EP1126017B1 - Process for making heavy duty detergent compositions and components thereof - Google Patents

Process for making heavy duty detergent compositions and components thereof Download PDF

Info

Publication number
EP1126017B1
EP1126017B1 EP00103515A EP00103515A EP1126017B1 EP 1126017 B1 EP1126017 B1 EP 1126017B1 EP 00103515 A EP00103515 A EP 00103515A EP 00103515 A EP00103515 A EP 00103515A EP 1126017 B1 EP1126017 B1 EP 1126017B1
Authority
EP
European Patent Office
Prior art keywords
fluidized bed
product
fluidised bed
fluidising chamber
components
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP00103515A
Other languages
German (de)
French (fr)
Other versions
EP1126017A1 (en
Inventor
Michael Jacob
Dr. Karlheinz Rümpler
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.)
Glatt Ingenieurtechnik GmbH
Original Assignee
Glatt Ingenieurtechnik GmbH
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=8167894&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP1126017(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Glatt Ingenieurtechnik GmbH filed Critical Glatt Ingenieurtechnik GmbH
Priority to DE50011442T priority Critical patent/DE50011442D1/en
Priority to AT00103515T priority patent/ATE307875T1/en
Priority to DK00103515T priority patent/DK1126017T3/en
Priority to EP00103515A priority patent/EP1126017B1/en
Priority to US09/609,110 priority patent/US6740632B1/en
Publication of EP1126017A1 publication Critical patent/EP1126017A1/en
Application granted granted Critical
Publication of EP1126017B1 publication Critical patent/EP1126017B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • 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
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • 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
    • C11D11/02—Preparation in the form of powder by spray drying

Definitions

  • the invention relates to a process for the preparation of heavy-duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis in a substantially horizontally oriented fluidized bed.
  • the disadvantage is that, depending on the quality of the mixture of the individual components a more or less inhomogeneous distribution of different components takes place. During transport and at the Storage can easily cause segregation of the components within the packaging or the container come. Due to the high dust content and the tendency to segregate will increase the quality of the detergent or detergent components deteriorated considerably. This works are very disadvantageous because these dusts in the most common cases are classified as harmful to health. Furthermore, there is with decreasing particle size increases in tendency to Dust explosions.
  • the object of the invention is to provide a method for Production of heavy-duty detergents and heavy-duty detergent components to develop in granular or agglomerated form on a dry matter basis, which is compared to the known granules by a homogeneous Composition of the granules or agglomerates of the individual Raw material components including the binder and the moisture characterized, a high resistance to mechanical stress has good water dispersibility and is low in dust are virtually dust-free.
  • the product is produced by fluidized bed agglomeration / granulation in a substantially horizontal aligned fluidized bed.
  • This is the solid in the Fluidized bed via a Bedüsungssystem a binder and / or Components in the form of solutions, suspensions or melts fed.
  • the binder content in the product can be 1 to 35% by weight.
  • Energy is a drying and solidification in the Bedüsungs Kunststoff the fluidized bed forming agglomerates / granules.
  • the feed temperature of the process air is in between 20 ° C to the decomposition temperature of the substances involved.
  • the process air from the fluidized bed entrained particles, in particular the fine dust, are in one in the Wirbe Anlagenapparat integrated with cross-sectional extensions provided expansion zone and in an adjoining Filter system separated from the air and into the fluidized bed returned and agglomerated there. This creates a low-dust or dust-free product with a grain size range of 0.2 to 2.00 mm.
  • the process described above for the preparation of the final product is in different process stages, e.g. Heating up, agglomerating, Coating, drying and cooling in a row in a single or multistage fluidized bed performed.
  • the advantage of the inventive method for the production of Heavy-duty detergents and heavy-duty detergent components in granules or Dry-based agglomerate form is that through the Fluidization of the material in the fluidized bed a uniform homogeneous composition of the individual granules or agglomerates from the individual raw material components including the binders and the corresponding moisture is created. A demixing of Components can no longer be done.
  • the granules or agglomerate has a uniform quality.
  • the production of granules or agglomerates by fluidized bed agglomeration / granulation has the further advantage that a firm, abriebarmes and low-dust end product is formed, the is readily dispersible in water.
  • Another advantage of the method according to the invention is that by the perfect encapsulation of the process by process control a health hazard in a single apparatus Contact with the supplied dusts is avoided. In addition, will the area of dust explosion hazard on the interior of the Fluidized bed apparatus reduced.
  • the process for the preparation of heavy duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis is done by Wirbarergesglomeration - / granulation one single- or multi-stage fluidized bed granulation plant, wherein the various process stages for the production of the final product such as Heating, agglomerating, coating, drying and cooling in a row be carried out in a fluidized bed 9.
  • the powdery starting material is on the solids entry 2 and a rotary valve 12 as a pressure seal to the environment of first process stage in the field of the fluid space II of the fluidized bed fed.
  • the supplied material goes through different process stages such as heating, agglomerating, coating, drying and cooling.
  • process air 1 with different Temperatures over the Zu Kunststoffschn 10 and an air distribution floor 11 of the fluidized bed 9 fed.
  • the supply air chambers form this 10 and the air distribution floor 11, as an upper limit, the Anströmteil 1, in which the process air 1 in the swirl space II introduced, distributed and evened out.
  • the temperature of the process air 1 for the agglomeration of the product is dependent on the decomposition temperature of each introduced Substance components and lies according to the substance components between 20 to 300 ° C.
  • the process air 1 for the cooling of the already granulated and dried material will be at the end of the process stages fed in front of the region of the product discharge 3.
  • the temperature the process air 1 for cooling is between - 20 to + 30 ° C and also depends on the individual fabric components in the final product. This will give the process optimal conditions in the fluidized bed 9 by adjusting the respective layer temperature created.
  • the vortex space II is in the lower area through the air distribution floor 11 with a substantially rectangular base and formed by vertical to slightly inclined side walls. there the side walls of the spinal space II can reach max. 10 ° from the Vertically inclined.
  • the of the process air 1 is flowed through from bottom to top the fluidized solid forming the fluidized bed 9.
  • the solid in the Fluidized bed 9 a binder, water and / or one or more Material components in the form of solutions, suspensions or melts fed.
  • the dry matter content in the spray medium is 0 up to 100% while including the binder content in the final product Humidity is 1 to 35%.
  • the spray system 8 consists of a known single or multi-fluid nozzle, where the injection direction from top to bottom or vice versa or can be inclined.
  • the spray system 8 is a homogeneous solid mixture, wherein Granules with a homogeneous composition of the respective Individual components are formed.
  • the expansion zone III closes on, in which the flow velocity of the process air 1 through Cross-sectional extensions is reduced.
  • the side walls of the Expansion zone III show a strong inclination of 15-45 ° Vertical on, so that a cross-sectional widening to the subsequent filter system IV takes place.
  • the expansion zone III is followed by an integrated filter system IV for dedusting the process air 1 and the simultaneous Return of the dust to the underlying fluidized bed 9 at.
  • the filter system IV consists of filter elements 7, the mechanically through the filter cleaning 6 and / or by compressed air 5 can be cleaned impulsively. The use of other well-known Filter elements is possible. Due to the integrated filter system IV Contact with the dusts is avoided and the dust explosion hazard reduced to the interior of the fluidized bed apparatus.
  • the purified process air leaves the system as exhaust 4 during the finished product also via a rotary valve 12 as Pressure completion via the product discharge 3 discharged from the system becomes.
  • the system can be further equipment, such as Explosion Suppression / Relief or in Support of Solids movement e.g. by vibration devices, added become.
  • detergent powder was ⁇ m agglomerated in a fluidized bed with two chambers in the upstream region and with a fluidization base area of 0.2 m 2 with a grain size smaller 200th 1.
  • chamber agglomeration Supply air temperature 150 ° C
  • Layer temperature 60 ° C
  • Spraying medium 30% binder solution in the product 10% binder content 5% water content
  • Second chamber cooling Cooling air temperature 25 ° C
  • Outlet temperature of detergent agglomerate 35 ° C Distribution of the vortex area 75% agglomeration 25% cooling
  • the invention relates to a process for the preparation of heavy-duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis in a substantially horizontally oriented fluidized bed.
  • the object of the invention is to detergent granules or to produce agglomerates characterized by a homogeneous composition from the individual raw material components including the Binders and moisture are characterized by high strength have mechanical stress, good in water dispersible and low in dust to almost dust-free.
  • this is achieved in that the production of the Product takes place in a fluidized bed.
  • This is the solid in the fluidized bed via a Bedüsungssystem a binder and / or components in the form of solutions, suspensions or Melting supplied.
  • Energy is a drying and solidification in the Bedüsungs Kunststoff the fluidized bed forming agglomerates / granules.
  • the feed temperature of the process air is in between 20 ° C to the decomposition temperature of the substances involved.
  • the entrained by the process air from the fluidized bed Particles are integrated in a fluidized bed apparatus Cross-sectional extensions provided expansion zone and in one subsequent filter system separated from the air and into the Fluidized bed returned and agglomerated there. This creates a dust-free or dust-free product with a grit area from 0.2 to 2.00 mm.

