EP1127609A2 - Method for processing a product in at least a mixing kneader - Google Patents

Method for processing a product in at least a mixing kneader Download PDF

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Publication number
EP1127609A2
EP1127609A2 EP01103153A EP01103153A EP1127609A2 EP 1127609 A2 EP1127609 A2 EP 1127609A2 EP 01103153 A EP01103153 A EP 01103153A EP 01103153 A EP01103153 A EP 01103153A EP 1127609 A2 EP1127609 A2 EP 1127609A2
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EP
European Patent Office
Prior art keywords
product
mixing kneader
kneader
mixing
kneading
Prior art date
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Granted
Application number
EP01103153A
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German (de)
French (fr)
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EP1127609A3 (en
EP1127609B1 (en
Inventor
Pierre-Alain Dr. Fleury
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List AG
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List AG
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Publication of EP1127609A3 publication Critical patent/EP1127609A3/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/47—Mixing liquids with liquids; Emulsifying involving high-viscosity liquids, e.g. asphalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
    • B01F27/70—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with paddles, blades or arms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/82—Combinations of dissimilar mixers
    • B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/834—Mixing in several steps, e.g. successive steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/22—Control or regulation
    • B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
    • B01F35/2214—Speed during the operation
    • B01F35/22142—Speed of the mixing device during the operation
    • B01F35/221422—Speed of rotation of the mixing axis, stirrer or receptacle during the operation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/75—Discharge mechanisms
    • B01F35/754—Discharge mechanisms characterised by the means for discharging the components from the mixer
    • B01F35/75455—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle
    • B01F35/754551—Discharge mechanisms characterised by the means for discharging the components from the mixer using a rotary discharge means, e.g. a screw beneath the receptacle using helical screws
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners

Definitions

  • the invention relates to a method for continuous Evaporation or for the thermal treatment of viscous viscous Products, especially elastomers and thermoplastics, in a mixing kneader with at least one with mixing or Kneading elements equipped stirrer shaft.
  • the corresponding separation processes are usually in stirred heat exchangers and so-called mixing kneaders carried out in which the product by appropriate Kneading and transport elements from one inlet to one Transported and simultaneously with the Heat exchange surfaces are brought into intensive contact.
  • mixing kneaders are, for example, in DE-PS 23 49 106, EP 0 517 068 A1 and DE 195 36 944 A1.
  • the present invention is based on the object heat transfer limited section of the evaporation optimize.
  • LIST-DTB mixer which is also used in the above mentioned DE-PS 23 49 106 is shown.
  • the product is not only a mixer from inlet to outlet transported, but by backmixing with a new product homogeneously mixed again throughout the apparatus.
  • the product is initially high in solvent still very liquid, so the evaporation takes place in the essentially about the contact heat coming from a heated Housing jacket, a heated shaft and / or heated Kneading counter elements comes.
  • the method according to the invention also has the advantage that with the increased work intensity foaming, that of the flash dosage of the product in the Mixing kneader originates, is broken, whereby the Heat energy input is further improved.
  • the for Evaporation required evaporation energy accordingly through the combination of contact heat and Maximized shear heat.
  • the possibility of evaporation of solvent to keep the product temperature constant allows a high degree of freedom in relation to the Regulation of the shear heat via the speed (shear gradient) and the degree of filling of the mixing kneader.
  • the product is in the downstream second mixer kneader by a corresponding geometry of the kneading elements Plug flow subjected.
  • this second mixer kneader the evaporation limited by mass transfer takes place, which is why twin-screw mixers are preferred be under the name LIST-ORP (EP 0 517 068 A1) and LIST-CRP (DE 195 36 944 A1) are on the market.
  • LIST-ORP EP 0 517 068 A1
  • LIST-CRP DE 195 36 944 A1
  • FIG 1 two mixing kneader 1 and 2 are together connected.
  • the mixing kneader 1 is a Kneader with a good backmixing, as for example under the Designation LIST-DTB is on the market. On this DTB relates to DE-PS 23 49 106.
  • a mixer kneader with good Backmixing is characterized in that the product in the entire mixing kneader is homogeneously mixed together.
  • the mixer kneader 2 is one Kneader with a so-called plug flow, such as. is on the market under the name LIST-CRP or LIST-ORP.
  • plug flow such as. is on the market under the name LIST-CRP or LIST-ORP.
  • the corresponding property rights for this are in EP 0 517 068 and DE 195 36 944 A1.
  • At a Mixing kneader with good plug flow is the product of Inlet transported to the outlet without an axial Mixing with the following product takes place. Therefore there is usually an inlet 3 for the Product at one end of the mixer kneader and an outlet 4, which in the present case as a discharge twin screw is formed at the other end of the mixer kneader 2.
  • the mixer kneader 1 has an inlet 5 approximately in the center of the mixer and a discharge twin screw 6 at the end of the mixing kneader 1.
  • each indicated two waves 7 and 8 or 9 and 10 which mixing, transport or kneading elements 11 are arranged are that rotate with the waves, like this among others in the above Property rights is described.
  • a feed line 12 to the inlet 5 there is a pump 13, a heat exchanger 14 and a pressure holding valve 15 switched on.
  • This referred to as a flash device Device preheats the product.
  • a large part of the liquid is in the mixer kneader 1 Part of the product evaporated, the Mixing kneader 1 heat is supplied.
  • a Housing shell 16 the kneader shafts 7 and 8 and the Kneading elements 11 are heated.
  • the evaporated The component leaves the mixer kneader 1 via a vapor dome 17, with a corresponding derivative 18 Condenser 19 and an inert gas pump 20 turned on are.
  • FIG. 2 also shows that the mixer kneader 1 can also have only one shaft 21.
  • This mixer kneader 2 also has a dome 24, which merges into a derivative 25, into which a condenser 26 or an inert gas pump 27 are switched on.
  • the kneading energy increases considerably due to the increasing viscosity of the product (up to 1300 Pas at 80 s -1 shear rate) without the contact heat transfer decreasing significantly. This means that a considerable amount of shear heat is added to the contact heat. At the same time, however, the solvent concentration is still high enough so that the entire energy input can be used to evaporate the solvent, so that the product temperature remains constant. This maximizes the effectiveness of the kneader in this area.
  • this product behavior in the Mixing kneader 1 with good remixing exploited by the Concentration of solvent always around 25% Cyclohexane is kept. This is done via a controller the supply amount of fresh product and over a Regulation of the kneading energy by means of the shaft speed and the degree of filling.
  • the solution so evaporated is by means of Discharge twin screw 6 from the mixer kneader 1 carried out continuously, simultaneously by shearing in warmed up the screw and into the mixer kneader 2 flashed.
  • this mixer kneader 2 is a material transfer limited drying section carried out, where essentially no surface evaporation takes place. The evaporation points, the entirety of which so-called drying mirror, pull more and back to the good inside. The liquid must diffuse.
  • the mixing kneader 2 is open for this process section Because of the shaft geometry and the kinematics with one maximum surface renewal, plug flow and good Product temperature control facility.
  • the degassed elastomer is finally discharged from the mixing kneader 2 with the second discharge twin screw 4.
  • the elastomer still contains a residual solvent content below 1000 ppm.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

Continuous evaporation or heat treatment of elastomers and thermoplastics is carried out in a mixer and kneader fitted with stirring shafts (7 - 10) on which mixing and kneading components (11) are mounted. New low viscosity solution is mixed with pre-evaporated viscous material, the viscosity and concentration of the solution being adjusted so that the energy input from mechanical kneading and heat transfer is maximised. An Independent claim is included for apparatus for carrying out the process with an inlet (5) for solution connected to a mixer/kneader (1) with good back mixing connected to a second mixer/kneader (2) with good forced flow.

Description

Die Erfindung betrifft ein Verfahren zum kontinuierlichen Eindampfen bzw. zur thermischen Behandlung von zähviskosen Produkten, insbesondere Elastomeren und Thermoplasten, in einem Mischkneter mit zumindest einer mit Misch- bzw. Knetelementen bestückten Rührwelle.The invention relates to a method for continuous Evaporation or for the thermal treatment of viscous viscous Products, especially elastomers and thermoplastics, in a mixing kneader with at least one with mixing or Kneading elements equipped stirrer shaft.

