WO1994013775A1 - Method of producing washing agents in powder form - Google Patents
Method of producing washing agents in powder form Download PDFInfo
- Publication number
- WO1994013775A1 WO1994013775A1 PCT/EP1993/003443 EP9303443W WO9413775A1 WO 1994013775 A1 WO1994013775 A1 WO 1994013775A1 EP 9303443 W EP9303443 W EP 9303443W WO 9413775 A1 WO9413775 A1 WO 9413775A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- detergent
- weight
- polyvinylpyrrolidone
- pvp
- powdered
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3769—(Co)polymerised monomers containing nitrogen, e.g. carbonamides, nitriles or amines
- C11D3/3776—Heterocyclic compounds, e.g. lactam
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
Definitions
- the present patent application relates to a process for the production of powder detergents containing polyvinyl pyrrolidone, by means of which the transfer of detached dyes during washing to other washed textiles is prevented.
- discoloration-inhibiting detergents care must therefore be taken that at most small amounts of strong electrolytes and in particular only small amounts of anionic surfactants are used. To achieve a sufficient washing performance, nonionic surfactants are therefore preferably used in larger quantities as a detergent component.
- Non-ionic surfactants have a liquid to pasty consistency at room temperature, so that when using larger amounts of non-ionic surfactants it is necessary to select the amount and type of these surfactants in such a way that the physical properties of the surfactants, in particular the flowability and flushing behavior of the pul ⁇ deformed detergents are not affected.
- This is sometimes a problem in the formulation of powder detergents, which is exacerbated by the addition of polyvinylpyrrolidone in the detergents. It was observed, for example, that powder detergents which, without a content of polyvinylpyrrolidone, had free-flowing properties and a problem-free rinsing behavior, behaved poorly in this regard even after adding only small amounts of polyvinylpyrrolidone.
- the object of the present invention was therefore to compensate for the disadvantage associated with the addition of polyvinylpyrrolidone in powder detergents of the deterioration in the flowability and the washing-in behavior by modifying the production process.
- this object is achieved by adding all or part of the polyvinylpyrrolidone to the spray-dried detergent in a separate working step in the preparation of the detergent by the customary spray drying of an aqueous slurry containing the detergent constituents.
- the present invention therefore relates to a process for the production of powdered detergents containing polyvinylpyrrolidone, which is characterized in that the polyvinylpyrrolidone is wholly or partly in the form of a separate mixture with other powdered detergent constituents, the powdered detergent which is the contains other detergent ingredients.
- the procedure described makes it possible to add polyvinylpyrrolidone in an amount of detergents required for the discoloration inhibition without impairing their free-flowing properties or detergent retention.
- the detergents to be produced according to the invention usually contain 10-30% by weight of surfactants, of which 5-10% by weight nonionic surfactants, 5-20% by weight of synthetic anionic surfactants and 1-5% by weight. of fatty acid soaps.
- inorganic builder salts such as, for example, zeolite A, sodium carbonate, sodium sulfate, sodium silicate or sodium triphosphate
- conventional detergent additives such as, for example, organic co-builders of the polycarboxylate type, carboxymethyl cellulose and water-soluble complexing agents , Anti-foaming agents, enzymes and fragrances.
- the polyvinylpyrrolidone content is preferably 0.5-5% by weight of the detergent.
- the separate mixture hereinafter called PVP concentrate, contains large amounts of PVP together with predominantly inorganic carrier components.
- the PVP content in this PVP concentrate can be 10-50% by weight, preferably 20-40% by weight.
- Such PVP concentrates preferably contain 20-40% by weight of polyvinylpyrrolidone in addition to 40-80% by weight of inorganic carrier salts and smaller amounts of water.
- These separate, high PVP-containing mixtures are preferably also produced by spray drying an aqueous slurry. However, it can also be produced by other conventional granulation processes, for example by spray mixing or extrusion processes.
- a further subject of the invention is therefore a pulverulent PVP concentrate containing PVP and inorganic carrier salts, which contains 20-40% by weight polyvinylpyrrolidone and 40-80% by weight inorganic carrier salts.
- the inorganic carrier salts preferably consist entirely or predominantly of detergent builders, preferably of water-insoluble zeolite ion exchangers, in particular of the zeolite A type.
- the PVP concentrate can also contain smaller amounts of surfactants and up to 20% by weight. % contain water.
- Another object of the invention is a detergent consisting of two granular components of different compositions, the first granular component containing no polyvinylpyrrolidone or no more than an amount of up to 2.5% by weight of polyvinylpyrrolidone which is not harmful to the flow properties, and the second one granular component 10-50 wt .-% polyvinyl pyrrolidone and an inorganic carrier, preferably a detergent builder salt, contains.
- Both the first granular component and the second, high PVP-containing component can be spray dried by appropriate slurry Ries or be produced by other known granulation. However, production by spray drying is preferred.
