EP1509736B1 - Drying method - Google Patents

Drying method Download PDF

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Publication number
EP1509736B1
EP1509736B1 EP03714606A EP03714606A EP1509736B1 EP 1509736 B1 EP1509736 B1 EP 1509736B1 EP 03714606 A EP03714606 A EP 03714606A EP 03714606 A EP03714606 A EP 03714606A EP 1509736 B1 EP1509736 B1 EP 1509736B1
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EP
European Patent Office
Prior art keywords
vacuum
drying
product
agitator
stirrer
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EP03714606A
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German (de)
French (fr)
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EP1509736A1 (en
Inventor
Reiner Laible
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Rosenmund VTA AG
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Rosenmund VTA AG
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    • 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 a vacuum contact drying in a device with a horizontally arranged, heated cylinder, a rotating with a very small wall distance stirrer and arranged on a stirrer chopper.
  • 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 the drying of plant extracts.
  • the device described in this document in addition to mixing / crushing, is a vacuum contact dryer for use in pharmaceutical drug (API) and chemical or fine chemical manufacturing, and has a horizontally disposed, heated cylinder with one rotating about a horizontal axis therein , heated stirrer
  • the products to be dried are predominantly products of the pharmaceutical active ingredient industry and fine chemicals, which in addition to water usually contain organic solvents which are to be removed or dried under a predetermined residual moisture content.
  • the wet products which are filled into the dryer for drying, come from centrifuges or filter nipples.
  • the moisture content of these wet products can fluctuate greatly, even with the same product.
  • Moisture ranges of 20-50% by weight of moisture or more are possible. This wide fluctuation range makes it considerably more difficult in conventional processes to achieve similar or approximately equal drying times for the same product.
  • Dry products are subject to further difficult-to-fulfill requirements. These include the most uniform grain size and particle size distribution possible (narrow range of sizes) in order to make the products reproducible and standardisable.
  • the invention has for its object to provide a method which does not have the aforementioned difficulties or significantly reduced compared to previous drying methods and in particular allows the processing of different starting materials in the sense of achieving similar, short and reproducible drying times while maintaining product quality.
  • This object is achieved according to the invention in that the course of the product temperature, the vacuum and the instantaneous evaporation rate are continuously measured and controlled on the basis of the measured values.
  • the method with the device suitable for this purpose is used to perform vacuum drying more effectively and makes it possible, in particular, to mix and distribute very varied products evenly, so that an always uniform heat input into the product is achieved.
  • This allows a vacuum control, which allows a controllable and uniform at any time evaporation of solvent or solvent mixtures. This, in turn, reduces mechanical stresses on the product and the machine and at the same time expands the use of the device to previously difficult to dry products such as suspensions, solutions and lumpy products.
  • a control that can be automatically adapted to the progress of the process makes it possible to use different drying parameters as criteria so that the process remains manageable and controllable at all times.
  • the parameters also provide criteria for control overshoot conditions, allowing the process to be continually advanced to achieve an effective process flow and which can then be automated through self-regulation.
  • a so-called IUT dryer known per se is used.
  • This has a arranged with a horizontal axis turned out Boiler cylinder 1.
  • the cylinder is designed for heating double-walled similar with welded Thompsonälen for channeling the heating medium over the entire surface over the entire cylindrical surface.
  • the heating medium is fed separately into up to 3 combined heating chamber units. For a completely uniform heating is possible 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 introduction system and a dust filter 2, which in turn is usually connected to a solvent recovery condenser followed by a vacuum pump.
  • a stirrer 3 is arranged, which is designed as a closed hollow profile with inserted drive shaft and is also heated.
  • the drive shaft of the stirrer is also arranged horizontally and coaxially with the boiler axis. Due to the fact that the boiler cylinder is turned out, a very small distance between stirrer and wall of 1-5 mm is possible, depending on the size of the machine.
  • the wing sides on the cylinder wall and front and back are wedge-shaped, in order to ensure in the direction of rotation lifting the product of the cylinder wall, the rear wall and the front door. This ensures that virtually no or only a very thin product layer can be built up on the wall, which only slightly influences the heat input. Thus, a sufficient heat input is always ensured at each point in the process.
  • the stirrer has on one wing side another stirrer (chopper) 4, the much higher speed as the stirrer is driven.
  • This so-called chopper is driven independently of the stirrer with 40-400 times higher speeds. So if the stirrer operates 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 runs around with the stirrer and thus always comes to the product to be processed resp. runs through the product with the stirrer.
  • the chopper is independent of the direction of rotation, ie it can run with the same direction of rotation as the stirrer or it can also be switched to reverse direction during the drying process.
  • the wings of the chopper have knife and flat shape.