Die industrielle Herstellung von zähviskosen Produkten, insbesondere von Elastomeren und Plasten erfolgt häufig unter Verwendung von Lösungsmitteln, wobei diese Lösungsmittel am Ende des Herstellprozesses durch thermische Abtrennung (Eindampfung) wieder entfernt werden müssen. Vor allem geht es im vorliegenden Ausführungsbeispiel um das kontinuierliche Eindampfen und Entgasen einer Elastomer-Lösung, wobei ein wärmeübergangslimitierter Abschnitt und ein stoffübergangslimitierter Abschnitt zu unterscheiden sind.The industrial production of viscous products, elastomers and plastics in particular are often used using solvents, these Solvent at the end of the manufacturing process thermal separation (evaporation) can be removed again have to. Above all, it deals with the present Embodiment to the continuous evaporation and Degassing an elastomer solution, being a heat transfer limited section and a A distinction must be made between the material transfer limited section.

Die entsprechenden Trennverfahren werden in der Regel in gerührten Wärmeaustauschern und sogenannten Mischknetern durchgeführt, in denen das Produkt durch entsprechende Knet- und Transportelemente von einem Einlass zu einem Auslass transportiert und gleichzeitig mit den Wärmeaustauschflächen in intensiven Kontakt gebracht wird. Derartige Mischkneter sind bspw. in der DE-PS 23 49 106, der EP 0 517 068 A1 und der DE 195 36 944 A1 beschrieben.The corresponding separation processes are usually in stirred heat exchangers and so-called mixing kneaders carried out in which the product by appropriate Kneading and transport elements from one inlet to one Transported and simultaneously with the Heat exchange surfaces are brought into intensive contact. Such mixer kneaders are, for example, in DE-PS 23 49 106, EP 0 517 068 A1 and DE 195 36 944 A1.

Der vorliegenden Erfindung liegt die Aufgabe zugrunde, den wärmeübergangslimitierten Abschnitt der Verdampfung zu optimieren.The present invention is based on the object heat transfer limited section of the evaporation optimize.

Zur Lösung dieser Aufgabe führt, dass in ein voreingedampftes viskoses Produktbett kontinuierlich neue niedrig viskose Produktlösung derart eingemischt wird, dass die Viskosität und Konzentration dieses Produktbettes so eingestellt wird, dass der Energieeintrag bestehend aus mechanischer Knetenergie und Wärmeübertragung über den Kontakt mit der Kneterwärmeaustauschfläche maximal ist.To solve this problem that leads to a pre-evaporated viscous product bed continuously new low-viscosity product solution is mixed in such a way that the viscosity and concentration of this product bed like this is set that the energy input consists of mechanical kneading energy and heat transfer via the Contact with the kneading heat exchange surface is maximum.

Dies geschieht bevorzugt in einem Mischkneter, der eine gute Rückmischung aufweist. Dabei handelt es sich bevorzugt um einen sogenannten LIST-DTB-Mischer, der auch in der oben erwähnten DE-PS 23 49 106 dargestellt ist. In diesem Mischer wird das Produkt nicht nur vom Einlass zum Auslass transportiert, sondern durch Rückmischung mit neuem Produkt im ganzen Apparat auch wieder homogen vermischt. This is preferably done in a mixing kneader, the one has good backmixing. It is preferred a so-called LIST-DTB mixer, which is also used in the above mentioned DE-PS 23 49 106 is shown. In this The product is not only a mixer from inlet to outlet transported, but by backmixing with a new product homogeneously mixed again throughout the apparatus.

Für das Produkt selbst wird vorab festgestellt, bei welchem Prozentsatz an vorhandenem, flüssigem Bestandteil die Summe aus Wärmeübertragung durch Kontaktwärme und Wärmeeinbringung durch Scherwärme maximal und damit die Verdampfungsgeschwindigkeit am höchsten ist. Dementsprechend wird dann versucht, in dem Mischkneter mit guter Rückmischung das Produkt auf diesem Prozentsatz mit Lösungsmittel zu halten, was durch dosierte kontinuierliche Zugabe von neuem Produkt geschieht, welches immer dünnflüssiger ist und einen höheren Prozentsatz eines Lösungsmittels beinhaltet. Auf diese Weise kann eine Konzentration eingestellt werden, bei welcher die erforderliche Verdampfungsenergie bestehend aus Kontaktwärme und Scherwärme optimiert ist.For the product itself, it is determined in advance which one Percentage of liquid component present the sum from heat transfer through contact heat and Maximum heat input by shear heat and thus the Evaporation rate is highest. Accordingly, an attempt is then made in the mixing kneader good backmixing with the product at this percentage Keep solvent what through metered continuous Adding new product happens, whichever is thinner and a higher percentage of one Includes solvent. In this way, a Concentration can be set at which the required evaporation energy consisting of Contact heat and shear heat is optimized.

