WO1994017122A1 - Procede de cristallisation et de polycondensation continues pour polyesters - Google Patents

Procede de cristallisation et de polycondensation continues pour polyesters Download PDF

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Publication number
WO1994017122A1
WO1994017122A1 PCT/CH1994/000006 CH9400006W WO9417122A1 WO 1994017122 A1 WO1994017122 A1 WO 1994017122A1 CH 9400006 W CH9400006 W CH 9400006W WO 9417122 A1 WO9417122 A1 WO 9417122A1
Authority
WO
WIPO (PCT)
Prior art keywords
polyester material
temperature
reactor
polyester
preheater
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.)
Ceased
Application number
PCT/CH1994/000006
Other languages
German (de)
English (en)
Inventor
Arthur Ruf
Edwin Boller
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.)
Buehler AG
Original Assignee
Buehler 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 Buehler AG filed Critical Buehler AG
Publication of WO1994017122A1 publication Critical patent/WO1994017122A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
    • B29B13/065—Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • B29B2009/165—Crystallizing granules

Definitions

  • the invention relates to a method for the continuous crystallization and polycondensation of polyester material according to the preamble of claim 1 and 2 respectively.
  • the pre-crystallized material Before entering the reactor, the pre-crystallized material has to be heated to about 200 ° C. to 225 ° C. in the core and dried. The residence time in the reactor is again several hours. Surface temperatures of up to approx. 230 ° C are reached, which is already above the melting point, cf. z. B. EP-B-85 643. This in turn leads to signs of stickiness and agglomeration of the material in the thermal solid phase treatment.
  • the invention is therefore based on the object, while avoiding the disadvantages of the prior art shown, of designing a process for the continuous crystallization and polycondensation of polyester material in such a way that exercises of the polyester material due to exothermic processes can be avoided.
  • this object is achieved in that, in a process procedure known per se, as described, for.
  • the material is subjected to intermediate cooling.
  • the material is heated in the preheater from an initial temperature of, for example, 120-190 ° C. to approximately 220 ° C. in a hot gas stream and completely warmed up in a dwell time of approximately three hours.
  • a degree of crystallinity of approx. 50% is achieved here.
  • the residence time in the reactor is 7-15 hours in a known manner. A degree of crystallinity of about 53% is achieved. This is followed by conventional cooling of the material to ensure that it can be stored.
  • the method according to the invention enables a higher application variance and an increased throughput of gas and polyester material. Material change and process change of an SSP system can be considerably simplified.
  • the material throughput is used as a control variable to avoid the beginning of the melting of the polyester granulate.
  • excess material is used, which results in a controlled temperature gradient. According to the invention, excess material is to be understood in the sense of a specific heat flow, derived from the required specific output
  • CPG mean specific thermal conductivity.
  • This variant of the invention is based on the surprising finding that an excess of gas tends to cause a deterioration in the temperature profile.
  • a process control with transient driving is also possible.
  • the material is preheated in a manner known per se in a few minutes in a gas stream of high temperature, but no total heating may occur. A degree of crystallinity of approx. 45% is achieved.
  • the polyester material is heated in a fluidizing gas stream, for example air.
  • the first fluidized bed is a bubbling fluidized bed with a mixed characteristic, in which the material has an average residence time of max. Is heated to about 160 ° C for 60 minutes.
  • This is followed by a fluid bed as the second fluidized bed Piston flow characteristics, with heating to approx. 170 ° C, with a minimum residence time of 2-25 minutes. This ensures trouble-free and complete crystallization even of sticky material, and agglomerate-free granules with a uniform degree of crystallization are obtained.
  • the polyester material is introduced into a preheater of an SSP reactor and in a period of about three hours to a temperature of about 215 ° C, max. 230 ° C heated with a hot inert gas stream (e.g. nitrogen). After passing through the preheating zone, the polyester material is intercooled from an average of 217 ° C. to approx. 210 ° C. in order to avoid overheating (exceeding the melting point) of the material in the subsequent reactor.
  • a hot inert gas stream e.g. nitrogen
  • the polyester material is again heated in the preheating zone of the reactor. In order to avoid the start of melting, however, an excess of material is used when a temperature of approximately 215 ° C. is reached.
  • the material throughput is set in such a way that 218 ° C. is not exceeded and the granulate does not stick together.
  • a temperature measurement is generally carried out in the process, and the data obtained can be compared with a simulation model.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

