EP1833874A1 - Procede et dispositif pour produire un granulat et/ ou des pieces moulees en polyester a faible teneur en acetaldehyde - Google Patents

Procede et dispositif pour produire un granulat et/ ou des pieces moulees en polyester a faible teneur en acetaldehyde

Info

Publication number
EP1833874A1
EP1833874A1 EP05809991A EP05809991A EP1833874A1 EP 1833874 A1 EP1833874 A1 EP 1833874A1 EP 05809991 A EP05809991 A EP 05809991A EP 05809991 A EP05809991 A EP 05809991A EP 1833874 A1 EP1833874 A1 EP 1833874A1
Authority
EP
European Patent Office
Prior art keywords
melt
polycondensation
discharge
drying
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05809991A
Other languages
German (de)
English (en)
Inventor
Kurt Hanimann
Werner Stibal
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Uhde Inventa Fischer AG
Original Assignee
Uhde Inventa Fischer AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Uhde Inventa Fischer AG filed Critical Uhde Inventa Fischer AG
Publication of EP1833874A1 publication Critical patent/EP1833874A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
    • 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
    • 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
    • C08G63/785—Preparation processes characterised by the apparatus used
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00823—Mixing elements
    • B01J2208/00831—Stationary elements
    • B01J2208/0084—Stationary elements inside the bed, e.g. 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
    • 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
    • B01J2219/00777—Baffles attached to the reactor wall horizontal
    • 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
    • B01J2219/00779—Baffles attached to the stirring means
    • 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
    • B01J2219/18—Details relating to the spatial orientation of the reactor
    • B01J2219/182—Details relating to the spatial orientation of the reactor horizontal