- a slurry is prepared which either contains no polyvinylpyrrolidone or only a portion of the polyvinylpyrrolidone provided in the recipe which is not harmful to the flowability and other constituents of the recipe, and this slurry is sprayed in the customary manner, gel can dispense with part of the water of the slurries due to the lower content of solids.
- the polyvinylpyrrolidone not contained in the slurry, together with the other inorganic detergent constituents also not contained in the slurry, is in turn processed into a second aqueous slurry and converted into a powdery state by spray drying.
- the mixing ratio depends on the amount of polyvinylpyrrolidone already contained in the first granular component and the desired PVP content of the end product, which is 0.5-5% by weight, preferably 3-5% by weight. should be. At least half of the total PVP contained in the finished detergent is preferably added in the form of a separate mixture (PVP concentrate). However, it is even more preferred to add at least 75% by weight of the PVP to the detergent in the form of the PVP concentrate.
- a preliminary detergent product was produced by spray drying, in which only a part of the total polyvinylpyrrolidone (PVP) provided in the recipe is contained. The remainder of the PVP is added in a mixing process in the form of a PVP-rich powder likewise produced by spray drying.
- PVP polyvinylpyrrolidone
- the preliminary detergent product contains:
- the finished product thus obtained had a bulk density of 410 g per liter and a much better trickle behavior (according to the so-called "package test") and a significantly improved washing-in behavior (according to the so-called “washing-in test”) than one otherwise identical detergent, the entire proportion of PVP of which was contained in the detergent intermediate.
- This finding is confirmed by a detergent which has the same composition, but in which the entire amount of PVP has been added to the detergent precursor in one mixing operation (Example V3).
- a preliminary detergent product which did not contain any PVP was prepared by spray drying.
- the "package test” is carried out as follows:
- a standard detergent package which is filled with washing powder and opened, is tilted through a device by certain angles and the type and amount of powder discharge, if necessary after shaking the package with the marks 1 (very good flowability) to 10 (very poorly flowable) rated.
- a commercially available washing machine dispenser which is particularly problematic with regard to its dispensing behavior, is charged with 100 g of detergent under defined filling conditions and flushed with a maximum of 10 liters of water. The amount of water in which the washing powder is completely rinsed out of the induction device or how large the detergent residue in the induction device is after the flow of 10 liters of water is then assessed.
Abstract
In the production of powder-form washing agents containing poly(vinyl pyrrolidone), the invention calls for all or part of the poly(vinyl pyrrolidone) to be added in the form of a separate mixture with other powder-form washing-agent ingredients to the powder-form washing agent containing the remaining ingredients.
Description
Verfahren zur Herstellung von pulverförmigen Waschmitteln Process for the preparation of powder detergents
Die vorliegende Patentanmeldung betrifft ein Verfahren zur Herstel¬ lung von pulverförmigen Waschmitteln mit einem Gehalt an Polyvinyl¬ pyrrolidon, durch den die Übertragung von abgelösten Farbstoffen während der Wäsche auf andere mitgewaschene Textilien verhindert wird.The present patent application relates to a process for the production of powder detergents containing polyvinyl pyrrolidone, by means of which the transfer of detached dyes during washing to other washed textiles is prevented.
Beim gleichzeitigen Waschen von gefärbten Textilien mit ungefärbten oder hellfarbigen Textilien wird häufig beobachtet, daß von den stärker gefärbten Textilien Farbstoff auf die ungefärbten Textilien oder hellfarbigen Textilien übertragen wird und dadurch der ur¬ sprüngliche Farbton verändert wird. In gleicher Weise gilt dies auch für die Übertragung von optischen Aufhellern, mit denen Textilien häufig vom Hersteller her oder durch das Waschen mit aufhellerhalti- gen Waschmitteln ausgerüstet sind. Diese unerwünschte Übertragung von Farbstoffen bzw. optischen Aufhellern zu verhindern oder zu ver-
ringern ist Gegenstand zahlreicher Patentanmeldungen. Ein für die gewünschte Verhinderung der Verfärbung gut geeignetes Mittel ist Polyvinylpyrrolidon. Ein Beispiel für Patentanmeldungen, in denen Polyvinylpyrrolidon alleine oder in Kombination mit anderen Wirk¬ stoffen in Waschmitteln beschrieben wird, ist die DE-22 32 353-B2; ein Beispiel für eine Patentanmeldung, in der Polyvinylpyrrolidon in Kombination mit anderen Wirkstoffen beschrieben wird, ist die DE-35 19012-A1. Nach der Lehre der DE-22 32 353-B2 ist es wesent¬ lich, daß das Waschmittel mit einem Zusatz von Polyvinylpyrrolidon im wesentlichen von anionischen oberflächenaktiven Mittel frei ist. Auch die Anwesenheit von starken Elektrolyten stört häufig die Wir¬ kung von Polyvinylpyrrolidon, wie der DE-35 19012-A1 zu entnehmen ist. Bei der Formulierung von verfärbungsinhibierenden Waschmitteln ist daher darauf zu achten, daß allenfalls geringe Mengen von star¬ ken Elektrolyten und insbesondere nur