WO2010057695A9 - Postcondensation de granulé de plastique - Google Patents

Postcondensation de granulé de plastique Download PDF

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Publication number
WO2010057695A9
WO2010057695A9 PCT/EP2009/061689 EP2009061689W WO2010057695A9 WO 2010057695 A9 WO2010057695 A9 WO 2010057695A9 EP 2009061689 W EP2009061689 W EP 2009061689W WO 2010057695 A9 WO2010057695 A9 WO 2010057695A9
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WO
WIPO (PCT)
Prior art keywords
reactor
arrangement
housing
reactor housing
outlet
Prior art date
Application number
PCT/EP2009/061689
Other languages
German (de)
English (en)
Other versions
WO2010057695A2 (fr
WO2010057695A3 (fr
Inventor
Miriam Fernanda Astegger
Peter Vollers
Original Assignee
Astegger, Johann, Josef
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Astegger, Johann, Josef filed Critical Astegger, Johann, Josef
Priority to EP09782815A priority Critical patent/EP2367622A2/fr
Priority to BRPI0915261A priority patent/BRPI0915261A2/pt
Publication of WO2010057695A2 publication Critical patent/WO2010057695A2/fr
Publication of WO2010057695A9 publication Critical patent/WO2010057695A9/fr
Publication of WO2010057695A3 publication Critical patent/WO2010057695A3/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/006—Baffles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/28—Moving reactors, e.g. rotary drums
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • C08G63/80—Solid-state polycondensation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/88—Post-polymerisation treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/88—Post-polymerisation treatment
    • C08G63/90—Purification; Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00029—Batch processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00031—Semi-batch or fed-batch processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00139—Controlling the temperature using electromagnetic heating
    • B01J2219/00141—Microwaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00139—Controlling the temperature using electromagnetic heating
    • B01J2219/00146—Infrared radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/00768—Baffles attached to the reactor wall vertical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/0077—Baffles attached to the reactor wall inclined
    • B01J2219/00772—Baffles attached to the reactor wall inclined in a helix

Definitions

  • the invention relates to a reactor arrangement for the energy-efficient postcondensation of polymers, the use of the reactor arrangement for the postcondensation of polycondensates or for the recycling of polyethylene terephthalate, as well as methods for the treatment of PET recycling material and the postcondensation of polymers such as polyamide or polyethylene terephthalate.
  • SSP Solid State Polymerization
  • stirred reactors which are used in a continuous process, more rarely in a semi-batch process, are also commonly used.
  • the advantage of the batch system is the relatively easily determinable initial viscosity, only over the reaction time, after the intermediate measurement. This advantage is particularly important in RECYCLING PET material where, as is known, the input viscosity is subject to large variations.
  • the heat source is almost always a hot wall of a double-walled reactor wall. This is not only technically very complicated, both in the production of the reactor and in the process, but also leads to a considerable safety risk by leaking hot oil.
  • DE 102 25 075 A1 describes a method and a device for the continuous postcondensation of plastic granules.
  • the reactor used with a rotating axis is designed double-walled, wherein between the walls heated oil is used as the heat transfer medium.
  • DE 2152245 A describes by way of example the classical postcondensation in a tumble dryer.
  • Hexanedioic acid and 1,6-diaminohexane react with elimination of water to form polyamide 6,6.
  • This water is formed during the postcondensation of polyamide and must be removed as efficiently as possible.
  • the granules but cooler than the environment, the water condenses on the granules or even unnecessarily long in the granules. This in turn results in long after-condensation times.
  • the object of the present invention is to provide a reactor and a process for the postcondensation of polymers, in which the heat input can be made more efficient and the degradation products can be transported away more easily, which reduces the after-condensation times and thus ensures better energy efficiency.
  • the object underlying the invention is achieved by a hermetically sealable Reactor arrangement 1 for crystallizing, after-condensing or decontaminating polycondensates comprising at least one heat source 3, which is characterized in that the reactor arrangement 1 has a fixed mandrel 11 about which the reactor housing 13 is rotatable.
  • the reactor arrangement is not hermetically sealable, undesirable oxidation and thus deterioration of the material often occur during recondensation or recycling.
  • Polycondensates can be, for example, PET flakes.