Definitions

  • the present invention relates to a method and an apparatus for producing low-acetaldehyde polyester granules and / or shaped articles from a melt discharged from a polycondensation.
  • the polyester may be, in particular, polyethylene terephthalate or its modified copolymers having acid-side modification amounts, e.g. of isophthalic acid or on the diol side e.g. of cyclohexadimethanol.
  • the material is particularly suitable as a packaging material in the form of films, films or hollow bodies such. Bottles.
  • acetaldehyde (hereinafter also: AA) as an undesirable by-product, wherein the AA content in the melt immediately after the Austragsaggregat usually 20 - 100 ppm , AA is very odor and taste intensive and disturbs especially in the food industry, because it diffuses even in a cold state in the food.
  • AA content in the preforms 1-3 ppm for water applications and 4-10 ppm for sweet drinks (CSDs). This means that, at least for these applications, the AA content has to be drastically reduced.
  • a first such method consists in chemically binding the AA by adding additives, so-called AA blockers.
  • additives can lead to yellowing and / or clouding of the material.
  • the AA blockers have to meet the requirements of the food industry. Their use is therefore limited. It is customary to dose AA blocker for high requirements, such as for water directly during injection molding, in order to compensate for the formation of AA occurring here.
  • Another method is to evaporate AA at elevated temperatures below the melting point. In general, this is done in combination with a solid phase postcondensation, wherein the degree of polycondensation is increased at a temperature between 190-230 ° and at the same time AA is deposited. To prevent thermo-oxidative damage, this is carried out in a stream of an inert gas such as nitrogen.
  • the granules thus obtained typically have an AA content of less than 1 ppm.
  • the treatment is time-consuming, requires large appliances, lasts almost a whole day and consumes a lot of energy.
  • the method is also applicable only to granules, but not if the melt coming from the polycondensation is directly e.g. an injection molding machine for the production of preforms is supplied.
  • Disk reactors operate on the principle that a horizontal cylindrical apparatus 20 with a diameter between 50 cm and 500 cm by controlling the continuous product entry (product in) and - product out to around one quarter to a maximum of half filled with melt. There is vacuum over the melt (vaper out). From the melt sump 21 shown dotted pull on a longitudinal shaft 22 or a basket-like structure arranged rotating disks, of which only two are designated 23, the melt high and drain them gravimetrically, whereby a large surface of the melt relative to the free space (vacuum ) is generated.
  • the level gradient forming in the sump 21 ensures inter alia the longitudinal flow of the melt through the reactor. It is usually by static internals such. Weirs, of which only two are designated 24, and controls the arrangement and speed of the rotating discs 23 in the reactor.
  • the sump 21 serves primarily to ensure the uniform loading of the discs 23 with melt.
  • Austrags Scheme 25 in which the melt at elevated viscosity for
  • the feed pressure to the discharge unit 26 is usually by arranging the Austragsaggregats at a certain distance from the bottom of the cylindrical apparatus 20 at the lower end of a collection process 27 still elevated.
  • the height of the liquid column can be up to 200 cm here.
  • the thermal degradation are formed in principle in this process in the melt continuously by-products, especially acetaldehyde.
  • the acetaldehyde can evaporate out of the melt due to the phase equilibrium, so that a very low AA content is established there in the melt. This is particularly the case on the discs 23, where thin product layers are formed.
  • the acetaldeyhyd formed in the thick sump layer 21 can only diffuse to the surface to a very small extent and thereby accumulates in the melt. If one takes the discharge area 25 with the aforementioned collection process 27, in which the entire polymer is no longer in contact with the vacuum in the reactor, the AA content can be up to
  • Discharge unit 26 in this method already significantly greater than 10 ppm.
  • the object of the invention is to specify how the AA content can be reduced in a simpler and more economical manner. This object is achieved according to the invention by a method as characterized in claim 1. An apparatus for carrying out the method is specified in claim 19.
  • the melt in the discharge region of a polycondensation is kept in contact with a gas space under reduced pressure at a temperature between 270 ° and 285 ° C.
  • the temperature of the melt in the discharge region of the polycondensation is preferably set to a value between 275 and 280 ° C.
  • the pressure in the gas space is preferably kept below 2 mbar, further preferably below 1 mbar.
  • melt with a discharge unit such. a discharge pump is discharged from the discharge of the polycondensation, it is advantageous if the melt is kept up to the discharge unit with the gas space in contact under reduced pressure. It should not arise before the Austragsaggregat the usual swamp there.
  • the apparatus preferred for carrying out the method according to the invention has, according to claim 19, a novel disk reactor in which, as far as possible, a sump is dispensed with.
  • the melt is transported directly from disk to disk by a combination of rotating disks and static scrapers attached to the circumference of the reactor.
  • static wipers convey the melt directly into the discharge unit, without any accumulation of melt occurring here as well.
  • the disk structure of the novel disk reactor is chosen so that no thick layers arise and the replacement of the product is ensured on the disc.
  • the discharge pump is flanged with a rectangular inlet flange directly to the reactor and under the last scrapers and discs of Agitator arranged.
  • the thickness of the melt layers throughout the reactor can be kept below 10 cm, predominantly even below 3 cm.
  • the new arrangement allows the controlled guidance of the melt on the discs as well as in ⁇ the longitudinal direction of the reactor, especially at high degrees of polymerization and relatively low temperature.
  • the melt leaves the polycondensation with an AA content of approximately 0 ppm. In any case, less than 5 ppm of AA content can be achieved. This means a drastic reduction in comparison to the AA content of 20-50 ppm which is customary per se at the outlet of the polycondensation directly after the discharge unit. In the amorphous granulate thereby reduces the AA content to ⁇ 10 ppm compared to> 50 ppm in the conventional method.
  • melt after its discharge from the polycondensation inter alia, to be used directly for the production of preforms on an injection molding machine, it can be used in polycondensation, e.g. by using a polycondensation (high-viscosity finisher), to an intrinsic viscosity between 0.5 - 0.9 dl / g, in particular between 0.70 - 0.85 di / g, can be adjusted.
  • a polycondensation high-viscosity finisher
  • melt from the polycondensation is discharged into at least one melt line, it is preferred if the melt in this at least one melt line is kept in the same temperature range as stated above for the discharge range of the polycondensation, so that it is not additionally present in the melt line to a thermal damage of the polymer material comes.
  • the residence time of the melt in the melt line (s) is up to granulation and / or the device used for the production of the preforms. (eg injection molding machine) is as short as possible.
  • the residence time in the melt line should not exceed 3 minutes, in particular 1 minute, until granulation.
  • the melt in the melt line should have a residence time ⁇ 5 min, preferably ⁇ 3 min.
  • the granulation can take place in a customary manner by pelletizers with a subsequent standard crystallization, wherein the granules are moved, for example with a stirrer or in a fluidized bed and with a drying gas at 150 - 200 0 C dried. Air is preferably used as the drying gas and the drying is carried out at 165-175 0 C.
  • the granulation can also be carried out by hot stripping with a subsequent direct crystallization by utilizing the intrinsic heat of the granules (latent heat crystallization) and with a drying as indicated above.
  • the AA content in the granules is reduced from ⁇ 10 ppm to at least ⁇ 2 ppm. Taking advantage of all measures described can be obtained according to the inventive method granules with an AA content of 1 ppm.
  • the viscosity increase which can be achieved with the solid-phase postcondensation to values required for the further processing can, as already mentioned, be achieved by suitable treatment of the melt still in the polycondensation.
  • the granules produced according to the invention results in about the same AA level and about the same formation rate for AA as in granules, which was prepared by the standard method mentioned above, including a solid phase postcondensation.
  • FIG. 1 shows a schemati ⁇ cher representation of a plant for the production of polyester granules and / or polyester moldings with low acetaldehyde content according to the invention
  • Fig. 2 is a schematic representation of a prior art disk reactor
  • Fig. 3 is a particularly suitable for carrying out the inventive method, modified disk reactor.
  • Fig. 1 denotes a polycondensation reactor (eg DISCAGE® of the Applicant), in which a melt of a polyester material is produced.
  • 2 is a discharge unit referred to, which simultaneously forms the discharge region of the polycondensation reactor 1 and closes and in which it may be a discharge pump.
  • FIG 3 shows a schematic representation of a novel polycondensation reactor which is preferably used in the context of the invention.
  • FIG. 2 is a disk reactor in the form of a horizontally-lying cylindrical apparatus 30 with disks arranged on a longitudinal shaft 32 or a basket-like structure, of which only two are designated by 33.
  • the reactor shown in FIG. In contrast to the reactor of FIG. 2, an unfavorable bottom product which is formed for the evaporation is dispensed with as far as possible.
  • the melt is transported directly from disk to disk 33 by static wipers attached to the circumference of the reactor, two of which are denoted by 34.
  • the melt In the discharge area 35, the melt is conveyed directly into the discharge unit or pump 37 by static wipers 36, so that no accumulation of melt takes place here as well. Also is dispensed to a collection process.
  • the pump 37 is flanged to a rectangular flange 38 directly to the reactor.
  • the continuous melt stream is connected to a gas space under reduced pressure everywhere, right up to the discharge area in a thin layer. It is just worked on the physical tear-off.
  • the discharge unit 2 conveys the polyester melt from the polycondensation reactor 1 under pressure into a melt line 3, which subsequently divides into the strands 3.1 and 3.2.
  • the strand 3.1 is divided again into strands 3.1.1 and 3.1.2.
  • the strand 3.1.1 leads to a standard granulation 4, for example using a conventional strand pelletizer.
  • the granules formed by this is fed to a standard crystallization 5, in which the granules are moved, for example by an agitator or on a fluidized bed.
  • a drying stage 6 in which the granules, for example, in a shaft dryer in the flow of a hot Drying gas is dried.
  • 7 denotes a container or a filling station for the finished granules.
  • the strand 3.1.2 leads to a granulation 8 by hot deduction and with a direct crystallization by utilizing the intrinsic heat of the granules.
  • the granules produced in this way are then fed to the aforementioned drying stage 6 and, via them, likewise pass into the container or the filling station 7.
  • the granulation can be driven directly into the drying stage 6 by hot-cutting. From there, the granules are then returned to the filling station 7.
  • the strand 3.2 leads to a tool 9 with which a molded part can be produced directly from the melt.
  • the tool 9 may in particular be an injection molding machine and the molding may be a bottle preform.
  • an injection site 10 is shown in dashed lines in conjunction with a static mixer, via which, if necessary, an AA blocker can be injected into the melt.
  • a corresponding injection site is provided and denoted by 1 1.
  • a filter 12 could also be provided in the melt line 3.
  • columns B - F are intrinsic values
  • Polycondensation are typical instead of drying according to the invention.
  • the polyester material is polyethylene terephthalate in all examples.
  • a polycondensation reactor according to FIG. 3 was used within a continuous process.
  • the IV values and the AA values were determined according to ASTM.
  • the degree of crystallinity was determined by the density method using the following conventional formula:
  • (a) granulation comprises:
  • Polycondensation reactor according to FIG. 2 continuous melt polycondensation: temperature 290 ° C.
  • (a) Granulation comprises: polycondensation reactor (continuous melt polycondensation): temperature 276 ° C.
  • (a) granulation comprises:
  • Polycondensation reactor continuous melt polycondensation: temperature 276 ° C. Vacuum 0.95 mbar
  • (a) Cleaning includes:
  • AA values can be lowered as much as required, for example, for the production of water bottles. Even after the remelting and further processing of granules produced according to the invention, the AA values remain at a level comparable to the prior art.

