EP1509736A1 - Drying method - Google Patents

Drying method

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Publication number
EP1509736A1
EP1509736A1 EP03714606A EP03714606A EP1509736A1 EP 1509736 A1 EP1509736 A1 EP 1509736A1 EP 03714606 A EP03714606 A EP 03714606A EP 03714606 A EP03714606 A EP 03714606A EP 1509736 A1 EP1509736 A1 EP 1509736A1
Authority
EP
European Patent Office
Prior art keywords
stirrer
vacuum
drying
product
chopper
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
EP03714606A
Other languages
German (de)
French (fr)
Other versions
EP1509736B1 (en
Inventor
Reiner Laible
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.)
Rosenmund VTA AG
Original Assignee
Rosenmund VTA AG
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 Rosenmund VTA AG filed Critical Rosenmund VTA AG
Publication of EP1509736A1 publication Critical patent/EP1509736A1/en
Application granted granted Critical
Publication of EP1509736B1 publication Critical patent/EP1509736B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • F26B21/10—Temperature; Pressure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
    • F26B11/12—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum

Definitions

  • the invention relates to a method for controlling vacuum contact drying in a device with a horizontally arranged, heated cylinder, a stirrer rotating around a very small distance from the wall and a chopper arranged on the stirrer.
  • EP-A-0 203 598 a device for mixing and / or crushing is known. From EP-A-0 753 306 it is known to use this device for drying plant extracts.
  • the device described in this document is designed as a vacuum contact dryer for use in pharmaceutical active ingredient (API) and chemical or fine chemical production and has a horizontally arranged, heated cylinder with a horizontal one around it Axis rotating, heated stirrer
  • the majority of the products to be dried are products from the pharmaceutical active ingredient industry and fine chemicals, which in addition to water usually contain organic solvents that have to be removed or dried to a predetermined residual moisture content.
  • the dry products are subject to further, difficult to meet requirements.
  • the invention has for its object to provide a method which does not have the aforementioned difficulties or significantly reduced compared to previous drying processes and in particular enables the processing of a wide variety of starting products in the sense of achieving similar, short and reproducible drying times with constant product quality.
  • This object is achieved according to the invention in that the course of the product temperature, the vacuum and the instantaneous evaporation capacity are continuously measured and regulated on the basis of the measured values.
  • the method with the suitable device serves to carry out vacuum drying more effectively and in particular makes it possible to mix and distribute very different products so uniformly that a uniform heat input into the product is always achieved.
  • This enables vacuum control, which allows evaporation of solvents or solvent mixtures, which is controllable and uniform at all times. This in turn reduces mechanical loads on the product and the machine and at the same time extends the use of the device to products that were previously difficult to dry, such as suspensions, solutions and lumpy products.
  • a control that can be automatically adapted to the process progress enables various drying parameters to be used as a criterion so that the process remains controllable and controllable at all times. The parameters also provide criteria for the switching conditions of the control, whereby the process can be continuously advanced in such a way that an effective process flow is achieved and which can then also be automated through self-regulation.
  • Fig. 1 is a front view of a dryer consisting of a boiler cylinder, attached filter housing and discharge valve
  • Fig. 2 is a side view of the system
  • Fig. 3 is a perspective view of the stirrer
  • FIG. 4 shows a schematic sectional illustration along the line AA in FIG. 3
  • a so-called IUT dryer known per se is used to carry out the method according to the invention.
  • This has a horizontal axis. turned boiler cylinder 1.
  • the cylinder is similarly designed for heating with double-walled heating channels for channeling the heating medium over the entire cylinder surface.
  • the heating medium is fed separately into up to 3 heating duct units that are combined into chambers. This enables completely uniform heating without significant intermediate cooling of the heating medium when flowing through the channels.
  • the rear wall is heated and the door.
  • the boiler cylinder is equipped with a product entry system and a dust filter 2, which in turn is usually connected to a condenser for solvent recovery with a subsequent vacuum pump.
  • a stirrer 3 is arranged in the boiler cylinder, which is designed as a closed hollow profile with an inserted drive shaft and is also heated.
  • the stirrer drive shaft is also horizontal and coaxial with the boiler axis. Because the bowl cylinder is turned out, a very small distance between the stirrer and the wall of 1-5 mm is possible depending on the size of the machine.
  • the wing sides on the cylinder wall as well as the front and rear are wedge-shaped to ensure that the product is lifted from the cylinder wall, the rear wall and the front door in the direction of rotation. This ensures that practically no or only a very thin product layer can be built up on the wall, which influences the heat input only slightly. This ensures sufficient heat input at all times during the process.
  • the stirrer has a further agitator (chopper) 4 on one side of the blade, which has a much higher speed when the stirrer is driven.
  • This so-called chopper is driven independently of the stirrer at 40-400 times higher speeds. If the stirrer works in the speed range up to 20 min -1 , the chopper reaches up to 800 min -1 and more. Since the chopper is mounted on the stirrer, it constantly rotates with the stirrer and thus always comes to the product to be processed or. runs through the product with the stirrer.
  • the chopper is independent of the direction of rotation, ie it can run in the same direction as the stirrer or can be switched to the opposite direction during the drying process.
  • the chopper's blades have a knife and flat shape.
  • a comb 5 - a so-called stator - can be screwed onto the stirrer blade through which the material is pulled.
  • the wings of the stator have a knife or flat shape like the chopper. This comes into play depending on the direction of rotation of the chopper. This means that in many cases difficult goods can be crushed by hammering and / or cutting and often, if required, grinding of the goods can also be achieved during drying.
  • the stirrer is equipped with a circumferential injection system 6. It is a line provided with nozzles which is attached behind the chopper on the impeller and rotates with the stirrer. Depending on the size of the machine, three to seven nozzles, through which three different types of media can be supplied, are characteristic of the injection line, namely
  • the device equipped in this way is able to dry a wide range of different products, namely from free-flowing products to those containing lumps to liquids (solutions or suspensions).
  • the combination of stirrer, chopper, stator and injection enables the machine to be dynamically adapted to the product properties that change during the drying process in such a way that uniform evaporation and thus short drying times are achieved at all times.