  • Hermetic in the sense of the invention means at least air and vacuum tight.
  • the reactor housing has, for example, a length in a range of 1 to 15 m.
  • the reactor housing has, for example, a diameter in a range of 0.5 to 3 m.
  • the wall thickness of the reactor housing 13 preferably has a thickness in a range of 1 to 10 mm.
  • the reactor arrangement 1 preferably has a conveying means 5 along the main axis of the reactor 7. Thereby, the material to be treated within the reactor 7 can be easily conveyed, for example, from the feed 29 to the outlet of the reactor assembly 37.
  • the reactor arrangement 1 according to the invention preferably has a vacuum pump 9. This allows vacuum to be applied in the reactor interior 15 and by-products such as water easier be transported away. Alternatively, the processes according to the invention can also be carried out under protective gas.
  • the fixed mandrel 11 is advantageously designed hollow.
  • the at least one heat source 3 can be arranged within the reactor housing 13, so that most of the heat energy in the reactor interior 15 in the treated material (for example granules or flakes) can be largely absorbed and barely penetrates to the outside.
  • the reactor arrangement according to the invention can be realized much more energy efficient than previously known reactors.
  • the fixed mandrel 11 has the further advantage that analytical and measuring instruments can be arranged in the axis with which the postcondensation process can be monitored much more easily in the current process.
  • the reactor housing 13 is preferably rotationally symmetrical with respect to the axis of rotation 7.
  • the reactor arrangement 1 according to the invention is equally suitable for example for semi-batch or batch operation and can also be cascaded.
  • Cascadable in the context of the invention means that individual reactor arrangements according to the invention can be connected in series and individual treatment phases (for example crystallization, postcondensation, cooling,...) Can be carried out successively in different reactor arrangements.
  • the reactor housing 13 is advantageously substantially tubular. Alternatively, the reactor housing can also be polygonal. Thus, the housing can also be at least 4- and at most 200-edged. This simplifies on the one hand the production of the reactor itself and on the other hand allows this embodiment of this reactor housing 13 a particularly easy transport of the polymers (as granules or pellets) or plastic flakes within the reactor assembly 1.
  • the fixed mandrel 11 through the main axis of rotation 7 along the tubular Reactor Housing 13.
  • the weight of reactor housing 13 rests primarily on storage devices located below the reactor, such as rollers or wheels 19.
  • Rollers or wheels 19 are advantageously arranged under the reactor housing 13, on which the reactor housing 13 is stably and statically stably suspended around the main axis of rotation 7, the axes of rotation of the rollers or wheels 19 being parallel to the main axis of rotation 7 of the reactor housing 13.
  • the reactor housing 13 may be supported on at least four wheels 19 or independently on at least two rollers 19.
  • the reactor housing 13 may be supported on at least four wheels 19 or independently on at least two rollers 19.
  • these rollers 19 are, for example, at a distance of at least the quarter radius the reactor housing 13 and at most provided at a distance from the diameter of the reactor housing 13.
  • wheels 19 are used, then for example those wheels 19 which have the same axis of rotation are connected to an axle. However, the wheels do not have to be connected to an axle and, for example, can each be driven separately.
  • rollers or wheels 19 are arranged for example on rotary rings, on which a drive 21 acts.
  • the axle with the wheels 19 or the respective roller 19 can be driven directly by a drive 21.
  • a preheating area 22a for example crystallization
  • a reactor area 22b for example aftercondensation
  • a cooling area 22c In the preheating region 22a, the introduced granules can be preheated.
  • the cooling region 22c the granules can be cooled accordingly.
  • a single-walled reactor housing 13 is advantageous, since in this way the waste heat can be transported away more easily.
  • the reactor housing 13 is partially or completely and in particular at least in the reactor region double-walled.
  • the reactor housing 13 is partially or completely and in particular at least in the reactor region double-walled.
  • the double-walled reactor housing 13 can also be designed so that the intermediate space is in communication with the reactor interior 15.
  • the two walls of the double wall are preferably thermally insulated from each other.
  • the reactor assembly 1 is commonly used in processes in which a vacuum is applied within the reactor housing 13. If there is now a connection between the interior of the reactor 15 and the intermediate space of the double-walled reactor housing 13, a highly efficient thermal insulation can be achieved particularly simply in such methods.