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 procédé permettant de produire un granulat ou des pièces moulées en polyester, à partir d'une matière fondue, provenant d'un système de polycondensation (1). Selon l'invention, pour obtenir une faible teneur en acétaldéhyde, la matière fondue est maintenue en liaison avec un espace de gaz, avec une pression réduite, dans la zone de décharge (2) du système de polycondensation, à une température comprise entre 270 et 285°C. Pour ce qui est du granulat, dans le cadre du procédé selon l'invention, une cristallisation standard (5) et un séchage (6) à l'air, comme gaz de séchage, suffisent. Les pièces moulées peuvent être produites directement à partir de la matière fondue, par ex. avec une machine à mouler par injection (9). Le dispositif selon l'invention comprend un système de polycondensation dont au moins le dernier niveau se présente sous forme de réacteur à disques dans lequel la matière fondue est transportée de disque en disque, la formation de sédiments étant évitée dans la plus large mesure possible, par une combinaison de disques rotatifs et de racles statiques montées sur la périphérie du réacteur. Dans la zone de décharge, la matière fondue est refoulée directement dans l'unité de décharge, par des racles statiques, sans qu'une accumulation de la matière fondue ne se forme.
EP05809991A 2004-12-07 2005-12-06 Procede et dispositif pour produire un granulat et/ ou des pieces moulees en polyester a faible teneur en acetaldehyde Withdrawn EP1833874A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH20262004 2004-12-07
PCT/CH2005/000723 WO2006060930A1 (fr) 2004-12-07 2005-12-06 Procede et dispositif pour produire un granulat et/ ou des pieces moulees en polyester a faible teneur en acetaldehyde