geringe Mengen von anionischen Tensiden verwendet werden. Zur Erzielung einer ausreichenden Wasch¬ leistung werden daher vorzugsweise nichtionische Tenside in größeren Mengen als Waschmittelbestandteil eingesetzt.When washing colored textiles with undyed or light-colored textiles at the same time, it is frequently observed that dye is transferred from the more colored textiles to the undyed textiles or light-colored textiles and the original color tone is thereby changed. In the same way, this also applies to the transfer of optical brighteners with which textiles are often equipped by the manufacturer or by washing with detergents containing brighteners. To prevent or prevent this undesired transfer of dyes or optical brighteners wrestling is the subject of numerous patent applications. Polyvinylpyrrolidone is a suitable agent for the desired prevention of discoloration. An example of patent applications in which polyvinylpyrrolidone is described alone or in combination with other active substances in detergents is DE-22 32 353-B2; An example of a patent application in which polyvinylpyrrolidone is described in combination with other active ingredients is DE-35 19012-A1. According to the teaching of DE-22 32 353-B2, it is essential that the detergent with the addition of polyvinylpyrrolidone is essentially free of anionic surface-active agents. The presence of strong electrolytes also frequently interferes with the action of polyvinylpyrrolidone, as can be seen from DE-35 19012-A1. When formulating discoloration-inhibiting detergents, care must therefore be taken that at most small amounts of strong electrolytes and in particular only small amounts of anionic surfactants are used. To achieve a sufficient washing performance, nonionic surfactants are therefore preferably used in larger quantities as a detergent component.
Nichtionische Tenside haben bei Raumtemperatur eine flüssige bis pastöse Konsistenz, so daß es erforderlich ist, beim Einsatz größe¬ rer Mengen nichtionischer Tenside Menge und Art dieser Tenside so auszuwählen, daß die physikalischen Eigenschaften der Tenside, hier insbesondere die Rieselfähigkeit und das Einspülverhalten der pul¬ verförmigen Waschmittel nicht beeinträchtigt werden. Dies stellt bei der Formulierung pulverförmiger Waschmittel mitunter ein Problem dar, das durch den Zusatz von Polyvinylpyrrolidon in den Waschmit¬ teln noch verstärkt wird. So wurde beobachtet, daß pulverförmige Waschmittel, die ohne einen Gehalt an Polyvinylpyrrolidon einwand¬ freie Rieselfähigkeit und ein problemloses Ausspülverhalten hatten, nach Zusatz auch von nur geringen Mengen Polyvinylpyrrolidon sich in dieser Hinsicht schlechter verhielten.
Die Aufgabe der vorliegenden Erfindung bestand daher darin, durch Modifizierung des Herstellverfahrens den mit dem Zusatz von Polyvi¬ nylpyrrolidon in pulverförmigen Waschmitteln verbundenen Nachteil der Verschlechterung der Rieselfähigkeit und des Einspülverhaltens auszugleichen.Non-ionic surfactants have a liquid to pasty consistency at room temperature, so that when using larger amounts of non-ionic surfactants it is necessary to select the amount and type of these surfactants in such a way that the physical properties of the surfactants, in particular the flowability and flushing behavior of the pul¬ deformed detergents are not affected. This is sometimes a problem in the formulation of powder detergents, which is exacerbated by the addition of polyvinylpyrrolidone in the detergents. It was observed, for example, that powder detergents which, without a content of polyvinylpyrrolidone, had free-flowing properties and a problem-free rinsing behavior, behaved poorly in this regard even after adding only small amounts of polyvinylpyrrolidone. The object of the present invention was therefore to compensate for the disadvantage associated with the addition of polyvinylpyrrolidone in powder detergents of the deterioration in the flowability and the washing-in behavior by modifying the production process.
Die Lösung dieser Aufgabe besteht erfindungsgemäß darin, daß man bei der Herstellung des Waschmittels durch die üblicherweise angewendete Sprühtrocknung eines die Waschmittelbestandteile enthaltenden wäßri¬ gen Slurries das Polyvinylpyrrolidon vollständig oder teilweise in einem separaten Arbeitsschritt dem sprühgetrockneten Waschmittel zusetzt. Gegenstand der vorliegenden Erfindung ist daher ein Verfah¬ ren zur Herstellung von pulverförmigen Waschmitteln mit einem Gehalt an Polyvinylpyrrolidon, das dadurch gekennzeichnet ist, daß man das Polyvinylpyrrolidon vollständig oder teilweise in Form eines separa¬ ten Gemischs mit anderen pulverförmigen Waschmittelbestandteilen dem pulverförmigen Waschmittel, das die übrigen Waschmittelbestandteile enthält, beimischt.According to the invention, this object is achieved by adding all or part of the polyvinylpyrrolidone to the spray-dried detergent in a separate working step in the preparation of the detergent by the customary spray drying of an aqueous slurry containing the detergent constituents. The present invention therefore relates to a process for the production of powdered detergents containing polyvinylpyrrolidone, which is characterized in that the polyvinylpyrrolidone is wholly or partly in the form of a separate mixture with other powdered detergent constituents, the powdered detergent which is the contains other detergent ingredients.