  • a comb 5 - a so-called stator - be screwed onto the stirrer blade, through which the material is pulled.
  • the blades of the stator have knife or flat shape as the chopper. This comes into effect depending on the direction of rotation of the chopper. Thus, difficult material can be crushed by hammering and / or cutting in many cases and thus during the drying often, if required, a grinding of the material can be achieved.
  • the stirrer is equipped with a circulating injection system 6.
  • This is a nozzle-equipped line which is mounted behind the chopper on the impeller and rotates with the stirrer.
  • three to seven nozzles are characteristic for the injection line, through which three different types of media can be supplied, namely liquids, gases or steam.
  • wetting (granulation), humidification and residual moisture discharge by means of gases as drag gases to achieve the lowest final moisture content possible.
  • the equipment thus equipped is able to dry a wide range of different products, from free-flowing products to those containing lumps to liquids (solutions or suspensions).
  • the combination of stirrer, chopper, stator and injection allows the machine to dynamically adjust the product properties that change during the drying process so that a uniform evaporation and thus a short drying time are achieved at all times.
  • the drying is carried out with the described device in batch operation, wherein the product is introduced into the cylinder and then stirrer, heating and vacuum are started.
  • the process sequence is then characterized in that initially relatively much solvent is evaporated off and the drying finally takes place from the product interior with a corresponding extension of the drying time. Finally, the desired final moisture in the product is reached and the product can after cooling and pressure relief are discharged through a located in the front door exhaust valve.
  • Control criteria include: the course of the product temperature, the course of the vacuum or evaporation, the amount of distillate and heating / cooling temperatures.
  • the product temperature and the amount of distillate represent the key quantities that determine the progress of the process and that provide the control with parameters for automatic adaptation.
  • the adaptation takes place via the vacuum, to a small extent also via the heating temperature.
  • the speeds of stirrer and chopper and its direction of rotation are auxiliary variables, which are also taken into account. As static mechanical additional auxiliary quantities, the distances of the blades of stator and chopper are added, which are already given by appropriate selection before drying.
  • the abscissa shows the drying time in min.
  • the left ordinate shows the vacuum (mbar) and temperatures (heating temperature, product temperature, Brüdentemperatur).
  • the right-hand ordinate indicates the absolute amount of evaporated solvent in liters.
  • Characteristic are the product temperature profile, which shows no waste or only very small waste (max 3-5 ° C) during drying, as well as the regulated vacuum in stages.
  • the solvent curve shows a uniform, rising course, which is typical with appropriate control.
  • the method of effective control can be divided into four to about ten main steps, whereby step-by-step criteria can be defined.
  • the number of steps depends on the type of product, the solvent and its evaporation characteristics (vapor pressure curve).
  • the heater is initially set to the maximum temperature still permissible for the product, ie the setpoint is set to this value and heating commences.
  • Stirrer and chopper run at medium speeds, the chopper mostly in a clockwise direction. This ensures a good mixing effect.
  • the vacuum is adjusted to about 500-300 mbar for safety reasons according to the vapor pressure curve of the most volatile solvents. It must be ensured that no evaporation takes place, which would lead to a lowering of the product temperature.
  • the next process step can be started, i. the beginning of the evaporation and the actual drying process.
  • the vacuum is adjusted to a value below the boiling point of the most volatile solvent, usually below 300 mbar. This results in a uniform solvent evaporation from the product, especially as long as free surface moisture is present according to the first drying section.
  • the controller ensures that the product temperature does not drop or only slightly drops - only then is it ensured that no recondensation of solvent takes place in the product - especially with large filling volumes. This would lead to clumping.
  • the controller adjusts the vacuum in terms of deterioration in order to reduce evaporation and to maintain the open pore state of the goods or to prevent too rapid shrinkage of the goods.
  • the multi-stage sequence of the actual drying to the end product begins.
  • 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 again the evaporation performance and the product temperature as in the second step.
  • the highest possible vacuum is used in the last step (typically approx. 3-5 mbar) until the required final moisture content is reached.
  • the required final moisture content is in the range of 0.5% - 1.5%.
  • the product temperature has proved to be a useful criterion, 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 which corresponds to the maximum permissible product temperature.
  • the device With its excellent heat transfer due to effective heating (special channels, multiple feed of the medium) and the mixing effect (stirrer, chopper, optionally with stator), the device is the prerequisite for being able to effectively apply the mentioned criteria of product temperature, vacuum and evaporation performance.
  • This applicability has been shown to be transferable to almost all types of products. Restrictions exist only for products that have a third drying section, ie all have the crystal moisture and chemically bound water. Here is only the height of the temperature and the exposure time prevail. Only to a small extent do the mixture and the vacuum have an effect.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Drying Of Solid Materials (AREA)