Landscapes

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

Abstract

Fluidized bed process to manufacture dry granular or powder washing agent produces homogenous dust-free product. A process to manufacture a dry granular or powder washing agent consists uses a horizontal fluidised bed. The processes, especially agglomeration, coating, drying and cooling, and take place in sequence in a single or multi-stage fluidized bed. The powdery first-stage starting material is fed to the fluidized bed chamber inlet zone. Process air is fed to all process stages from beneath the fluidized bed. The process temperature (20 to 300 degrees C) and air feed temperature (-20 to +30 degrees C) for product agglomeration is dependent upon the break-down temperature of the individual components making up the end-product. Binding agents, water and other ingredients such as solutions, suspensions or molten substances are introduced over the fluidized bed by spray or jet, the percentage dry matter being in the range 0 -100. The ingredients are fluidized to form homogenized granules.

Description

Die Erfindung betrifft ein Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten in Granulat- oder Agglomeratform auf Trockenstoffbasis in einer im wesentlichen horizontal ausgerichteten Wirbelschicht.The invention relates to a process for the preparation of heavy-duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis in a substantially horizontally oriented fluidized bed.

Es ist bekannt, bei der Produktion von Waschmitteln oder Vollwaschmittelkomponenten die jeweiligen Einzelkomponenten durch Sprühtrocknung oder Sprühgranulierung herzustellen und anschließend die so hergestellten Einzelkomponenten enstprechend der Rezeptur zu vermischen. Eine Vereinigung von unterschliedlichen Einzelpartikeln erfolgt dabei bei der Vermischung nicht.It is known in the production of detergents or heavy duty detergent components the individual components by spray drying or spray granulation and then the so produced individual components according to the recipe mix. An association of different individual particles does not take place during mixing.

Nachteilig ist, daß je nach Qualität der Mischung der Einzelkomponenten eine mehr oder weniger inhomogene Verteilung der verschiedenen Komponenten erfolgt. Beim Transport und bei der Lagerung kann es leicht zur Entmischung der Komponenten innerhalb der Verpackung bzw. der Container kommen. Durch den hohen Staubanteil und der Neigung zur Entmischung wird die Qualität der Waschmittel bzw. Waschmittelkomponenten erheblich verschlechtert. Dieses wirkt sich sehr nachteilig aus, da diese Stäube in den häufigsten Fällen als gesundheitsschädlich einzustufen sind. Weiterhin besteht mit abnehmender Partikelgröße eine größer werdende Neigung zu Staubexplosionen.The disadvantage is that, depending on the quality of the mixture of the individual components a more or less inhomogeneous distribution of different components takes place. During transport and at the Storage can easily cause segregation of the components within the packaging or the container come. Due to the high dust content and the tendency to segregate will increase the quality of the detergent or detergent components deteriorated considerably. This works are very disadvantageous because these dusts in the most common cases are classified as harmful to health. Furthermore, there is with decreasing particle size increases in tendency to Dust explosions.

