch das Vorsehen mehrerer Vorwölbungen im
Preßstempel ggf. noch zu verstärken. Die Preßdrücke können so belassen werden, wie es für
die Herstellung zweischichtiger Tabletten üblich ist. wobei diese Preßdrücke in Abhängigkeit
von der Zusammensetzung der einzelnen Schichten stark schwanken können. In den nachfolgenden
Beispielen sind Preßdrücke für konkrete Zusammensetzungen angegeben. A noticeable effect of strengthening the connection between the two layers
the toothing between the
Die durch das erfindungsgemäße Herstellungsverfahren auf der Oberseite 23 der oberen
Schicht 20 entstehenden Vertiefungen 24 können so belassen werden oder vorzugsweise mit
einem weiteren Material verfüllt werden, das gleichzeitig auch noch weitere Funktionen beim
Einsatz der Tabletten übernehmen kann. In der dargestellten Ausführungsform ist ein Formkörper
30 in der (zumindest in ihrem unteren Teil) komplementär ausgebildeten Vertiefung 24
in geeigneter Weise, bspw. durch einen Kleber, fixiert. Dabei weist der Formkörper 30 der
dargestellten Ausführungsform einen Kern 31 und eine zusätzliche Schutzumhüllung 32 auf.
um ihn z.B. während der Lagerung zu schützen und bei Gebrauch die Freisetzung der Inhaltsstofte
des Kern 31 zu steuern.The by the manufacturing method according to the invention on the
Die Zusammensetzungen der Tablette bzw. Formkörper können je nach Einsatz in breitem Umfang variieren. Verschiedene Möglichkeiten im bevorzugten Einsatzbereich sind in den folgenden Beispielen dargestellt.The compositions of the tablet or shaped body can vary widely depending on the use Vary scope. Different possibilities in the preferred area of application are in the following examples.
Die Zusammensetzungen der Tabletten in den Beispielen 1 bis 7 repräsentieren Geschirrspülmittelzusammensetzungen, wobei bei den Tabletten der Beispiele 2 bis 7 die Vertiefungen in der Oberseite der obersten Schicht mit verschiedenen Formkörpern verfüllt sind. Beispiel 8 beschreibt eine Waschverstärkertablette und eine Waschmitteltablette.The compositions of the tablets in Examples 1 to 7 represent dishwashing detergent compositions the depressions in the tablets of Examples 2 to 7 are filled with various shaped bodies in the top of the top layer. example 8 describes a detergent tablet and a detergent tablet.
Weitere Einsatzbereiche für mehrschichtige Tabletten - nicht nur im Bereich von Reinigungsmitteln - sind aber denkbar. Dabei kann der Fachmann in jedem Falle auf die ihm bekannten oder von ihm entwickelten Rezepturen und Verfahrensweisen zurückgreifen, da er zur Verwirklichung des erfindungsgemäßen Verfahrens lediglich den Preßstempel modifizieren und ggf. Preßdrücke angleichen müßte.Further areas of application for multi-layer tablets - not only in the area of cleaning agents - but are conceivable. In this case, the person skilled in the art can rely on those known to him or recipes and procedures developed by him, since he only modify the ram to implement the method according to the invention and if necessary would have to equalize pressures.
Die folgende Tabelle bezieht sich auf die Zusammensetzung der beiden Schichten einer zweischichtigen
Geschirrspülmitteltablette (Gewichtsverhältnis ca. 50 : 50), wobei Schicht 1 die
erste (untere) Schicht darstellt, die in Schritt (b) lediglich leicht zusammengedrückt wird (ohne
eigentliche Komprimierung), was aber ausreichend ist, um eine glatte Oberfläche mit der
entsprechenden Vertiefung in der Oberseite auszubilden. Nach Einfüllen der zweiten Zusammensetzung
erfolgt das Pressen der endgültigen Tablette mit einem Preßdruck von ca. 100
kN/cm2.