Publications (1)

Publication Number Publication Date
EP1833874A1 true EP1833874A1 (fr) 2007-09-19

Family

ID=34974986

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05809991A Withdrawn EP1833874A1 (fr) 2004-12-07 2005-12-06 Procede et dispositif pour produire un granulat et/ ou des pieces moulees en polyester a faible teneur en acetaldehyde

Country Status (6)

Country Link
US (1) US8470220B2 (fr)
EP (1) EP1833874A1 (fr)
KR (1) KR101250302B1 (fr)
CN (1) CN101072810B (fr)
RU (1) RU2412955C2 (fr)
WO (1) WO2006060930A1 (fr)

Families Citing this family (5)

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Publication number Priority date Publication date Assignee Title
US10745517B2 (en) 2012-09-26 2020-08-18 Polymetrix Ag Process and apparatus for direct crystallization of polycondensates
ES2539610T3 (es) 2012-09-26 2015-07-02 Polymetrix Ag Procedimiento y dispositivo para la cristalización directa de polímeros bajo gas inerte
WO2015199798A2 (fr) 2014-04-22 2015-12-30 Plastipak Packaging, Inc. Pastille et précurseur contenant de la matière recyclée
AT521534A2 (de) 2018-07-03 2020-02-15 Next Generation Recyclingmaschinen Gmbh Verfahren zur Herstellung einer Polykondensatschmelze aus einem Primärmaterial und einem Sekundärmaterial
DE102018216250B4 (de) * 2018-09-24 2023-12-14 Thyssenkrupp Ag Reaktor zur Entgasung einer Polymerschmelze und Polykondensation

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DE2559290B2 (de) * 1975-12-31 1979-08-02 Davy International Ag, 6000 Frankfurt Verfahren zur kontinuierlichen Herstellung von hochmolekularem PoIyäthylenterephthalat
IT1251953B (it) * 1991-10-18 1995-05-27 M & G Ricerche Spa Procedimento per la produzione di resine poliestere ad elevato peso molecolare.
DE19503053B4 (de) * 1995-02-01 2005-08-18 Zimmer Ag Verfahren zur direkten Herstellung von Polyester-Verpackungen
DE19505680C1 (de) * 1995-02-20 1996-05-23 Inventa Ag Kondensations-Spritzgußverfahren zur Herstellung von Flaschenvorformlingen aus Polyethylenterephthalat und/oder seinen Copolyestern sowie nach diesem Verfahren herstellbare Vorformlinge
US5648032A (en) * 1995-08-01 1997-07-15 Eastman Chemical Company Process for producing polyester articles having low acetaldehyde content
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US5980797A (en) 1997-03-20 1999-11-09 Eastman Chemical Company Apparatus and method for molding polyester articles having low acetaldehyde content directly from the melt formation using flash tank devoltatilization
US6284866B1 (en) * 1999-12-07 2001-09-04 Wellman, Inc. Method of preparing modified polyester bottle resins
US6274212B1 (en) * 2000-02-22 2001-08-14 The Coca-Cola Company Method to decrease the acetaldehyde content of melt-processed polyesters
DE10045719B4 (de) * 2000-09-15 2018-01-11 Inventa-Fischer Gmbh & Co. Kg Verfahren zur Herstellung von Polyestern mit reduziertem Gehalt an Acetaldehyd
CA2515692A1 (fr) * 2003-10-17 2005-05-19 Bkg Bruckmann & Kreyenborg Granuliertechnik Gmbh Procede de traitement thermique de granules de polyester
US7358324B2 (en) * 2005-12-06 2008-04-15 Dak Americas Llc Manufacturing method of co-polyester resins for clear mono-layer containers with improved gas barrier characteristics

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Also Published As

Publication number Publication date
CN101072810B (zh) 2012-05-16
CN101072810A (zh) 2007-11-14
KR101250302B1 (ko) 2013-04-03
US20090302489A1 (en) 2009-12-10
WO2006060930A1 (fr) 2006-06-15
RU2007120623A (ru) 2009-01-20
KR20080028835A (ko) 2008-04-01
RU2412955C2 (ru) 2011-02-27
US8470220B2 (en) 2013-06-25

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