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

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 a vacuum contact drying in a device with a horizontally arranged, heated cylinder, a rotating with a very small wall distance stirrer and arranged on a stirrer chopper.

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 Vakuumkontakttrockner 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 the drying of plant extracts. The device described in this document, in addition to mixing / crushing, is a vacuum contact dryer for use in pharmaceutical drug (API) and chemical or fine chemical manufacturing, and has a horizontally disposed, heated cylinder with one rotating about a horizontal axis therein , 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 products to be dried are predominantly products of the pharmaceutical active ingredient industry and fine chemicals, which in addition to water usually contain organic solvents which are to be removed or dried under 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 Produkteigenschaften, 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 mostly relatively long drying times occur. The product range, ie the product properties, must be within a relatively narrow range, ie strongly standardized, in order to be able to dry reproducibly in acceptable times. Some products, such as liquids (Solutions or suspensions) are not or only insufficiently and after adjustments (conversions) to dry.

Zumeist stammen die Nassprodukte, die in den Trockner zur Trocknung eingefüllt werden, aus Zentrifugen oder Filternutschen. 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.In most cases, the wet products, which are filled into the dryer for drying, come from centrifuges or filter nipples. The moisture content of these wet products can fluctuate greatly, even with the same product. Moisture ranges of 20-50% by weight of moisture or more are possible. This wide fluctuation range makes it considerably more difficult in conventional processes to achieve similar or approximately equal drying times for the same product.

Physikalische Eigenschaften der Produkte (Viskosität, Aggregatzustand 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, state of solid or liquid, shrinkage), which arise or change in the course of drying, are added and make it impossible to complete the drying to the desired final moisture in previously known systems often or extend the drying times extremely.

An die Trockenprodukte (Fertigprodukte) werden weitere, schwierig zu erfüllende Anforderungen gestellt. Dazu gehören eine möglichst gleichförmige Korngrösse und Kornverteilung (enges Grössenspektrum), um die Produkte reproduzierbar und standardisierbar machen zu können.Dry products (finished products) are subject to further difficult-to-fulfill requirements. These include the most uniform grain size and particle size distribution possible (narrow range of sizes) in order to make the products reproducible and standardisable.

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 met inadequately. Often, a high additional effort (post-drying, grinding, granulation) is required to meet 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. This makes the achievement almost identical Meant drying times for the same product, but comes in the total of several batch-drying on the same apparatus. These properties include final moisture, color and fineness of the goods and 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 methods and in particular allows the processing of different starting materials in the sense of achieving similar, short and reproducible drying times while maintaining 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 rate are continuously measured and controlled 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.The method with the device suitable for this purpose is used to perform vacuum drying more effectively and makes it possible, in particular, to mix and distribute very varied products evenly, so that an always uniform heat input into the product is achieved. This allows a vacuum control, which allows a controllable and uniform at any time evaporation of solvent or solvent mixtures. This, in turn, reduces mechanical stresses on the product and the machine and at the same time expands the use of the device to previously difficult to dry products such as suspensions, solutions and lumpy products.