  • the drying is carried out with the device described in batch operation, the product being filled into the cylinder and the stirrer, heating and vacuum then being started.
  • the process sequence is then characterized by the fact that a relatively large amount of solvent is first evaporated and the drying finally takes place from the inside of the product with a corresponding extension of the drying time. Finally, the desired final moisture content in the material is reached and the product can cool down and pressure relief can be discharged through an outlet valve located in the front door.
  • Control criteria are: course of the product temperature, course of the vacuum or evaporation, amount of distillate and heating / cooling temperatures.
  • the product temperature and the amount of distillate are the key parameters that determine the process progress and provide the control parameters for the automatic adjustment.
  • the adjustment is done via the vacuum, to a small extent also via the heating temperature.
  • the speeds of the stirrer and chopper and their direction of rotation are auxiliary variables that are also taken into account.
  • the static, mechanical auxiliary variables are the spacing of the knives from the stator and chopper, which are given before the drying process by appropriate selection.
  • the setting of the parameters that are processed in the control is shown on the basis of the drying curve of a vitamin precursor shown in FIG.
  • Characteristic are the product temperature curve, which shows no waste or only very little waste (max. 3-5 ° C) during drying, as well as the vacuum regulated in stages.
  • the solvent curve shows a steady, rising course, which is typical with appropriate control.
  • the process for effective control can be divided into four to about ten main steps, with step-by-step criteria being defined from step to step.
  • the number of steps depends on the type of product
  • the heating is first set to the maximum temperature that is still permissible for the product, ie the setpoint is set to this value and heating begins.
  • the stirrer and chopper run at medium speeds, the chopper mostly clockwise. This ensures a good mixing effect.
  • the vacuum is set to approx. 500-300 mbar according to the vapor pressure curve of the mostly volatile solvents. It must be ensured that no evaporation takes place that would lead to a lowering of the product temperature.
  • the next process step can be started, ie the start of the evaporation and the actual drying process.
  • the vacuum is set to a value below the boiling point of the most volatile solvent, usually below 300 mbar. This creates a uniform evaporation of solvent from the product, especially as long as the surface moisture is free according to the first
  • Drying section is present.
  • the control By adjusting the vacuum, the control now ensures that the product temperature does not drop or only drops slightly - only then is it ensured that there is no back-condensation of solvent in the product - especially with large filling volumes. This would lead to clumping.
  • By keeping the vacuum too rapid evaporation on the surface of the material with shrinkage of the material or the pores is prevented. If the pores shrink, the liquid transport in the mass transport controlled second drying section would be massively impeded, which leads to very long drying times.
  • control adjusts the vacuum in the sense of a deterioration in order to reduce evaporation and to maintain the open pore condition of the goods or to prevent the goods from shrinking too quickly.
  • This state of constant vacuum is maintained as long as a constant evaporation capacity is maintained and the product temperature remains constant or the increase does not exceed certain limits. If the evaporation capacity drops, the multi-stage process of the actual drying process begins up to the end product (dry product). The vacuum is gradually increased by 20-30 mbar (steps of 10 mbar are also possible and useful depending on the product). The criteria up to the end of the step are, as in the second step, the evaporation capacity and the product temperature. Finally, the last step is to operate with the highest possible vacuum (typically approx. 3-5 mbar) until the required final moisture is reached.
  • the final moisture required for most products is in the range 0.5% - 1.5%.
  • the product temperature has also proven to be a usable criterion here, which - when the material is dry - is equal to the actual value of the jacket heating temperature; provided that a heating temperature has been selected that corresponds to the maximum permissible product temperature.
  • the product is then cooled and emptied.
  • the device With its excellent heat transfer as a result of effective heating (special channels, multiple supply of the medium) and the mixing effect (stirrer, chopper, optionally with stator), the device is the prerequisite for being able to effectively apply the criteria of product temperature, vacuum and evaporation capacity. This applicability has been shown to be applicable to almost all types of products.

Abstract

The vacuum contact drying takes place in a device with a horizontally-arranged heated cylinder ( 1 ), a stirrer circulating with a very small wall separation, a blade ( 4 ) arranged on the stirrer and optionally an injection line ( 6 ), also arranged on the stirrer, for the introduction of liquid, gaseous, or vaporized media. According to the invention, the drying may be controlled whereby the value for the product temperature, the vacuum and the instantaneous evaporation power are continuously measured and regulated on the basis of the measured values.

Description

Trocknungsverfahrendrying process
Die Erfindung betrifft ein Verfahren zur Steuerung einer Vakuumkontakttrocknung in einer Vorrichtung mit einem horizontal angeordneten, beheizten Zylinder, einem mit sehr geringen Wandabstand umlaufenden Rührer und einem am Rührer angeordneten Zerhacker.The invention relates to a method for controlling vacuum contact drying in a device with a horizontally arranged, heated cylinder, a stirrer rotating around a very small distance from the wall and a chopper arranged on the stirrer.
Aus EP-A-0 203 598 ist eine Einrichtung zum Mischen und/oder Zerkleinern bekannt. Aus EP-A-0 753 306 ist es bekannt, diese Einrichtung zur Trocknung von Pflanzenextrakten einzusetzen. Die in diesem Dokument beschriebene Einrichtung ist über das Mischen/Zerkleinern hinaus als Vaku- umkontakttrockner zum Einsatz in der Pharmawirkstoff (API) - und der Chemie- bzw. Feinchemie-Herstellung ausgeführt und besitzt einen horizontal angeordneten, beheizten Zylinder mit einem darin um eine horizontale Achse rotierenden, beheizten RührerFrom EP-A-0 203 598 a device for mixing and / or crushing is known. From EP-A-0 753 306 it is known to use this device for drying plant extracts. In addition to mixing / crushing, the device described in this document is designed as a vacuum contact dryer for use in pharmaceutical active ingredient (API) and chemical or fine chemical production and has a horizontally arranged, heated cylinder with a horizontal one around it Axis rotating, heated stirrer
Bei den zu trocknenden Produkten handelt es sich zum überwiegenden Teil um Produkte der pharmazeutischen Wirkstoffindustrie und der Feinchemie, die neben Wasser meist organische Lösungsmittel enthalten, die zu entfernen oder unter einen vorgegebenen Restfeuchtegehalt zu trocknen sind.The majority of the products to be dried are products from the pharmaceutical active ingredient industry and fine chemicals, which in addition to water usually contain organic solvents that have to be removed or dried to a predetermined residual moisture content.