Die Aufgabe der Erfindung besteht darin, ein Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten in Granulat- oder Agglomeratform auf Trockenstoffbasis zu entwickeln, das sich gegenüber den bekannten Granulaten durch eine homogene Zusammensetzung der Granulate oder Agglomerate aus den einzelnen Rohstoffkomponenten inklusive dem Bindemittel und der Feuchtigkeit auszeichnet, eine hohe Festigkeit gegenüber mechanischer Beanspruchung aufweist, gut in Wasser dispergierbar und staubarm bis nahezu staubfrei sind.The object of the invention is to provide a method for Production of heavy-duty detergents and heavy-duty detergent components to develop in granular or agglomerated form on a dry matter basis, which is compared to the known granules by a homogeneous Composition of the granules or agglomerates of the individual Raw material components including the binder and the moisture characterized, a high resistance to mechanical stress has good water dispersibility and is low in dust are virtually dust-free.

Die Aufgabe wird erfindungsgemäß mit den Merkmalen des Anspruches 1 gelöst. Vorteilhafte Ausgestaltungen des Verfahrens sind in den Unteransprüchen angegeben.The object is achieved according to the invention with the features of the claim 1 solved. Advantageous embodiments of the method are in the Subclaims specified.

Die Herstellung des Produktes erfolgt durch Wirbelschichtagglomeration /-granulation in einer im wesentlichen horizontal ausgerichteten Wirbelschicht. Dabei wird dem Feststoff in der Wirbelschicht über ein Bedüsungssystem ein Bindemittel und/oder Komponenten in Form von Lösungen, Suspensionen oder Schmelzen zugeführt. Der Bindemittelgehalt im Produkt kann Werte von 1 bis 35 Mass.-% einnehmen. Durch die über die Prozeßluft eingebrachte Energie erfolgt eine Trocknung und Verfestigung der sich im Bedüsungsbereich der Wirbelschicht bildenden Agglomerate/Granulate. Dabei liegt die Zuführungstemperatur der Prozeßluft zwischen 20 °C bis zur Zersetzungstemperatur der beteiligten Stoffe. Durch Einstellung der Trocknungsparameter kann die Produktfeuchte variiert werden. Werte ab 0 Mass.-% aufwärts je nach Flüssigkeitseintrag sind möglich. Die durch die Prozeßluft aus der Wirbelschicht mitgerissenen Partikel, insbesondere der Feinstaub, werden in einer im Wirbeschichtapparat intergrierten mit Querschnittserweiterungen versehenen Expansionszone und in einem daran anschließenden Filtersystem von der Luft getrennt und in das Wirbelschichtbett zurückgeführt und dort agglomeriert. Damit entsteht ein staubarmes bzw. staubfreies Produkt mit einem Körnungsbereich von 0,2 bis 2,00 mm.The product is produced by fluidized bed agglomeration / granulation in a substantially horizontal aligned fluidized bed. This is the solid in the Fluidized bed via a Bedüsungssystem a binder and / or Components in the form of solutions, suspensions or melts fed. The binder content in the product can be 1 to 35% by weight. By introduced via the process air Energy is a drying and solidification in the Bedüsungsbereich the fluidized bed forming agglomerates / granules. In this case, the feed temperature of the process air is in between 20 ° C to the decomposition temperature of the substances involved. By Setting the drying parameters can reduce the product moisture be varied. Values from 0% by mass upwards depending on the liquid input are possible. The process air from the fluidized bed entrained particles, in particular the fine dust, are in one in the Wirbeschichtapparat integrated with cross-sectional extensions provided expansion zone and in an adjoining Filter system separated from the air and into the fluidized bed returned and agglomerated there. This creates a low-dust or dust-free product with a grain size range of 0.2 to 2.00 mm.

Der oben beschriebene Prozeß zur Herstellung des Endproduktes wird in verschiedenen Prozeßstufen wie z.B. Aufheizen, Agglomerieren, Coaten, Trocknen und Kühlen hintereinander in einer ein- oder mehrstufigen Wirbelschicht durchgeführt.The process described above for the preparation of the final product is in different process stages, e.g. Heating up, agglomerating, Coating, drying and cooling in a row in a single or multistage fluidized bed performed.

Der Vorteil des erfindungsgemäßen Verfahrens zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten in Granulat- oder Agglomeratform auf Trockenstoffbasis besteht darin, daß durch die Fluidisierung des Materials in der Wirbelschicht eine gleichmäßige homogene Zusammensetzung der einzelnen Granulate oder Agglomerate aus den einzelnen Rohstoffkomponenten einschließlich den Bindemitteln und der entsprechenden Feuchtigkeit entsteht. Eine Entmischung der Komponenten kann dadurch nicht mehr erfolgen.The advantage of the inventive method for the production of Heavy-duty detergents and heavy-duty detergent components in granules or Dry-based agglomerate form is that through the Fluidization of the material in the fluidized bed a uniform homogeneous composition of the individual granules or agglomerates from the individual raw material components including the binders and the corresponding moisture is created. A demixing of Components can no longer be done.

Das Granulat oder Agglomerat weist eine einheitliche Qualität auf. Die Herstellung der Granalien oder Agglomerate mittels Wirbelschichtagglomeration /-granulation hat weiterhin den Vorteil, daß ein festes, abriebarmes sowie staubarmes Endprodukt entsteht, das in Wasser gut dispergierbar ist.The granules or agglomerate has a uniform quality. The production of granules or agglomerates by fluidized bed agglomeration / granulation has the further advantage that a firm, abriebarmes and low-dust end product is formed, the is readily dispersible in water.