Ist das Produkt bei hohem Lösungsmittelanteil anfänglich noch sehr flüssig, so erfolgt das Verdampfen im wesentlichen über die Kontaktwärme, die aus einem geheiztem Gehäusemantel, einer geheizten Welle und/oder geheizten Knetgegenelementen kommt. Je viskoser das Produkt durch die Eindampfung wird, desto mehr nimmt die Kontaktwärmeübertragung ab und umso mehr Scherwärme kommt hinzu, wobei die Summe von beiden ein Maximum durchläuft. Ab einer bestimmten Verminderung des Prozentsatzes an flüssigen Bestandteilen nimmt jedoch die Verdampfungsgeschwindigkeit ganz erheblich ab, da nicht mehr genügend Lösungsmittel vom Gutsinneren an die Oberfläche nachgeliefert werden kann. Erfindungsgemäss soll deshalb der Bestandteil an bspw. Lösungsmittel in einem Prozentbereich gehalten werden, der nahe am Maximum aber unbedingt noch oberhalb dieser Einbruchstelle der Verdampfungsgeschwindigkeit liegt. The product is initially high in solvent still very liquid, so the evaporation takes place in the essentially about the contact heat coming from a heated Housing jacket, a heated shaft and / or heated Kneading counter elements comes. The more viscous the product through Evaporation becomes, the more it takes Contact heat transfer from and the more shear heat comes added, the sum of both going through a maximum. From a certain decrease in the percentage however, liquid components take the Evaporation rate drops considerably since not more enough solvent from the good to the Surface can be supplied later. According to the invention therefore the component of e.g. solvent in one Percentage range are kept, but close to the maximum necessarily above this break-in point Evaporation rate is.

Das erfindungsgemässe Verfahren hat ferner den Vorteil, dass bei der erhöhten Arbeitsintensität eine Schaumbildung, die von der Flash-Dosierung des Produktes in den Mischkneter herrührt, gebrochen wird, wodurch der Wärmeenergieeintrag nochmals verbessert wird. Die zur Eindampfung benötigte Verdampfungsenergie wird dementsprechend durch die Kombination von Kontaktwärme und Scherwärme maximiert. Die Möglichkeit über die Verdampfung von Lösungsmittel die Produkttemperatur konstant zu halten erlaubt einen hohen Freiheitsgrad in Bezug auf die Regulierung der Scherwärme über die Drehzahl (Schergefälle) und den Füllgrad des Mischkneters.The method according to the invention also has the advantage that with the increased work intensity foaming, that of the flash dosage of the product in the Mixing kneader originates, is broken, whereby the Heat energy input is further improved. The for Evaporation required evaporation energy accordingly through the combination of contact heat and Maximized shear heat. The possibility of evaporation of solvent to keep the product temperature constant allows a high degree of freedom in relation to the Regulation of the shear heat via the speed (shear gradient) and the degree of filling of the mixing kneader.

Im nachgeschalteten zweiten Mischkneter wird das Produkt durch eine entsprechende Geometrie der Knetelemente einer Pfropfenströmung unterworfen. In diesem zweiten Mischkneter findet die stoffübergangslimitierte Eindampfung statt, weshalb hier bevorzugt zweiwellige Mischkneter verwendet werden, die unter dem Namen LIST-ORP (EP 0 517 068 A1) und LIST-CRP (DE 195 36 944 A1) im Handel sind. In diesem Mischkneter mit Pfropfenströmung ist wesentlich, dass die Oberfläche des Produktes möglichst schnell erneuert wird, da von dieser Oberfläche die Flüssigkeit abdampft. Da sich die Verdunstungsstellen mehr und mehr in das Gutsinnere zurückziehen, müss die Produktoberfläche durch intensivers Kneten permanent erneuert werden. Ferner ist eine gute Produkttemperaturkontrolle notwendig. The product is in the downstream second mixer kneader by a corresponding geometry of the kneading elements Plug flow subjected. In this second mixer kneader the evaporation limited by mass transfer takes place, which is why twin-screw mixers are preferred be under the name LIST-ORP (EP 0 517 068 A1) and LIST-CRP (DE 195 36 944 A1) are on the market. In this Mixing kneader with plug flow is essential that the Surface of the product is renewed as quickly as possible, because the liquid evaporates from this surface. That I the evaporation points more and more into the good interior withdraw, the product surface must intensify Kneading can be renewed permanently. It is also a good one Product temperature control necessary.

