EP1572853A1 - Method for the production of suspensions comprising bleaching agents - Google Patents

Method for the production of suspensions comprising bleaching agents

Info

Publication number
EP1572853A1
EP1572853A1 EP03782278A EP03782278A EP1572853A1 EP 1572853 A1 EP1572853 A1 EP 1572853A1 EP 03782278 A EP03782278 A EP 03782278A EP 03782278 A EP03782278 A EP 03782278A EP 1572853 A1 EP1572853 A1 EP 1572853A1
Authority
EP
European Patent Office
Prior art keywords
phthalimidoperoxyhexanoic acid
grinding
microns
production
phthalimidoperoxyhexanoic
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.)
Granted
Application number
EP03782278A
Other languages
German (de)
French (fr)
Other versions
EP1572853B1 (en
Inventor
Matthias Sunder
Christian Schoth
Theodor Völkel
Dieter Nickel
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP1572853A1 publication Critical patent/EP1572853A1/en
Application granted granted Critical
Publication of EP1572853B1 publication Critical patent/EP1572853B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2006—Monohydric alcohols
    • C11D3/201—Monohydric alcohols linear
    • C11D3/2013—Monohydric alcohols linear fatty or with at least 8 carbon atoms in the alkyl chain
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
    • 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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2006—Monohydric alcohols
    • C11D3/201—Monohydric alcohols linear
    • 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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2041—Dihydric alcohols
    • C11D3/2044—Dihydric alcohols linear
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3945—Organic per-compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3947—Liquid compositions
    • 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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2003—Alcohols; Phenols
    • C11D3/2065—Polyhydric alcohols

Definitions

  • the invention relates to a process for the production of flowable phthalimidoperoxyhexanoic acid containing suspension and their use for the production of liquid detergents or cleaning agents.
  • Phthalimidoperoxyhexanoic acid is known, for example, from European patents EP 0 349 940 and EP 0 325 328. Their use in liquid detergents or cleaning agents is described, for example, in European patent applications EP 0 442 549, EP 0 477 190, EP 0 484 095 or EP 1 010 750 or in international patent applications WO 00/27960, WO 00/27971 or WO 00 / 29536 known. In the course of its production from aqueous systems, it is usually obtained in relatively large crystals which can bake together and which is commercially available as a so-called "wet cake".
  • the grinding can be carried out in conventional wet grinding devices.
  • the grinding is preferably carried out using a toothed disc or a ball mill.
  • the grinding is preferably carried out until the average particle size (d 5 o, determined with a laser diffraction spectrometer) of the phthalimidoperoxyhexanoic acid is in the range of 10 .mu.m to 40 .mu.m, in particular from 12 microns to 30 microns is located.
  • the grinding is carried out until the size of at least 90% of the particles (d 9 o, also determinable with a laser diffraction spectrometer) of the phthalimidoperoxyhexanoic acid is below 80 ⁇ m, in particular below 50 ⁇ m.
  • This can be the "wet cake” already mentioned, which can easily contain particles of up to 1 mm, or else particles produced from it by drying and optionally granulation. Any adhering water does not have to be removed further, but can also be introduced into the alcoholic slurry, in which case the alcohol component of the alcoholic slurry must be correspondingly water-miscible.
  • the alcohol component of the alcoholic slurry is liquid at the grinding temperature and that the phthalimidoperoxyhexanoic acid is essentially insoluble in it.
  • Substantially insoluble should be understood to mean that the phthalimidoperoxyhexanoic acid dissolves in the alcohol component at most 10 times better, preferably at most 2 times better and particularly preferably not better than in water.
  • the grinding temperature is preferably at room temperature, but it can also be higher due to the energy input during the grinding process, but should remain below the boiling point of the alcohol at normal pressure.
  • the Ci to C 3 alcohols with up to 3 OH groups and mixtures thereof are particularly suitable.
  • the alcohol is preferably selected from the group comprising ethanol, propanol, isopropanol, ethanediol, 1,2-propanediol, glycerol and mixtures thereof.
  • the content of phthalimidoperoxyhexanoic acid in the alcoholic slurry is preferably in the range from 10% by weight to 90% by weight, in particular from 50% by weight to 85% by weight.
  • Flowable, non-sedimenting suspensions of phthalimidoperoxyhexanoic acid in the alcohol component are obtained in the manner described.
  • Flowable is understood to mean that it flows out at least partially from an open vessel with a corresponding inclination under the influence of gravity and can be easily pumped as part of its industrial processing.
  • a suspension obtainable by the process according to the invention is preferably used for the production of liquid washing or cleaning agents.
  • a bleach-containing liquid washing or cleaning agent which contains a suspension obtainable by the process according to the invention can be aqueous or essentially anhydrous and, in addition to the suspension obtainable by the process according to the invention, can contain all the other usual ingredients of such compositions, provided that they are not unacceptably negative of phthalimidoperoxyhexanoic acid interact.
  • Such an agent preferably has an acidic pH, which is in particular in the range from pH 2.5 to pH 6.5, preferably in the range from pH 3.5 to pH 5.5, and is optionally adjusted by the presence of acids which are compatible with the system may have been.
  • the phthalimidoperoxyhexanoic acid also remains sedimentation-stable in the liquid detergents or cleaning agents by the process according to the invention.
  • ingredients of such detergents or cleaning agents can also be milled in the same alcoholic slurry with the phthalimidoperoxyhexanoic acid if they are in the alcoholic component Slurry the presence of the phthalimidoperoxyhexanoic acid and grind to the same grain size as the phthalimidoperoxyhexanoic acid.
  • Phthalimidoperoxyhexanoic acid granules (Eureco®, manufacturer Ausimont) were slurried in isopropyl alcohol. The 70% by weight slurry was sheared intensively in a grinding bowl by means of a toothed disk at a peripheral speed of 10 m / s for 15 minutes. .