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.A control that can be automatically adapted to the progress of the process makes it possible to use different drying parameters as criteria so that the process remains manageable and controllable at all times. The parameters also provide criteria for control overshoot conditions, allowing the process to be continually advanced to achieve an effective process flow and which can then be automated through self-regulation.

Im folgenden wird anhand der beiliegenden Zeichnungen ein Ausführungsbeispiel der Erfindung beschrieben. Es zeigen

Fig. 1
eine Frontansicht eines Trockners bestehend aus Kesselzylinder, aufgesetztem Filtergehäuse und Austragsventil
Fig. 2
eine Seitenansicht der Anlage
Fig. 3
eine perspektivische Ansicht des Rührers mit Zerhacker, Stator und Eindüsungsleitung als wichtigsten Bauteilen.
Fig. 4
eine schematische Schnittdarstellung entlang der Linie A - A in Fig. 3
Fig. 5
eine typische Trocknungsverlaufskurve mit Kondensatmengenverlauf, Produkttemperaturverlauf, Heiztemperaturverlauf und Vakuumverlauf.
In the following an embodiment of the invention will be described with reference to the accompanying drawings. Show it
Fig. 1
a front view of a dryer consisting of boiler cylinder, mounted filter housing and discharge valve
Fig. 2
a side view of the plant
Fig. 3
a perspective view of the stirrer with chopper, stator and injection line as the main components.
Fig. 4
a schematic sectional view taken along the line A - A in Fig. 3rd
Fig. 5
a typical drying curve with condensate flow, product temperature, heating temperature 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 ausgedrehten Kesselzylinder 1. Der Zylinder ist zur Beheizung doppelwandig ähnlich ausgeführt mit aufgeschweissten Heizkanälen zur Kanalisierung des Heizmediums vollflächig über die gesamte Zylinderfläche. Je nach Grösse 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 Türe.To carry out the process according to the invention, a so-called IUT dryer known per se is used. This has a arranged with a horizontal axis turned out Boiler cylinder 1. The cylinder is designed for heating double-walled similar with welded Heizkanälen for channeling the heating medium over the entire surface over the entire cylindrical surface. Depending on the size of the machine, the heating medium is fed separately into up to 3 combined heating chamber units. For a completely uniform heating is possible 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 Kesselachse 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 Abheben 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 introduction system and a dust filter 2, which in turn is usually connected to a solvent recovery condenser followed by a vacuum pump. In the boiler cylinder, a stirrer 3 is arranged, which is designed as a closed hollow profile with inserted drive shaft and is also heated. The drive shaft of the stirrer is also arranged horizontally and coaxially with the boiler axis. Due to the fact that the boiler cylinder is turned out, a very small distance between stirrer and wall of 1-5 mm is possible, depending on the size of the machine. The wing sides on the cylinder wall and front and back are wedge-shaped, in order to ensure in the direction of rotation lifting the product of the cylinder wall, the rear wall and the front door. This ensures that virtually no or only a very thin product layer can be built up on the wall, which only slightly influences the heat input. Thus, a sufficient heat input is always ensured at each point in 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 on one wing side another stirrer (chopper) 4, the much higher speed as the stirrer is driven. This so-called chopper is driven independently of the stirrer with 40-400 times higher speeds. So if the stirrer operates 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 runs around with the stirrer and thus always comes to the product to be processed resp. runs through the product with the stirrer. The chopper is independent of the direction of rotation, ie it can run with the same direction of rotation as the stirrer or it can also be switched to reverse direction during the drying process. The wings of the chopper have 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 - be screwed onto the stirrer blade, through which the material is pulled. The blades of the stator have knife or flat shape as the chopper. This comes into effect depending on the direction of rotation of the chopper. Thus, difficult material can be crushed by hammering and / or cutting in many cases and thus during the drying often, if required, a grinding of the material can be achieved.