  • slats 23 are advantageously integrally formed with at least one preferably controllable or adjustable passage 25 in the fins 23 to the reactor housing 13.
  • these slats 23 have the advantage that the dwell time and / or filling level of plastic granulate or recycled material can be controlled separately in each individual section of the reactor interior 15, which is bounded by the slats 23. Due to the fact that the lamellae 23 are formed directly on the reactor housing 13, it is not possible for the otherwise threatening jamming of the conveyor worm or conveyor spiral in the reactor housing 13 to occur.
  • the size of the passage 25 can be varied.
  • the residence time and / or the fill level of the granules, the flakes or the recycled material can be constantly adapted not only in advance but over the duration of the process.
  • the passage 25 may be an adjustable flap. With this adjustable flap, the angle of attack can be regulated. In addition, the direction of rotation of the flap can be regulated.
  • the heat source 3 is at least one in particular controlled infrared radiator.
  • a microwave radiator can be used. So far, due to the different design of the reactors, infrared radiators could not be used for the postcondensation of polymer material or for the recycling of, for example, PET. Due to the new design of the reactor with a fixed mandrel 11 infrared radiator can be arranged in this fixed mandrel inside the reactor housing 13 in the reactor interior 15. The fact that plastic and water absorb medium-wave or short-wave infrared radiation excellent, the granules heats up better than the planar atmosphere or the reactor housing 13.
  • an infrared radiator with the greatest intensity is selected at a wavelength in a range of 1 to 4.5 ⁇ m.
  • the radiant energy is absorbed particularly well by the polycondensate.
  • the heat could be transferred directly from the heated reactor wall to the material to be treated only with much longer wave heat radiation.
  • the heated wall of the tumble dryer previously used could not be heated above 250 0 C, otherwise the material would be melted.
  • this longer-wave thermal radiation is very poorly absorbed by polycondensate.
  • only little energy can be transported with longer-wave radiation.
  • radiation exchange is the only possible form of heat transfer in a vacuum.
  • the at least one infrared radiator 3 can be arranged in the stationary mandrel 11.
  • the infrared radiator 3 may be directed downwards in the direction of the rollers or wheels 19.
  • the granulate or the recycling material will namely be located in the reactor interior 15 of gravity, because typically in the lower region of the reactor interior 15.
  • a pyrometer 27 may be provided to constantly monitor and / or regulate the material temperature of the material to be treated.
  • a pyrometer 27 and independently a heat source 3 is provided for each individual section separated by fins 23.
  • the reactor housing 13 rotates constantly around the mandrel 11.
  • the fixed dome 11 has the further advantage that the feed 29 can be provided within this axis and so be configured without rotation as usual and thus very low maintenance.
  • generators for high-frequency fields 31 for example high-frequency generators or electrostatic electrodes
  • the fixed mandrel 11 itself does not have to contain a vacuum.
  • the reactor arrangement 1 advantageously comprises a delivery spiral 33 at the outlet of the reactor interior 35, which raises and / or conveys the treated material towards the outlet of the reactor arrangement 37.
  • This conveyor spiral extends, for example, on the side of the outlet of the reactor interior 35 over the entire diameter of the reactor interior 15.
  • a vacuum lock 39 in particular a double vacuum lock 39 for synchronous loading and unloading is provided at the feed 29 and the outlet of the reactor assembly 37.
  • a postcondensation process or a recycling process can be operated quasi-continuously or semi-continuously.
  • At least two projecting rings 41 are advantageously formed on the reactor housing 13. These rings 41 are advantageously so high that cables can be laid through the rings on the reactor wall 13 along. In particular, the rings 41 are at least 4 mm high. These can act as spacers so that mechanical, electrical and / or electronic components can be arranged on the outer surface of the reactor housing 13. These may be control devices for the flaps 25, for example. For example, these rings 41 put on the wheels or rollers 19. With slip rings can be transferred to these components on the outside of the reactor housing 13, for example, power or energy in a different form (for example, via hydraulic to control the flaps 25). There can also be laid cables.
  • At least one water bath 43 may be provided below the reactor housing 13, which is filled so high with water that the rings 41 dive into the water bath, but for example, the reactor housing 13 is not immersed in the water bath.