Abstract

A process for the production of a flowable suspension containing phthalimidoperoxyhexanoic acid by combining phthalimidoperoxyhexanoic acid in granular form with a liquid alcohol and grinding the combination to form a flowable suspension of the phthalimidoperoxyhexanoic acid in the alcohol.

Description

Verfahren zur Herstellung von bleichmittelhaltigen Suspensionen Process for the production of suspensions containing bleach
Die Erfindung betrifft ein Verfahren zur Herstellung von fließfähigen Phthalimidoperoxyhexansäure enthaltenden Suspension und deren Verwendung zur Herstellung flüssiger Wasch- oder Reinigungsmittel.The invention relates to a process for the production of flowable phthalimidoperoxyhexanoic acid containing suspension and their use for the production of liquid detergents or cleaning agents.
Phthalimidoperoxyhexansäure ist beispielsweise aus den europäischen Patenten EP 0 349 940 und EP 0 325 328 bekannt. Ihr Einsatz in flüssigen Wasch- oder Reinigungsmitteln ist beispielsweise in den europäischen Patentanmeldungen EP 0 442 549, EP 0 477 190, EP 0 484 095 oder EP 1 010 750 oder den internationalen Patentanmeldungen WO 00/27960, WO 00/27971 oder WO 00/29536 bekannt. Sie fällt im Rahmen ihrer Herstellung aus wäßrigen Systemen normalerweise in relativ großen Kristallen an, die miteinander verbacken können und als sogenannter "wet cake" kommerziell verfügbar ist. Die physikalisch stabile Einarbeitung der Phthalimidoperoxyhexansäure in flüssige Mittel macht zum einen wegen der Größe und damit Schwere der Teilchen und zum zweiten wegen der Breite der Teilchengrößenverteilung Schwierigkeiten. In der internationalen Patentanmeldung WO 00/27969 wird ein zweistufiges Mahlverfahren für den aus der Herstellung der Phthalimidoperoxyhexansäure resultierenden "wet cake" vorgeschlagen, um zu durchschnittlichen Teilchengrößen unter 100 μm zu kommen. Die europäische Patentanmeldung EP 0 890 635 empfiehlt, Phthalimidoperoxyhexansäure in angesäuertem Wasser, das auch Entschäumer, Aniontensid, nichtionisches Tensid, Wasserstoffperoxid und/oder anorganische Salze enthalten kann, zu vermählen. In der europäischen Patentanmeldung EP 1 074 607 wird vorgeschlagen, wasserbasierte Dispersionen der Phthalimidoperoxyhexansäure durch die Zugabe bestimmter Polymere zu stabilisieren.Phthalimidoperoxyhexanoic acid is known, for example, from European patents EP 0 349 940 and EP 0 325 328. Their use in liquid detergents or cleaning agents is described, for example, in European patent applications EP 0 442 549, EP 0 477 190, EP 0 484 095 or EP 1 010 750 or in international patent applications WO 00/27960, WO 00/27971 or WO 00 / 29536 known. In the course of its production from aqueous systems, it is usually obtained in relatively large crystals which can bake together and which is commercially available as a so-called "wet cake". The physically stable incorporation of phthalimidoperoxyhexanoic acid into liquid medium makes difficulties on the one hand because of the size and thus the weight of the particles and on the other hand because of the breadth of the particle size distribution. International patent application WO 00/27969 proposes a two-stage grinding process for the "wet cake" resulting from the production of phthalimidoperoxyhexanoic acid in order to achieve average particle sizes below 100 μm. European patent application EP 0 890 635 recommends grinding phthalimidoperoxyhexanoic acid in acidified water, which can also contain defoamers, anionic surfactants, nonionic surfactants, hydrogen peroxide and / or inorganic salts. In European patent application EP 1 074 607 it is proposed to stabilize water-based dispersions of phthalimidoperoxyhexanoic acid by adding certain polymers.