Alle bisher bekannten Trockner und Verfahren sind dadurch gekennzeichnet, dass zunächst meist relativ lange Trocknungszeiten auftreten. Das Produktspektrum, d.h. die Pro- dukteigenschaften, müssen dabei in einem relativ engen Bereich liegen, also stark standardisiert sein, um dabei überhaupt reproduzierbar in akzeptablen Zeiten trocknen zu können. Einige Produkte, wie beispielsweise Flüssigkeiten (Lösungen oder Suspensionen) sind nicht oder nur unzureichend und nach Anpassungen (Umbauten) zu trocknen.All previously known dryers and processes are characterized in that initially relatively long drying times usually occur. The product range, ie the product properties, must be in a relatively narrow range, ie be highly standardized, in order to be able to dry reproducibly in acceptable times. Some products, such as liquids (Solutions or suspensions) are not or only inadequate and must be dried after adjustments (conversions).
Zumeist stammen die Nassprodukte, die in den Trockner zur Trocknung eingefüllt werden, aus Zentrifugen oder Filter- nutschen. Die Feuchtegehalte dieser Nassprodukte können stark schwanken, auch bei gleichem Produkt. Es sind Feuchtebereiche von 20-50 Gew.% Feuchte oder mehr möglich. Dieser weite Schwankungsbereich erschwert es in konventionellen Verfahren erheblich, ähnliche oder annähernd gleiche Trocknungszeiten für gleiches Gut zu erzielen.Most of the wet products that are put into the dryer for drying come from centrifuges or filter filters. The moisture content of these wet products can fluctuate greatly, even with the same product. Humidity ranges from 20-50 wt.% Moisture or more are possible. This wide fluctuation range makes it considerably more difficult in conventional processes to achieve similar or approximately the same drying times for the same good.
Physikalische Eigenschaften der Produkte (Viskosität, Ag- gregatzustand fest oder flüssig, Schrumpfung) , die sich im Verlauf der Trocknung ergeben oder ändern, kommen hinzu und machen eine vollständige Durchführung der Trocknung auf die gewünschte Endfeuchte in bisher bekannten Systemen oftmals unmöglich oder verlängern die Trocknungszeiten extrem.Physical properties of the products (viscosity, aggregate state solid or liquid, shrinkage), which result or change during the course of drying, are added and often make it completely impossible to carry out the drying to the desired final moisture content in previously known systems or extend the drying times extreme.
An die Trockenprodukte (Fertigprodukte) werden weitere, schwierig zu erfüllende Anforderungen gestellt. Dazu gehören eine möglichst gleichförmige Korngrösse und Kornverteilung (enges Grössenspektru ) , um die Produkte reproduzierbar und standardisierbar machen zu können.The dry products (finished products) are subject to further, difficult to meet requirements. This includes a grain size and grain distribution that is as uniform as possible (narrow size spectrum) in order to make the products reproducible and standardizable.
Dies sind Anforderungen, die bisher nur unzureichend erfüllt wurden. Oft ist ein hoher Zusatzaufwand (Nachtrocknung, Mahlung, Granulierung) erforderlich, um diese Anforderungen zu erreichen.These are requirements that have so far been insufficiently met. A lot of additional effort (post-drying, grinding, granulation) is often required to achieve these requirements.
Ein weiteres wichtiges und oftmals unabdingbares Kriterium bei der Herstellung von aktiven Wirkstoffen und feinchemischen Produkten ist die Reproduzierbarkeit der Trocknungsergebnisse. Damit ist das Erreichen nahezu identischer Trocknungszeiten für gleiches Produkt gemeint, das aber in der Gesamtheit aus mehreren Batchtrocknungen auf gleichem Apparat stammt. Zu diesen Eigenschaften zählen u.a. Endfeuchte, Farbe und Feinheit des Gutes sowie Erhaltung der chemisch-pharmazeutischen Wirksamkeit. Indirekte Eigenschaften sind dabei Trocknungszeit und Energieverbrauch.Another important and often indispensable criterion in the production of active ingredients and fine chemical products is the reproducibility of the drying results. The achievement is almost identical Drying times are meant for the same product, but which as a whole comes from several batch drying operations on the same apparatus. These properties include final moisture, color and fineness of the goods as well as preservation of the chemical-pharmaceutical effectiveness. Indirect properties are drying time and energy consumption.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren zu schaffen, welches die vorgenannten Schwierigkeiten nicht aufweist bzw. gegenüber bisherigen Trocknungsverfahren deutlich reduziert und insbesondere die Bearbeitung unterschiedlichster Ausgangsprodukte im Sinne des Erzielens einander ähnlicher, kurzer und reproduzierbarer Trocknungszeiten bei gleichbleibender Produktqualität ermöglicht.The invention has for its object to provide a method which does not have the aforementioned difficulties or significantly reduced compared to previous drying processes and in particular enables the processing of a wide variety of starting products in the sense of achieving similar, short and reproducible drying times with constant product quality.
Diese Aufgabe wird gemäss der Erfindung dadurch gelöst, dass der Verlauf der Produkttemperatur, das Vakuum und die momentane Verdampfungsleistung kontinuierlich gemessen und aufgrund der Messwerte geregelt werden.This object is achieved according to the invention in that the course of the product temperature, the vacuum and the instantaneous evaporation capacity are continuously measured and regulated on the basis of the measured values.