Ein weiterer Vorteil des erfindungsgemäßen Verfahrens besteht darin, daß durch die vollkommende Kapselung des Prozesses durch Prozeßführung in einem einzigen Apparat eine Gesundheitsgefährdung durch Kontakt mit den zugeführten Stäuben vermieden wird. Außerdem wird der Bereich der Staubexplosionsgefährdung auf den Innenraum des Wirbelschichtapparates reduziert.Another advantage of the method according to the invention is that by the perfect encapsulation of the process by process control a health hazard in a single apparatus Contact with the supplied dusts is avoided. In addition, will the area of dust explosion hazard on the interior of the Fluidized bed apparatus reduced.

Die Erfindung wird anhand von Ausführungsbeispielen näher erläutert. In der dazugehörigen Zeichnung ist ein Querschnitt durch eine Wirbelschichtgranulationsanlage schematisch dargestellt. The invention will be explained in more detail with reference to exemplary embodiments. In the accompanying drawing is a cross section through a Fluidized bed granulation system shown schematically.

Das Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten in Granulat- oder Agglomeratform auf Trockenstoffbasis erfolgt durch Wirbeschichtagglomeration -/granulation einer ein- oder mehrstufigen Wirbelschichtgranulationsanlage, wobei die verschiedenen Prozeßstufen zur Herstellung des Endproduktes wie Aufheizen, Agglomerieren, Coaten, Trocknen und Kühlen hintereinander in einer Wirbelschicht 9 durchgeführt werden.The process for the preparation of heavy duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis is done by Wirbarergesglomeration - / granulation one single- or multi-stage fluidized bed granulation plant, wherein the various process stages for the production of the final product such as Heating, agglomerating, coating, drying and cooling in a row be carried out in a fluidized bed 9.

Das pulverförmige Ausgangsmaterial wird über den Feststoffeintrag 2 und eine Zellenradschleuse 12 als Druckabschluß zur Umgebung der ersten Prozeßstufe im Bereich des Wirbelraums II der Wirbelschicht zugeführt. Entsprechend den spezifischen Materialbedingungen durchläuft das zugeführte Material unterschiedliche Prozeßstufen wie Aufheizen, Agglomerieren, Coaten, Trocknen und Kühlen. Der jeweiligen Prozeßstufe wird Prozeßluft 1 mit unterschiedlichen Temperaturen über die Zuluftkammern 10 und einem Luftverteilungsboden 11 der Wirbelschicht 9 zugeführt. Dabei bilden die Zuluftkammern 10 und der Luftverteilungsboden 11, als obere Begrenzung, den Anströmteil 1, in dem die Prozeßluft 1 in den Wirbelraum II eingebracht, verteilt und vergleichmäßigt wird.The powdery starting material is on the solids entry 2 and a rotary valve 12 as a pressure seal to the environment of first process stage in the field of the fluid space II of the fluidized bed fed. According to the specific material conditions the supplied material goes through different process stages such as heating, agglomerating, coating, drying and cooling. Of the process step is process air 1 with different Temperatures over the Zuluftkammern 10 and an air distribution floor 11 of the fluidized bed 9 fed. The supply air chambers form this 10 and the air distribution floor 11, as an upper limit, the Anströmteil 1, in which the process air 1 in the swirl space II introduced, distributed and evened out.

Die Temperatur der Prozeßluft 1 für die Agglomeration des Produktes ist abhängig von der Zersetzungstemperatur der einzelnen eingebrachten Stoffkomponenten und liegt entsprechend der Stoffkomponenten zwischen 20 bis 300 °C. Die Prozeßluft 1 für die Kühlung des bereits granulierten und getrockneten Materials wird am Ende der Prozeßstufen vor dem Bereich des Produktsaustrages 3 zugeführt. Die Temperatur der Prozeßluft 1 für die Kühlung liegt zwischen - 20 bis + 30 ° C und richtet sich auch nach den einzelnen Stoffkomponenten im Endprodukt. Damit werden für das Verfahren optimale Bedingungen in der Wirbelschicht 9 durch Einstellung der jeweiligen Schichttemperatur geschaffen.The temperature of the process air 1 for the agglomeration of the product is dependent on the decomposition temperature of each introduced Substance components and lies according to the substance components between 20 to 300 ° C. The process air 1 for the cooling of the already granulated and dried material will be at the end of the process stages fed in front of the region of the product discharge 3. The temperature the process air 1 for cooling is between - 20 to + 30 ° C and also depends on the individual fabric components in the final product. This will give the process optimal conditions in the fluidized bed 9 by adjusting the respective layer temperature created.

Der Wirbelraum II wird in den unteren Bereich durch den Luftverteilungsboden 11 mit im wesentlichen rechteckiger Grundfläche und durch senkrechte bis leicht geneigte Seitenwände gebildet. Dabei können die Seitenwände des Wirbelraums II bis max. 10° von der Senkrechten geneigt angeordnet sein. In dem Wirbelraum II, der von der Prozeßluft 1 von unten nach oben durchströmt wird, befindet sich der fluidisierte Feststoff, der die Wirbelschicht 9 bildet. Im Bereich des Wirbelraums II wird über den gesamten Prozeßbereich mittels eines Sprüh- oder Bedüsungssystems 8 dem Feststoff in der Wirbelschicht 9 ein Bindemittel, Wasser und/oder ein oder mehrere Materialkomponenten in Form von Lösungen, Suspensionen oder Schmelzen zugeführt. Der Trockenstoffanteil im Sprühmedium beträgt dabei 0 bis 100 %, während der Binderanteil im Endprodukt einschließlich Feuchte 1 bis 35 % beträgt.The vortex space II is in the lower area through the air distribution floor 11 with a substantially rectangular base and formed by vertical to slightly inclined side walls. there the side walls of the spinal space II can reach max. 10 ° from the Vertically inclined. In the vortex space II, the of the process air 1 is flowed through from bottom to top the fluidized solid forming the fluidized bed 9. In the area of the vortex space II is over the entire process area by means of a spray or Bedüsungssystems 8 the solid in the Fluidized bed 9 a binder, water and / or one or more Material components in the form of solutions, suspensions or melts fed. The dry matter content in the spray medium is 0 up to 100% while including the binder content in the final product Humidity is 1 to 35%.