Überraschenderweise wurde gefunden, daß man auf einfacherem Wege sehr stabile flüssige Suspension von Phthalimidoperoxyhexansäure erhalten kann, wenn man nicht in Wasser, sondern in bestimmten organischen Flüssigkeiten arbeitet. Gegenstand des Patentes ist ein Verfahren zur Herstellung einer fließfähigen Phthalimidoperoxyhexansäure enthaltenden Suspension durch Vermahlung von Phthalimidoperoxyhexansäure in alkoholischer Aufschlämmung.Surprisingly, it has been found that very stable liquid suspensions of phthalimidoperoxyhexanoic acid can be obtained in a simpler way if one does not work in water but in certain organic liquids. The subject of the patent is a process for the production of a suspension containing flowable phthalimidoperoxyhexanoic acid by grinding phthalimidoperoxyhexanoic acid in an alcoholic slurry.
Die Vermahlung kann dabei in üblichen Naßmahlvorrichtungen vorgenommen werden. Bevorzugt wird die Vermahlung mit Hilfe einer Zahnscheibe oder einer Kugelmühle durchgeführt.The grinding can be carried out in conventional wet grinding devices. The grinding is preferably carried out using a toothed disc or a ball mill.
Die Vermahlung wird vorzugsweise so lange vorgenommen, bis die mittlere Teilchengröße (d5o, bestimmbar mit einem Laserbeugungsspektrometer) der Phthalimidoperoxyhexansäure im Bereich von 10 μm bis 40 μm, insbesondere von 12 μm bis 30 μm liegt. In einer bevorzugten Ausführungsform der Erfindung nimmt man die Vermahlung so lange vor, bis die Größe von mindestens 90 % der Teilchen (d9o, bestimmbar ebenfalls mit einem Laserbeugungsspektrometer) der Phthalimidoperoxyhexansäure unter 80 μm, insbesondere unter 50 μm liegt. Bei einem Mahlverfahren versteht sich von selbst, daß man von einer gröberen Qualität ausgeht. Bei dieser kann es sich um den bereits genannten "wet cake" handeln, der ohne weiteres Teilchen bis zu 1 mm enthalten kann, oder auch um durch Trocknen und gegebenenfalls Granulation aus diesem erzeugte Partikel. Eventuell anhaftendes Wasser muß nicht weiter entfernt werden, sondern kann mit in die alkoholischer Aufschlämmung eingebracht werden, wobei für diesen Fall die Alkoholkomponente der alkoholischen Aufschlämmung entsprechend wassermischbar sein muß.The grinding is preferably carried out until the average particle size (d 5 o, determined with a laser diffraction spectrometer) of the phthalimidoperoxyhexanoic acid is in the range of 10 .mu.m to 40 .mu.m, in particular from 12 microns to 30 microns is located. In a preferred embodiment of the invention, the grinding is carried out until the size of at least 90% of the particles (d 9 o, also determinable with a laser diffraction spectrometer) of the phthalimidoperoxyhexanoic acid is below 80 μm, in particular below 50 μm. With a grinding process it goes without saying that a coarser quality is assumed. This can be the "wet cake" already mentioned, which can easily contain particles of up to 1 mm, or else particles produced from it by drying and optionally granulation. Any adhering water does not have to be removed further, but can also be introduced into the alcoholic slurry, in which case the alcohol component of the alcoholic slurry must be correspondingly water-miscible.