Des weiteren ist der Rührer mit einem umlaufenden Eindüsungssystem 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 Maschinengrösse drei bis sieben Düsen, durch die drei verschiedene Medienarten zugeführt werden können, nämlich Flüssigkeiten, Gase oder Dampf. Damit sind Benetzung (Granulierung), Befeuchtung und Restfeuchteaustrag mittels Gasen als Schleppgasen zur Erzielung niedrigster Endfeuchten möglich.Furthermore, the stirrer is equipped with a circulating injection system 6. This is a nozzle-equipped line which is mounted behind the chopper on the impeller and rotates with the stirrer. Depending on the machine size, three to seven nozzles are characteristic for the injection line, through which three different types of media can be supplied, namely liquids, gases or steam. Thus, wetting (granulation), humidification and residual moisture discharge by means of gases as drag gases to achieve the lowest final moisture content possible.

Mit dieser Anordnung sind sowohl Produktaufwirbelung als auch Produkteinzug möglich. Phasenänderungen (flüssig/fest) wie auch Klumpenbildung kann damit frühzeitig effektiv begegnet bzw. diese verhindert werden. Dadurch wird über den gesamten Prozess ein für die Verdampfung gleichmässiger 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.With this arrangement, both Produktaufwirbelung and product collection are possible. Phase changes (liquid / solid) as well as lump formation can thus be effectively counteracted at an early stage or prevented. As a result, a uniform product state for evaporation is maintained throughout the process. Combined with the extremely small wall clearances (1-5 mm depending on the size of the machine), there is an even heat input into the material, resulting in short drying times. The heat input consists of the transition from wall to heap, heat transport in the heap and transmission between the individual particles together. The chopper effect produces a uniformly fine product.

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 equipment thus equipped is able to dry a wide range of different products, from free-flowing products to those containing lumps to liquids (solutions or suspensions). The combination of stirrer, chopper, stator and injection allows the machine to dynamically adjust the product properties that change during the drying process so that a uniform evaporation and thus a short drying time 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 dadurch 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 described device in batch operation, wherein the product is introduced into the cylinder and then stirrer, heating and vacuum are started. The process sequence is then characterized in that initially relatively much solvent is evaporated off and the drying finally takes place from the product interior with a corresponding extension of the drying time. Finally, the desired final moisture in the product is reached and the product can after cooling and pressure relief are discharged through a located in the front door exhaust valve.

Das Zusammenspiel der Komponenten Trockner, Vakuumsystem mit Kondensation und Heizung/Kühlung erfolgt gemäss einer Steuerung, die es erlaubt, die üblichen Prozessschritte Befüllen, Aufheizen, Verdampfen und Trocknen, Abkühlen, Produktaustrag 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 in accordance with a controller, which makes it possible to optimally combine the usual process steps of filling, heating, evaporation and drying, cooling, product discharge. Criteria are the changes in the product properties, which the controller indirectly records, processes and adjusts settings.

Steuerungskriterien sind dabei: Verlauf der Produkttemperatur, Verlauf des Vakuums bzw. der Verdampfung, Destillatmenge 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 Hilfsgrössen, die ebenfalls berücksichtigt werden. Als statischmechanische weitere Hilfsgrössen kommen die Abstände der Messer von Stator und Zerhacker hinzu, die durch entsprechende Auswahl bereits vor der Trocknung gegeben sind.Control criteria include: the course of the product temperature, the course of the vacuum or evaporation, the amount of distillate and heating / cooling temperatures. The product temperature and the amount of distillate represent the key quantities that determine the progress of the process and that provide the control with parameters for automatic adaptation. The adaptation takes place via the vacuum, to a small extent also via the heating temperature. The speeds of stirrer and chopper and its direction of rotation are auxiliary variables, which are also taken into account. As static mechanical additional auxiliary quantities, the distances of the blades of stator and chopper are added, which are already given by appropriate selection before drying.

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 pharmaceutical ingredients, z. B. Antibiotika, Antihistaminika etc.) und Feinchemikalien, sowie Zwischenprodukte, welcher mittels der genannten Einrichtung und der angewendeten Steuerungskriterien erreicht wird.Based on the drying curve of a vitamin precursor shown in Figure 4, the setting of the parameters is displayed, which are processed in the controller. This drying process is typical of the product types mentioned active ingredients (API = active pharmaceutical ingredients, such as antibiotics, antihistamines, etc.) and fine chemicals, as well as intermediates, which by means of the said facility and the applied control criteria.