Weitere Vorteile, Merkmale und Einzelheiten der Erfindung ergeben sich aus der nachfolgenden Beschreibung bevorzugter Ausführungsbeispiele sowie anhand der Zeichnung; diese zeigt in

  • Figur 1 eine Seitenansicht einer erfindungsgemässen Vorrichtung zum Behandeln eines Produktes in zumindest einem Mischkneter;
  • Figur 2 eine Frontansicht eines Teils der Vorrichtung gemäss Figur 1.
    • Further advantages, features and details of the invention result from the following description of preferred exemplary embodiments and from the drawing; this shows in
  • FIG. 1 shows a side view of an inventive device for treating a product in at least one mixing kneader;
  • FIG. 2 shows a front view of part of the device according to FIG. 1.

    • In Figur 1 sind zwei Mischkneter 1 und 2 miteinander verbunden. Bei dem Mischkneter 1 handelt es sich um einen Kneter mit einer guten Rückmischung, wie er bspw. unter der Bezeichnung LIST-DTB auf dem Markt ist. Auf diesen DTB bezieht sich die DE-PS 23 49 106. Ein Mischkneter mit guter Rückmischung zeichnet sich dadurch aus, dass das Produkt im gesamten Mischkneter homogen miteinander vermischt wird.In Figure 1, two mixing kneader 1 and 2 are together connected. The mixing kneader 1 is a Kneader with a good backmixing, as for example under the Designation LIST-DTB is on the market. On this DTB relates to DE-PS 23 49 106. A mixer kneader with good Backmixing is characterized in that the product in the entire mixing kneader is homogeneously mixed together.

    Bei dem Mischkneter 2 handelt es sich dagegen um einen Kneter mit einer sogenannten Propfenströmung, wie er bspw. unter dem Namen LIST-CRP oder LIST-ORP auf dem Markt ist. Die entsprechenden Schutzrechte hierfür sind in der EP 0 517 068 und der DE 195 36 944 A1 veröffentlicht. Bei einem Mischkneter mit guter Propfenströmung wird das Produkt vom Einlass zum Auslass transportiert, ohne dass eine axiale Vermischung mit dem nachfolgenden Produkt stattfindet. Deshalb befindet sich in der Regel ein Einlass 3 für das Produkt an einem Ende des Mischkneters und ein Auslass 4, der im vorliegenden Fall als eine Austragsdoppelschnecke ausgebildet ist, am anderen Ende des Mischkneters 2. In contrast, the mixer kneader 2 is one Kneader with a so-called plug flow, such as. is on the market under the name LIST-CRP or LIST-ORP. The corresponding property rights for this are in EP 0 517 068 and DE 195 36 944 A1. At a Mixing kneader with good plug flow is the product of Inlet transported to the outlet without an axial Mixing with the following product takes place. Therefore there is usually an inlet 3 for the Product at one end of the mixer kneader and an outlet 4, which in the present case as a discharge twin screw is formed at the other end of the mixer kneader 2.

    Der Mischkneter 1 besitzt dagegen einen Einlass 5 etwa in der Mitte des Mischkneters und eine Austragsdoppelschnecke 6 am Ende des Mischkneters 1. In beiden Mischknetern sind jeweils zwei Wellen 7 und 8 bzw. 9 und 10 angedeutet, an denen Misch-, Transport- bzw. Knetelemente 11 angeordnet sind, die mit den Wellen drehen, wie dies unter anderem in den o. g. Schutzrechten beschrieben ist.In contrast, the mixer kneader 1 has an inlet 5 approximately in the center of the mixer and a discharge twin screw 6 at the end of the mixing kneader 1. In both mixing kneaders each indicated two waves 7 and 8 or 9 and 10 which mixing, transport or kneading elements 11 are arranged are that rotate with the waves, like this among others in the above Property rights is described.

    In einer Zuleitung 12 zu dem Einlass 5 ist eine Pumpe 13, ein Wärmetauscher 14 und ein Druckhalteventil 15 eingeschaltet. Diese als Flasheinrichtung bezeichnete Vorrichtung heizt das Produkt vor.In a feed line 12 to the inlet 5 there is a pump 13, a heat exchanger 14 and a pressure holding valve 15 switched on. This referred to as a flash device Device preheats the product.