Wesentlich ist, daß die Alkoholkomponente der alkoholischen Aufschlämmung bei der Mahltemperatur flüssig ist und die Phthalimidoperoxyhexansäure dabei in ihr im wesentlichen unlöslich ist. Unter im wesentlichen unlöslich soll dabei verstanden werden, daß sich die Phthalimidoperoxyhexansäure in der Alkoholkomponente höchstens 10 mal besser, vorzugsweise höchstens 2 mal besser und besonders bevorzugt nicht besser als in Wasser löst. Die Mahltemperatur liegt vorzugsweise bei Raumtemperatur, sie kann allerdings wegen des Energieeintrags beim Mahlvorgang auch höher liegen, sollte jedoch unterhalb des Siedepunkts des Alkohols bei Normaldruck bleiben. In Frage kommen insbesondere die Ci- bis C3 -Alkohole mit bis zu 3 OH-Gruppen und deren Mischungen. Vorzugsweise wird der Alkohol ausgewählt aus der Gruppe umfassend Ethanol, Propanol, Isopropanol, Ethandiol, 1,2-Propandiol, Glycerin und deren Mischungen.It is essential that the alcohol component of the alcoholic slurry is liquid at the grinding temperature and that the phthalimidoperoxyhexanoic acid is essentially insoluble in it. Substantially insoluble should be understood to mean that the phthalimidoperoxyhexanoic acid dissolves in the alcohol component at most 10 times better, preferably at most 2 times better and particularly preferably not better than in water. The grinding temperature is preferably at room temperature, but it can also be higher due to the energy input during the grinding process, but should remain below the boiling point of the alcohol at normal pressure. The Ci to C 3 alcohols with up to 3 OH groups and mixtures thereof are particularly suitable. The alcohol is preferably selected from the group comprising ethanol, propanol, isopropanol, ethanediol, 1,2-propanediol, glycerol and mixtures thereof.
Der Gehalt an Phthalimidoperoxyhexansäure in der alkoholischen Aufschlämmung liegt vorzugsweise im Bereich von 10 Gew.-% bis 90 Gew.-%, insbesondere von 50 Gew.- % bis 85 Gew.-%.The content of phthalimidoperoxyhexanoic acid in the alcoholic slurry is preferably in the range from 10% by weight to 90% by weight, in particular from 50% by weight to 85% by weight.
Auf die beschriebene Weise erhält man fließfähige, nicht sedimentierende Suspensionen der Phthalimidoperoxyhexansäure in der Alkoholkomponente. Unter fließfähig wird dabei verstanden, daß sie aus einem offenen Gefäß bei entsprechender Neigung unter Einwirkung der Schwerkraft wenigstens anteilsweise ausfließt und im Rahmen ihrer industriellen Weiterverarbeitung ohne weiteres gepumpt werden kann.Flowable, non-sedimenting suspensions of phthalimidoperoxyhexanoic acid in the alcohol component are obtained in the manner described. Flowable is understood to mean that it flows out at least partially from an open vessel with a corresponding inclination under the influence of gravity and can be easily pumped as part of its industrial processing.
Eine nach dem erfindungsgemäßen Verfahren erhältliche Suspension wird vorzugsweise zur Herstellung flüssiger Wasch- oder Reinigungsmittel verwendet. Ein bleichehaltiges flüssiges Wasch- oder Reinigungsmittel, das eine nach dem erfindungsgemäßen Verfahren erhältliche Suspension enthält, kann wäßrig oder im wesentlichen wasserfrei sein und außer der nach dem erfindungsgemäßen Verfahren erhältlichen Suspension alle weiteren üblichen Inhaltstofe solcher Mittel enthalten, sofern sie nicht in unzumutbar negativer Weise mit der Phthalimidoperoxyhexansäure wechselwirken. Ein solches Mittel weist vorzugsweise einen sauren pH- Wert auf, der insbesondere im Bereich von pH 2,5 bis pH 6,5, vorzugsweise im Bereich von pH 3,5 bis pH 5,5, liegt und gegebenenfalls durch die Anwesenheit systemverträglicher Säuren eingestellt worden sein kann.A suspension obtainable by the process according to the invention is preferably used for the production of liquid washing or cleaning agents. A bleach-containing liquid