EP1863862A1 - Procede et dispositif de production de vide en plusieurs etapes dans le cadre de la production de polyesters - Google Patents

Procede et dispositif de production de vide en plusieurs etapes dans le cadre de la production de polyesters

Info

Publication number
EP1863862A1
EP1863862A1 EP05819253A EP05819253A EP1863862A1 EP 1863862 A1 EP1863862 A1 EP 1863862A1 EP 05819253 A EP05819253 A EP 05819253A EP 05819253 A EP05819253 A EP 05819253A EP 1863862 A1 EP1863862 A1 EP 1863862A1
Authority
EP
European Patent Office
Prior art keywords
injection
diol
vapors
vapor
condenser
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Withdrawn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
EP05819253A
Other languages
German (de)
English (en)
Inventor
Micha TRÖGER
Christof Fischer
Michael Reisen
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.)
Lurgi Zimmer GmbH
Original Assignee
Lurgi Zimmer GmbH
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 Lurgi Zimmer GmbH filed Critical Lurgi Zimmer GmbH
Publication of EP1863862A1 publication Critical patent/EP1863862A1/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Withdrawn legal-status Critical Current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
    • 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
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
    • 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
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • 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
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/002—Nozzle-type elements
    • 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
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/46—Polyesters chemically modified by esterification
    • 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