  • separate water baths 43 are provided in the cooling area 22c and the preheating area 22a, which are connected to each other in a circulating manner. The water can be circulated in these different baths 43, for example.
  • the ring 41 can be cooled in the vicinity of the outlet of the reactor interior 31 and thus also cool the exiting granulate or recycled material.
  • the thus heated water bath 43 can be used for preheating the incoming material, for example by the feed 29.
  • the ring 41 arranged there, for example can be correspondingly heated by the water bath 43, which has an effect particularly under protective gas.
  • additional cooling rings may be provided on the outer wall. These are advantageously made of silver or copper. These may adopt a so-called "double T-shape, wherein a band-shaped part of the cooling ring on the outer wall of the Reactor housing 13 rests, from which centered, for example, a cooling rib is integrally formed. In turn, a wide free-standing band is formed on this cooling fin, which can then dip into one of the water baths 43, for example.
  • the reactor housing 13 is fixedly mounted on the rollers or wheels 19.
  • the mandrel 11 and the discharge unit 58 are "freely” suspended in the reactor housing 13 via the bearing / vacuum seals 17 and 55.
  • the components such as the feed 29, feed to the pump 9 and supply to the outlet of the reactor assembly 37 are provided with elastic sections (See Fig. 1).
  • the mandrel 11 is practically only “loosely” suspended in the reactor interior 13. Co-rotation of the dome 11 and / or the discharge unit 58 can be prevented by simple, conventional measures. This has the advantage that when the thermal expansion of the reactor housing 13 by a few millimeters or centimeters, for example, the feed 29 or the outlet from the reactor assembly 37 "mitwandern" can.
  • the object underlying the invention is achieved by the use of the reactor arrangement 1 according to the invention for the recycling of polyethylene terephthalate or for the postcondensation of polycondensates, in particular nylon, polyethylene terephthalate (PET), polycarbonates or copolymers or blends (for example PBT / PS, PBT / ASA , PBT / ABS, PBT / PC, PET / ABS, PET / PC, PBT / PRT / PC, PBT / PET, PA / PE or PA / ABS).
  • PET polyethylene terephthalate
  • polycarbonates or copolymers or blends for example PBT / PS, PBT / ASA , PBT / ABS, PBT / PC, PET / ABS, PET / PC, PBT / PRT / PC, PBT / PET, PA / PE or PA / ABS).
  • the reactor arrangement according to the invention can be used in both batch and semi-batch processes.
  • the object underlying the invention is achieved by a batch process for the postcondensation or for the preparation of polymer material such as generally polycondensate or especially PET recycled material with the reactor assembly 1 according to the invention, wherein a) in a first step, the rotating reactor charged with polymer material, so that, in particular in the region of the fins 23, the desired levels are reached, b) in a second step, the reactor heats c) or at least from a temperature in the amount of 150 0 C creates a vacuum or the reactor with Protective gas flows, d) in a further step, the reactor housing 13 rotates about the fixed mandrel 11 until the desired target viscosity of the polymer material is reached, and e) discharges the polymer material from the reactor in a further step.
  • step c) creates a vacuum already at 100 0 C at the latest or flooding the reactor at the latest at this temperature with a protective gas.
  • This process according to the invention is carried out, for example, as a batch process.
  • a PET recycling material with different viscosity is used.
  • the plant is, for example, over the fixed mandrel 11 is charged with the feed 29 until the tubular reactor housing 13 - has reached the desired levels in the heating area.
  • those reached after the loading time for example, is heated and from about 100 0 C vacuum drawn.
  • the viscosity can now be accurately determined over the reaction time. If this is reached or calculated, for example, the discharge starts, whereby the cooling can be sectoral.
  • the advantage here is that the loading and unloading times can be partially included.
  • a sampler 44 is provided in the reactor wall of the reactor housing.
  • This can for example be a passage with pipe connection and, for example, a double ball valve.
  • the method according to the invention there are significant advantages. Due to the much better adjustable temperature gradient and, for example, by the infrared heater, a much better energy yield can be achieved.
  • the loading and unloading times can be included. There is less energy peak load.
  • the preheating and the cooling can be realized by a simple water bath 43.
  • at least two water baths 43 are used, which are connected to one another.