washing or cleaning agent which contains a suspension obtainable by the process according to the invention can be aqueous or essentially anhydrous and, in addition to the suspension obtainable by the process according to the invention, can contain all the other usual ingredients of such compositions, provided that they are not unacceptably negative of phthalimidoperoxyhexanoic acid interact. Such an agent preferably has an acidic pH, which is in particular in the range from pH 2.5 to pH 6.5, preferably in the range from pH 3.5 to pH 5.5, and is optionally adjusted by the presence of acids which are compatible with the system may have been.
Als besonderer Vorteil ist zu erwähnen, daß die Phthalimidoperoxyhexansäure durch das erfindungsgemäße Verfahren auch sedimentationsstabil in den flüssigen Wasch- oder Reinigungsmitteln verbleibt.It should be mentioned as a particular advantage that the phthalimidoperoxyhexanoic acid also remains sedimentation-stable in the liquid detergents or cleaning agents by the process according to the invention.
Gewünschtenfalls können gleichzeitig mit der Phthalimidoperoxyhexansäure auch weitere Inhaltsstoffe derartiger Wasch- oder Reinigungsmittel in der gleichen alkoholischen Aufschlämmung vermählen werden, wenn sie sich in der alkoholischen Komponente in Gegenwart der Phthalimidoperoxyhexansäure aufschlämmen lassen und auf die gleiche Korngröße wie die Phthalimidoperoxyhexansäure gemahlen werden sollen. If desired, other ingredients of such detergents or cleaning agents can also be milled in the same alcoholic slurry with the phthalimidoperoxyhexanoic acid if they are in the alcoholic component Slurry the presence of the phthalimidoperoxyhexanoic acid and grind to the same grain size as the phthalimidoperoxyhexanoic acid.
BeispieleExamples
Beispiel 1example 1
Phthalimidoperoxyhexansäure-Granulat (Eureco®, Hersteller Ausimont) wurde in Isopropylalkohol aufgeschlämmt. Die 70-gewichtsprozentige Aufschlämmung wurde in einem Mahlbecher mittels Zahnscheibe bei 10 m/s Umfangsgeschwindigkeit 15 Minuten intensiv geschert. Man erhielt eine gut fließfähige strukturviskose Paste Bl. Eine Partikelgrößenanalyse in einem Laserbeugungsspektrometer ergab folgende Werte: dio = 4,6 μm, d5o = 20 μm, d ü = 41 μm.Phthalimidoperoxyhexanoic acid granules (Eureco®, manufacturer Ausimont) were slurried in isopropyl alcohol. The 70% by weight slurry was sheared intensively in a grinding bowl by means of a toothed disk at a peripheral speed of 10 m / s for 15 minutes. . A free-flowing pseudoplastic paste Bl A particle size analysis was obtained in a laser diffraction spectrometer gave the following values: dio = 4.6 .mu.m, d 5 o = 20 microns, d u = 41 microns.
Beispiel 2Example 2
Phthalimidoperoxyhexansäure-Granulat (Eureco®, Hersteller Ausimont) wurde in 1,2- Propandiol aufgeschlä mt. Die 62, 5 -gewichtsprozentige AufscUämmung wurde in einem Mahlbecher mittels Zahnscheibe bei 14,5 m/s Umfangsgeschwindigkeit 12 Minuten intensiv geschert. Man erhielt eine gut fließfähige strukturviskose Paste. Eine Partikelgrößenanalyse in einem Laserbeugungsspektrometer ergab folgende Werte: dio = 2,6 μm, d5o = 13 μm, d90 = 31 μm. Phthalimidoperoxyhexanoic acid granules (Eureco®, manufacturer Ausimont) were slurried in 1,2-propanediol. The 62.5% by weight slurry was sheared intensively for 12 minutes in a grinding bowl by means of a toothed disc at a peripheral speed of 14.5 m / s. A readily flowable pseudoplastic paste was obtained. A particle size analysis in a laser diffraction spectrometer gave the following values: dio = 2.6 .mu.m, d = 5 o 13 microns, d 90 = 31 microns.