Das Verfahren mit der dafür geeigneten Einrichtung dienen dazu, Vakuumtrocknungen effektiver durchzuführen und ermöglicht es insbesondere, sehr verschiedenartige Produkte so gleichmässig zu mischen und zu verteilen, dass ein stets gleichförmiger Wärmeeintrag in das Produkt erzielt wird. Dadurch wird eine Vakuumsteuerung ermöglicht, die eine zu jedem Zeitpunkt kontrollierbare und gleichmässige Abdampfung von Lösungsmittel oder auch Lösungsmittelgemischen erlaubt. Dies wiederum vermindert mechanische Belastungen auf Produkt und Maschine und erweitert gleichzeitig damit den Einsatz der Einrichtung auf bisher schwierig zu trocknende Produkte wie Suspensionen, Lösungen und klumpige Produkte. Eine dem Prozessfortschritt automatisch anpassbare Steuerung ermöglicht es, verschiedene Trocknungsparameter so als Kriterium einzusetzen, dass der Prozess zu jeder Zeit beherrschbar und steuerbar bleibt. Die Parameter liefern zudem Kriterien für Weiterschaltbedingungen der Steuerung, wodurch der Prozess kontinuierlich so voran gebracht werden kann, dass ein effektiver Prozessablauf erreicht wird und welcher dann auch automatisiert werden kann durch eine Selbstregelung .The method with the suitable device serves to carry out vacuum drying more effectively and in particular makes it possible to mix and distribute very different products so uniformly that a uniform heat input into the product is always achieved. This enables vacuum control, which allows evaporation of solvents or solvent mixtures, which is controllable and uniform at all times. This in turn reduces mechanical loads on the product and the machine and at the same time extends the use of the device to products that were previously difficult to dry, such as suspensions, solutions and lumpy products. A control that can be automatically adapted to the process progress enables various drying parameters to be used as a criterion so that the process remains controllable and controllable at all times. The parameters also provide criteria for the switching conditions of the control, whereby the process can be continuously advanced in such a way that an effective process flow is achieved and which can then also be automated through self-regulation.
Im folgenden wird anhand der beiliegenden Zeichnungen ein Ausführungsbeispiel der Erfindung beschrieben. Es zeigenIn the following an embodiment of the invention will be described with reference to the accompanying drawings. Show it
Fig. 1 eine Frontansicht eines Trockners bestehend aus Kesselzylinder, aufgesetztem Filtergehäuse und AustragsventilFig. 1 is a front view of a dryer consisting of a boiler cylinder, attached filter housing and discharge valve
Fig. 2 eine Seitenansicht der AnlageFig. 2 is a side view of the system
Fig. 3 eine perspektivische Ansicht des Rührers mitFig. 3 is a perspective view of the stirrer
Zerhacker, Stator und Eindüsungsleitung als wichtigsten Bauteilen.Chopper, stator and injection line as the most important components.
Fig. 4 eine schematische Schnittdarstellung entlang der Linie A - A in Fig. 3FIG. 4 shows a schematic sectional illustration along the line AA in FIG. 3
Fig. 5 eine typische Trocknungsverlaufskurve mit Kondensatmengenverlauf, Produkttemperaturverlauf, Heiztemperaturverlauf und Vakuum- verlauf.5 shows a typical drying curve with condensate quantity curve, product temperature curve, heating temperature curve and vacuum curve.
Zur Durchführung des erfindungsgemässen Verfahrens kommt ein an sich bekannter sog. IUT-Trockner zum Einsatz. Dieser besitzt einen mit horizontaler Achse angeordneten ausge- drehten Kesselzylinder 1. Der Zylinder ist zur Beheizung doppelwandig ähnlich ausgeführt mit aufgeschweissten Heizkanälen zur Kanalisierung des Heizmediums vollflächig über die gesamte Zylinderfläche. Je nach Grosse der Maschine wird das Heizmedium getrennt in bis zu 3 zu Kammern zusammengeführten Heizkanaleinheiten zugeführt. Damit ist eine vollkommen gleichmässige Beheizung möglich ohne erhebliche Zwischenabkühlung des Heizmediums beim Durchströmen der Kanäle. Darüber hinaus ist die Rückwand beheizt sowie die Tü- re.A so-called IUT dryer known per se is used to carry out the method according to the invention. This has a horizontal axis. turned boiler cylinder 1. The cylinder is similarly designed for heating with double-walled heating channels for channeling the heating medium over the entire cylinder surface. Depending on the size of the machine, the heating medium is fed separately into up to 3 heating duct units that are combined into chambers. This enables completely uniform heating without significant intermediate cooling of the heating medium when flowing through the channels. In addition, the rear wall is heated and the door.
Der Kesselzylinder ist mit einem Produkteintragsystem und einem Staubfilter 2 ausgerüstet, welches üblicherweise wiederum an einen Kondensator zur Lösungsmittelrückgewinnung mit darauf folgender Vakuumpumpe angeschlossen ist. Im Kesselzylinder ist ein Rührer 3 angeordnet, der als geschlossenes Hohlprofil mit eingeschobener Antriebswelle ausgebildet und ebenfalls beheizt ist. Die Antriebswelle des Rührers ist ebenfalls horizontal und koaxial mit der Kessel- achse angeordnet. Dadurch, dass der Kesselzylinder ausgedreht ist, ist ein sehr geringer Abstand zwischen Rührer und Wand von 1-5 mm je nach Baugrösse der Maschine möglich. Die Flügelseiten an der Zylinderwand sowie Front- und Rückseite sind keilförmig gebaut, um in Drehrichtung ein Abhe- ben des Produktes von der Zylinderwand, der Rückwand und der Fronttüre zu gewährleisten. Somit wird sichergestellt, dass praktisch keine oder nur eine sehr dünne Produktschicht an der Wand aufgebaut werden kann, die den Wärmeeintrag nur wenig beeinflusst. So ist zu jedem Zeitpunkt des Prozesses stets ein ausreichender Wärmeeintrag sichergestellt .The boiler cylinder is equipped with a product entry system and a dust filter 2, which in turn is usually connected to a condenser for solvent recovery with a subsequent vacuum pump. A stirrer 3 is arranged in the boiler cylinder, which is designed as a closed hollow profile with an inserted drive shaft and is also heated. The stirrer drive shaft is also horizontal and coaxial with the boiler axis. Because the bowl cylinder is turned out, a very small distance between the stirrer and the wall of 1-5 mm is possible depending on the size of the machine. The wing sides on the cylinder wall as well as the front and rear are wedge-shaped to ensure that the product is lifted from the cylinder wall, the rear wall and the front door in the direction of rotation. This ensures that practically no or only a very thin product layer can be built up on the wall, which influences the heat input only slightly. This ensures sufficient heat input at all times during the process.