  • the object on which the invention is based is achieved by a semi-batch process for recycling or postcondensing polymers such as polycondensates, in particular polymers such as polyamide or polyethylene terephthalate, with the reactor arrangement 1 according to the invention, where a) the under reduced pressure or inert gas polymer is fed via the stationary mandrel 11, the reactor housing 13 being rotated about the fixed mandrel 11, b) conveying the polymer with the conveying means 5 along the main axis of the reactor 7 towards the outlet of the reactor arrangement 37 and, at the same time, with the heat source 3 heated, c) the polymer at the outlet of the reactor interior 35 cools and then transported with a delivery spiral 33 in the direction of the outlet of the reactor assembly 37, and d) discharges the polymer at the outlet of the reactor assembly 37.
  • polymers such as polycondensates, in particular polymers such as polyamide or polyethylene terephthalate
  • This method is carried out, for example, as a semi-batch method.
  • This method can not only be used for the pure postcondensation of polycondensate, but also, for example, for the recycling of PET.
  • this mode is intended for example for recondensing nylon.
  • new material is introduced in portions into the rotating tubular reactor housing 13 via the fixed axis 11 via the vacuum locks.
  • the slats 23 regulate the level and the residence time in the individual sections.
  • Infrared heating 3 regulates delay-free and precisely the product temperature via the sectoral pyrometers.
  • the medium wave infrared heater effectively heats the pellets "from the inside", which is what the Drying and crystallization very fast. The heat in this construction is properly inside, and the jacket is always cooler, which supports the removal of the split-off products.
  • tubular reactor housing 13 If the tubular reactor housing 13 is now filled to the extent that the material has already arrived at the outlet, it is cooled there (simply on the outer wall 13, which dips with the outer rings 41 in a water bath 43) and then lifted by the spiral 33 and to Output vacuum lock 37,39 transported. This happens, for example, by a fixed inside stretched spiral on the output inner tube.
  • the initial viscosity is adjusted once and remains the same for the same materials.
  • the material to be treated (for example, granules, pellets or flakes) is heated at least in one of the separated for example, by the slats 23 sections in the interior of the reactor 15 to a temperature in a range from about 230 to about 250 0 C.
  • amorphous starting material or flakes can be introduced through the feed 29 in the reactor interior 15 and the first portions of the reactor interior 15, which are formed for example by the fins 23, can be used at a temperature slightly above the glass transition temperature of the Starting materials from the amorphous material to produce a crystalline material.
  • the first sections can thus be used, for example, for crystallization.
  • higher temperatures can be set in the further sections in order to carry out the processes according to the invention (for example aftercondensation) accordingly.
  • the object underlying the invention is achieved by a process for producing polycondensate having a constant viscosity from recycled material, characterized in that the product of one of the processes A according to the invention having a specific viscosity with a polycondensate B having a higher Viscosity mixes while the mixing ratio automatically adjusted so that the viscosity of the mixture product AB is constant at a desired value between the viscosities of the two different mixing components A and B, which is controlled by viscosity measurements before and / or after the mixer.
  • the mixture product AB can subsequently be extruded and, independently of this, further processed to pellets or granules after the extrusion.
  • the mixture product AB can also be further processed, for example, directly into PET bottle blanks.
  • the polycondensate B having a higher viscosity can also be obtained by one of the methods according to the invention, wherein the parameters (for example temperature, duration of treatment,...) Are set such that a higher viscosity than in the case of the polycondensate A is obtained.
  • the viscosity can be measured by the method described in the article "A Real-time Ultrasonic Technique for Viscosity Monitoring during Polymer Processing", AIP Conf. Proc, 7 July 2008, Volume 1027, pages 1217-1219.
  • FIG. 1 shows a cross section through the reactor arrangement 1 according to the invention along the main axis of the reactor 7.
  • Figure 2 shows a cross section through the reactor assembly 1 according to the invention at the position 45, as shown in Figure 1.
  • the cross-sectional plane is perpendicular to the main axis of the reactor 7.
  • Figure 2 the arrangement of the water bath 43 is illustrated.
  • FIG. 3 shows a cross section through the reactor arrangement 1 according to the invention at a position where a lamella 23 is located.
  • FIG. 4 shows the conveyor spiral 33.
  • Figure 5 shows a cross section through the reactor assembly 1 at a position where a blade 23 is located.