Durch die geschilderte Verfahrensweise ist es möglich, Polyvinylpyr¬ rolidon in einer für die Verfärbungsinhibierung erforderlichen Menge Waschmitteln zuzusetzen, ohne deren Rieselfähigkeit oder Einspülver¬ halten zu verschlechtern. Die erfindungsgemäß herzustellenden Wasch¬ mittel enthalten üblicherweise 10 - 30 Gew.-% an Tensiden, davon 5 - 10 Gew.-% nichtionogene Tenside, 5 - 20 Gew.-% an synthetischen an¬ ionischen Tensiden und 1 - 5 Gew.-% an Fettsäure-Seifen. Daneben enthalten sie 40 - 60 Gew.-% anorganische Buildersalze wie z.B. Zeo- lith A, Natriumcarbonat, Natriumsulfat, Natriumsilikat oder Natriu - triphosphat neben geringeren Mengen üblicher Waschmitteladditive wie z.B. organische Co-Builder vom Typ der Polycarboxylate, Carboxyme- thylcellulose, wasserlösliche Komplexbildner, Antischaummittel , Enzyme und Duftstoffe. Der Gehalt an Polyvinylpyrrolidon beträgt bevorzugt 0,5 - 5 Gew.-% des Waschmittels.
Das separate Gemisch, im folgenden PVP-Konzentrat genannt, enthält hohe Mengen von PVP zusammen mit überwiegend anorganischen Trägerbe¬ standteilen. Der Gehalt an PVP in diesem PVP-Konzentrat kann 10 - 50 Gew.-%, bevorzugt 20 - 40 Gew.-%, betragen. Bevorzugt enthalten sol¬ che PVP-Konzentrate 20 - 40 Gew.-% Polyvinylpyrrolidon neben 40 - 80 Gew.-% anorganischen Trägersalzen und kleineren Mengen an Wasser. Die Herstellung dieser separaten, hoch PVP-haltigen Gemische erfolgt bevorzugt ebenfalls durch Sprühtrocknung eines wäßrigen Slurry. Es kann aber auch nach anderen üblichen Granulierverfahren, z.B. durch Sprühmisch- oder Extrusionsverfahren hergestellt werden.The procedure described makes it possible to add polyvinylpyrrolidone in an amount of detergents required for the discoloration inhibition without impairing their free-flowing properties or detergent retention. The detergents to be produced according to the invention usually contain 10-30% by weight of surfactants, of which 5-10% by weight nonionic surfactants, 5-20% by weight of synthetic anionic surfactants and 1-5% by weight. of fatty acid soaps. In addition, they contain 40-60% by weight of inorganic builder salts such as, for example, zeolite A, sodium carbonate, sodium sulfate, sodium silicate or sodium triphosphate, in addition to smaller amounts of conventional detergent additives, such as, for example, organic co-builders of the polycarboxylate type, carboxymethyl cellulose and water-soluble complexing agents , Anti-foaming agents, enzymes and fragrances. The polyvinylpyrrolidone content is preferably 0.5-5% by weight of the detergent. The separate mixture, hereinafter called PVP concentrate, contains large amounts of PVP together with predominantly inorganic carrier components. The PVP content in this PVP concentrate can be 10-50% by weight, preferably 20-40% by weight. Such PVP concentrates preferably contain 20-40% by weight of polyvinylpyrrolidone in addition to 40-80% by weight of inorganic carrier salts and smaller amounts of water. These separate, high PVP-containing mixtures are preferably also produced by spray drying an aqueous slurry. However, it can also be produced by other conventional granulation processes, for example by spray mixing or extrusion processes.
Ein weiterer Erfindungsgegenstand ist daher ein pulverför iges PVP- Konzentrat, enthaltend PVP und anorganische Trägersalze, das 20 - 40 Gew.-% Polyvinylpyrrolidon und 40 - 80 Gew.-% anorganischer Träger¬ salze enthält. Die anorganischen Trägersalze bestehen dabei vorzugs¬ weise ganz oder zum überwiegenden Teil aus Waschmittelbuildern, be¬ vorzugt aus wasserunlöslichen Zeolith-Ionenaustauschern, insbesonde¬ re vom Typ Zeolith A. Das PVP-Konzentrat kann auch kleinere Mengen an Tensiden und bis zu 20 Gew.-% an Wasser enthalten.A further subject of the invention is therefore a pulverulent PVP concentrate containing PVP and inorganic carrier salts, which contains 20-40% by weight polyvinylpyrrolidone and 40-80% by weight inorganic carrier salts. The inorganic carrier salts preferably consist entirely or predominantly of detergent builders, preferably of water-insoluble zeolite ion exchangers, in particular of the zeolite A type. The PVP concentrate can also contain smaller amounts of surfactants and up to 20% by weight. % contain water.