Der Rührer besitzt auf einer Flügelseite ein weiteres Rührorgan (Zerhacker) 4, das mit wesentlich höherer Drehzahl als der Rührer angetrieben wird. Dieser sog. Zerhacker wird unabhängig vom Rührer mit 40-400 mal höheren Drehzahlen angetrieben. Wenn also der Rührer im Drehzahlbereich bis 20 min-1 arbeitet, erreicht der Zerhacker bis zu 800 min-1 und mehr. Da der Zerhacker auf dem Rührer montiert ist, läuft er ständig mit dem Rührer um und kommt so immer zu dem zu bearbeitenden Produkt resp. läuft mit dem Rührer durch das Produkt. Der Zerhacker ist drehrichtungsunabhängig, d.h. er kann mit gleicher Drehrichtung wie der Rührer laufen oder auch während des Trocknungsprozesses auf Gegendrehsinn umgeschaltet werden. Die Flügel des Zerhackers besitzen Messer- und Flachform.The stirrer has a further agitator (chopper) 4 on one side of the blade, which has a much higher speed when the stirrer is driven. This so-called chopper is driven independently of the stirrer at 40-400 times higher speeds. If the stirrer works in the speed range up to 20 min -1 , the chopper reaches up to 800 min -1 and more. Since the chopper is mounted on the stirrer, it constantly rotates with the stirrer and thus always comes to the product to be processed or. runs through the product with the stirrer. The chopper is independent of the direction of rotation, ie it can run in the same direction as the stirrer or can be switched to the opposite direction during the drying process. The chopper's blades have a knife and flat shape.
Optional kann auf der Zerhackerseite des Rührers ein Kamm 5 - ein sog. Stator - auf dem Rührerflügel angeschraubt sein, durch den das Gut hindurchgezogen wird. Die Flügel des Stators weisen Messer- bzw. Flachform wie der Zerhacker auf. Dies kommt je nach Drehrichtung des Zerhackers zur Geltung. Damit kann in vielen Fällen schwieriges Gut durch Hämmern und/oder Schneiden zerkleinert und damit während der Trocknung oftmals auch, falls gefordert, eine Mahlung des Gutes erreicht werden.Optionally, on the chopper side of the stirrer, a comb 5 - a so-called stator - can be screwed onto the stirrer blade through which the material is pulled. The wings of the stator have a knife or flat shape like the chopper. This comes into play depending on the direction of rotation of the chopper. This means that in many cases difficult goods can be crushed by hammering and / or cutting and often, if required, grinding of the goods can also be achieved during drying.
Des weiteren ist der Rührer mit einem umlaufenden Eindü- sungssystem 6 ausgerüstet. Dabei handelt es sich um eine mit Düsen versehene Leitung die hinter dem Zerhacker auf dem Rührflügel angebracht ist und mit dem Rührer umläuft. Charakteristisch für die Eindüsungsleitung sind je nach Ma- schinengrösse drei bis sieben Düsen, durch die drei ver- schiedene Medienarten zugeführt werden können, nämlichFurthermore, the stirrer is equipped with a circumferential injection system 6. It is a line provided with nozzles which is attached behind the chopper on the impeller and rotates with the stirrer. Depending on the size of the machine, three to seven nozzles, through which three different types of media can be supplied, are characteristic of the injection line, namely
Flüssigkeiten, Gase oder Dampf. Damit sind Benetzung (Granulierung) , Befeuchtung und Restfeuchteaustrag mittels Gasen als Schleppgasen zur Erzielung niedrigster Endfeuchten möglich. Mit dieser Anordnung sind sowohl Produktaufwirbelung als auch Produkteinzug möglich. Phasenänderungen (flüssig/fest) wie auch Klumpenbildung kann damit frühzeitig effektiv be- gegnet bzw. diese verhindert werden. Dadurch wird über den gesamten Prozess ein für die Verdampfung gleich ässiger Produktzustand aufrechterhalten. Verbunden mit den extrem geringen Wandabständen (1-5 mm je nach Maschinengrösse) ergibt sich ein gleichmässiger Wärmeeintrag in das Gut, aus dem kurze Trocknungszeiten resultieren. Der Wärmeeintrag setzt sich dabei aus dem Übergang Wand zu Haufwerk, Wärmetransport im Haufwerk und Übertragung zwischen den Einzelpartikeln zusammen. Durch die Zerhackerwirkung wird ein gleichmässig feines Gut hergestellt.Liquids, gases or steam. This enables wetting (granulation), humidification and residual moisture discharge using gases as trailing gases to achieve the lowest final moisture levels. With this arrangement, both product swirling and product intake are possible. Phase changes (liquid / solid) as well as clump formation can thus be effectively countered at an early stage or prevented. This maintains a uniform product condition for evaporation throughout the entire process. Combined with the extremely small wall clearances (1-5 mm depending on the machine size), there is even heat input into the goods, which results in short drying times. The heat input is made up of the transition from the wall to the aggregate, heat transport in the aggregate and transfer between the individual particles. The chopper effect produces an evenly fine material.
Die so ausgerüstete Einrichtung ist in der Lage, ein weites Spektrum unterschiedlichster Produkte zu trocknen, nämlich von rieselfähigen Produkten über solche, die Klumpen enthalten bis zu Flüssigkeiten (Lösungen oder Suspensionen) . Die Kombination aus Rührer, Zerhacker, Stator und Eindüsung ermöglicht es, die Maschine den sich während des Trocknungsvorgangs ändernden Produkteigenschaften dynamisch so anzupassen, dass jederzeit eine gleichmässige Verdampfung und damit kurze Trocknungszeit erreicht wird.The device equipped in this way is able to dry a wide range of different products, namely from free-flowing products to those containing lumps to liquids (solutions or suspensions). The combination of stirrer, chopper, stator and injection enables the machine to be dynamically adapted to the product properties that change during the drying process in such a way that uniform evaporation and thus short drying times are achieved at all times.