Definitions

  • the present invention relates to a process for the multi-stage vacuum generation and condensation and recycling of the evacuated, glycols and reaction by-products containing vapors of the polycondensation in the polyester production and a corresponding device.
  • Polyesters are prepared by adding at least one dicarboxylic acid, for example terephthalic acid or naphthalenedicarboxylic acid, or their methyl esters with at least one alkylene glycol, for example ethylene glycol or 1,4-butanediol, to which may be added minor amounts of a cyclic or aromatic diol such as 1,4-cyclohexanedimethanol , is first esterified or transesterified, then precondensed under elimination of water and a little glycol at moderate vacuum and finally polycondensed with elimination of glycol and a little water at high vacuum.
  • dicarboxylic acid for example terephthalic acid or naphthalenedicarboxylic acid
  • alkylene glycol for example ethylene glycol or 1,4-butanediol
  • 1,4-cyclohexanedimethanol 1,4-cyclohexanedimethanol
  • EP 0 685 502 discloses a process for the generation of vacuum as well as condensation and recycling of the exhausted vapors of polyester polycondensation, in which the glycol required for operating the glycol vapor jet pumps and the mixing condensers is recirculated without filtration and / or purification by distillation even over a prolonged period of operation and the excess glycol, including the condensed reaction byproducts, can be recycled to the polyester production process, if possible without removal and without additional purification.
  • the object of the present invention is to improve a method and a corresponding device for vacuum generation and condensation and recirculation of the exhausted vapor of the polyester polycondensation so that a trouble-free direct suction of emerging from the reactors vapors is made possible.
  • the inventive method for multi-stage vacuum generation in the production of polyesters or copolyesters by esterification of dicarboxylic acids and diols or by transesterification of dicarboxylic acid esters and diols is characterized by the following steps: Vapors from a final reactor are sucked directly into a first jet nozzle and compacted there , The compressed vapors form a vapor / motive vapor mixture with supplied motive steam and are conducted in a first injection condenser in cocurrent with injected diol. The injected diol and the diol-wetted walls of the first injection condenser largely condenses the vapor / motive vapor mixture.
  • direct current means that the vapor / vapor mixture and the injected diol emerge in a stream at the end of the injection condenser.
  • a part of the injected diol from the spray nozzles can initially also move transversely to the flow direction of the vapor / vapor mixture when entering the injection capacitor, but after a short flight the diol droplets strike the opposite wall of the injection capacitor and run there as a diol - film or they move in cocurrent with the vapor /maschinedampf- mixture to the end of the injection condenser.
  • the condensates from the at least one injection condenser are combined in a common immersion tank and used as Sprühdioi for the first injection condenser and optionally further injection condensers.
  • the temperature of the spray diol for the first injection capacitor is preferably set by cooling a partial flow of the combined condensates from the injection condensers and the temperature of the spray diol for the subsequent injection condensers by partial recycling of this cooled partial flow.
  • a portion of the condensates from the injection condensers is vaporized in an evaporator and the steam, for example, after overheating at 5 to 25 0 C, the jet nozzles supplied as motive steam.
  • the liquid phase emerging from the evaporator can be recycled directly into the polyester production process.
  • An additional preferred embodiment provides that vapors of the precondensation stage are sucked directly through a further jet nozzle.
  • the injection condensers open at their lower end to form an upwardly closed annular space in each case in a funnel-shaped extended section of a down metered barometric drainpipe.
  • a vapor-drive steam mixture from a diffuser preferably vertically, from above into the first and possibly further injection condensers and oligomers and polymers directly via a heated drip edge drip into injected diol and solidify into small solid particles. Caking on the walls is prevented by the film of film flowing down the wall. The resulting particles fall at the lower end of the injection condenser in the liquid and are discharged with this.
  • the liquid coming from the injection condenser is preferably collected in a desiccant container, in which the solid components are separated by sieving and a downstream filter to the extent that trouble-free operation is ensured.
  • Particles of solids collecting at the bottom of the container may from time to time be collected and disposed of by means of a slurry tanker or sieve trolley.
  • the diol liberated from the solids is cooled via the cooler and returned to the first or another injection condenser.
  • the present process is particularly suitable for vacuum generation for the polycondensation of homo- or copolyester precondensates, provided that the diol component forming the polyester predominantly consists of ethylene glycol, 1,3-propanediol and / or 1,4-butanediol.
  • Preferred field of application is the preparation of polyalkylene terephthalates and their low-modified copolymers, that is to say up to about 20 mol% of comonomers.
  • the suction lines for this purpose emanating from separate, corresponding to the desired vacuum levels.
  • the Dioldampf is superheated, preferably by 5 to 25 0 C.
  • All injection capacitors are operated according to the invention so that the diol phase including the higher-boiling components, especially the oligomers, as completely as possible condensed while the lower-boiling reaction products, predominantly water next to Diolspalt arean such as acetaldehyde in ethylene glycol or tetrahydrofuran at 1, 4-butanediol, together with the non-condensable components, in particular the leakage air, as far as possible remain in the gas phase.
  • Diolspalt arean such as acetaldehyde in ethylene glycol or tetrahydrofuran at 1, 4-butanediol
  • the operating conditions required for this purpose are determined in a known manner from the individual partial vapor pressures, which in turn depend on the chemical nature of the components, the respective proportions, the temperature and the total pressure, and must be determined for each individual application using conventional methods.
  • This mode of operation causes a purification of the diol from the lower-boiling impurities, so that a circulation of the diol condensate as Sprühdiol for the mixing capacitors without further measures is possible.
  • a portion of the diol condensate is recirculated as motive steam of the jet nozzles, this part being freed at the same time for steam generation from the higher-boiling impurities which are discharged from the evaporator as the bottom phase.
  • the low pressure of the motive steam, the steam generator can be operated at also low pressure, that is below 1 bar absolute. Evaporation at a relatively low temperature is therefore possible with the result that the evaporator sump phase is exposed to only a small thermal load.
  • the sump phase can therefore be recycled in the majority of applications without further purification in the polyester manufacturing process.
  • the condensable components of the gas phase from the mixing condensers are condensed in the last stage and together with in the closed Diolniklauf this stage fed diol recycled in the polyester production process.
  • the non-condensable components are discharged from the process and supplied, for example, to an exhaust gas combustion.
  • the vapor / motive vapor mixture passes into a first injection condenser 4, in which the propellant vapor 3 and the condensable part of the vapor 1 are condensed by means of injected diol 5.
  • the height h between funnel space and immersion tank 6 is dimensioned such that when setting a pressure equilibrium in the sense of communicating tubes, the liquid level in the funnel space assumes the height required for carrying out the method.
  • collecting solid particles are collected from time to time by means of a Ausschlämm observationsers 9 or a Siebwagens 10 and disposed of.
  • the diol liberated from the solids is passed through a diol Pump 11 out to a cooler 12, where it is cooled and from there back to the first injection condenser 4 and a second and third injection condenser 13, 14, respectively.
  • the non-condensable part of the vapor is fed to a second jet nozzle 15, compressed there to a pressure between 20 and 40 millibar and passes together with vapors of Vorpolykondensation 16, which is compressed via a separate jet nozzle 17, vertically from above into the second injection capacitor 13.
  • Die oligomers and low-viscosity polymers entrained with the vapor of the prepolycondensation 16 drop over a heatable drip edge directly into the injected diol 18 and solidify into small particles. Baking on the walls of the second injection capacitor 13 is also prevented here by the film of film flowing down the walls. The resulting particles fall at the lower end of the second injection condenser 13 in the liquid and are discharged with this.
  • the liquid coming from the second injection condenser 13 is also collected in the immersion tank 6, and solids are separated as necessary.
  • the uncondensed portion of the vapors from the second injection condenser 13 is passed into a third jet nozzle 19 and further compressed there by means of motive steam 3 to a pressure of 40 to 120 millibars.
  • the vapor /maschinedampfger ⁇ isch exiting from the third jet nozzle 19 is partially condensed in the third injection condenser 14, and the remaining residual vapor is supplied to a suitable compression to atmospheric pressure, for example by means of a Diolringpumpe 22. Since in the third injection condenser 14 substantially previously purified vapors, At this point, a simpler conventional capacitor design is conceivable.