Die folgenden Beispiele 2 bis 7 betreffen ebenfalls zweischichtige Geschirrspülmitteltabletten, wobei die Zusammensetzung an einzelnen Schichten der Tablette gegenüber denjenigen von Beispiel 1 (wenn überhaupt) nur geringfügig verändert sind. In den einzelnen Beispielen sind zur Veranschaulichung konkrete Anwendungsbeispiele verschiedener Formkörper beschrieben. die in die bei dem erfindungsgemäßen Verfahren entstehende Vertiefung in der Oberseite der obersten (zweiten) Schicht eingesetzt und bspw. mit Kleber fixiert werden können. Das eigentliche Herstellungsverfahren der Tablette, insbesondere die in Beispiel 1 beschriebenen Preßdrücke, bleiben unverändert. The following Examples 2 to 7 also relate to two-layer dishwasher tablets, the composition on individual layers of the tablet compared to those of Example 1 are only slightly changed (if at all). In the individual examples concrete examples of use of various moldings are described for illustration. the in the resulting in the process according to the invention in the Top of the top (second) layer can be used and can be fixed with glue, for example. The actual manufacturing process of the tablet, especially those described in Example 1 Press pressures remain unchanged.
Durch die rasche Auflösezeit des Formkörpers (< 1 min) wird die darin enthaltene Protease schneller freigesetzt als die in der Tablette enthaltene und kann dadurch ihre Wirkung bereits direkt am Anfang des Hauptspülganges entfalten. Durch das Auflösen der Tablette während des Aufwärmeprozesses werden erneut frische Enzyme (Protease und Amylase) in die Spüllauge freigesetzt. Due to the rapid dissolution time of the shaped body (<1 min), the protease contained therein becomes Released faster than that contained in the tablet and may already have its effect unfold directly at the beginning of the main wash cycle. By dissolving the tablet while During the warm-up process, fresh enzymes (protease and amylase) are added to the rinsing solution released.
Ähnlich wie Beispiel 1, mit dem Unterschied. daß hier am Anfang des Hauptspülganges sowohl Protease als auch Amylase freigesetzt werden.Similar to example 1, with the difference. that here at the beginning of the main wash cycle both Protease as well as amylase are released.
Die Tablette entspricht in ihrer Zusammensetzung im wesentlichen derjenigen der Beispiele 1 und 2, mit dem Unterschied, daß in Schicht 2 der Tablette warmwasserstabile Protease bzw. Amylase eingesetzt wird. Die Zusammensetzung des Formkörpers entspricht derjenigen des Formkörpers von Beispiel 2.The composition of the tablet essentially corresponds to that of Examples 1 and 2, with the difference that protease or amylase which is stable in hot water is used in layer 2 of the tablet. The composition of the shaped body corresponds to that of the shaped body from Example 2.
Durch das zeitversetzte Auflösen von Tablette und Formkörper können sich die unterschiedlichen Wirkungsprofile der verschiedenen Protease- und Amylasetypen optimal entfalten. Der Formkörper setzt am Anfang des Hauptspülganges kaltwasseraktive Protease und Amylase frei. Durch das Auflösen der Tablette während des Aufwärmeprozesses werden bleichstabile warmwasserstabile Enzyme in die Spüllauge freigesetzt.Due to the delayed dissolution of the tablet and the shaped body, the different ones can Optimally develop the effect profiles of the different types of proteases and amylases. The Shaped body sets cold water-active protease and amylase at the beginning of the main wash cycle free. By dissolving the tablet during the warm-up process, it becomes bleach-stable enzymes stable in hot water are released into the rinsing solution.
Durch dieses Ausführungsform ist eine zeitversetzte Auflösung von in Lösung nicht kompatibler Lipase und Protease möglich. With this embodiment, a time-shifted resolution is not compatible in solution Lipase and protease possible.
Durch diese Ausführungsform ist eine zeitversetzte Auflösung von in Lösung mit Bleichmitteln nicht kompatiblen Enzymen möglich. This embodiment enables a time-delayed dissolution of in solution with bleaching agents incompatible enzymes possible.
Durch die Auflösung des Formkörpers am Anfang des Hauptspülganges kann die freigesetzte Persäure unter den notwendigen sauren Bedingungen wirken. Durch späteres Auflösen der Tablette wird die übliche optimale alkalische Spülbedingung für Protease und Amylase erreicht.By dissolving the molded body at the beginning of the main wash cycle, the released one can Peracid act under the necessary acidic conditions. By later dissolving the Tablet, the usual optimal alkaline rinsing condition for protease and amylase is reached.