Das Sprühsystem 8 besteht aus einer bekannten Ein- oder Mehrstoffdüse, wobei die Eindüsrichtung von oben nach unten oder umgekehrt bzw. geneigt erfolgen kann. Durch die Gestaltung des Wirbelraums II und der Zuführung von zusätzlichen Komponenten über das Sprühsystem 8 erfolgt eine homogene Feststoffvermischung, wobei Granulate mit einer homogenen Zusammensetzung aus den jeweiligen Einzelkomponenten gebildet werden.The spray system 8 consists of a known single or multi-fluid nozzle, where the injection direction from top to bottom or vice versa or can be inclined. By the design of the swirling room II and the supply of additional components over the Spray system 8 is a homogeneous solid mixture, wherein Granules with a homogeneous composition of the respective Individual components are formed.

Oberhalb des Wirbelraums II schließt sich die Expansionszone III an, in der die Strömungsgeschwindigkeit der Prozeßluft 1 durch Querschnittserweiterungen verringert wird. Die Seitenwände der Expansionszone III weisen eine starke Neigung von 15-45° zur Senkrechten auf, so daß eine Querschnittserweiterung bis zum anschließenden Filtersystem IV erfolgt. Durch die Verringerung der Strömungsgeschwindigkeit der Prozeßluft 1 erfolgt eine Vorabscheidung von aus dem Wirbelraum II mitgerissenen Partikeln, die wieder in den Wirbelraum rückgeführt werden.Above the spinal space II, the expansion zone III closes on, in which the flow velocity of the process air 1 through Cross-sectional extensions is reduced. The side walls of the Expansion zone III show a strong inclination of 15-45 ° Vertical on, so that a cross-sectional widening to the subsequent filter system IV takes place. By reducing the Flow rate of the process air 1 is a pre-separation of entrained from the vortex space II particles that are again in be returned to the vertebral space.

An die Expansionszone III schließt sich ein integriertes Filtersystem IV zur Entstaubung der Prozeßluft 1 und zur gleichzeitigen Rückkehrung des Staubes in die darunterliegende Wirbelschicht 9 an. Das Filtersystem IV besteht aus Filterelementen 7, die mechanisch durch die Filterabreinigung 6 und/oder durch Druckluft 5 impulsmäßig gereinigt werden können. Der Einsatz anderer bekannter Filterelemente ist möglich. Durch das integrierte Filtersystem IV wird ein Kontakt mit den Stäuben vermieden und die Staubexplosionsgefährdung auf den Innenraum des Wirbelschichtapparates reduziert.The expansion zone III is followed by an integrated filter system IV for dedusting the process air 1 and the simultaneous Return of the dust to the underlying fluidized bed 9 at. The filter system IV consists of filter elements 7, the mechanically through the filter cleaning 6 and / or by compressed air 5 can be cleaned impulsively. The use of other well-known Filter elements is possible. Due to the integrated filter system IV Contact with the dusts is avoided and the dust explosion hazard reduced to the interior of the fluidized bed apparatus.

Die gereinigte Prozeßluft verläßt das System als Abluft 4 während das Fertigprodukt ebenfalls über eine Zellenradschleuse 12 als Druckabschluß über den Produktaustrag 3 aus dem System ausgetragen wird.The purified process air leaves the system as exhaust 4 during the finished product also via a rotary valve 12 as Pressure completion via the product discharge 3 discharged from the system becomes.

Der Anlage können weitere Ausrüstungsteile, beispielsweise zur Explosionsunterdrückung /-entlastung oder zur Unterstützung der Feststoffbewegung z.B. durch Vibrationseinrichtungen, hinzugefügt werden.The system can be further equipment, such as Explosion Suppression / Relief or in Support of Solids movement e.g. by vibration devices, added become.

In einem konkreten Fall wurde Waschmittelpulver mit einer Körnung kleiner 200 µm in einer Wirbelschicht mit zwei Kammern im Anströmbereich und mit einer Wirbelbodenfläche von 0,2 m2 agglomeriert. 1. Kammer Agglomeration Zulufttemperatur 150 °C Schichttemperatur 60 °C Sprühmedium 30 %ige Binderlösung im Produkt 10 % Binderanteil 5 % Wasseranteil 2. Kammer Kühlung Kühllufttemperatur 25° C Austrittstemperatur Waschmittelagglomerat 35 °C Aufteilung der Wirbelfläche 75 % Agglomeration 25 % Kühlung In a concrete case, detergent powder was μ m agglomerated in a fluidized bed with two chambers in the upstream region and with a fluidization base area of 0.2 m 2 with a grain size smaller 200th 1. chamber agglomeration Supply air temperature 150 ° C Layer temperature 60 ° C Spraying medium 30% binder solution in the product 10% binder content 5% water content Second chamber cooling Cooling air temperature 25 ° C Outlet temperature of detergent agglomerate 35 ° C Distribution of the vortex area 75% agglomeration 25% cooling

Es wurden feste und gleichmäßig homogene Agglomerate mit einer Korngröße von 400 bis 800 µm, ohne Staubanteile < 200 µm erzeugt, die gut in Wasser löslich sind.There were solid and uniformly homogeneous agglomerates with a Grain size of 400 to 800 μm, produced without dust particles <200 μm, which are well soluble in water.

Zusammenfassend läßt sich folgendes feststellen:In summary, the following can be stated:

Die Erfindung betrifft ein Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten in Granulat- oder Agglomeratform auf Trockenstoffbasis in einer im wesentlichen horizontal ausgerichteten Wirbelschicht.The invention relates to a process for the preparation of heavy-duty detergents and heavy duty detergent components in granular or agglomerate form on a dry basis in a substantially horizontally oriented fluidized bed.