Landscapes

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

Abstract

L'invention concerne un procédé et un dispositif correspondant permettant de produire du vide en plusieurs étapes, lors de la production de polyesters ou de copolyesters, par estérification d'acides dicarboxyliques et de diols ou par transestérification d'esters d'acides dicarboxyliques et de diols en plusieurs étapes de réaction. Ledit procédé se caractérise par les tapes suivantes: 1) les vapeurs chaudes (1) sortant d'un réacteur terminal sont aspirées directement dans une première tuyère (2) où elles sont comprimées; 2) les vapeurs chaudes (1) comprimées forment, conjointement avec un gaz propulseur (3) acheminé, un mélange vapeurs chaudes-vapeur pour vide et sont acheminées dans un premier condenseur à jet (4) en flux commun avec un diol (5) injecté; 3) le mélange vapeurs chaudes-vapeur pour le vide est condensé dans une large mesure par le diol (5) injecté et sur les parois imprégnées de diol du premier condenseur à jet (3); 4) les polymères extraits du premier condensateur à jet (4) avec le diol (5) sortant sont séparés.
EP05819253A 2005-03-19 2005-12-09 Procede et dispositif de production de vide en plusieurs etapes dans le cadre de la production de polyesters Withdrawn EP1863862A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005012732A DE102005012732A1 (de) 2005-03-19 2005-03-19 Verfahren und Vorrichtung zur mehrstufigen Vakuumerzeugung bei der Polyesterherstellung
PCT/EP2005/013185 WO2006099895A1 (fr) 2005-03-19 2005-12-09 Procede et dispositif de production de vide en plusieurs etapes dans le cadre de la production de polyesters

Publications (1)

Publication Number Publication Date
EP1863862A1 true EP1863862A1 (fr) 2007-12-12

Family

ID=36084362

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05819253A Withdrawn EP1863862A1 (fr) 2005-03-19 2005-12-09 Procede et dispositif de production de vide en plusieurs etapes dans le cadre de la production de polyesters

Country Status (8)

Country Link
EP (1) EP1863862A1 (fr)
JP (1) JP2008533251A (fr)
KR (1) KR20070122494A (fr)
CN (1) CN1903908A (fr)
DE (1) DE102005012732A1 (fr)
EA (1) EA200702018A1 (fr)
TW (1) TW200634048A (fr)
WO (1) WO2006099895A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106633277A (zh) 2009-12-02 2017-05-10 巴斯夫欧洲公司 光敏分子和金属配合物作为氧清除剂成分的用途
DE102011007543A1 (de) * 2011-04-15 2012-10-18 Aquafil Engineering Gmbh Vorrichtung und Verfahren zur Kondensation von Dämpfen unter Vakuum
US10576393B2 (en) * 2015-12-18 2020-03-03 General Electric Company System and method for condensing moisture in a bioreactor gas stream

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4419397A1 (de) * 1994-06-03 1995-12-14 Zimmer Ag Verfahren zur mehrstufigen Vakuumerzeugung bei der Polyester-Herstellung
DE10111343A1 (de) * 2001-03-08 2002-09-12 Gea Jet Pumps Gmbh Verfahren zur Vakuumerzeugung bei der Polyester-Herstellung
DE10318747B4 (de) * 2003-04-25 2006-04-20 Zimmer Ag Verfahren zur Vakuumerzeugung bei der Herstellung von Polymeren

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2006099895A1 *

Also Published As

Publication number Publication date
CN1903908A (zh) 2007-01-31
DE102005012732A1 (de) 2006-09-21
EA200702018A1 (ru) 2008-04-28
TW200634048A (en) 2006-10-01
WO2006099895A1 (fr) 2006-09-28
JP2008533251A (ja) 2008-08-21
KR20070122494A (ko) 2007-12-31

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