  • the passage of the blade 23 is designed differently to the passage 25 in Figure 3.
  • water includes not only water but also water one or more additives, such as are common in a water bath for temperature control, for example. It is also possible alternatively or additionally to use other coolants or heat carriers than water.
  • the reactor arrangement 1 essentially consists of a tubular reactor housing 13 and the stationary mandrel 11, into which plastic granules or PET recycling material are introduced through the stationary mandrel 11 into the reactor interior 15 through the feed 29.
  • the tubular reactor housing 13 is rotatably supported by the bearings 17 around the fixed mandrel 11.
  • fins 23 are formed in the interior. These fins 23 each have a passage adjustable 25. Thus, these slats 23 with the passage 25, the conveyor 5.
  • infrared radiators are arranged as a heat source 3. These are coupled to a pyrometer 27 for temperature control and adjustment.
  • a unit of infrared radiator 3 and pyrometer 27 is provided for each space between two fins 23.
  • the infrared radiator 3 are directed downwards and irradiate introduced by the feed 29 and conveyed by the conveyor 5 material (such as granules or flakes) in the reactor interior 15.
  • 47 corresponding window 47 are provided in the fixed mandrel.
  • At least the interior of the reactor 15 is sealed to the outside so that a vacuum can be applied in the reactor interior 15.
  • a vacuum pump 9 is connected to the reactor interior 15.
  • the reactor interior 15 is sealed against the outside world so that created a vacuum can be.
  • the bearing 17 in the vicinity of the feed 29 is correspondingly airtight.
  • the substantially tubular reactor housing 13 has rings 41, which in turn are mounted on rollers 19. These rollers 19 are connected to a common axis 49, which in turn is connected to a drive 21. In total, there are four such rollers 19 with two axes 49, which are arranged substantially parallel under the reactor.
  • a high-frequency generator 31 may be provided to the post-condensing of the granules, as in the prior art already known to accelerate. Depending on the angle of attack of the apertures of the fins 25, the granules are conveyed correspondingly faster or slower from one section between two fins 23 to the other.
  • These passages of the fins 25 may be, for example, flaps.
  • flaps 25 can be controlled from outside on the reactor wall 13 located control devices 53. Because of the rings 41, the reactor housing 13 always keeps a certain distance from the other components of the reactor arrangement 1 according to the invention. The necessary power supply for these control devices for the flaps 53 can take place via so-called slip rings, which are not shown separately in FIG. Depending on the angle of attack of the flaps 25, therefore, the granules, as already mentioned, are conveyed from one section between two lamellae 23 to the other. At the end of the reactor housing 13, the granules then reaches the outlet of the reactor interior 35 and lands through it in the conveyor spiral 33. With this conveyor spiral, the granules are raised approximately at the level of the stationary mandrel 11.
  • the treated granules then fall into a funnel leading to the outlet the reactor assembly 37 leads.
  • the outlet of the reactor assembly 37 as well as the feed 29 and the bearings / seals 11 and 55 are hermetically sealed to the outside with a double vacuum lock.
  • the part of the reactor arrangement 1 according to the invention which comprises the outlet of the reactor arrangement 37 and the vacuum pump 9 is stationary in this exemplary embodiment.
  • the rotating reactor housing 13 is hereby connected to a vacuum seal 55.
  • the signals for the control device for the flaps 53 or measured values can be transmitted, for example, by appropriate signal processing and wireless LAN 57 for further processing.
  • the reactor interior 15 is flooded with nitrogen, for example, in a first step. Thereafter, the reactor interior 15 is charged via the feed 29 with PET recycling material.
  • the reactor housing 13 already rotates about the fixed mandrel 11.
  • the flaps 25 in the fins 23 are adjusted by means of the control devices 53 so that with each revolution of the reactor housing 13, some recycled PET material in the next section between two fins 23 is further promoted , If the desired filling level with PET recycling material is reached in each of the sections between the lamellae 23, the flaps 25 are closed by means of the control device for the flaps 53, so that transport no longer takes place.
  • the interior of the reactor 15 is heated during the rotation of the reactor housing 13 by means of the infrared radiator 3 to a temperature of about 230 0 C and applied a vacuum by means of the vacuum pump 9.