Ein weiterer Gegenstand der Erfindung ist ein Waschmittel, bestehend aus zwei granulären Komponenten unterschiedlicher Zusammensetzung, wobei die erste granuläre Komponente kein Polyvinylpyrrolidon oder nicht mehr als eine für die Rieselfähigkeit unschädliche Menge bis 2,5 Gew.-% Polyvinylpyrrolidon neben üblichen Waschmittelkomponenten enthält und die zweite granuläre Komponente 10 - 50 Gew.-% Polyvi¬ nylpyrrolidon und einen anorganischen Träger, bevorzugt ein Wasch- mittel-Buildersalz, enthält.Another object of the invention is a detergent consisting of two granular components of different compositions, the first granular component containing no polyvinylpyrrolidone or no more than an amount of up to 2.5% by weight of polyvinylpyrrolidone which is not harmful to the flow properties, and the second one granular component 10-50 wt .-% polyvinyl pyrrolidone and an inorganic carrier, preferably a detergent builder salt, contains.
Sowohl die erste granuläre Komponente als auch die zweite, hoch PVP- haltige Komponente können durch Sprühtrocknung entsprechender Slur-
ries oder durch andere bekannte Granulierverfahren hergestellt wer¬ den. Bevorzugt ist jedoch die Herstellung durch Sprühtrocknung.Both the first granular component and the second, high PVP-containing component can be spray dried by appropriate slurry Ries or be produced by other known granulation. However, production by spray drying is preferred.
Bei der erfindungsgemäßen Verfahrensweise setzt man einen Slurry an, der entweder kein Polyvinylpyrrolidon oder nur einen für die Rie¬ selfähigkeit unschädlichen Anteil des in der Rezeptur vorgesehenen Polyvinylpyrrolidons sowie weitere Bestandteile der Rezeptur enthält und versprüht diesen Slurry auf übliche Weise, wobei man in der Re¬ gel wegen des geringeren Gehalts an Feststoffen auf einen Teil des Wassers des Slurries verzichten kann. Das im Slurry nicht enthaltene Polyvinylpyrrolidon wird zusammen mit den ebenfalls nicht in dem Slurry enthaltenen weiteren anorganischen Waschmittelbestandteilen seinerseits zu einem zweiten wäßrigen Slurry verarbeitet und durch Sprühtrocknen in einen pulverförmigen Zustand überführt.In the procedure according to the invention, a slurry is prepared which either contains no polyvinylpyrrolidone or only a portion of the polyvinylpyrrolidone provided in the recipe which is not harmful to the flowability and other constituents of the recipe, and this slurry is sprayed in the customary manner, gel can dispense with part of the water of the slurries due to the lower content of solids. The polyvinylpyrrolidone not contained in the slurry, together with the other inorganic detergent constituents also not contained in the slurry, is in turn processed into a second aqueous slurry and converted into a powdery state by spray drying.
Das Mischungsverhältnis richtet sich dabei nach dem bereits in der ersten granulären Komponente enthaltenen Menge an Polyvinylpyrro¬ lidon und dem gewünschten PVP-Gehalt des Endproduktes, der bei 0,5 - 5 Gew.-%, bevorzugt bei 3 - 5 Gew.-%, liegen sollte. Bevorzugt wird wenigstens die Hälfte des insgesamt im fertigen Waschmittel enthal¬ tenen PVP in Form eines separaten Gemischs (PVP-Konzentrat) zuge¬ setzt. Noch mehr bevorzugt ist es aber, wenigstens 75 Gew.-% des PVP in Form des PVP-Konzentrats dem Waschmittel beizumischen.
The mixing ratio depends on the amount of polyvinylpyrrolidone already contained in the first granular component and the desired PVP content of the end product, which is 0.5-5% by weight, preferably 3-5% by weight. should be. At least half of the total PVP contained in the finished detergent is preferably added in the form of a separate mixture (PVP concentrate). However, it is even more preferred to add at least 75% by weight of the PVP to the detergent in the form of the PVP concentrate.
B e i s p i e l eB e i s p i e l e
Beispiel 1example 1
Durch Sprühtrocknung wurde ein Waschmittel-Vorprodukt hergestellt, bei dem nur ein Teil des in der Rezeptur insgesamt vorgesehenen Po¬ lyvinylpyrrolidon (PVP) enthalten ist. Der Rest PVP wird in einem Mischvorgang in Form eines ebenfalls durch Sprühtrocknung herge¬ stellten PVP-reichen Pulvers hinzugefügt.A preliminary detergent product was produced by spray drying, in which only a part of the total polyvinylpyrrolidone (PVP) provided in the recipe is contained. The remainder of the PVP is added in a mixing process in the form of a PVP-rich powder likewise produced by spray drying.
