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EP1032641A2 - Procede ameliore destine a la production de granules tensioactifs avec une densite en vrac elevee - Google Patents

Procede ameliore destine a la production de granules tensioactifs avec une densite en vrac elevee

Info

Publication number
EP1032641A2
EP1032641A2 EP98961137A EP98961137A EP1032641A2 EP 1032641 A2 EP1032641 A2 EP 1032641A2 EP 98961137 A EP98961137 A EP 98961137A EP 98961137 A EP98961137 A EP 98961137A EP 1032641 A2 EP1032641 A2 EP 1032641A2
Authority
EP
European Patent Office
Prior art keywords
fluidized bed
surfactant
air
liquid
granules
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
EP98961137A
Other languages
German (de)
English (en)
Other versions
EP1032641B1 (fr
Inventor
Olaf Blochwitz
Georg Assmann
Andreas Syldath
Ditmar Kischkel
Karl-Heinz Schmid
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.)
Cognis IP Management GmbH
Original Assignee
Cognis Deutschland GmbH and Co KG
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 Cognis Deutschland GmbH and Co KG filed Critical Cognis Deutschland GmbH and Co KG
Publication of EP1032641A2 publication Critical patent/EP1032641A2/fr
Application granted granted Critical
Publication of EP1032641B1 publication Critical patent/EP1032641B1/fr
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
    • 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions

Definitions

  • the invention relates to a process for producing detergent-containing granules with a bulk density above 500 g / l, which are active in washing and cleaning, from a surfactant preparation which has a non-surfactant liquid component, in particular water, and which operates under normal pressure at temperatures between 20 and 80 ° C is in liquid to pasty form, by granulation and simultaneous drying in a fluidized bed above an inflow floor provided with through-openings for the fluidizing gas, in particular fluidizing air, drying being understood to mean the partial or complete removal of the non-surfactant liquid component.
  • the invention is therefore based on the object of improving the economy of the method of the type mentioned.
  • the duration of an uninterrupted operation of a corresponding system is to be extended considerably.
  • the quality of the product obtained should be improved so that there is no longer any risk of black or brown spots ("specks") on the preferably white granules.
  • the passage openings are covered by a grid with mesh sizes smaller than 600 microns.
  • the grid can be arranged inside or above the passage openings. However, the grid preferably lies directly below the passage openings of the inflow floor.
  • a metal gauze with the appropriate mesh size can be sintered onto the underside of a known inflow floor or attached in some other way.
  • the metal gauze preferably consists of the same material as the inflow floor, in particular of stainless steel.
  • the fine-meshed grid prevents particles from falling through, especially when the granulation system stops unscheduled, but in the case of heavy particles with bulk weights around 1000 g / l are prevented even during operation.
  • the mesh size of said grid is preferably between 200 and 400 ⁇ m.
  • the top is switched off cleans the inflow floor during operation by means of a slide, scratch or the like.
  • Such cleaning can be done manually or automatically.
  • the scratch or scraper used can be made of a thermally resistant plastic, e.g. B. polytetrafluoroethylene (PTFE) exist to exclude damage to the inflow floor with certainty.
  • PTFE polytetrafluoroethylene
  • fatty alcohol sulfates may be mentioned, which can hydrolyze at elevated temperatures.
  • the inflow floor used has a pressure loss of at most 10 mbar and in particular at most 6 mbar.
  • oversize ie granules with grain sizes above the desired range
  • fine grain ie the granules with grain sizes below the desired range
  • the undersize obtained during sieving be returned to the fluidized bed, which is above the desired particle size but below one oversized grain that is of a predetermined size grinds and likewise returns to the fluidized bed and the oversized grain that is above the specified size is collected, cooled and only then ground and returned to the fluidized bed.
  • the specified grain size is preferably about 10 mm.
  • the desired grain size range is preferably 0.4 to 1.6 mm.
  • the surfactant preparation form used has a surfactant concentration of 35 to 95% by weight.
  • Particularly suitable compositions of the preparation form are mentioned in EP 0 603 207 B1, to which reference is expressly made to supplement the disclosure.
  • the aqueous surfactant preparation form used has a relatively high viscosity of 3,000 to 20,000 mPas. This toughness requires two-component atomization.
  • a fine distribution of the droplets has the further advantage of a relatively large surface area of the droplet or particle compared to the volume, so that it not only dries up quickly, but also completely, and there is no gelatinous sticky area inside, which is present during storage and use of the finished product can lead to problems.
  • the surfactant preparation form is sprayed into the fluidized bed by means of at least one nozzle which has at least one additional nozzle channel for compressed air, in particular swirl air, for fine atomization of the surfactant preparation form.
  • the nozzle channel for the compressed air is preferably on the outside and the channel for the surfactant preparation form is on the inside.
  • the nozzles can be attached in different ways inside the fluidized bed apparatus. It is known, for example, to attach the nozzles to holders in the interior of the fluidized bed apparatus. On the brackets and on the supply lines for the nozzles that necessarily run inside the fluidized bed apparatus in this case, product components are disadvantageously deposited, so that cleaning is necessary from time to time. Another disadvantage with this arrangement is a possible disturbance of the fluidized bed by the brackets and supply lines. This arrangement of the nozzles with their supply lines has so far been chosen in order to ensure that a uniform spraying of the fluidized bed is achieved from top to bottom.
  • the inventors have now surprisingly found that the required uniform spraying of the fluidized bed from top to bottom is ensured even if the nozzles are attached directly to the inner wall of the fluidized bed apparatus. In this case, they are slanted downwards directed. It is therefore proposed in a further advantageous embodiment of the invention that the surfactant preparation form is sprayed in by means of nozzles which are arranged on the inside of the side wall of the fluidized bed apparatus, the feed lines for the nozzles running outside the fluidized bed apparatus. In addition to avoiding caking, the arrangement of the feed lines has the additional advantage that leaks in the feed lines can be recognized immediately by the operating personnel and can be remedied easily from the outside. With this arrangement of the nozzles, injection at different heights is also possible.
  • This seed material is preferably produced granules with a grain size that is too small or corresponding granules with a grain size that is too large, which have been ground and sieved.
  • the preferred inlet temperature of the fluidized air is 80 to 230 ° C
  • the preferred air outlet temperature is 30 to 120 ° C.
  • the product drawn off from the fluidized bed is cooled in a product cooler before it is packaged.
  • a product cooler In contrast to the previous method, it is advantageous if, instead of ambient air for cooling, an already cooled supply air is used, in particular at a temperature of 5 to 8 ° C, so that in any case, even on very hot summer days, a product temperature of less than 35 ° C with certainty.
  • the lower absolute humidity of this pre-cooled cooling air also has advantages for the wash- and cleaning-active granules, since this removes further (residual) moisture from the product, which results in increased storage stability.
  • a filter is preferably installed in or on the product cooler, the filter dust of which is returned to the fluidized bed as seed material. The cooler works especially self-promoting.
  • the following filter system for the actual fluidized bed system is also advantageous.
  • a separate cyclone for separating particles from an external filter system is provided.
  • the design of the filter depends on the material properties of the product to be granulated and the amount of dust generated.
  • the way the burner is used can be direct or indirect.
  • the hot exhaust gas from the burner comes into direct contact with the fluidized bed.
  • a heat exchanger is interposed, in which the exhaust gases the fluidizing gas, for. B. air, heat.
  • Figure 1 shows a device suitable for performing the method according to the invention in a schematic representation.
  • the surfactant preparation form to be dried and granulated is passed from stirred templates 1 of different sizes via metering pumps 2 and a line 3 to the fluidized bed granulation dryer 4.
  • the templates 1 are connected to the lines 3 for the nozzles 8 so that different pumps 2 and nozzles 8 from the templates 1 can be operated.
  • a mixture of the contents of different templates 1 for setting the desired recipe is possible in this way.
  • Another advantage is the possibility of switching from one nozzle 8 to another nozzle 8 in the event of malfunctions without the operation of the granulation dryer 4 having to be interrupted.
  • the fluidized bed granulator dryer 4 essentially consists of two areas, namely an upper area with the fluidized bed zone 5 above an inflow floor 6 provided with passage openings.
  • the air required to maintain the fluidized bed which also serves for drying, flows out of the lower, particularly hot area 7 up through the through openings of the inflow base 6.
  • the inflow base 6 consists of six circular sector-shaped elements, a central circular opening for the downpipe 13 being kept free.
  • the bottom 6 can also be in one piece.
  • the inflow floor is equipped with holes with a diameter of 2 mm, which are spaced 10 mm apart (hole division).
  • the particle stream moves upwards on the outer wall and from there to the central discharge area, where it is classified by means of the classifying air flowing upward in the downpipe 13.
  • the granules above a certain grain size range fall down through the downpipe 13 to the rotary valve 14; the smaller and lighter particles move in the vicinity of the inflow bottom again outwards to the side wall of the fluidized bed granulator dryer 4.
  • the pasty surfactant preparation form is fed via line 3 to six nozzles 8, where it is divided into particularly fine droplets by means of compressed air of approximately 3 bar, which is fed to the nozzles via line 9 and swirled within the nozzles 8.
  • the nozzles 8 are attached to the inside of the side wall of the fluidized bed granulator dryer 4 and are directed obliquely downwards, the spray direction being adjustable from the outside.
  • the droplets hit the particles of the fluidized bed, are dried at the same time and allow the particles of the fluidized bed to grow into larger granules.
  • the finely divided solids required for the process, the so-called germs are fed to the fluidized bed via lines 10, 11, 12.
  • the germs come from different sources, as will be explained below.
  • the granules are discharged via a down pipe 13 and a rotary valve 14 and fed to a cooler 15.
  • classifier air is allowed to enter the downpipe 13 from below.
  • This detail is not shown in FIG. 1.
  • the still relatively hot granules are cooled with air heated to 5 to 8 ° C., which is supplied via a line 16, leave the cooler 15 via a further rotary valve 17 and are fed from a conveyor belt 8 to a screening plant 19.
  • the exhaust air from the cooler 15 is cleaned with a bag or pocket filter 20, the filtered fine particles being returned to the fluidized bed as seed material.
  • the screening plant 19 consists of at least two screening decks 21. Oversize 22 with a size of more than 10 mm is collected, cooled and only ground later, when this oversize has also cooled to the inside, so that this grain is continuously crystallized. Coarse grains with a grain size below 10 mm, but above the desired grain size range, are fed into a roller mill (roller mill) 25 via a screw 23 and a pneumatic steep conveyor section 24 and milled there. The gap width of the roller mill can be set between 0.4 mm and 1.2 mm. The ground material can either be passed to the screening plant 19 (line 26) or back into the fluidized bed immediately above the inflow floor (line 27).
  • the good grain obtained from the screening plant 19, that is to say the granules within the desired grain size range, are drawn off and packed via the line 28.
  • a filter system 29 with a bag or pocket filter based on needle felt for the exhaust air and a burner 30 for heating the fluidized air supplied via the line 31 are provided.
  • a so-called direct mode of operation of the burner is used.
  • the system is also equipped with an emergency chimney 33 behind the burner 30. In this way, the hot air from the burner (residual heat) can be released directly to the environment in an emergency without additionally heating or fluidizing the organic components in the fluidized bed.
  • the source of the fire is quickly extinguished by water injection from a specially installed facility. Since no more supply air is sent through the fluidized bed, a fire cannot be started again and the supply of oxygen is cut off at the same time.
  • the exhaust air from the filter system 29 can be used again as supply air for the burner 30 or the corresponding heat exchanger. In this way, air recirculation can be achieved without emissions.
  • the fine particles obtained in the filter system 29 are also added to the fluidized bed again as seed material via a cellular wheel sluice 32 and the line 12.
  • clearing locks are understood to mean locks for powder or granules with a possibility of forced clearing. It is favorable to use such clearing locks in the area between the fluidized bed and the rotary valve 14, in front of the rotary valve 32 of the main filter 29 and between the cooler 15 and the downstream rotary valve 17. In the case of sticky products, this prevents the rotary valve from sticking.
  • FIG. 2 an exemplary embodiment of the method according to the invention is shown again in summary with the aid of a product flow diagram.
  • the reference symbols used here have the same meaning as in FIG. 1.
  • the solid lines indicate continuous, the dashed lines a discontinuous execution of the corresponding process steps.
  • the product produced in the fluidized bed granulator dryer 4 is cooled down in the fluidized bed cooler 15 before it is placed on a tumbler screen 19.
  • the gut grain arrives at the filling 34; the oversize is fed via a feed 35 and a dosage 36 to a roller mill 25.
  • the oversize can also be collected in a further template 37 and filled into big bags 38 and stored.
  • the big bags can later be emptied in doses (reference number 39) and fed to the roller mill 25.
  • the particularly large oversize is also stored in big bags 40 and later fed to said roller mill 25 or another roller mill 41, the ground product in turn being filled into big bags 42 for later use.
  • the ground product obtained from the roller mill 25 is fed either to the fluidized bed granulation dryer 4 as seed material (line 43) or to the fluidized bed cooler 15 (line 44).
  • the fluidized bed granulation dryer 4 is also supplied with germ material from other sources, namely fine grain from the exhaust gas filter 29, from a silo 45 and from the big bags 42.
  • the table below shows parameters of two process examples according to the invention. Sodium salts were used as sulfates. "Fatty alcohol sulfate” here means sulfates made from a fatty alcohol mixture in the following proportions:
  • Ci2 fatty alcohol 13% by weight
  • the rest of 100% by weight is distributed among other fatty alcohols.