Aus der folgenden Tabelle ergibt sich eine beispielhafte Formulierung für eine zweischichtige
Waschverstärkertablette. Die erste (untere) Schicht macht dabei gewichtsmäßig ca. 74 % der
Gesamttablette aus. während die zweite (obere) Schicht ca. 26 % ausmacht.
Aus der folgenden Tabelle ergibt sich eine beispielhafte Formulierung für eine Waschmitteltablette wobei die beiden Schichten in diesem Falle in einem Gewichtsverhältnis von 70 (untere (1.) Schicht) zu 30 (obere (2.) Schicht) stehen. The following table shows an exemplary formulation for a detergent tablet, in which case the two layers are in a weight ratio of 70 (lower (1st) layer) to 30 (upper (2nd) layer).
Im folgenden werden verschiedene Möglichkeiten für Formkörper beschrieben, die bei der soeben beschriebenen zweischichtigen Waschverstärkertablette bzw. Waschmitteltablette zum Einsatz kommen können.The following describes various options for moldings that are used in the just described two-layer detergent tablet or detergent tablet for Can come into play.
Die Freisetzung einer Säure in den Spülgängen einer Waschmaschine soll sowohl der Entfernung von Inkrustierungen als auch der Neutralisierung von alkalischen Rückständen dienen. Vorteilhafterweise werden für diesen Zweck schwache Säuren eingesetzt, wie bspw. Amidosulfonsäure und/oder Maleinsäure. Üblicherweise handelt es sich bei diesen Materialien um Feststoffe. The release of an acid in the wash cycles of a washing machine is said to be both removal of incrustations as well as the neutralization of alkaline residues serve. Weak acids are advantageously used for this purpose, such as For example, amidosulfonic acid and / or maleic acid. Usually these are Materials around solids.
Das Herstellungsverfahren stellt sich wie folgt dar:The manufacturing process is as follows:
Eine Mischung aus 1.05 g Amidosulfonsäure und 0,45 Maleinsäure werden in einer Rotationspresse unter einem Druck von 890 kg/cm2 zu einem Formkörper ausgeformt.A mixture of 1.05 g of amidosulfonic acid and 0.45 maleic acid is formed in a rotary press under a pressure of 890 kg / cm 2 to give a shaped body.
Unter Berücksichtigung ähnlicher Erwägungen wie in Beispiel 7a wird ein entsprechender Formkörper wie folgt hergestellt:Taking into account similar considerations as in Example 7a, a corresponding one Shaped body produced as follows:
0,1975 g Duftstoff werden auf 0,0525 g feinverteilte Kieselsäure absorbiert, um ein freifließendes körniges Material zu ergeben. Die resultierenden 0,25 g werden mit 0,6 g mikrokristalliner Cellulose und 0,15 g quervernetztem Polyvinylpyrrolidon vermischt. Die Mischung wird in einer Rundpresse mit einem Innendurchmesser von 10 mm unter einem Druck von 2900 kg/cm2 tablettiert, um einen elliptischen Formkörper mit einer Höhe von 13,1 mm und einem Gewicht von ca. 1 g zu ergeben.0.1975 g of fragrance is absorbed onto 0.0525 g of finely divided silica to give a free-flowing granular material. The resulting 0.25 g is mixed with 0.6 g of microcrystalline cellulose and 0.15 g of cross-linked polyvinylpyrrolidone. The mixture is tableted in a round press with an inner diameter of 10 mm under a pressure of 2900 kg / cm 2 to give an elliptical shaped body with a height of 13.1 mm and a weight of approx. 1 g.
Der Einsatz von Chlorbleiche im Spülgang einer Waschmaschine dient der Verbesserung der Reinigungswirkung und entfaltet gleichzeitig eine zusätzliche Desinfektionswirkung.The use of chlorine bleach in the washing cycle of a washing machine serves for improvement the cleaning effect and at the same time has an additional disinfecting effect.