    In dem Mischkneter 1 wird ein grosser Teil des flüssigen Bestandteils des Produktes ausgedampft, wobei dem Mischkneter 1 Wärme zugeführt wird. Hierzu können bspw. ein Gehäusemantel 16, die Kneterwellen 7 und 8 bzw. die Knetelemente 11 beheizt werden. Der ausgedampfte Bestandteil verlässt den Mischkneter 1 über ein Brüdendom 17, wobei in eine entsprechende Ableitung 18 ein Kondensator 19 und eine Inertgaspumpe 20 eingeschaltet sind.A large part of the liquid is in the mixer kneader 1 Part of the product evaporated, the Mixing kneader 1 heat is supplied. For example, a Housing shell 16, the kneader shafts 7 and 8 and the Kneading elements 11 are heated. The evaporated The component leaves the mixer kneader 1 via a vapor dome 17, with a corresponding derivative 18 Condenser 19 and an inert gas pump 20 turned on are.

    In Figur 2 ist im übrigen dargestellt, dass der Mischkneter 1 auch nur eine Welle 21 aufweisen kann.FIG. 2 also shows that the mixer kneader 1 can also have only one shaft 21.

    Das von dem flüssigen Bestandteil weitgehend befreite Produkt wird aus dem Mischkneter 1 durch die Austragsdoppelschnecke 6 ausgetragen und über eine Leitung 22 und ein Druckhalteventil 23 dem Einlass 3 des Mischkneters 2 zugeführt. Auch dieser Mischkneter 2 weist einen Brüdendom 24 auf, der in eine Ableitung 25 übergeht, in die ein Kondensator 26 bzw. eine Inertgaspumpe 27 eingeschaltet sind.That is largely freed from the liquid component Product is from the mixer kneader 1 through the Discharge twin screw 6 discharged and via a line 22 and a pressure holding valve 23 the inlet 3 of the Mixing kneader 2 supplied. This mixer kneader 2 also has a dome 24, which merges into a derivative 25, into which a condenser 26 or an inert gas pump 27 are switched on.

    Die Funktionsweise der vorliegenden Erfindung wird anhand eines Beispiels näher erläutert:The operation of the present invention is illustrated of an example:

    In 77% Cylohexan ist bspw. ein Elastomer, nämlich Styrol-Butadien-Styrol (SBS), gelöst. In einem Batch-Versuch wurde das Eindampf- und Entgasungsverhalten dieses gelösten Elastomer untersucht und die Verdampfungsgeschwindigkeit über die Zeit dargestellt. Von 77% bis auf 40% Lösungsmittelkonzentration ist die Verdampfungsgeschwindigkeit hauptsächlich von der Kontaktwärme des Produktes mit dem geheizten Gehäusemantel, den geheizten Wellen 7 und 8 und den geheizten Knetelementen 11 abhängig.For example, in 77% cyclohexane there is an elastomer, namely styrene-butadiene-styrene (SBS). In a batch trial the evaporation and degassing behavior of this solved Elastomer examined and the rate of evaporation represented over time. From 77% to 40% Solvent concentration is the rate of evaporation mainly from the contact heat of the product with the heated casing, the heated shafts 7 and 8 and the heated kneading elements 11 dependent.

    Im Bereich von 40% bis 25% des Lösungsmittels nimmt die Knetenergie infolge der steigenden Viskosität des Produktes (bis 1300 Pas bei 80 s-1 Schergefälle) erheblich zu, ohne dass dabei die Kontaktwärmeübertragung wesentlich abnimmt. Das bedeutet, dass zu der Kontaktwärme eine erhebliche Scherwärme hinzutritt. Gleichzeitig ist aber die Lösungsmittelkonzentration noch hoch genugt, damit der gesamte Energieeintrag zur Verdampfung des Lösungsmittels genutzt werden kann, so dass die Produkttemperatur konstant bleibt. Damit wird in diesem Bereich die Effektivität des Kneters maximiert.In the range of 40% to 25% of the solvent, the kneading energy increases considerably due to the increasing viscosity of the product (up to 1300 Pas at 80 s -1 shear rate) without the contact heat transfer decreasing significantly. This means that a considerable amount of shear heat is added to the contact heat. At the same time, however, the solvent concentration is still high enough so that the entire energy input can be used to evaporate the solvent, so that the product temperature remains constant. This maximizes the effectiveness of the kneader in this area.