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)
  • Glanulating (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé de production de granulés contenant des tensioactifs, ayant une action de lavage ou de nettoyage ainsi qu'une densité en vrac supérieure à 500 g/l. Ces granulés sont produits à partir d'une forme de préparation tensioactive qui possède des composantes liquides non tensioactives et qui, à une pression normale pour des températures comprises entre 20 et 80 °C, se présente sous une forme liquide à pâteuse. Ce procédé consiste en la granulation et simultanément le séchage dans un lit fluidisé au-dessus d'un fond doté d'ouvertures et destiné au flux affluent de gaz fluidisé. Pour améliorer la rentabilité de ce procédé, les ouvertures sont remplies d'une grille ayant une maille inférieure à 600 νm.
EP98961137A 1997-11-14 1998-11-05 Procede ameliore destine a la production de granules tensioactifs avec une densite en vrac elevee Expired - Lifetime EP1032641B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19750424A DE19750424A1 (de) 1997-11-14 1997-11-14 Verbessertes Verfahren zum Herstellen von Tensidgranulaten mit einem hohen Schüttgewicht
DE19750424 1997-11-14
PCT/EP1998/007060 WO1999025805A2 (fr) 1997-11-14 1998-11-05 Procede ameliore destine a la production de granules tensioactifs avec une densite en vrac elevee