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 abscissa shows the drying time in min., The left ordinate shows the vacuum (mbar) and temperatures (heating temperature, product temperature, Brüdentemperatur). Finally, the right-hand ordinate indicates the absolute amount of evaporated 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 gleichmässigen, ansteigenden Verlauf, welcher typisch ist bei entsprechender Steuerung.Characteristic are the product temperature profile, which shows no waste or only very small waste (max 3-5 ° C) during drying, as well as the regulated vacuum in stages. The solvent curve shows a uniform, 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, dem Lösungsmittel und dessen Verdampfungscharakteristik (Dampfdruckkurve)abhängig.The method of effective control can be divided into four to about ten main steps, whereby step-by-step criteria can be defined. The number of steps depends on the type of product, the solvent and its evaporation characteristics (vapor pressure curve).

Nach dem Einfüllen wird zunächst die Heizung auf die maximal 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.After filling, the heater is initially set to the maximum temperature still permissible for the product, ie the setpoint is set to this value and heating commences. Stirrer and chopper run at medium speeds, the chopper mostly in a clockwise direction. This ensures a good mixing effect. At the same time, the vacuum is adjusted to about 500-300 mbar for safety reasons according to the vapor pressure curve of the most volatile solvents. It must be ensured that no evaporation takes place, which would lead to a lowering of the product temperature.

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 gleichmässige Lösungsmittelverdampfung aus dem Produkt, besonders solange freie Oberflächenfeuchte entsprechend dem ersten 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 Flüssigkeitstransport im Stofftransport kontrollierten zweiten Trocknungsabschnitt massiv behindert, was zu sehr langen Trocknungszeiten führt.When the product temperature has finally reached about 30 ° C (+ - 2 ° C) and thus energy has been introduced into the product, the next process step can be started, i. the beginning of the evaporation and the actual drying process. The vacuum is adjusted to a value below the boiling point of the most volatile solvent, usually below 300 mbar. This results in a uniform solvent evaporation from the product, especially as long as free surface moisture is present according to the first drying section. By adjusting the vacuum, the controller ensures that the product temperature does not drop or only slightly drops - only then is it ensured that no recondensation of solvent takes place in the product - especially with large filling volumes. This would lead to clumping. Furthermore, by keeping the vacuum too fast evaporation at the Gutsoberfläche with shrinkage of the material or the pores is prevented. With shrinkage of the pores, the liquid transport in the mass transport controlled second drying section would be hindered massively, resulting in 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.Nevertheless, should the product temperature fall below a certain limit, the controller adjusts the vacuum in terms of deterioration in order to reduce evaporation and to maintain the open pore state of the goods or to prevent too rapid shrinkage of the goods.

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.This state of constant vacuum is maintained as long as on the one hand a constant evaporation performance is maintained and on the other hand the product temperature remains constant or the rise does not exceed certain limits.

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 (typischerweise ca. 3-5 mbar), bis die geforderte Endfeuchte erreicht ist.When the evaporation rate drops, the multi-stage sequence of the actual drying to the end product (dry product) begins. 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 again the evaporation performance and the product temperature as in the second step. Finally, the highest possible vacuum is used in the last step (typically approx. 3-5 mbar) until the required final moisture content is reached.

Für die meisten Produkte liegt die geforderte Endfeuchte im Bereich 0.5% - 1.5%. Hierbei hat sich als verwendbares Kriterium 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.For most products, the required final moisture content is in the range of 0.5% - 1.5%. In this case, the product temperature has proved to be a useful criterion, 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 which corresponds to the maximum permissible product temperature.

Abschliessend erfolgen die Abkühlung und die Entleerung des Produktes.Finally, the cooling and the emptying of the product.

Die Einrichtung stellt mit ihrem ausgezeichneten Wärmeübergang 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 Anwendbarkeit hat sich als auf nahezu alle Arten von Produkten übertragbar gezeigt.
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.With its excellent heat transfer due to effective heating (special channels, multiple feed of the medium) and the mixing effect (stirrer, chopper, optionally with stator), the device is the prerequisite for being able to effectively apply the mentioned criteria of product temperature, vacuum and evaporation performance. This applicability has been shown to be transferable to almost all types of products.
Restrictions exist only for products that have a third drying section, ie all have the crystal moisture and chemically bound water. Here is only the height of the temperature and the exposure time prevail. Only to a small extent do the mixture and the vacuum have an effect.