Das Waschmittel-Vorprodukt enthält:The preliminary detergent product contains:
12,2 Gew.-% Alkylbenzolsulfonat-Na12.2% by weight of alkylbenzenesulfonate Na
8.2 Gew.-% Fettalkoholethoxylat 2,4 Gew.-% Seife8.2% by weight of fatty alcohol ethoxylate 2.4% by weight of soap
20,8 Gew.-% Soda 33,2 Gew.-% Zeolith A20.8% by weight of soda 33.2% by weight of zeolite A
2.3 Gew.-% PVP2.3% by weight of PVP
Rest Wasser und sonstige Bestandteile in geringenRest of water and other ingredients in small
Mengenamounts
Diesem Waschmittel-Vorprodukt wurden 3,3 Gew.-% eines sprühgetrock¬ neten Pulvers beigemischt, das die folgenden Bestandteile enthielt:3.3% by weight of a spray-dried powder which contained the following constituents were mixed into this preliminary detergent product:
PVP-KonzentratPVP concentrate
30,0 Gew.-% PVP30.0 wt% PVP
53,0 Gew.-% Zeolith A53.0% by weight of zeolite A
1.4 Gew.-% Fettalkoholethoxylat 15,2 Gew.-% Wasser1.4% by weight of fatty alcohol ethoxylate 15.2% by weight of water
0,3 Gew.-% Natronlauge
Zusätzlich wurden diesem Gemisch noch geringe Mengen weiterer Wasch¬ mittel-Bestandteile wie Duftstoffe, Schaumregulatoren und Enzyme zu¬ gesetzt.0.3% by weight sodium hydroxide solution In addition, small amounts of further detergent components such as fragrances, foam regulators and enzymes were added to this mixture.
Das so erhaltene Fertig-Produkt hatte ein Schüttgewicht von 410 g pro Liter und ein wesentlich besseres Riesel-Verhalten (nach dem sogenannten "Paket-Test") und ein deutlich verbessertes Einspülver¬ halten (nach dem sogenannten "Einspül-Test") als ein sonst gleich zusammengesetztes Waschmittel, dessen gesamter Anteil an PVP in dem Waschmittel-Vorprodukt enthalten war. Dieser Befund wird durch ein Waschmittel bestätigt, das die gleiche Zusammensetzung hat, bei dem aber die gesamte PVP-Menge dem Waschmittel-Vorprodukt in einem Mischvorgang hinzugefügt wurde (Beispiel V3).The finished product thus obtained had a bulk density of 410 g per liter and a much better trickle behavior (according to the so-called "package test") and a significantly improved washing-in behavior (according to the so-called "washing-in test") than one otherwise identical detergent, the entire proportion of PVP of which was contained in the detergent intermediate. This finding is confirmed by a detergent which has the same composition, but in which the entire amount of PVP has been added to the detergent precursor in one mixing operation (Example V3).
Beispiel 2Example 2
Durch Sprühtrocknung wurde ein Waschmittel-Vorprodukt hergestellt, das kein PVP enthielt.A preliminary detergent product which did not contain any PVP was prepared by spray drying.
Waschmitte1-VorproduktWaschmitte1 intermediate
13,5 Gew.-% Alkylbenzolsulfonat13.5% by weight alkylbenzenesulfonate
2.7 Gew.-% Talgfettalkoholethoxylat2.7% by weight of tallow fatty alcohol ethoxylate
2.8 Gew.-% Seife 22,9 Gew.-% Soda 32,0 Gew.-% Zeolith A2.8% by weight of soap 22.9% by weight of soda 32.0% by weight of zeolite A
2,7 Gew.-% Wasserglas2.7% by weight water glass
9,1 Gew.-% Polyacrylsäure-Maleinsäure-Copoly er, Na 0,7 Gew.-% Carboxymethylcellulose Rest Wasser
Zu 79 Gew.-% Waschmittel-Vorprodukt wird in einem Mischprozeß 6 Gew.-% Fettalkoholethoxylat, 4 Gew.-% eines Schauminhibitor-Com- pounds, 0,7 Gew.-% eines Enzympräparats, 0,3 Gew.-% Duftstoff und 10 Gew.-% des PVP-Konzentrats gemäß Beispiel 1 zugesetzt.9.1% by weight of polyacrylic acid-maleic acid copoly er, Na 0.7% by weight of carboxymethyl cellulose balance water 6% by weight of fatty alcohol ethoxylate, 4% by weight of a foam inhibitor compound, 0.7% by weight of an enzyme preparation, 0.3% by weight of fragrance are added to 79% by weight of preliminary detergent product in a mixing process and 10% by weight of the PVP concentrate according to Example 1 were added.