Publications (2)

Publication Number Publication Date
EP1032641A2 true EP1032641A2 (fr) 2000-09-06
EP1032641B1 EP1032641B1 (fr) 2006-08-30

Family

ID=7848693

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98961137A Expired - Lifetime EP1032641B1 (fr) 1997-11-14 1998-11-05 Procede ameliore destine a la production de granules tensioactifs avec une densite en vrac elevee

Country Status (5)

Country Link
US (1) US6362157B1 (fr)
EP (1) EP1032641B1 (fr)
DE (2) DE19750424A1 (fr)
ES (1) ES2272014T3 (fr)
WO (1) WO1999025805A2 (fr)

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DE19820943A1 (de) 1998-05-11 1999-11-18 Henkel Kgaa Alkylsulfat-Granulate
ES2184523T3 (es) * 1998-10-26 2003-04-01 Procter & Gamble Procedimientos para obtener una composicion detergente granular que tiene un aspecto y solubilidad mejoradas.
DE19850100A1 (de) 1998-10-29 2000-05-04 Henkel Kgaa Polymer-Granulate durch Wirbelschichtgranulation
DE19911040A1 (de) * 1999-03-12 2000-09-21 Cognis Deutschland Gmbh Tensidgranulate
US6894018B1 (en) 1999-06-21 2005-05-17 The Procter & Gamble Company Process for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles
DE10003124A1 (de) 2000-01-26 2001-08-09 Cognis Deutschland Gmbh Verfahren zur Herstellung von Tensidgranulaten
DE50011442D1 (de) 2000-02-18 2005-12-01 Glatt Ingtech Gmbh Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten
EP1340806A1 (fr) * 2000-11-08 2003-09-03 Ajinomoto Co., Inc. Agent de surface granulaire et son procede de production
DE10159388A1 (de) * 2001-12-04 2003-06-12 Henkel Kgaa Verfahren zur Herstellung von umhüllten Bleichaktivatorgranulaten
DE10159386A1 (de) 2001-12-04 2003-06-12 Henkel Kgaa Verfahren zur Herstellung von Bleichaktivatorgranulaten
JP2007509188A (ja) * 2003-05-02 2007-04-12 クラリアント・プロドゥクテ・（ドイチュラント）・ゲゼルシャフト・ミト・ベシュレンクテル・ハフツング 顆粒状アンモニウムニトリルの製造方法
CN102435049B (zh) * 2011-10-27 2014-12-31 西王药业有限公司 无水葡萄糖干燥设备及干燥工艺
EP2982486B1 (fr) * 2014-08-04 2018-02-21 Andras Szücs Procédé et appareil pour produire de granulés en matière plastique remodelés, et granulés en matière plastique remodelés ainsi produits
DE102018208932A1 (de) * 2018-06-06 2019-12-12 Glatt Gesellschaft Mit Beschränkter Haftung Anströmboden für einen Fluidisierungsapparat

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Also Published As

Publication number Publication date
DE19750424A1 (de) 1999-05-20
DE59813704D1 (de) 2006-10-12
EP1032641B1 (fr) 2006-08-30
US6362157B1 (en) 2002-03-26
WO1999025805A3 (fr) 1999-07-22
WO1999025805A2 (fr) 1999-05-27
ES2272014T3 (es) 2007-04-16

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