Unter Berücksichtigung der Erwägungen in den Beispielen 7a und 7b können derartige Formkörper wie folgt hergestellt werden: Taking into account the considerations in Examples 7a and 7b, such Shaped bodies can be produced as follows:
1 g Chlorbleiche, z.B. reines Natriumdichlorisocyanurat. kann in einer geeigneten Presse unter einem Druck von 5.600 kg/cm2 zu einem Formkörper verpreßt werden.1 g of chlorine bleach, e.g. pure sodium dichloroisocyanurate. can be pressed into a shaped body in a suitable press under a pressure of 5,600 kg / cm 2 .
Im vorliegenden Beispiel umfaßt der Formkörper mehrere Substanzen, die im Spülgang einer Waschmaschine ihre jeweiligen Wirkungen entfalten sollen. Im konkreten Fall handelt es sich um die Kombination eines Weichspülers. eines Mittels zur Verringerung des Aufbaus statischer Elektrizität im Gewebe und eines Mittels zur Verbesserung der erneuten Feuchtigkeitsaufnahme durch das Gewebe.In the present example, the shaped body comprises several substances in the rinse cycle a washing machine should have their respective effects. Act in the specific case it is the combination of a fabric softener. a means of reducing the Build-up of static electricity in the tissue and a means to improve the renewed Moisture absorption through the fabric.
Eine Aufschlämmung aus 58 % Harnstoff, 18 % Dimethyldistearylammoniumchlorid (DMDSAC) (90 %), 8 % eines C9-11-Alkohols, ethoxyliert mit 9 Mol Ethylenoxid, und 16 % Wasser wurde hergestellt. Die Aufschlämmung wurde sprühgetrocknet, um ein kömiges Material mit einer Dichte von 580 g/l und der folgenden Zusammensetzung zu erhalten: 68,8 Gew.-% Harnstoff, 19,2 Gew.-% DMDSAC, 9,5 Gew.-% nicht-ionisches Tensid und 2,5 Gew.-% Wasser.A slurry of 58% urea, 18% dimethyldistearylammonium chloride (DMDSAC) (90%), 8% of a C 9-11 alcohol, ethoxylated with 9 moles of ethylene oxide, and 16% water was prepared. The slurry was spray dried to obtain a granular material with a density of 580 g / l and the following composition: 68.8% by weight urea, 19.2% by weight DMDSAC, 9.5% by weight not -ionic surfactant and 2.5% by weight water.
4 g der körnigen Zusammensetzung wurden mit 1 g Cellulose vermischt. Die Mischung wurde in einer Rundpresse mit einem Innendurchmesser von 25 mm und einem Druck von 80 kg/cm2 tablettiert, um einen elliptischen Formkörper mit einer Höhe von 14 mm und einem Gewicht von 5 g zu erhalten. 4 g of the granular composition were mixed with 1 g of cellulose. The mixture was tableted in a round press with an inner diameter of 25 mm and a pressure of 80 kg / cm 2 to obtain an elliptical shaped body with a height of 14 mm and a weight of 5 g.
Stabilitätstests. bei denen insbesondere die mechanische Beanspruchung während eines Transports simuliert werden, haben eine meßbar bessere Stabilität der gemäß den Beispielen hergestellten Tabletten ergeben, wenn diese mit denselben Preßdrücken hergestellt werden. wie sie üblicherweise für die Herstellung von zweischichtigen Tabletten verwendet werden.Stability tests. where in particular the mechanical stress during a Transports simulated have a measurably better stability according to the examples tablets produced if they are produced with the same compression pressures. as usually used for the production of two-layer tablets.
Die in der vorstehenden Beschreibung, den Ansprüchen sowie der Zeichnung offenbarten Merkmale der Erfindung können sowohl einzeln als auch in beliebiger Kombination für die Verwirklichung der Erfindung in ihren verschiedenen Ausführungsformen wesentlich sein.Those disclosed in the above description, the claims and the drawing Features of the invention can be used both individually and in any combination Realization of the invention in its various embodiments may be essential.
Claims (20)
- Method of producing a tablet, in particular a detergent tablet, with at least a first and a second layer, characterised by the following steps:a) introducing a first metered quantity of a first particulate composition into a mould well of a tablet press;b) pressing the first metered quantity at a first pressing pressure by means of a die, which has at least one protuberance on its pressing surface in order to make a first pressed layer with a hollow(s) in its top surface matching the protuberance(s) on the die;c) introducing a second metered quantity of a second particulate composition into the mould well of the tablet press on top of the first pressed layer; andd) pressing the second metered quantity at a second pressing pressure by means of the die, in order to make a second pressed layer with a corresponding hollow(s) in its surface.