Der "Paket-Test" wird wie folgt durchgeführt:The "package test" is carried out as follows:
Ein Waschmittel-Normpaket, das mit Waschpulver gefüllt und geöffnet ist, wird durch eine Apparatur um bestimmte Winkel gekippt und die Art und Menge des Pulverauslaufs, gegebenenfalls nach Rütteln des Pakets mit den Noten 1 (sehr gut rieselfähig) bis 10 (sehr schlecht rieselfähig) bewertet.A standard detergent package, which is filled with washing powder and opened, is tilted through a device by certain angles and the type and amount of powder discharge, if necessary after shaking the package with the marks 1 (very good flowability) to 10 (very poorly flowable) rated.
Der "Einspül-Test" wurde wie folgt durchgeführt:The "induction test" was carried out as follows:
Eine handelsübliche Waschmaschinen-Einspülvorrichtung, die hinsicht¬ lich ihres EinspülVerhaltens als besonders problematisch gilt, wird unter definierten Einfüllbedingungen mit 100 g Waschmittel beschickt und mit maximal 10 Liter Wasser durchspült. Danach wird bewertet, mit welcher Wassermenge das Waschpulver vollständig aus der Einspül¬ vorrichtung ausgespült wird bzw. wie groß der Waschmittelrückstand in der Einspülvorrichtung nach dem Durchfluß von 10 Liter Wasser ist.A commercially available washing machine dispenser, which is particularly problematic with regard to its dispensing behavior, is charged with 100 g of detergent under defined filling conditions and flushed with a maximum of 10 liters of water. The amount of water in which the washing powder is completely rinsed out of the induction device or how large the detergent residue in the induction device is after the flow of 10 liters of water is then assessed.
Testergebnisse: Beispiele V3Test results: Examples V3
Vorprodukt Beispiel 1 mit 3,0 Gew.-% PVPIntermediate Example 1 with 3.0 wt .-% PVP
Paket-Test Einspül-Test 2 1 Wasser 2 1 Wasser Rückstand 8,3 g rückstands¬ rückstands¬ frei frei
Package test induction test 2 1 water 2 1 water residue 8.3 g residue-free
Claims
1. Verfahren zur Herstellung von pulverförmigen Waschmitteln mit einem Gehalt an Polyvinylpyrrolidon, dadurch gekennzeichnet, daß man das Polyvinylpyrrolidon vollständig oder teilweise in Form eines separaten Gemischs mit anderen pulverförmigen Wasch¬ mittelbestandteilen dem pulverförmigen Waschmittel, das die übrigen Waschmittelbestandteile enthält, beimischt.1. A process for the preparation of powdered detergents containing polyvinylpyrrolidone, characterized in that the polyvinylpyrrolidone is wholly or partly mixed in the form of a separate mixture with other powdered detergent constituents in the powdered detergent which contains the other detergent constituents.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das pul- verför ige Waschmittel 0,5 - 5 Gew.-% Polyvinylpyrrolidon ent¬ hält und das Polyvinylpyrrolidon ganz oder teilweise in Form eines pulverförmigen PVP-Konzentrats beigemischt wird, das 10 - 50 Gew.-% Polyvinylpyrrolidon auf einem anorganischen Träger enthält.2. The method according to claim 1, characterized in that the powder-form detergent contains 0.5-5% by weight of polyvinylpyrrolidone and the polyvinylpyrrolidone is wholly or partly mixed in the form of a powdered PVP concentrate which is 10-50 Contains wt .-% polyvinylpyrrolidone on an inorganic carrier.
3. Pulverförmiges PVP-Konzentrat zur Verwendung in einem Verfahren gemäß Anspruch 1 oder 2, enthaltend PVP und anorganische Träger¬ salze, dadurch gekennzeichnet, daß es 20 - 40 Gew.-% Polyvinyl¬ pyrrolidon und 40 - 80 Gew.-% anorganische Trägersalze enthält.3. Powdery PVP concentrate for use in a process according to claim 1 or 2, containing PVP and inorganic Träger¬ salts, characterized in that it contains 20 - 40 wt .-% polyvinyl pyrrolidone and 40 - 80 wt .-% inorganic carrier salts contains.
4. Pulverförmiges PVP-Konzentrat, dadurch gekennzeichnet, daß die anorganischen Trägersalze aus Waschmittel-Buildern, bevorzugt aus Zeolith A, bestehen.4. Powdery PVP concentrate, characterized in that the inorganic carrier salts consist of detergent builders, preferably of zeolite A.
5. Waschmittel, bestehend aus zwei granulären Komponenten unter¬ schiedlicher Zusammensetzung, dadurch gekennzeichnet, daß die erste granuläre Komponente kein Polyvinylpyrrolidon oder nicht mehr als eine für die Rieselfähigkeit unschädliche Menge bis 2,5 Gew.-% PVP neben üblichen Waschmittelkomponenten enthält und ,die zweite granuläre Komponente 10 - 50 Gew.-% Polyvinylpyrrolidon und einen anorganischen Träger, bevorzugt ein Waschmittel-Buil- dersalz, enthält.5. Detergent, consisting of two granular components of different composition, characterized in that the first granular component contains no polyvinylpyrrolidone or not more than an amount of 2.5% by weight of PVP which is harmless to the free-flowing properties in addition to conventional detergent components and second granular component contains 10-50% by weight of polyvinylpyrrolidone and an inorganic carrier, preferably a detergent builder salt.