Claims

Patentansprüche claims
1. Verfahren zur Herstellung einer fließfahigen Phthalimidoperoxyhexansäure enthaltenden Suspension durch Vermahlung von Phthalimidoperoxyhexansäure in alkoholischer Aufschlämmung.1. Process for the production of a flowable suspension containing phthalimidoperoxyhexanoic acid by grinding phthalimidoperoxyhexanoic acid in an alcoholic slurry.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man die Vermahlung mit Hilfe einer Zahnscheibe oder einer Kugelmühle durcMührt.2. The method according to claim 1, characterized in that the grinding is carried out by means of a toothed disc or a ball mill.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Alkohol ausgewählt wird aus den d- bis C3- Alkoholen mit bis zu 3 OH-Gruppen und deren Mischungen.3. The method according to claim 1 or 2, characterized in that the alcohol is selected from the d- to C 3 - alcohols with up to 3 OH groups and mixtures thereof.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß der Alkohol ausgewählt wird aus der Gruppe umfassend Ethanol, Propanol, Isopropanol, Ethandiol, 1,2- Propandiol, Glycerin und deren Mischungen.4. The method according to claim 3, characterized in that the alcohol is selected from the group comprising ethanol, propanol, isopropanol, ethanediol, 1,2-propanediol, glycerol and mixtures thereof.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der Gehalt an Phthalimidoperoxyhexansäure in der alkoholischen Aufschlämmung im Bereich von 10 Gew.-% bis 90 Gew.-%, insbesondere von 50 Gew.-% bis 85 Gew.-%, liegt.5. The method according to any one of claims 1 to 4, characterized in that the content of phthalimidoperoxyhexanoic acid in the alcoholic slurry in the range of 10 wt .-% to 90 wt .-%, in particular from 50 wt .-% to 85 wt .-% %, lies.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß man die Vermahlung so lange vornimmt, bis die mittlere Teilchengröße (d5u, bestimmbar mit einem Laserbeugungsspektrometer) der Phthalimidoperoxyhexansäure im Bereich von 10 μm bis 40 μm, insbesondere von 12 μm bis 30 μm liegt.6. The method according to any one of claims 1 to 5, characterized in that the grinding is carried out until the average particle size (d 5u , determinable with a laser diffraction spectrometer) of phthalimidoperoxyhexanoic acid in the range from 10 microns to 40 microns, in particular from 12 microns up to 30 μm.
7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß man die Vermahlung so lange vornimmt, bis die Größe von mindestens 90 % der Teilchen (d9o, bestimmbar mit einem Laserbeugungsspektrometer) der Phthalimidoperoxyhexansäure unter 80 μm, insbesondere unter 50 μm liegt.7. The method according to any one of claims 1 to 6, characterized in that the grinding is carried out until the size of at least 90% of the particles (d 9 o, determinable with a laser diffraction spectrometer) of the phthalimidoperoxyhexanoic acid below 80 microns, especially below 50 μm.
8. Verwendung einer nach dem Verfahren gemäß einem der Ansprüche 1 bis 7 erhältlichen Suspension zur Herstellung flüssiger Wasch- oder Reinigungsmittel. 8. Use of a suspension obtainable by the process according to one of claims 1 to 7 for the production of liquid washing or cleaning agents.
9. Bleichehaltiges flüssiges Wasch- oder Reinigungsmittel, dadurch gekennzeichnet, daß es eine nach dem Verfahren gemäß einem der Ansprüche 1 bis 7 erhältliche Suspension enthält.9. bleach-containing liquid washing or cleaning agent, characterized in that it contains a suspension obtainable by the process according to one of claims 1 to 7.
10. Mittel nach Anspruch 9, dadurch gekennzeichnet, daß es einen sauren pH- Wert, insbesondere im Bereich von pH 2,5 bis pH 6,5, aufweist. 10. Composition according to claim 9, characterized in that it has an acidic pH, in particular in the range from pH 2.5 to pH 6.5.
EP03782278A 2002-12-17 2003-12-02 Method for the production of suspensions comprising bleaching agents Expired - Lifetime EP1572853B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10259262A DE10259262B3 (en) 2002-12-17 2002-12-17 Process for the production of suspensions containing bleach
DE10259262 2002-12-17
PCT/EP2003/013565 WO2004055149A1 (en) 2002-12-17 2003-12-02 Method for the production of suspensions comprising bleaching agents

Publications (2)

Publication Number Publication Date
EP1572853A1 true EP1572853A1 (en) 2005-09-14
EP1572853B1 EP1572853B1 (en) 2007-05-16

Family

ID=32519070

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03782278A Expired - Lifetime EP1572853B1 (en) 2002-12-17 2003-12-02 Method for the production of suspensions comprising bleaching agents

Country Status (8)

Country Link
US (1) US7183247B2 (en)
EP (1) EP1572853B1 (en)
JP (1) JP4467438B2 (en)
AT (1) ATE362514T1 (en)
AU (1) AU2003289937A1 (en)
DE (2) DE10259262B3 (en)
ES (1) ES2285224T3 (en)
WO (1) WO2004055149A1 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004019139A1 (en) * 2004-04-16 2005-11-10 Henkel Kgaa Liquid-crystalline washing or cleaning agent with particulate bleach
GB0509377D0 (en) * 2005-05-09 2005-06-15 Reckitt Benckiser Nv Detergent composition
DE102005054565A1 (en) * 2005-11-14 2007-05-16 Henkel Kgaa Oxidizing agent containing fragrant consumer products