Die Trocknungen werden mit der beschriebenen Einrichtung im Chargenbetrieb durchgeführt, wobei das Produkt in den Zylinder eingefüllt wird und anschliessend Rührer, Heizung und Vakuum gestartet werden. Der Prozessablauf ist dann da- durch gekennzeichnet, dass zunächst relativ viel Lösungsmittel abgedampft wird und die Trocknung schliesslich aus dem Produktinneren erfolgt mit entsprechender Verlängerung der Trocknungszeit. Schliesslich wird die gewünschte Endfeuchte im Gut erreicht und das Produkt kann nach Abkühlung und Druckentlastung durch ein in der Fronttüre befindliches Auslassventil entladen werden.The drying is carried out with the device described in batch operation, the product being filled into the cylinder and the stirrer, heating and vacuum then being started. The process sequence is then characterized by the fact that a relatively large amount of solvent is first evaporated and the drying finally takes place from the inside of the product with a corresponding extension of the drying time. Finally, the desired final moisture content in the material is reached and the product can cool down and pressure relief can be discharged through an outlet valve located in the front door.
Das Zusammenspiel der Komponenten Trockner, Vakuumsystem mit Kondensation und Heizung/Kühlung erfolgt gemäss einer Steuerung, die es erlaubt, die üblichen Prozessschritte Be- füllen, Aufheizen, Verdampfen und Trocknen, Abkühlen, Pro- duktaustrag optimal zu kombinieren. Kriterien sind dabei die Veränderungen der Produkteigenschaften, welche die Steuerung indirekt erfasst, verarbeitet und Einstellungen anpasst .The interaction of the components dryer, vacuum system with condensation and heating / cooling takes place according to a control system that allows the usual process steps of filling, heating, evaporating and drying, cooling, and product discharge to be optimally combined. Criteria are the changes in product properties, which the control indirectly captures, processes and adjusts settings.
Steuerungskriterien sind dabei: Verlauf der Produkttemperatur, Verlauf des Vakuums bzw. der Verdampfung, Destillat- menge sowie Heiz/Kühltemperaturen. Produkttemperatur und Destillatmenge stellen dabei die Schlüsselgrössen dar, die den Prozessfortschritt bestimmen und die der Steuerung Kenngrössen für die automatische Anpassung liefern. Die Anpassung erfolgt dabei über das Vakuum, zu geringem Teil auch über die Heiztemperatur. Die Drehzahlen von Rührer und Zerhacker sowie dessen Drehrichtung sind dabei Hilfsgrös- sen, die ebenfalls berücksichtigt werden. Als statischmechanische weitere Hilfsgrössen kommen die Abstände der Messer von Stator und Zerhacker hinzu, die durch entspre- chende Auswahl bereits vor der Trocknung gegeben sind.Control criteria are: course of the product temperature, course of the vacuum or evaporation, amount of distillate and heating / cooling temperatures. The product temperature and the amount of distillate are the key parameters that determine the process progress and provide the control parameters for the automatic adjustment. The adjustment is done via the vacuum, to a small extent also via the heating temperature. The speeds of the stirrer and chopper and their direction of rotation are auxiliary variables that are also taken into account. The static, mechanical auxiliary variables are the spacing of the knives from the stator and chopper, which are given before the drying process by appropriate selection.
Anhand der in Fig.4 gezeigten Trocknungsverlaufskurven einer Vitaminvorstufe wird die Einstellung der Parameter dargestellt, die in der Steuerung verarbeitet werden. Dieser Trocknungsverlauf ist typisch für die genannten Produktgattungen aktive Wirkstoffe (API = active pharmaceuti- cal ingredients, z. B. Antibiotika, Antihistaminika etc.) und Feinchemikalien, sowie Zwischenprodukte, welcher mit- tels der genannten Einrichtung und der angewendeten Steuerungskriterien erreicht wird.The setting of the parameters that are processed in the control is shown on the basis of the drying curve of a vitamin precursor shown in FIG. This course of drying is typical of the product types of active ingredients mentioned (API = active pharmaceutical ingredients, e.g. antibiotics, antihistamines etc.) and fine chemicals, as well as intermediate products which by means of the facility mentioned and the control criteria applied.
Auf der Abszisse ist die Trocknungszeit in min, auf der linken Ordinate sind Vakuum (mbar) und Temperaturen (Heiztemperatur, Produkttemperatur, Brüdentemperatur) dargestellt. Schliesslich zeigt die rechte Ordinate die absolut abgedampfte Lösungsmittelmenge in Liter an.The drying time in minutes is shown on the abscissa, vacuum (mbar) and temperatures (heating temperature, product temperature, vapor temperature) are shown on the left ordinate. Finally, the right ordinate shows the absolutely evaporated amount of solvent in liters.
Charakteristisch sind der Produkttemperaturverlauf, der keinen Abfall bzw. nur sehr geringe Abfälle (max. 3-5 °C) während der Trocknung zeigt, sowie das in Stufen einregulierte Vakuum. Die Lösungsmittelkurve zeigt einen gleich- massigen, ansteigenden Verlauf, welcher typisch ist bei entsprechender Steuerung.Characteristic are the product temperature curve, which shows no waste or only very little waste (max. 3-5 ° C) during drying, as well as the vacuum regulated in stages. The solvent curve shows a steady, rising course, which is typical with appropriate control.
Das Verfahren zur effektiven Steuerung lässt sich in vier bis ca. zehn Hauptschritte unterteilen, wobei sich von Schritt zu Schritt Weiterschaltkriterien definieren lassen. Die Zahl der Schritte ist von der Art des Produktes, demThe process for effective control can be divided into four to about ten main steps, with step-by-step criteria being defined from step to step. The number of steps depends on the type of product
Lösungsmittel und dessen Verdampfungscharakteristik (Dampfdruckkurve) abhängig.Solvent and its evaporation characteristics (vapor pressure curve) dependent.