6. Pulverförmiges Waschmittel nach Anspruch 5, dadurch gekennzeich¬ net, daß es 10 - 30 Gew.-% Tenside und zwar 5 - 20 Gew.-% nicht¬ ionische Tenside, 5 - 20 Gew.-% synthetische anionische Tenside und 1 - 5 Gew.-% Fettsäure-Seifen sowie 40 - 60 Gew.-% anorga¬ nische Buildersalze und 0,5 - 5 Gew.-% Polyvinylpyrrolidon ent¬ hält. 6. Powdered detergent according to claim 5, characterized gekennzeich¬ net that it 10-30 wt .-% surfactants, namely 5-20 wt .-% non-ionic surfactants, 5-20 wt .-% synthetic anionic surfactants and 1- Contains 5% by weight of fatty acid soaps and 40-60% by weight of inorganic builder salts and 0.5-5% by weight of polyvinylpyrrolidone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP94902706A EP0674702A1 (en) | 1992-12-16 | 1993-12-07 | Method of producing washing agents in powder form |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP4242482.8 | 1992-12-16 | ||
| DE19924242482 DE4242482A1 (en) | 1992-12-16 | 1992-12-16 | Process for the preparation of powdered detergents |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1994013775A1 true WO1994013775A1 (en) | 1994-06-23 |
Family
ID=6475440
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP1993/003443 WO1994013775A1 (en) | 1992-12-16 | 1993-12-07 | Method of producing washing agents in powder form |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0674702A1 (en) |
| DE (1) | DE4242482A1 (en) |
| WO (1) | WO1994013775A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0719856A1 (en) * | 1994-12-29 | 1996-07-03 | The Procter & Gamble Company | Softening-through-the-wash laundry detergent compositions |
| EP0800570A1 (en) * | 1994-12-29 | 1997-10-15 | The Procter & Gamble Company | Laundry detergent composition comprising substantially water-insoluble polymeric dye transfer inhibiting agent |
| WO2000025906A1 (en) * | 1998-10-29 | 2000-05-11 | Henkel Kommanditgesellschaft Auf Aktien | Polymer granules produced by fluidized bed granulation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0075818A2 (en) * | 1981-09-28 | 1983-04-06 | BASF Aktiengesellschaft | Granular bleach activator |
| EP0114308A1 (en) * | 1982-12-24 | 1984-08-01 | Henkel Kommanditgesellschaft auf Aktien | Spray-dried multi-component washing agent |
| EP0327927A2 (en) * | 1988-02-06 | 1989-08-16 | Henkel Kommanditgesellschaft auf Aktien | Detergent additive |
| EP0421664A2 (en) * | 1989-10-02 | 1991-04-10 | Rohm And Haas Company | Polymer-containing granulates |
-
1992
- 1992-12-16 DE DE19924242482 patent/DE4242482A1/en not_active Withdrawn
-
1993
- 1993-12-07 WO PCT/EP1993/003443 patent/WO1994013775A1/en not_active Application Discontinuation
- 1993-12-07 EP EP94902706A patent/EP0674702A1/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0075818A2 (en) * | 1981-09-28 | 1983-04-06 | BASF Aktiengesellschaft | Granular bleach activator |
| EP0114308A1 (en) * | 1982-12-24 | 1984-08-01 | Henkel Kommanditgesellschaft auf Aktien | Spray-dried multi-component washing agent |
| EP0327927A2 (en) * | 1988-02-06 | 1989-08-16 | Henkel Kommanditgesellschaft auf Aktien | Detergent additive |
| EP0421664A2 (en) * | 1989-10-02 | 1991-04-10 | Rohm And Haas Company | Polymer-containing granulates |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0719856A1 (en) * | 1994-12-29 | 1996-07-03 | The Procter & Gamble Company | Softening-through-the-wash laundry detergent compositions |
| EP0800570A1 (en) * | 1994-12-29 | 1997-10-15 | The Procter & Gamble Company | Laundry detergent composition comprising substantially water-insoluble polymeric dye transfer inhibiting agent |
| EP0800570A4 (en) * | 1994-12-29 | 1998-01-28 | Procter & Gamble | Laundry detergent composition comprising substantially water-insoluble polymeric dye transfer inhibiting agent |
| WO2000025906A1 (en) * | 1998-10-29 | 2000-05-11 | Henkel Kommanditgesellschaft Auf Aktien | Polymer granules produced by fluidized bed granulation |
| US6841614B1 (en) | 1998-10-29 | 2005-01-11 | Henkel Kommanditgesellschaft Auf Aktien | Polymer granules produced by fluidized bed granulation |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0674702A1 (en) | 1995-10-04 |
| DE4242482A1 (en) | 1994-06-23 |
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