Die Aufgabe der Erfindung besteht darin, Waschmittelgranulate oder -agglomerate herzustellen, die sich durch eine homogene Zusammensetzung der aus den einzelnen Rohstoffkomponenten inklusive dem Bindemittel und der Feuchtigkeit auszeichnen, eine hohe Festigkeit gegenüber mechanischer Beanspruchung aufweisen, gut in Wasser dispergierbar und staubarm bis nahezu staubfrei sind.The object of the invention is to detergent granules or to produce agglomerates characterized by a homogeneous composition from the individual raw material components including the Binders and moisture are characterized by high strength have mechanical stress, good in water dispersible and low in dust to almost dust-free.

Erfindungsgemäß wird das dadurch erreicht, daß die Herstellung des Produktes in einer Wirbelschicht erfolgt. Dabei wird dem Feststoff in der Wirbelschicht über ein Bedüsungssystem ein Bindemittel und/oder Komponenten in Form von Lösungen, Suspensionen oder Schmelzen zugeführt. Durch die über die Prozeßluft eingebrachte Energie erfolgt eine Trocknung und Verfestigung der sich im Bedüsungsbereich der Wirbelschicht bildenden Agglomerate/Granulate. Dabei liegt die Zuführungstemperatur der Prozeßluft zwischen 20 °C bis zur Zersetzungstemperatur der beteiligten Stoffe. Durch Einstellung der Trocknungstemperatur kann die Produktfeuchte variiert werden. Die durch die Prozeßluft aus der Wirbelschicht mitgerissenen Partikel werden in einer im Wirbelschichtapparat integrierten mit Querschnittserweiterungen versehenen Expansionszone und in einem daran anschließenden Filtersystem von der Luft getrennt und in das Wirbelschichtbett zurückgeführt und dort agglomeriert. Damit entsteht ein staubarmes bzw. staubfreies Produkt mit einem Körnungsbereich von 0,2 bis 2,00 mm.According to the invention this is achieved in that the production of the Product takes place in a fluidized bed. This is the solid in the fluidized bed via a Bedüsungssystem a binder and / or components in the form of solutions, suspensions or Melting supplied. By introduced via the process air Energy is a drying and solidification in the Bedüsungsbereich the fluidized bed forming agglomerates / granules. In this case, the feed temperature of the process air is in between 20 ° C to the decomposition temperature of the substances involved. By Setting the drying temperature, the product moisture can be varied become. The entrained by the process air from the fluidized bed Particles are integrated in a fluidized bed apparatus Cross-sectional extensions provided expansion zone and in one subsequent filter system separated from the air and into the Fluidized bed returned and agglomerated there. This creates a dust-free or dust-free product with a grit area from 0.2 to 2.00 mm.

Claims (3)

  1. Process for producing heavy duty detergents and heavy duty detergent components in granulated or agglomerated form based on dry substance in a substantially horizontally aligned fluidised bed, characterised in that
    a) the various stages of the process for producing the end product such as, for example, heating, agglomerating, coating, drying and cooling, are carried out one after the other in a single- or multi-stage fluidised bed,
    b) the powdered starting material is fed into the first stage of the process in the region of the fluidising chamber of the fluidised bed,
    c) the processing air is supplied to the various stages of the process underneath the fluidised bed, the temperature of the processing air or air supply for the agglomeration of the product being dependent on the temperature of decomposition of the individual components of the end product and being 20 to 300°C, while the processing air for the cooling is at -20 to +30°C,
    d) in the region of the fluidising chamber, over the entire processing area, a binder, water and/or one or more material components in the form of solutions, suspensions or melts are fed into the solid in the fluidised bed by means of a spraying or sprinkling system, the dry content of the spray medium being 0 to 100%,
    e) in the region of the fluidising chamber the solids are mixed by fluidising and in this way granules of homogeneous composition are formed from the individual components,
    f) the flow rate of the processing air supplied to the fluidising chamber from below is reduced in the expansion zone located above the fluidising chamber by means of widened cross sections, and at the same time particles picked up from the fluidising chamber are deposited and the deposited particles are recycled into the fluidising chamber,
    g) the depositing and recycling of the dust from the process into the fluidising chamber takes place in an adjacent integrated filter system with cleaning mechanism, which is provided above the expansion zone.
  2. Process according to claim 1, characterised in that the content of binder in the product including moisture is from 1 to 35%.
  3. Process according to claims I and 2, characterised in that the introduction of the raw material into the fluidised bed and the removal of the finished product from the fluidised bed take place with the pressure being sealed off from the surrounding area.
EP00103515A 2000-02-18 2000-02-18 Process for making heavy duty detergent compositions and components thereof Expired - Lifetime EP1126017B1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DE50011442T DE50011442D1 (en) 2000-02-18 2000-02-18 Process for the preparation of heavy-duty detergents and heavy-duty detergent components
AT00103515T ATE307875T1 (en) 2000-02-18 2000-02-18 METHOD FOR PRODUCING SOLUTIONAL DETERGENTS AND SOLUTIONAL DETERGENT COMPONENTS
DK00103515T DK1126017T3 (en) 2000-02-18 2000-02-18 Process for the preparation of high-efficiency detergents and components of high-efficiency detergents
EP00103515A EP1126017B1 (en) 2000-02-18 2000-02-18 Process for making heavy duty detergent compositions and components thereof
US09/609,110 US6740632B1 (en) 2000-02-18 2000-06-30 Process for manufacturing industrial detergent and components thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP00103515A EP1126017B1 (en) 2000-02-18 2000-02-18 Process for making heavy duty detergent compositions and components thereof

Publications (2)

Publication Number Publication Date
EP1126017A1 EP1126017A1 (en) 2001-08-22
EP1126017B1 true EP1126017B1 (en) 2005-10-26

Family

ID=8167894

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00103515A Expired - Lifetime EP1126017B1 (en) 2000-02-18 2000-02-18 Process for making heavy duty detergent compositions and components thereof

Country Status (5)

Country Link
US (1) US6740632B1 (en)
EP (1) EP1126017B1 (en)
AT (1) ATE307875T1 (en)
DE (1) DE50011442D1 (en)
DK (1) DK1126017T3 (en)