- Method as claimed in claim 1, characterised in that steps (c) and (d) are respectively repeated in order to obtain a third and optionally other layers.
- Method as claimed in claim 1 or 2, characterised in that the hollow(s) made in the uppermost layer using the method proposed by the invention is (are) filled.
- Method as claimed in claim 3, characterised in that the hollow(s) in the uppermost layer of the tablet (is) are filled by pouring in a free-flowing, hardenable composition.
- Method as claimed in claim 3, characterised in that the hollows(s) is (are) filled by introducing and then pressing a particulate composition.
- Method as claimed in claim 3, characterised in that the hollow(s) is (are) filled by introducing one or more moulded pieces.
- Method as claimed in claim 6, characterised in that when placed in the hollow(s), the moulded piece(s) stand proud of the top face of the tablet.
- Method as claimed in claim 6 or 7, characterised in that the moulded piece(s) is (are) fixed in the hollow(s), producing a bond between the tablet and the moulded piece that will remain secure during transport.
- Method as claimed in claim 8, characterised in that the moulded piece(s) is (are) fixed in the hollow(s) by means of a glue.
- Multi-layered tablet, in particular a detergent tablet, which is produced as claimed in one of the preceding claims.
- Tablet (1) with at least a first pressed layer (10) and a second pressed layer (20) arranged on top, characterised in that the first layer (10) has a hollow (12) in the surface (11) to which the second layer (20) is joined, the second layer (20) has a protuberance (22) which complements the hollow (12) and locates in the hollow (12), the top face (23) of the second layer (20) having a hollow (24) complementing the protuberance (22).
- Tablet as claimed in claim 11, in which a third and optionally other layers are disposed above the second layer (20).
- Tablet as claimed in claim 11 or 12, in which the hollow(s) in the uppermost layer (20) of the tablet is (are) filled.
- Tablet as claimed in claim 13, in which the hollow(s) in the uppermost layer (20) of the tablet is (are) filled by pouring in a free-flowing hardenable composition.
- Tablet as claimed in claim 13, in which the hollow(s) (24) is (are) filled by introducing and then pressing a particulate composition.
- Tablet as claimed in claim 13, in which the hollow(s) (24) is (are) filled by introducing one or more moulded pieces (30).
- Tablet as claimed in claim 16, in which the moulded piece(s) (30) stand proud of the top face (23) of the uppermost layer (20).
- Tablet as claimed claim 16 or 17, in which the moulded piece(s) (30) is (are) fixed in the hollow(s) (24) with a substance which produces a bond between the tablet (1) and the moulded piece(s) (30) that will remain secure during transport.
- Tablet as claimed in claim 18, in which the moulded piece (30) is fixed in the hollow(s) (24) by a glue.
