EP0591488A1 - Procede de fabrication d'un polyester ainsi que son utilisation - Google Patents

Procede de fabrication d'un polyester ainsi que son utilisation

Info

Publication number
EP0591488A1
EP0591488A1 EP93907749A EP93907749A EP0591488A1 EP 0591488 A1 EP0591488 A1 EP 0591488A1 EP 93907749 A EP93907749 A EP 93907749A EP 93907749 A EP93907749 A EP 93907749A EP 0591488 A1 EP0591488 A1 EP 0591488A1
Authority
EP
European Patent Office
Prior art keywords
polyester
polycondensation
ppm
antimony
produced
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Withdrawn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
EP93907749A
Other languages
German (de)
English (en)
Inventor
Stephan Müller
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.)
Viscosuisse SA
Original Assignee
Rhone Poulenc Viscosuisse SA
Societe de la Viscose Suisse SA
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 Rhone Poulenc Viscosuisse SA, Societe de la Viscose Suisse SA filed Critical Rhone Poulenc Viscosuisse SA
Publication of EP0591488A1 publication Critical patent/EP0591488A1/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Withdrawn legal-status Critical Current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
    • C08G63/82—Preparation processes characterised by the catalyst used
    • C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
    • 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
    • C08G63/82—Preparation processes characterised by the catalyst used
    • C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C08G63/86—Germanium, antimony, or compounds thereof
    • C08G63/863—Germanium or compounds thereof

Definitions

  • the invention relates to a process for producing a polyester or a copolyester from polyethylene terephthalate units by polycondensation by means of a mixed catalyst comprising several components, at least one component being a lithium salt or a germanium salt, the polyester 20 and the use thereof.
  • polyester The production of a polyester is known.
  • an acid component such as terephthalic acid or its methyl ester and a
  • glycol component such as ethylene glycol directly esterified in a first process stage or subjected to a transesterification reaction and subjected to the actual polycondensation in a second process step. This requires catalysts from
  • EP-A-0425215 describes a process in which an Mn / Li / Co / Sb catalyst is used in the polycondensation. Lithium in combination with antimony is said to accelerate the polycondensation massively.
  • FR-A-2 570 077 mentions the use of lithium germanate as a catalyst for polycondensation. No embodiment is mentioned from what concentrations and how it works.
  • the sodium germanate of the examples has been solubilized via the alkali metal oxide or carbonate by known reaction with germanium dioxide, the Na.Ge ratio being approximately 0.5: 1.
  • the sodium germanate is used to accelerate the polycondensation in a reaction mixture which is incompletely inhibited with phosphate compounds.
  • the object of the invention is the economical production of an antimony-free polyester without reducing the known quality of the polyester.
  • a molar ratio of Li: Ge of about 12: 1 to 1: 1 has proven to be a polycondensation catalyst. proven to be particularly suitable.
  • the polyester produced should contain less than 50 ppm Li, preferably 20-45 ppm Li and 20-50 ppm Ge.
  • the invention will be explained using examples.
  • glycol phase in which excess glycol is distilled off, 5.0 g of titanium dioxide (0.05%, Hombitan-LWS, trademark of Sachtleben, FRG) and 7.5 g of Irganox 1010 (0.075%, trademark) are used at 240 ° C from CIBA-GEIGY AG, Switzerland) dosed as a suspension in ethylene glycol.
  • the glycol phase is terminated at 245 ° C.
  • the granulated polymer is dried and crystallized in a double cone dryer using the following method:
  • the 8-10 kg polymer are first heated to 90 ° C (1 h) and then 115 ° C (1 h) heated up. The heating continues: final temperature
  • the dried and crystallized polymers are spun into dtex 55f24 threads using the following process:
  • the threads are then drawn in a laboratory stretching system in one step to a residual elongation of 28 ⁇ 2%.
  • the thread is passed over a heating surface with a temperature of 200 ° C.
  • the temperature of the godet 1 is 85 ° C.
  • the deduction godet is cold. It is stretched at a take-off speed of 100 m / min. The stretch ratio is approximately 3.3.
  • lithium acetate is very well suited as a cocatalyst together with germanium for the polycondensation.
  • the polycondensation time could be reduced so much that at the same time a reduction in the required amount of germanium was made possible.
  • the germanium content could be reduced by more than half.
  • the process is particularly suitable for the production of glossy polyester products.
  • Example 7 Both the combination “a lot of lithium and a little germanium” (examples 1 and 2) and the combination “with almost the same amount of lithium and germanium” (example 7) show favorable polycondensation times.
  • a disadvantage of Examples 1 and 2 is the excessive coloring in the yellow area on the thread (large Db value).
  • Example 7 is both lighter (positive DL value) and more neutral in color (smaller Da and Db value).