    Unterhalb von 23% Lösungsmittel verlangsamt sich die Verdampfungsgeschwindigkeit drastisch. Dies kommt daher, weil an der Produktoberfläche nicht mehr genügend Lösungsmittel vorhanden ist und der Lösungsmittelnachschub aus dem Inneren gebremst ist. Damit verlangsamt sich die Trocknungsgeschwindigkeit erheblich. Der Beginn dieser Geschwindigkeitsabnahme ist durch einen scharfen Knick in der Trocknungskurve gekennzeichnet.Below 23% solvent, the slows down Evaporation rate drastically. This is because because there is no longer enough on the product surface Solvent is present and the solvent replenishment is braked from the inside. This slows down the Drying speed considerably. The beginning of this Decrease in speed is due to a sharp kink marked on the drying curve.

    Erfindungsgemäss wird dieses Produktverhalten in dem Mischkneter 1 mit guter Rückmischung ausgenutzt, indem die Konzentration des Lösungsmittels immer bei etwa 25% Cyclohexan gehalten wird. Dies erfolgt über eine Steuerung der Zulaufmenge an frischem Produkt und über eine Regulierung der Knetenergie mittels der Wellendrehzahl und dem Füllgrad.According to the invention, this product behavior in the Mixing kneader 1 with good remixing exploited by the Concentration of solvent always around 25% Cyclohexane is kept. This is done via a controller the supply amount of fresh product and over a Regulation of the kneading energy by means of the shaft speed and the degree of filling.

    Als weiterer Vorteil konnte beobachtet werden, dass bei Einhaltung dieser Konzentration keine Schaumbildung auftritt, was zu einem besseren Wärmedurchgangskoeffizienten führt. Die verfahrensgemässe Fahrweise des Mischkneters 1 ist von grossem Einfluss auf den "Scale-up" des hier durchgeführten wärmeübergangsbestimmten Trockungsabschnittes.As a further advantage, it was observed that at Adherence to this concentration no foaming occurs, resulting in a better heat transfer coefficient leads. The procedural driving style of the Mixing kneader 1 has a major influence on the "scale-up" of the heat transfer determined here Drying section.

    Die so eingedampfte Lösung wird mittels der Austragdoppelschnecke 6 aus dem Mischkneter 1 kontinuierlich ausgetragen, gleichzeitig durch Scherung in der Schnecke aufgewärmt und in den Mischkneter 2 eingeflasht. In diesem Mischkneter 2 wird ein stoffübergangslimitierter Trocknungsabschnitt durchgeführt, bei dem im wesentlichen keine Oberflächenverdunstung mehr stattfindet. Die Verdunstungsstellen, deren Gesamtheit den sogenannten Trocknungsspiegel darstellt, ziehen sich mehr und mehr in das Gutsinnere zurück. Die Flüssigkeit muss diffundieren. The solution so evaporated is by means of Discharge twin screw 6 from the mixer kneader 1 carried out continuously, simultaneously by shearing in warmed up the screw and into the mixer kneader 2 flashed. In this mixer kneader 2 is a material transfer limited drying section carried out, where essentially no surface evaporation takes place. The evaporation points, the entirety of which so-called drying mirror, pull more and back to the good inside. The liquid must diffuse.

    Für diesen Verfahrensabschnitt ist der Mischkneter 2 auf Grund der Wellengeometrie und der Kinematik mit einer maximalen Oberflächenerneuerung, Propfenströmung und guter Produkttemperatur-Kontrollmöglichkeit ausgestattet.The mixing kneader 2 is open for this process section Because of the shaft geometry and the kinematics with one maximum surface renewal, plug flow and good Product temperature control facility.

    Das entgaste Elastomer wird am Schluss mit der zweiten Austragdoppelschnecke 4 aus dem Mischkneter 2 ausgetragen. Das Elastomer beinhaltet noch einen Restlösungsmittelgehalt unter 1000 ppm.