- Tablet as claimed in one of claims 11 to 19, the tablet being a detergent tablet.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19922578 | 1999-05-17 | ||
DE19922578A DE19922578C2 (en) | 1999-05-17 | 1999-05-17 | Process for the production of a multilayer tablet, in particular detergent tablet, and product which can be produced thereafter |
PCT/EP2000/004478 WO2000070008A1 (en) | 1999-05-17 | 2000-05-17 | Method of producing a multi-layer detergent tablet |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1179042A1 EP1179042A1 (en) | 2002-02-13 |
EP1179042B1 true EP1179042B1 (en) | 2003-12-10 |
Family
ID=7908277
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00929538A Revoked EP1179042B1 (en) | 1999-05-17 | 2000-05-17 | Method of producing a multi-layer tablet |
Country Status (8)
Country | Link |
---|---|
US (1) | US6809073B2 (en) |
EP (1) | EP1179042B1 (en) |
AT (1) | ATE256174T1 (en) |
AU (1) | AU768494B2 (en) |
CA (1) | CA2372193C (en) |
DE (2) | DE19922578C2 (en) |
ES (1) | ES2211543T3 (en) |
WO (1) | WO2000070008A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2089501A1 (en) * | 2006-10-27 | 2009-08-19 | Henkel AG & Co. KGaA | Detergent or cleaning agent moulded bodies |
EP2097503A1 (en) * | 2006-10-27 | 2009-09-09 | Henkel AG & Co. KGaA | Detergent or cleaning agent moulded bodies |
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DE19963569B4 (en) | 1999-12-29 | 2006-11-16 | Reckitt Benckiser N.V. | Composition for use in a dishwasher |
GB0003592D0 (en) * | 2000-02-17 | 2000-04-05 | Procter & Gamble | Detergent tablet |
GB0015350D0 (en) * | 2000-06-23 | 2000-08-16 | Reckitt Benckiser Nv | Improvements in or relating to compositions |
EP1319058B1 (en) * | 2000-09-20 | 2006-02-01 | Reckitt Benckiser Inc. | Improvements in enzyme containing tablets |
DE10108153A1 (en) | 2000-09-28 | 2002-10-24 | Henkel Kgaa | Tray tablets and process for their manufacture |
DE10061421A1 (en) * | 2000-12-09 | 2002-06-20 | Henkel Kgaa | Process for the production of glued molded articles |
DE10111780B8 (en) * | 2001-03-13 | 2005-02-10 | Isaak Dr. Abramov | Effervescent tablet, pill or dragee, as well as the process for its preparation |
GB2382342A (en) * | 2001-11-27 | 2003-05-28 | Reckitt Benckiser Nv | Water-softening tablet |
DE10221559B4 (en) * | 2002-05-15 | 2009-04-30 | Henkel Ag & Co. Kgaa | Detergent and detergent tablets with active phase |
US20050148488A1 (en) * | 2002-05-15 | 2005-07-07 | Maren Jekel | Detergent tablets with active phase |
DE10336796B4 (en) * | 2003-08-08 | 2005-05-19 | Henkel Kgaa | Washing or cleaning agents |
DE10352961A1 (en) * | 2003-11-13 | 2005-06-23 | Henkel Kgaa | Shock-resistant tablet |
GB2415200A (en) | 2004-06-19 | 2005-12-21 | Reckitt Benckiser Nv | Process for producing a detergent tablet |
DE102004051557A1 (en) * | 2004-10-22 | 2006-04-27 | Henkel Kgaa | Detergent or detergent dosing unit |
GB2419838A (en) * | 2004-11-03 | 2006-05-10 | Reckitt Benckiser Nv | Making a tablet of three layers |
GB0616439D0 (en) * | 2006-08-18 | 2006-09-27 | Reckitt Benckiser Nv | Detergent composition |
GB0616444D0 (en) * | 2006-08-18 | 2006-09-27 | Reckitt Benckiser Nv | Detergent composition |
DE102007032892B4 (en) * | 2007-07-14 | 2009-12-24 | Refractory Intellectual Property Gmbh & Co. Kg | Tundish mass and a method for creating a humid Tundishmasse |
US20090032063A1 (en) * | 2007-07-30 | 2009-02-05 | Haas Geoffrey R | Solid cleaning composition and method of use |
PL2053120T3 (en) | 2007-10-26 | 2017-04-28 | Dalli-Werke Gmbh & Co. Kg | Washing or cleaning agent shaped body with dyeable relief structure |
ITMI20100789A1 (en) * | 2010-05-05 | 2011-11-06 | Ica Spa | MULTIPURPOSE TABLET FOR FABRICS AND ITS PROCESS OF PROCESSING |