Family Cites Families (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2214708A (en) 1988-01-20 1989-09-06 Philips Nv A method of manufacturing a semiconductor device
DE3823172C2 (en) * 1988-07-08 1998-01-22 Hoechst Ag Omega-phthalimidoperoxihexanoic acid, process for its preparation and its use
US4992194A (en) 1989-06-12 1991-02-12 Lever Brothers Company, Division Of Conopco Inc. Stably suspended organic peroxy bleach in a structured aqueous liquid
GB9003200D0 (en) 1990-02-13 1990-04-11 Unilever Plc Aqueous liquid bleach composition
CA2054466A1 (en) 1990-11-02 1992-05-03 Gregory Van Buskirk Liquid nonaqueous detergent with stable, solubilized peracid
JPH06511243A (en) * 1991-10-04 1994-12-15 アクゾ　ナムローゼ　フェンノートシャップ Suspension and flocculation method of amidoperoxyacids
US5480577A (en) * 1994-06-07 1996-01-02 Lever Brothers Company, Division Of Conopco, Inc. Encapsulates containing surfactant for improved release and dissolution rates
JP2958506B2 (en) * 1994-06-15 1999-10-06 花王株式会社 Method for producing fine solid builder
US5858945A (en) * 1996-06-26 1999-01-12 Lever Brothers Company, Division Of Conopco, Inc. Peracid granules containing citric acid monohydrate for improved dissolution rates
DK0932631T3 (en) 1996-10-30 2000-12-18 Akzo Nobel Nv Process for preparing initiator compositions comprising polyvinyl alcohol and surfactant
IT1293587B1 (en) * 1997-07-08 1999-03-08 Manitoba Italia Spa COMPOSITIONS BASED ON PERCARBOXYLIC ACIDS AS STAIN REMOVER AND SANITIZERS
US5981456A (en) * 1997-07-23 1999-11-09 Lever Brothers Company Automatic dishwashing compositions containing water soluble cationic or amphoteric polymers
EP1001008A1 (en) 1998-11-10 2000-05-17 The Procter & Gamble Company Liquid aqueous bleaching compositions comprising a sulphonated anionic surfactant
AU1521999A (en) 1998-11-10 2000-06-05 Procter & Gamble Company, The Bleaching compositions
WO2000027966A1 (en) 1998-11-10 2000-05-18 The Procter & Gamble Company Bleaching compositions
EP1010751B1 (en) * 1998-12-14 2005-04-20 The Procter & Gamble Company Bleaching compositions
EP1010750A1 (en) 1998-12-14 2000-06-21 The Procter & Gamble Company Bleaching compositions
US6699828B1 (en) * 1999-06-28 2004-03-02 The Procter & Gamble Company Aqueous liquid detergent compositions comprising an effervescent system
IT1313598B1 (en) 1999-08-04 2002-09-09 Ausimont Spa WATER DISPERSIONS OF PERCARBOXYL ACIDS
US6537958B1 (en) * 1999-11-10 2003-03-25 The Procter & Gamble Company Bleaching compositions
AU2002236655A1 (en) * 2000-12-21 2002-07-01 The Procter And Gamble Company A motorized hand-held scrubbing and dispensing device and a method of use therefor
HUP0401100A2 (en) * 2001-01-16 2004-11-29 Unilever N.V. Dentifrice composition
US6475977B1 (en) * 2001-03-16 2002-11-05 Unilever Home & Personal Care Usa, Division Of Conopco, Inc. Water soluble sachet with a dishwasher composition

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004055149A1 *

Also Published As

Publication number Publication date
DE50307304D1 (en) 2007-06-28
DE10259262B3 (en) 2004-08-05
JP2006516658A (en) 2006-07-06
US20050233928A1 (en) 2005-10-20
ATE362514T1 (en) 2007-06-15
JP4467438B2 (en) 2010-05-26
ES2285224T3 (en) 2007-11-16
AU2003289937A1 (en) 2004-07-09
EP1572853B1 (en) 2007-05-16
WO2004055149A1 (en) 2004-07-01
US7183247B2 (en) 2007-02-27