Claims (10)

  1. A method for the control of vacuum contact drying in a device with a horizontally arranged heated cylinder (1), with an agitator (3) rotating with a very small wall clearance, with a chopper (4) arranged on the agitator (3) and with an injection line (6), likewise arranged on the agitator (3), for the introduction of liquid, gaseous or vaporous media, characterized in that the profile of the product temperature and the vacuum are continuously measured and are regulated on the basis of the measurement values.
  2. The method as claimed in claim 1, characterized in that the instantaneous evaporative capacity is measured and is used as a regulated variable.
  3. The method as claimed in one of claims 1-2, characterized in that the moist initial material after being introduced into the device, is comminuted and homogenized.
  4. The method as claimed in claim 3, characterized in that the evaporative capacity is kept constant, in order to achieve a short drying time, irrespective of the type of initial material.
  5. The method as claimed in one of claims 1-4, characterized in that the vacuum is lowered in steps, and the evaporative capacity is thereby kept constant during the entire drying.
  6. The method as claimed in one of claims 1-5, characterized in that the material temperature is measured for determining the residual moisture.
  7. The method as claimed in one of claims 1-6, characterized in that a carrier gas is introduced directly into the product, in order to achieve residual moistures in the ppm range.
  8. A device for vacuum contact drying, with a horizontally arranged cylinder (1), with an agitator (3) rotating with a very small wall clearance, and with a chopper (4) arranged on the agitator, characterized by a heated cylinder (4) and means for the continuous measurement of the profile of the product temperature and of the vacuum and for regulating these parameters.
  9. The device as claimed in claim 8, characterized by an injection line (6), likewise arranged on the agitator (3), for the introduction of liquid, gaseous or vaporous media.
  10. The use of a device as claimed in claims 8 and 9 for vacuum contact drying.
EP03714606A 2002-05-02 2003-04-30 Drying method Expired - Lifetime EP1509736B1 (en)

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CH00747/02A CH695427A5 (en) 2002-05-02 2002-05-02 Drying process.
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PCT/CH2003/000278 WO2003093744A1 (en) 2002-05-02 2003-04-30 Drying method

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US8056256B2 (en) * 2008-09-17 2011-11-15 Slack Associates, Inc. Method for reconditioning FCR APG-68 tactical radar units
US8701307B2 (en) 2008-09-17 2014-04-22 Howard C. Slack Method for cleaning and reconditioning FCR APG-68 tactical radar units
EP2689833A3 (en) 2012-07-27 2015-05-13 Marion Mixers, Inc. Mixing apparatus

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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
ATE33765T1 (en) * 1983-12-21 1988-05-15 Gergely Gerhard METHOD AND DEVICE FOR THE HEAT TREATMENT OF POWDER OR GRANULES.
DE3519613A1 (en) 1985-05-31 1986-12-04 Killer Verfahrenstechnik Dr DEVICE FOR MIXING AND / OR MILLING
US4882851A (en) * 1987-04-13 1989-11-28 The Fitzpatrick Co. Apparatus and method for batch drying using a microwave vacuum system
DE4441350C1 (en) * 1994-11-21 1996-06-13 Bohle L B Pharmatech Gmbh Infrared spectroscopic measuring system for moisture content of materials in mixer and dryer plant
DE19525026A1 (en) 1995-07-10 1997-01-16 Plantamed Arzneimittel Gmbh Process for the preparation of pharmaceutical preparations with a higher content of essential oils and phenols
US5958156A (en) * 1996-03-15 1999-09-28 Kemp Development Corporation Process for treating a particulate material within a rotating retort

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AU2003218859A1 (en) 2003-11-17
DE50306667D1 (en) 2007-04-12
ATE355499T1 (en) 2006-03-15
CH695427A5 (en) 2006-05-15
WO2003093744A1 (en) 2003-11-13

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