Nach dem Einfüllen wird zunächst die Heizung auf die maxi- mal für das Produkt noch zulässige Temperatur eingestellt, d.h. der Sollwert wird auf diesen Wert gesetzt und die Aufheizung beginnt. Rührer und Zerhacker laufen bei mittleren Drehzahlen, der Zerhacker zumeist im Uhrzeigersinn. Damit ist eine gute Mischwirkung sichergestellt. Gleichzeitig wird das Vakuum aus Sicherheitsgründen entsprechend der Dampfdruckkurve der meist leichtflüchtigen Lösungsmittel auf ca. 500-300 mbar eingestellt. Dabei ist sicherzustellen, dass noch keine Verdampfung stattfindet, die zu einer Absenkung der Produkttemperatur führen würde. Wenn die Produkttemperatur schliesslich etwa 30 °C (+- 2°C) erreicht hat und damit Energie in das Produkt eingetragen wurde, kann der nächste Verfahrensschritt gestartet werden, d.h. der Beginn der Verdampfung und des eigentlichen Trocknungsvorgangs. Das Vakuum wird auf einen Wert unterhalb des Siedepunktes des leichtestflüchtigen Lösungsmittels eingestellt, meist unter 300 mbar. Damit entsteht eine gleich- massige Lösungsmittelverdampfung aus dem Produkt, besonders solange freie Oberflächenfeuchte entsprechend dem erstenAfter filling, the heating is first set to the maximum temperature that is still permissible for the product, ie the setpoint is set to this value and heating begins. The stirrer and chopper run at medium speeds, the chopper mostly clockwise. This ensures a good mixing effect. At the same time, for safety reasons, the vacuum is set to approx. 500-300 mbar according to the vapor pressure curve of the mostly volatile solvents. It must be ensured that no evaporation takes place that would lead to a lowering of the product temperature. When the product temperature has finally reached approximately 30 ° C (+ - 2 ° C) and energy has thus been introduced into the product, the next process step can be started, ie the start of the evaporation and the actual drying process. The vacuum is set to a value below the boiling point of the most volatile solvent, usually below 300 mbar. This creates a uniform evaporation of solvent from the product, especially as long as the surface moisture is free according to the first
Trocknungsabschnitt vorliegt. Die Steuerung sorgt nun durch Einstellung des Vakuums dafür, dass die Produkttemperatur nicht oder nur leicht absinkt - nur dann ist sichergestellt, dass im Produkt - speziell bei grossen Füllvolumina - keine Rückkondensation von Lösungsmittel erfolgt. Diese würde zu Verklumpungen führen. Weiterhin wird durch Halten des Vakuums eine zu schnelle Verdampfung an der Gutsoberfläche mit Schrumpfung des Gutes bzw. der Poren verhindert. Bei Schrumpfung der Poren würde der Flüssigkeits- transport im Stofftransport kontrollierten zweiten Trocknungsabschnitt massiv behindert, was zu sehr langen Trocknungszeiten führt.Drying section is present. By adjusting the vacuum, the control now ensures that the product temperature does not drop or only drops slightly - only then is it ensured that there is no back-condensation of solvent in the product - especially with large filling volumes. This would lead to clumping. By keeping the vacuum, too rapid evaporation on the surface of the material with shrinkage of the material or the pores is prevented. If the pores shrink, the liquid transport in the mass transport controlled second drying section would be massively impeded, which leads to very long drying times.
Sollte trotzdem die Produkttemperatur unter eine gewisse Grenze absinken, passt die Steuerung das Vakuum im Sinne einer Verschlechterung an, um die Verdampfung zu verringern und den offenen Porenzustand des Gutes aufrecht zu erhalten bzw. eine zu schnelle Schrumpfung des Gutes zu verhindern.Should the product temperature nevertheless fall below a certain limit, the control adjusts the vacuum in the sense of a deterioration in order to reduce evaporation and to maintain the open pore condition of the goods or to prevent the goods from shrinking too quickly.
Dieser Zustand konstanten Vakuums wird so lange beibehalten, wie zum einen eine konstante Verdampfungsleistung aufrechterhalten wird und zum anderen die Produkttemperatur konstant bleibt bzw. der Anstieg gewisse Grenzen nicht überschreitet . Bei Abfallen der Verdampfungsleistung beginnt der mehrstufige Ablauf der eigentlichen Trocknung bis zum Endprodukt (Trockenprodukt) . Das Vakuum wird schrittweise um 20-30 mbar (Schritte von 10 mbar sind auch möglich und sinnvoll je nach Produkt) erhöht. Die Kriterien bis zum Schrittende sind dann wieder wie beim zweiten Schritt die Verdampfungsleistung und die Produkttemperatur. Schliesslich wird im letzten Schritt mit höchst möglichem Vakuum gefahren (typi- scherweise ca. 3-5 mbar), bis die geforderte Endfeuchte erreicht ist.This state of constant vacuum is maintained as long as a constant evaporation capacity is maintained and the product temperature remains constant or the increase does not exceed certain limits. If the evaporation capacity drops, the multi-stage process of the actual drying process begins up to the end product (dry product). The vacuum is gradually increased by 20-30 mbar (steps of 10 mbar are also possible and useful depending on the product). The criteria up to the end of the step are, as in the second step, the evaporation capacity and the product temperature. Finally, the last step is to operate with the highest possible vacuum (typically approx. 3-5 mbar) until the required final moisture is reached.
Für die meisten Produkte liegt die geforderte Endfeuchte im Bereich 0.5% - 1.5%. Hierbei hat sich als verwendbares Kri- terium auch die Produkttemperatur erwiesen, die - wenn das Gut trocken ist - gleich dem Ist-Wert der Mantel- Heiztemperatur ist; vorausgesetzt es wurde eine Heiztemperatur gewählt, die der maximal zulässigen Produkttemperatur entspricht .The final moisture required for most products is in the range 0.5% - 1.5%. The product temperature has also proven to be a usable criterion here, which - when the material is dry - is equal to the actual value of the jacket heating temperature; provided that a heating temperature has been selected that corresponds to the maximum permissible product temperature.
Abschliessend erfolgen die Abkühlung und die Entleerung des Produktes .The product is then cooled and emptied.