    Figure 00100001
    The degassed elastomer is finally discharged from the mixing kneader 2 with the second discharge twin screw 4. The elastomer still contains a residual solvent content below 1000 ppm.
    Figure 00100001

    Claims (10)

    Verfahren zum kontinuierlichen Eindampfen bzw. zur thermischen Behandlung von zähviskosen Produkten, insbesondere Elastomeren und Thermoplasten, in einem Mischkneter mit zumindest einer mit Misch- bzw. Knetelementen (11) bestückten Rührwelle (7-10, 21),
    dadurch gekennzeichnet,
    dass in ein voreingedampftes viskoses Produktbett kontinuierlich neue niedrig viskose Produktlösung derart eingemischt wird, dass die Viskosität und Konzentration dieses Produktbettes so eingestellt wird, dass der Energieeintrag bestehend aus mechanischer Knetenergie und Wärmeübertragung über den Kontakt mit der Kneterwärmeaustauschfläche maximal ist.    Process for the continuous evaporation or for the thermal treatment of viscous products, in particular elastomers and thermoplastics, in a mixing kneader with at least one stirring shaft (7-10, 21) equipped with mixing or kneading elements (11),
    characterized by
    that new, low-viscosity product solution is continuously mixed into a pre-evaporated viscous product bed in such a way that the viscosity and concentration of this product bed is adjusted so that the energy input consisting of mechanical kneading energy and heat transfer via contact with the kneading heat exchange surface is maximum.         Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass eine Knetenergie durch Veränderung der Drehzahl und/oder des Füllgrades des Mischkneters (1) beeinflusst wird.A method according to claim 1, characterized in that a kneading energy is influenced by changing the speed and / or the degree of filling of the mixing kneader (1). Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das Produkt in dem Mischkneter (1) kontinuierlich rückgemischt wird.A method according to claim 1 or 2, characterized in that the product is continuously back-mixed in the mixing kneader (1). Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Produkt kontinuierlich aus dem Mischkneter (1) ausgetragen und in einen zweiten Mischkneter (2) eingegeben wird. Method according to one of claims 1 to 3, characterized in that the product is continuously discharged from the mixing kneader (1) and fed into a second mixing kneader (2). Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass das Produkt beim Austragen aus dem Mischkneter (1) aufgeheizt wird, bevor es in den Mischkneter (2) gelangt.A method according to claim 4, characterized in that the product is heated up when it is discharged from the mixing kneader (1) before it reaches the mixing kneader (2). Verfahren nach Anspruch 4 oder 5, dadurch gekennzeichnet, dass das Produkt in dem zweiten Mischkneter (2) einer Pfropfenströmung unterworfen wird.A method according to claim 4 or 5, characterized in that the product is subjected to a plug flow in the second mixing kneader (2). Verfahren nach Anspruch 6, dadurch gekennzeichnet, dass das Produkt in dem zweiten Mischkneter (2) einer grossen Oberflächenerneuerung sowie guter Produkttemperaturkontrolle unterworfen wird.A method according to claim 6, characterized in that the product in the second mixing kneader (2) is subjected to a large surface renewal and good product temperature control. Verfahren nach wenigstens einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass als Produkt eine ein Lösungsmittel enthaltende Elastomer-Lösung behandelt wird.Method according to at least one of claims 1 to 7, characterized in that an elastomer solution containing a solvent is treated as the product. Vorrichtung zur Durchführung des Verfahrens nach wenigstens einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, dass ein Einlauf (5) für das Produkt mit einem Mischkneter (1) mit guter Rückmischung und dieser mit einem Mischkneter (2) mit guter Propfenströmung in Verbindung steht.Device for carrying out the method according to at least one of Claims 1 to 8, characterized in that an inlet (5) for the product is connected to a mixing kneader (1) with good backmixing and this is connected to a mixing kneader (2) with good plug flow. Vorrichtung nach Anspruch 9, dadurch gekennzeichnet, dass an den Auslauf von jedem der beiden Mischkneter (1, 2) eine Austragdoppelschnecke (4, 6) anschliesst.Apparatus according to claim 9, characterized in that a discharge twin screw (4, 6) connects to the outlet of each of the two mixing kneaders (1, 2).
    EP01103153A 2000-02-24 2001-02-10 Method for processing a product in at least a mixing kneader Expired - Lifetime EP1127609B1 (en)

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    US9925693B2 (en) 2013-04-04 2018-03-27 Arlanxeo Deutschland Gmbh Method for removing volatile components from elastomer-containing media and degassing devices therefor
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    EP3288735B1 (en) * 2015-04-30 2024-07-03 ExxonMobil Chemical Patents Inc. Process for halogenating olefinic-derived elastomers in the bulk phase

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