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10221742A1 (en) * 2002-05-16 2003-12-04 Henkel Kgaa Builder granules
DE10322062A1 (en) * 2003-05-15 2004-12-02 Glatt Ingenieurtechnik Gmbh Method and device for applying liquids in a solid flow of a spouted bed apparatus
WO2004108911A2 (en) * 2003-06-11 2004-12-16 Glatt Ingenieurtechnik Gmbh Method for production of enzyme granules and enzyme granules produced thus
DE10326231B4 (en) * 2003-06-11 2016-04-07 Glatt Ingenieurtechnik Gmbh Process for the preparation of enzyme granules
US20080022940A1 (en) * 2003-07-11 2008-01-31 Bradley Kirsch Composite Absorbent Particles with Superabsorbent Material
US20080029039A1 (en) * 2003-07-11 2008-02-07 Dennis Jenkins Dry Bed Agglomeration Process and Product Formed Thereby
US20090217882A1 (en) * 2003-07-11 2009-09-03 Dennis Jenkins Dry Bed Agglomeration Process and Product Formed Thereby
US20080251027A1 (en) * 2003-07-11 2008-10-16 Bradley Kirsch Shaped Absorbent Particles
TWI356712B (en) 2004-05-24 2012-01-21 Nycomed Pharma As Agglomeration of a calcium-containing compound by
DE102004028883A1 (en) * 2004-06-15 2006-01-05 Glatt Ingenieurtechnik Gmbh Process for the granulation of malt extracts
ES2306431T3 (en) 2005-02-03 2008-11-01 Nycomed Pharma As GRANULATION BY FUSION OF A COMPOSITION CONTAINING A COMPOUND BASED ON CALCIUM.
AU2006211023B2 (en) 2005-02-03 2012-05-24 Takeda Nycomed As Fast wet-massing method for the preparation of calcium-containing compositions
PL1861073T5 (en) * 2005-03-04 2012-09-28 Takeda As Process for the production of calcium compositions in a continuous fluid bed
UA95093C2 (en) 2005-12-07 2011-07-11 Нікомед Фарма Ас Method for the preparation of calcium-containing compound
DE602006016641D1 (en) 2005-12-07 2010-10-14 Nycomed Danmark Aps PRE-PAINTED CALCIUM-CONTAINING COMPOSITIONS
US7776110B2 (en) 2007-06-21 2010-08-17 The Clorox Company Agglomerated animal litter
DE102007051093A1 (en) * 2007-10-24 2009-04-30 Henkel Ag & Co. Kgaa Detergent or detergent compounds and their preparation
US8277557B2 (en) 2009-08-07 2012-10-02 Borregaard Industries Limited Agglomerated particulate lignosulfonate

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1341557A (en) * 1970-06-02 1973-12-25
US4323312A (en) * 1977-08-26 1982-04-06 Werner Glatt Fluidized bed apparatus
US4689297A (en) * 1985-03-05 1987-08-25 Miles Laboratories, Inc. Dust free particulate enzyme formulation
US4734290A (en) * 1985-12-12 1988-03-29 Mallinckrodt, Inc. Process for preparing a coated-particle salt substitute composition
US4919847A (en) * 1988-06-03 1990-04-24 Colgate Palmolive Co. Process for manufacturing particulate detergent composition directly from in situ produced anionic detergent salt
GB8818613D0 (en) * 1988-08-05 1988-09-07 Paterson Zochonis Uk Ltd Detergents
EP0441092A1 (en) * 1990-02-08 1991-08-14 Niro Holding A/S A method and apparatus for heat treating a particulate product
US5814501A (en) * 1990-06-04 1998-09-29 Genencor International, Inc. Process for making dust-free enzyme-containing particles from an enzyme-containing fermentation broth
DE4127323A1 (en) * 1991-08-20 1993-02-25 Henkel Kgaa METHOD FOR PRODUCING TENSIDE GRANULES
DE4304015A1 (en) * 1993-02-11 1994-08-18 Henkel Kgaa Process for the production of granules
DK62994A (en) * 1993-11-15 1995-05-16 Niro Holding As Apparatus and method for making an agglomerated material
DE4422607A1 (en) * 1994-06-28 1996-01-04 Henkel Kgaa Process for producing granules in a fluidized bed and apparatus for carrying out the process
DE19524464C2 (en) * 1995-07-10 2000-08-24 Cognis Deutschland Gmbh Process for the production of sugar surfactant granules
DE19750424A1 (en) * 1997-11-14 1999-05-20 Henkel Kgaa Production of detergent granules with high bulk density

Also Published As

Publication number Publication date
US6740632B1 (en) 2004-05-25
DE50011442D1 (en) 2005-12-01
EP1126017A1 (en) 2001-08-22
DK1126017T3 (en) 2006-02-06
ATE307875T1 (en) 2005-11-15