La présente invention concerne une procédé de cristallisation et de polycondensation continues de polyesters. Il s'agit d'éviter des dégâts par oxydation du polyester pendant le traitement SSP tout en augmentant la variété des applications de la polycondensation en phase solide. Selon cette invention, le problème est résolu par le fait que l'on expose, lors de la cristallisation et polycondensation connues en soi, le polyester à un refroidissement intermédiaire à 5 °C environ après son passage dans un dispositif de préchauffage et avant l'entrée dans le réacteur.
PCT/CH1994/000006 1993-01-21 1994-01-11 Procede de cristallisation et de polycondensation continues pour polyesters Ceased WO1994017122A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH17993A CH684697A5 (de) 1993-01-21 1993-01-21 Verfahren zum kontinuierlichen Kristallisieren und Polykondensieren von Polyestermaterial.
CH179/93-5 1993-01-21

Publications (1)

Publication Number Publication Date
WO1994017122A1 true WO1994017122A1 (fr) 1994-08-04

Family

ID=4181071

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CH1994/000006 Ceased WO1994017122A1 (fr) 1993-01-21 1994-01-11 Procede de cristallisation et de polycondensation continues pour polyesters

Country Status (2)

Country Link
CH (1) CH684697A5 (fr)
WO (1) WO1994017122A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2007022994A1 (fr) 2005-08-26 2007-03-01 Lurgi Zimmer Gmbh Procede et dispositif pour reduire la teneur en acetaldehyde d'un granulat de polyester
US7262263B2 (en) 2001-11-30 2007-08-28 Brigitta Otto Method and apparatus for producing solid-state polycondensed polyesters
US7977448B2 (en) 2004-03-04 2011-07-12 Lurgi Zimmer Gmbh Method for producing highly condensed solid-phase polyesters
US8063176B2 (en) 2006-03-16 2011-11-22 Lurgi Zimmer Gmbh Method and device for the crystallization of polyester material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2008523A1 (fr) * 1968-05-14 1970-01-23 Glanzstoff Ag
US4161578A (en) * 1978-05-12 1979-07-17 Bepex Corporation Process for solid phase polymerization of polyester
EP0085643A2 (fr) * 1982-02-02 1983-08-10 The Goodyear Tire & Rubber Company Procédé de préparation de polyesters à haut poids moléculaire
EP0091566A1 (fr) * 1982-04-02 1983-10-19 Karl Fischer Industrieanlagen Gmbh Procédé et dispositif pour la post-condensation de polycondensats
EP0379684A2 (fr) * 1988-12-23 1990-08-01 Bühler Ag Procédé et dispositif pour la cristallisation en continu de polyester

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2008523A1 (fr) * 1968-05-14 1970-01-23 Glanzstoff Ag
US4161578A (en) * 1978-05-12 1979-07-17 Bepex Corporation Process for solid phase polymerization of polyester
EP0085643A2 (fr) * 1982-02-02 1983-08-10 The Goodyear Tire & Rubber Company Procédé de préparation de polyesters à haut poids moléculaire
EP0091566A1 (fr) * 1982-04-02 1983-10-19 Karl Fischer Industrieanlagen Gmbh Procédé et dispositif pour la post-condensation de polycondensats
EP0379684A2 (fr) * 1988-12-23 1990-08-01 Bühler Ag Procédé et dispositif pour la cristallisation en continu de polyester

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US5656719A (en) * 1995-02-20 1997-08-12 Ems-Inventa Ag Condensation injection molding process for producing bottle preforms of polyethylene terephthalate and/or its copolyesters and resultant preforms
US7262263B2 (en) 2001-11-30 2007-08-28 Brigitta Otto Method and apparatus for producing solid-state polycondensed polyesters
US7977448B2 (en) 2004-03-04 2011-07-12 Lurgi Zimmer Gmbh Method for producing highly condensed solid-phase polyesters
WO2007022994A1 (fr) 2005-08-26 2007-03-01 Lurgi Zimmer Gmbh Procede et dispositif pour reduire la teneur en acetaldehyde d'un granulat de polyester
US7521522B2 (en) 2005-08-26 2009-04-21 Lurgi Zimmer Gmbh Method and device to reduce the acetaldehyde content of polyester granulate
US8063176B2 (en) 2006-03-16 2011-11-22 Lurgi Zimmer Gmbh Method and device for the crystallization of polyester material

Also Published As

Publication number Publication date
CH684697A5 (de) 1994-11-30

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