Similar Documents

Publication Publication Date Title
CH655325A5 (en) WATER-BASED, THIXOTROPICAL DISHWASHER, IN PARTICULAR FOR AUTOMATIC DISHWASHER.
DE3128336A1 (en) "METHOD FOR PRODUCING COATED NUCLEAR BLEACHING ACTIVATORS"
DE60309070T2 (en) DISTRIBUTED PERSONAL COMPOUNDS WITH CONTROLLED RELEASE, A METHOD OF PREPARING THEM AND THEIR USE
DE69533590T2 (en) METHOD FOR PRODUCING FINE-PARTICULAR SOLID BUILDING PARTICLES
DE1296297B (en) Detergent tablet not coated with silicates
DE3536106A1 (en) METHOD FOR PRODUCING FINE-POWDERED SILICON DIOXIDE
CH631946A5 (en) TYPE A CRYSTALLINE ZEOLITE POWDER
WO1985001039A1 (en) Stabilized aqueous zeolite suspension
EP0283791B1 (en) Aqueous bleaching suspensions containing peroxycarboxylic acid, their preparation and their use
CH631948A5 (en) TYPE A CRYSTALLINE ZEOLITE POWDER
DE10259262B3 (en) Process for the production of suspensions containing bleach
EP0889003A1 (en) Synthetic magnesium silicate
DE2704310A1 (en) PROCESS FOR THE PRODUCTION OF Aqueous SUSPENSIONS OF FINE PARTICULAR, WATER-INSOLUBLE SILICATES, ENABLED FOR CATION EXCHANGE
DE60122771T2 (en) FINE ZEOLITE PARTICLES
DE60121283T2 (en) Carrier particles and detergent particles
DE3720277C2 (en)
DE1592409C2 (en) Process for hydrocassing titanium dioxide pigments in aqueous suspension
DE19900156A1 (en) Highly pure amorphous silicic acid preparing method
EP0006618A1 (en) Use of aluminium silicate granules as cation exchangers
DD292432A5 (en) METHOD FOR PRODUCING A FINE-PARTICULAR TYPE 4A CRYSTALLINE ZEOLITE POWDER WITH PREDETERMINABLE GRAIN SIZE DISTRIBUTION
EP0633923B1 (en) Granular, phosphate-free additive containing non-ionic surface-active agents for washing and cleaning agents
EP0889004A1 (en) Process for the preparation of a synthetic layered silicate of the hectorite type
EP1347037B1 (en) Detergent additive with a high nonionic surfactant content and good dissolution properties
DE19757217A1 (en) Particulate detergent and cleaning agent
WO2004035470A2 (en) Method for producing dust-free alkaline earth peroxides

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20050507

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL LT LV MK

GRAC Information related to communication of intention to grant a patent modified

Free format text: ORIGINAL CODE: EPIDOSCIGR1

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

DAX Request for extension of the european patent (deleted)
GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: GERMAN

REF Corresponds to:

Ref document number: 50307304

Country of ref document: DE

Date of ref document: 20070628

Kind code of ref document: P

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070816

GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 20070823

ET Fr: translation filed
NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2285224

Country of ref document: ES

Kind code of ref document: T3

REG Reference to a national code

Ref country code: IE

Ref legal event code: FD4D

REG Reference to a national code

Ref country code: HU

Ref legal event code: AG4A

Ref document number: E002199

Country of ref document: HU

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

Ref country code: IE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20071016

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070816

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20080219

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070817

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

BERE Be: lapsed

Owner name: HENKEL K.G.A.A.

Effective date: 20071231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20071231

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20071231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20071231

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20071231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20071202

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20070516

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CZ

Payment date: 20141113

Year of fee payment: 12

Ref country code: SK

Payment date: 20141112

Year of fee payment: 12

Ref country code: ES

Payment date: 20141111

Year of fee payment: 12

Ref country code: GB

Payment date: 20141126

Year of fee payment: 12

Ref country code: DE

Payment date: 20141125

Year of fee payment: 12

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20141125

Year of fee payment: 12

Ref country code: HU

Payment date: 20141111

Year of fee payment: 12

Ref country code: FR

Payment date: 20141208

Year of fee payment: 12

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20141126

Year of fee payment: 12

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 50307304

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CZ

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151202

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 362514

Country of ref document: AT

Kind code of ref document: T

Effective date: 20151202

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20151202

REG Reference to a national code

Ref country code: SK

Ref legal event code: MM4A

Ref document number: E 2264

Country of ref document: SK

Effective date: 20151202

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20160831

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151203

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151202

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20160701

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151202

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151231

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151202

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151202

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20151203