  • the reactor housing 13 will then continue around the stationary mandrel 11 rotates until the desired target viscosity of the recycled material is reached.
  • the viscosity can be readily determined by a sampler 44 located on the reactor housing 13.
  • the flaps 25 are placed in the blades 23 via the control device 53 so that a maximum transport rate is achieved and the PET recycled material is conveyed into the conveyor spiral 33.
  • the conveyor spiral 33 subsequently raises the PET recycling material at the level of the stationary dome 11.
  • the PET recycling material is conveyed with a transport spindle 34 as far as the funnel, which leads to the outlet of the reactor arrangement 37.
  • the treated PET recycling material is discharged from the reactor assembly 1 according to the invention.
  • the semi-batch process for example, for the post-condensation of polyamide or polyethylene terephthalate from.
  • granules of polyamide or polyethylene terephthalate are introduced via the feed 29 into the reactor interior 15 in a similar manner.
  • the reactor interior 15 is always under vacuum, which is generated via the vacuum pump 9.
  • the polymer is conveyed along the major axis of the reactor 7 towards the outlet of the reactor assembly 37 and, in the meantime, with infrared heaters 3 fixed in the hollow Dorn 11 are mounted, heated to about 240 0 C.
  • This temperature is controlled by the arranged next to the infrared radiators pyrometers 27 and adjusted if necessary.
  • a water bath 43 is located below the reactor housing 13, so that the reactor housing 13 is not wetted with water, but the rings 41 are immersed in the water bath. This has the particular advantage that the treated granules can be cooled down at the level of the last section, since there located nearby ring 41 is cooled by the water bath 43 and can dissipate heat from the reactor housing 13 at this point accordingly.
  • the granules in the vicinity of the feed 29 can be preheated in the same way by the nearby there ring 41, since the ring 41 there can absorb heat from the water and there pass on to the reactor housing 13.
  • the granules are then conveyed with the conveyor spiral 33 to the outlet of the reactor arrangement 37.
  • This process for recondensing polymer can be carried out quasi-continuously, since in the double vacuum lock 39, for example, raw granules can be introduced simultaneously through the feed 29 and at the same time a similar amount of treated granules can be removed through the double vacuum lock 39 at the outlet of the reactor assembly 37.
  • the vacuum is thereby insignificantly impaired for the time in which the internal valve of the double vacuum lock 39 is opened. Depending on the configuration of the vacuum pump 9, this impairment can be kept short.
  • a somewhat lower temperature is set with the infrared radiators 3 in the first sections of the reactor interior between the lamellae 23, so that these sections can serve for the crystallization. Namely, amorphous material can be used as the input material. This has been difficult with conventional methods.
  • the temperature set in the first sections is typically just above the glass transition temperature of the polymer used.
  • the processes according to the invention can also always be carried out under protective gas.
  • Figure 2 shows a cross section perpendicular to the main axis of the reactor 7 at the position 45, as shown in Figure 1.
  • the ring 41, the reactor housing 13, the reactor interior 15, the main axis of the reactor 7 and the rollers 19 are shown.
  • the water bath 43 is shown. It should be noted that the level of the water bath 43 wets the ring 41 but does not have to wet the wall of the reactor housing 13.
  • FIG. 3 shows a cross section perpendicular to the main axis of the reactor 7 at the point where a lamella 23 is located.
  • the reactor housing 13 and the lamella 23 are shown with the passage of the lamella 25.
  • the passage of the lamella 25 is designed in this case as a one-legged flap. This flap can have different angles of attack, so that the granules are transported at a correspondingly different speed from one side of the reactor 13 to the other side.
  • the also shown control device for the flap 53 is in this case for ease of understanding a simple lever. Alternatively, a worm wheel can be used.
  • FIG. 4 shows the image of the conveyor spiral 33, which extends in the direction of the outlet of the reactor interior 35 over the full diameter of the reactor interior 15. It then tapers so far that it can lift the granules approximately at the level of the outlet channel 54 and can transport via the transport spindle 34 and the funnel to the outlet of the reactor arrangement 37.