Landscapes

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

Abstract

Dans un procédé de fabrication sans antimoine d'un polyester composé d'unités de téréphtalate de polyéthylène, après la transestérification, on utilise en vue de la polycondensation un catalyseur mixte composé de 10 à 75 ppm de lithium et de 15 à 80 ppm de germanium. Le polyester exempt d'antimoine obtenu est utilisé dans la fabrication de bouteilles, de feuilles, de films, de fibres, de filaments et d'articles moulés.
EP93907749A 1992-04-27 1993-04-21 Procede de fabrication d'un polyester ainsi que son utilisation Withdrawn EP0591488A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CH1348/92 1992-04-27
CH134892 1992-04-27
PCT/CH1993/000105 WO1993022367A1 (fr) 1992-04-27 1993-04-21 Procede de fabrication d'un polyester ainsi que son utilisation

Publications (1)

Publication Number Publication Date
EP0591488A1 true EP0591488A1 (fr) 1994-04-13

Family

ID=4208378

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93907749A Withdrawn EP0591488A1 (fr) 1992-04-27 1993-04-21 Procede de fabrication d'un polyester ainsi que son utilisation

Country Status (11)

Country Link
EP (1) EP0591488A1 (fr)
JP (1) JPH06509386A (fr)
AR (1) AR246751A1 (fr)
AU (1) AU3886593A (fr)
CA (1) CA2111969A1 (fr)
CZ (1) CZ17494A3 (fr)
HU (1) HU212446B (fr)
PL (1) PL306375A1 (fr)
SK (1) SK9094A3 (fr)
TW (1) TW227006B (fr)
WO (1) WO1993022367A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100210220B1 (ko) * 1991-01-16 1999-07-15 페터 라인탈러, 페터 헤르만 폴리에스테르의 제조 방법, 폴리에스테르 및 그의 용도
WO1994013732A1 (fr) * 1992-12-04 1994-06-23 Toray Industries, Inc. Film de polyester a stratification thermique
BG100572A (en) * 1995-06-01 1996-12-31 Enichem S.P.A. Low speed crystallization polyesters and catalytic system for their preparation
US6953768B2 (en) 2002-11-26 2005-10-11 Teck Cominco Metals Ltd. Multi-component catalyst system for the polycondensation manufacture of polyesters

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3651017A (en) * 1967-12-29 1972-03-21 Kurashiki Rayon Co Process for the preparation of polyesters
US3635900A (en) * 1969-10-28 1972-01-18 Fmc Corp Polyester condensation process using alkali metal germanates

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9322367A1 *

Also Published As

Publication number Publication date
TW227006B (fr) 1994-07-21
HUT69043A (en) 1995-08-28
HU212446B (en) 1996-06-28
CZ17494A3 (en) 1994-06-15
AU3886593A (en) 1993-11-29
AR246751A1 (es) 1994-09-30
CA2111969A1 (fr) 1993-11-11
PL306375A1 (en) 1995-03-20
JPH06509386A (ja) 1994-10-20
HU9400236D0 (en) 1994-05-30
WO1993022367A1 (fr) 1993-11-11
SK9094A3 (en) 1994-08-10

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Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

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17P Request for examination filed

Effective date: 19931228

AK Designated contracting states

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Designated state(s): AT BE CH DE ES FR GB IE IT LI LU NL PT SE

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: RHONE-POULENC VISCOSUISSE SA

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 19961101