Similar Documents

Publication Publication Date Title
EP1126017B1 (en) Process for making heavy duty detergent compositions and components thereof
DE69712226T2 (en) METHOD AND DEVICE FOR SPRAY DRYING AND CLEANING METHOD FOR SUCH A DEVICE
DE19826570C2 (en) Process for the production of fertilizer granules containing urea and ammonium sulfate
EP0163836A1 (en) Process and apparatus for the production of granules
DE3043440A1 (en) GRANULATION METHOD AND DEVICE
EP1279433B1 (en) Process for coating of baby food
EP1638678B1 (en) Method for production of enzyme granules and enzyme granules produced thus
DE10326231B4 (en) Process for the preparation of enzyme granules
DE10146778B4 (en) Process and fluidized-bed plant for the production of compact solid particles
DE19904657B4 (en) Process for the preparation of heavy-duty detergents and heavy-duty detergent components
EP1407814B1 (en) Process and apparatus with a fluidised bed apparatus for producing granules
DE10132177A1 (en) Process for the production of granules in a circulating fluidized bed, apparatus for carrying out this process and granules obtained by this process
DD140987B1 (en) CONTINUOUS MANUFACTURING METHOD GRANULATED WASHING AND CLEANING AGENT IN SWIVEL LAYERED APPARATUS
EP1593424B1 (en) Process for encapsulation of substances sensitive to oxidation as well as fragrance and flavorant compounds in granular form
EP0047794B1 (en) Process for the uniform close-formation coating of separate particles of free flowing material, and apparatus for carrying it out
DD228458A1 (en) METHOD FOR THE CONTINUOUS PREPARATION OF DETERGENT GRANULATE PRODUCTS
DE19724142B4 (en) Process for the production of granulated mixed fertilizer
AT404098B (en) METHOD FOR PRODUCING GRANULATED CONTINUOUS POWDER
EP0564713A2 (en) Process for solidifying powders containing metal, apparatus for solidifying and obtained solids
AT409345B (en) Fluidized bed apparatus and process for producing granules
DE60203609T2 (en) METHOD FOR DRYING A LIQUID OR A PASTE AND DRYING SYSTEM THEREFOR
DE2940263A1 (en) Appts. for spray coating granular materials - has agitating device and air suspension arrangement to ensure uniform mixing
EP1609848A1 (en) Process for granulation of malt extracts
DE102004008020A1 (en) Preparing enzyme granules, useful in nutritional, cleaning and pharmaceutical compositions, by spraying enzyme solution into gas stream containing solid particles, followed by drying and granulation
DE10035556A1 (en) Production of granulates and agglomerates in fluidized beds from solids, suspensions, slurries, emulsions or melts comprises additionally adding microbes in additional spraying liquid to produce defined granulate grain size

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: 20000927

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

AX Request for extension of the european patent

Free format text: AL;LT;LV;MK;RO;SI

RIN1 Information on inventor provided before grant (corrected)

Inventor name: RUEMPLER, DR. KARLHEINZ

Inventor name: JACOB, MICHAEL

AKX Designation fees paid

Free format text: AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

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 CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

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: CH

Ref legal event code: NV

Representative=s name: HANS RUDOLF GACHNANG PATENTANWALT

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: GERMAN

REF Corresponds to:

Ref document number: 50011442

Country of ref document: DE

Date of ref document: 20051201

Kind code of ref document: P

REG Reference to a national code

Ref country code: SE

Ref legal event code: TRGR

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: 20060126

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 FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060206

REG Reference to a national code

Ref country code: DK

Ref legal event code: T3

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: 20060228

Ref country code: LU

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

Effective date: 20060228

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

Effective date: 20060208

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

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: 20060327

ET Fr: translation filed
PLBI Opposition filed

Free format text: ORIGINAL CODE: 0009260

26 Opposition filed

Opponent name: HENKEL KOMMANDITGESELLSCHAFT AUF AKTIEN VTP/PATENT

Effective date: 20060717

PLAX Notice of opposition and request to file observation + time limit sent

Free format text: ORIGINAL CODE: EPIDOSNOBS2

NLR1 Nl: opposition has been filed with the epo

Opponent name: HENKEL KOMMANDITGESELLSCHAFT AUF AKTIEN VTP/PATENT

PLBB Reply of patent proprietor to notice(s) of opposition received

Free format text: ORIGINAL CODE: EPIDOSNOBS3

PLBP Opposition withdrawn

Free format text: ORIGINAL CODE: 0009264

PLBD Termination of opposition procedure: decision despatched

Free format text: ORIGINAL CODE: EPIDOSNOPC1

PLBM Termination of opposition procedure: date of legal effect published

Free format text: ORIGINAL CODE: 0009276

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

Free format text: STATUS: OPPOSITION PROCEDURE CLOSED

27C Opposition proceedings terminated

Effective date: 20070601

NLR2 Nl: decision of opposition

Effective date: 20070601

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: 20051026

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

Ref country code: IE

Payment date: 20120203

Year of fee payment: 13

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

Ref country code: BE

Payment date: 20120102

Year of fee payment: 13

Ref country code: IT

Payment date: 20120227

Year of fee payment: 13

Ref country code: FI

Payment date: 20120221

Year of fee payment: 13

Ref country code: GB

Payment date: 20120202

Year of fee payment: 13

Ref country code: DK

Payment date: 20120210

Year of fee payment: 13

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

Ref country code: SE

Payment date: 20121130

Year of fee payment: 14

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

Ref country code: AT

Payment date: 20120210

Year of fee payment: 13

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

Ref country code: FR

Payment date: 20130320

Year of fee payment: 14

Ref country code: DE

Payment date: 20130208

Year of fee payment: 14

Ref country code: CH

Payment date: 20130308

Year of fee payment: 14

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

Ref country code: NL

Payment date: 20130215

Year of fee payment: 14

BERE Be: lapsed

Owner name: *GLATT INGENIEURTECHNIK G.M.B.H.

Effective date: 20130228

REG Reference to a national code

Ref country code: DK

Ref legal event code: EBP

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 307875

Country of ref document: AT

Kind code of ref document: T

Effective date: 20130228

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

Effective date: 20130218

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

Ref country code: AT

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

Effective date: 20130228

Ref country code: FI

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

Effective date: 20130218

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

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

Ref country code: GB

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

Effective date: 20130218

Ref country code: IE

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

Effective date: 20130218

Ref country code: BE

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

Effective date: 20130228

Ref country code: DK

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

Effective date: 20130228

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 50011442

Country of ref document: DE

REG Reference to a national code

Ref country code: NL

Ref legal event code: V1

Effective date: 20140901

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

Ref country code: SE

Ref legal event code: EUG

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: 20140228

Ref country code: NL

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

Effective date: 20140901

Ref country code: LI

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

Effective date: 20140228

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST

Effective date: 20141031

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 NON-PAYMENT OF DUE FEES

Effective date: 20140219

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 50011442

Country of ref document: DE

Effective date: 20140902

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

Ref country code: DE

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

Effective date: 20140902

Ref country code: FR

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

Effective date: 20140228

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: 20140218