  • FIG. 5 corresponds approximately to FIG. 3 with the difference that a two-legged flap is depicted as the passage of the lamellae 25.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

L'invention concerne un ensemble réacteur destiné à la postcondensation de polymères, l'utilisation de cet ensemble réacteur pour la postcondensation de nylon ou de polyéthylène téréphtalate ou pour le recyclage de polyéthylène téréphtalate, ainsi que des procédés de préparation de matériaux de recyclage de PET et de postcondensation de polymères tels que le polyamide ou le polyéthylène téréphtalate.
PCT/EP2009/061689 2008-11-21 2009-09-09 Postcondensation de granulé de plastique WO2010057695A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP09782815A EP2367622A2 (fr) 2008-11-21 2009-09-09 Postcondensation de granulé de plastique
BRPI0915261A BRPI0915261A2 (pt) 2008-11-21 2009-09-09 reator hermeticamente vedado para cristalização, pós-condensação ou descontaminação de condensados de polímero, uso do reator, processo intermitente para a pós-condensação para o processamento de polímeros, processo semi-intermitente para a reciclagen ou pós-condensação de polímeros e processo para a produção de condensado de polímero

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008058313.8 2008-11-21
DE200810058313 DE102008058313A1 (de) 2008-11-21 2008-11-21 Nachkondensieren von Kunststoffgranulat

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WO2010057695A2 WO2010057695A2 (fr) 2010-05-27
WO2010057695A9 true WO2010057695A9 (fr) 2010-08-26
WO2010057695A3 WO2010057695A3 (fr) 2010-11-04

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BR (1) BRPI0915261A2 (fr)
DE (1) DE102008058313A1 (fr)
WO (1) WO2010057695A2 (fr)

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Publication number Priority date Publication date Assignee Title
DE102011052185A1 (de) 2011-07-27 2013-01-31 Johann Josef Astegger Reaktoranordnung
GB2507488A (en) * 2012-10-30 2014-05-07 Ashe Morris Ltd Rotating flow reactor with extended flow path
WO2015040562A1 (fr) 2013-09-19 2015-03-26 Christian Schiavolin Procédé de traitement et appareil de traitement pour substance liquide
CN103752225B (zh) * 2014-01-04 2015-06-10 衢州昀睿工业设计有限公司 具有双上升动能的自循环合成反应器
DE102015009754A1 (de) * 2015-07-29 2017-02-02 Torsten Heitmann Kristallisator bzw. Reaktor und Verfahren zur kontinuierlichen Züchtung von Kristallen bzw. kontinuierlichen Reaktionsführung

Family Cites Families (8)

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Publication number Priority date Publication date Assignee Title
DE1745532C3 (de) * 1967-05-19 1974-12-05 Davy International Ag, 6000 Frankfurt Polykondensationsreaktor
BE773707A (fr) 1970-10-23 1972-01-31 Sandoz Sa Procede de preparation de polycondensats a poids moleculaire eleve
DE2142456A1 (de) * 1971-08-25 1973-03-01 Rudolf Dr Beck Reaktor zur kontinuierlichen aufbereitung von polymeren
DE10225075A1 (de) 2002-02-07 2003-11-20 Ohl Appbau & Verfahrenstechnik Verfahren und Vorrichtung zur kontinuierlichen Nachkondensation von Kunststoffgranulat, wie beispielsweise Polyester oder Nylon
DE102004050356A1 (de) 2003-11-21 2005-07-28 Gala Industries, Inc. Verfahren und Vorrichtung für das Herstellen von kristallinem PET-Granulat
DE102005013701A1 (de) 2005-03-24 2006-09-28 Krones Ag Verfahren und Vorrichtung zur Dekontamination von Kunststoffflakes
DE102006016534A1 (de) * 2006-04-07 2007-10-11 Ohl Engineering Gmbh Pet Recycling Technoligies Vorrichtung sowie Apparatur und Verfahren zur Behandlung von Materialien bei erhöhter Temperatur und unter Bewegung und unter Vakuum
WO2007131728A1 (fr) * 2006-05-11 2007-11-22 Aquafil Engineering Gmbh Procédé et dispositif de polymérisation en continu d'un polymère en phase solide

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DE102008058313A1 (de) 2010-06-02
WO2010057695A2 (fr) 2010-05-27
BRPI0915261A2 (pt) 2016-02-16
WO2010057695A3 (fr) 2010-11-04
EP2367622A2 (fr) 2011-09-28

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