Die Einrichtung stellt mit ihrem ausgezeichneten Wärmeüber- gang infolge effektiver Beheizung (Spezialkanäle, Mehrfachzuführung des Mediums) und der Mischwirkung (Rührer, Zerhacker, optional mit Stator) die Voraussetzung dar, die genannten Kriterien Produkttemperatur, Vakuum und Verdampfungsleistung effektiv anwenden zu können. Diese Anwendbar- keit hat sich als auf nahezu alle Arten von Produkten übertragbar gezeigt.With its excellent heat transfer as a result of effective heating (special channels, multiple supply of the medium) and the mixing effect (stirrer, chopper, optionally with stator), the device is the prerequisite for being able to effectively apply the criteria of product temperature, vacuum and evaporation capacity. This applicability has been shown to be applicable to almost all types of products.
Einschränkungen gibt es nur von Produkten, die einen dritten Trocknungsabschnitt aufweisen, also alle die Kristallfeuchte und chemisch gebundenes Wasser aufweisen. Hier ist allein die Höhe der Temperatur und die Einwirkungszeit massgebend. Nur in geringem Umfang wirken sich dabei Mischung und Vakuum aus. There are only restrictions for products that have a third drying section, i.e. all that contain crystal moisture and chemically bound water. Here is only the height of the temperature and the exposure time are decisive. Mixing and vacuum only have a minor effect.

Claims

Patentansprüche claims
1. Verfahren zur Steuerung einer Vakuumkontakttrocknung in einer Vorrichtung mit einem horizontal angeordneten, beheizten Zylinder, einem mit sehr geringen Wandabstand umlaufenden Rührer, einem am Rührer angeordneten Zerhacker und einer ebenfalls am Rührer angeordneten Eindüsleitung zum Einbringen flüssiger, gasförmi- ger oder dampfförmiger Medien, dadurch gekennzeichnet, dass der Verlauf der Produkttemperatur und das Vakuum kontinuierlich gemessen und aufgrund der Messwerte geregelt werden.1. Method for controlling vacuum contact drying in a device with a horizontally arranged, heated cylinder, a stirrer rotating around a very small distance from the wall, a chopper arranged on the stirrer and a spray line also arranged on the stirrer for introducing liquid, gaseous or vaporous media, thereby characterized that the course of the product temperature and the vacuum are continuously measured and regulated based on the measured values.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die momentane Verdampfungsleistung gemessen und als Regelgrösse verwendet wird.2. The method according to claim 1, characterized in that the instantaneous evaporation power is measured and used as a control variable.
3. Verfahren nach einem der Ansprüche 1-2, dadurch ge- kennzeichnet, dass das feuchte Ausgangsgut nach dem3. The method according to any one of claims 1-2, characterized in that the moist starting material after the
Einfüllen in die Einrichtung zerkleinert und homogenisiert wird.Filling into the facility is crushed and homogenized.
4. Verfahren nach Anspruch 3 , dadurch gekennzeichnet, dass die Verdampfungsleistung konstant gehalten wird, um eine kurze Trocknungszeit unabhängig von der Art des Ausgangsgutes zu erzielen.4. The method according to claim 3, characterized in that the evaporation rate is kept constant in order to achieve a short drying time regardless of the type of starting material.
5. Verfahren nach einem der Ansprüche 1 - 4 , dadurch gekennzeichnet, dass das Vakuum stufenförmig abgesenkt und dadurch während der gesamten Trocknung die Verdampfungsleistung konstant gehalten wird. 5. The method according to any one of claims 1-4, characterized in that the vacuum is lowered stepwise and thereby the evaporation rate is kept constant during the entire drying.
6. Verfahren nach einem der Ansprüche 1 - 5 , dadurch gekennzeichnet, dass die Gutstemperatur zur Bestimmung der Restfeuchte gemessen wird.6. The method according to any one of claims 1-5, characterized in that the good temperature is measured to determine the residual moisture.
7. Verfahren nach einem der Ansprüche 1 - 6, dadurch gekennzeichnet, dass ein Schleppgas direkt in das Produkt eingeleitet wird, um Restfeuchten im ppm Bereich zu erzielen.7. The method according to any one of claims 1-6, characterized in that an entraining gas is introduced directly into the product in order to achieve residual moisture in the ppm range.
8. Vorrichtung zur Vakuumkontakttrocknung mit einem horizontal angeordneten, beheizten Zylinder, einem mit sehr geringen Wandabstand umlaufenden Rührer und einem am Rührer angeordneten Zerhacker, gekennzeichnet durch Mittel zur kontinuierlichen Messung des Verlaufs der Produkttemperatur und des Vakuums und zur Regelung dieser Parameter.8. Device for vacuum contact drying with a horizontally arranged, heated cylinder, a stirrer rotating around a very small distance from the wall and a chopper arranged on the stirrer, characterized by means for continuously measuring the course of the product temperature and the vacuum and for regulating these parameters.
9. Vorrichtung nach Anspruch 8, gekennzeichnet durch eine ebenfalls am Rührer angeordnete Eindüsleitung zum Einbringen flüssiger, gasförmiger oder dampfförmiger Medien9. The device according to claim 8, characterized by a also arranged on the stirrer injection line for introducing liquid, gaseous or vaporous media
10. Verwendung einer Vorrichtung mit einem horizontal angeordneten, beheizten Zylinder, einem mit sehr ge- ringen Wandabstand umlaufenden Rührer, einem am Rührer angeordneten Zerhacker, sowie Mitteln zur Messung und Regelung des Verlaufs der Produkttemperatur und des Vakuums zur Vakuumkontakttrocknung. 10. Use of a device with a horizontally arranged, heated cylinder, a stirrer rotating with a very small wall clearance, a chopper arranged on the stirrer, and means for measuring and regulating the course of the product temperature and the vacuum for vacuum contact drying.
EP03714606A 2002-05-02 2003-04-30 Drying method Expired - Lifetime EP1509736B1 (en)

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US4183673A (en) * 1976-02-23 1980-01-15 The Gillette Company Marbleization of plastic materials
US4876802A (en) * 1983-12-21 1989-10-31 Gerhard Gergely Process and means for the heat treatment of powdery or granulate material
DE3470665D1 (en) * 1983-12-21 1988-06-01 Gergely Gerhard Process and apparatus for treating a powder or a granulate by applying heat
DE3519613A1 (en) * 1985-05-31 1986-12-04 Killer Verfahrenstechnik Dr DEVICE FOR MIXING AND / OR MILLING
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