WO2011151192A1 (en) * | 2010-06-02 | 2011-12-08 | Henkel Ag & Co. Kgaa | Dishwasher products in a compacted form |
WO2011151190A1 (en) * | 2010-06-02 | 2011-12-08 | Henkel Ag & Co. Kgaa | Dishwasher products in a compacted form |
DE102010051226A1 (en) | 2010-11-12 | 2012-05-31 | Dental Care Innovation Gmbh | Rinse-off tray with abrasive components |
WO2012118180A1 (en) * | 2011-03-03 | 2012-09-07 | 武田薬品工業株式会社 | Laminated tablet and manufacturing method therefor |
FR3021666B1 (en) | 2014-05-28 | 2017-12-08 | Eurotab | CAVITY MULTILAYER TABLET, DEVICE AND METHOD FOR COMPACTING SUCH TABLET |
US20160145542A1 (en) * | 2014-11-25 | 2016-05-26 | Milliken & Company | Cleaning Composition |
AU2018214552B2 (en) | 2017-02-02 | 2021-12-23 | Water Pik, Inc. | Tablet comprising abrasive for dental cleaning |
US20220251485A1 (en) * | 2021-02-09 | 2022-08-11 | Urnex Brands, Llc | Dual function milk, milkstone cleaning tablet |
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EP0979866A1 (en) * | 1998-07-17 | 2000-02-16 | The Procter & Gamble Company | Detergent tablet |
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DE3541146A1 (en) * | 1985-11-21 | 1987-05-27 | Henkel Kgaa | MULTILAYERED DETERGENT TABLETS FOR MACHINE DISHWASHER |
GB9711829D0 (en) * | 1997-06-06 | 1997-08-06 | Unilever Plc | Detergent compositions |
GB2327949A (en) * | 1997-08-02 | 1999-02-10 | Procter & Gamble | Detergent tablet |
US6274538B1 (en) * | 1997-11-10 | 2001-08-14 | The Procter & Gamble Company | Detergent compositions |
DE29823506U1 (en) * | 1998-05-25 | 1999-06-17 | Henkel Kgaa | Detergent tablets with trough |
IES990573A2 (en) * | 1998-07-17 | 2000-03-08 | Procter & Gamble | Detergent tablet |
ES2168835T3 (en) * | 1998-07-17 | 2002-06-16 | Procter & Gamble | METHOD TO PREPARE DETERGENT TABLETS. |
DE29911486U1 (en) * | 1998-07-17 | 1999-11-18 | Procter & Gamble | Detergent tablet |
GB9901688D0 (en) * | 1999-01-26 | 1999-03-17 | Unilever Plc | Detergent compositions |
-
1999
- 1999-05-17 DE DE19922578A patent/DE19922578C2/en not_active Revoked
-
2000
- 2000-05-17 WO PCT/EP2000/004478 patent/WO2000070008A1/en active IP Right Grant
- 2000-05-17 ES ES00929538T patent/ES2211543T3/en not_active Expired - Lifetime
- 2000-05-17 AT AT00929538T patent/ATE256174T1/en not_active IP Right Cessation
- 2000-05-17 EP EP00929538A patent/EP1179042B1/en not_active Revoked
- 2000-05-17 DE DE50004732T patent/DE50004732D1/en not_active Revoked
- 2000-05-17 CA CA002372193A patent/CA2372193C/en not_active Expired - Lifetime
- 2000-05-17 AU AU47579/00A patent/AU768494B2/en not_active Ceased
-
2001
- 2001-11-15 US US10/000,641 patent/US6809073B2/en not_active Expired - Lifetime
Patent Citations (1)
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EP0979866A1 (en) * | 1998-07-17 | 2000-02-16 | The Procter & Gamble Company | Detergent tablet |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2089501A1 (en) * | 2006-10-27 | 2009-08-19 | Henkel AG & Co. KGaA | Detergent or cleaning agent moulded bodies |
EP2097503A1 (en) * | 2006-10-27 | 2009-09-09 | Henkel AG & Co. KGaA | Detergent or cleaning agent moulded bodies |
Also Published As
Publication number | Publication date |
---|---|
US20020147125A1 (en) | 2002-10-10 |
EP1179042A1 (en) | 2002-02-13 |
DE19922578A1 (en) | 2000-11-23 |
AU768494B2 (en) | 2003-12-11 |
WO2000070008A1 (en) | 2000-11-23 |
DE50004732D1 (en) | 2004-01-22 |
US6809073B2 (en) | 2004-10-26 |
CA2372193C (en) | 2008-07-29 |
CA2372193A1 (en) | 2000-11-23 |
ATE256174T1 (en) | 2003-12-15 |
DE19922578C2 (en) | 2003-12-24 |
ES2211543T3 (en) | 2004-07-16 |
AU4757900A (en) | 2000-12-05 |
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