Polyester polycondensation with catalyst and a catalyst enhancer

a polycondensation and catalyst technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of high polycondensation activity, color problems in the resulting polyester, and the need for an extremely long time period to achieve significant reduction of the need for suitable catalysts

Inactive Publication Date: 2002-03-14
ARKEMA INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polycondensation reactions that produce polyesters require an extremely long period of time that is significantly reduced by a suitable catalyst.
However, titanyl oxalate catalysts when used as polycondensation catalysts for polyesters have caused color problems in the resulting polyester.
However, only potassium titanyl oxalate and ammonium ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

examples 1-20

and A-G

[0055] Catalyst evaluation was performed with a {fraction (3 / 16)} stainless steel, 2 L reactor, fitted with a ball valve at the bottom of the reactor. The vessel was equipped with 3 inlet ports, one outlet port, one thermowell port and one pressure transducer port, and was vertically stirred by an electric motor with amperage monitoring. The laboratory experimental were all conducted on a 4.0 mole scale, using as polyester forming reactants, BHET and a normal bottle resin autoclave recipe. The experimental catalysts were added at the time of BHET charging.

[0056] Bis(2-hydroxyethyl)terephthalate (BHET) and catalyst were added to the reactor and the contents blanketed with nitrogen. The mixtures were heated under reduced pressure with constant stirring. The ethylene glycol (EG) produced during the polymerization was removed and trapped. The polymerization was at 280.degree. C. , under the vacuum of typically around 1 torr. The reaction was terminated when the stirrer torque rea...

example b

[0060] Example B catalyst-2 ppm titanium from potassium titanyl oxalate-reaction time=118 mins.

[0061] Example C catalyst-6 ppm titanium potassium titanyl oxalate-reaction time=71 mins.

[0062] Example D catalyst-25 ppm antimony from antimony (III) oxide-reaction time=122 mins.

[0063] Example 1 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm potassium oxalate-reaction time=111 mins.

[0064] Example 2 catalyst-90 ppm potassium oxalate+25 ppm antimony from antimony (III) oxide-reaction time=120 mins.

[0065] Example 3 catalyst-180 ppm potassium oxalate+50 ppm antimony from antimony (III) oxide-reaction time=130 mins.

[0066] Example 4 catalyst-90 ppm potassium oxalate+100 ppm antimony from antimony (III) oxide-reaction time=112 mins.

[0067] Example 5 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm potassium oxalate+25 ppm antimony from antimony (III) oxide-reaction time=105 mins.

[0068] Example E catalyst-240 ppm antimony from antimony (III) oxide-reaction time=90 mins...

example f

[0069] Example F catalyst-240 ppm antimony from antimony (III) oxide-reaction time=100 mins.

[0070] Example 6 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm potassium oxalate+25 ppm antimony from antimony (III) oxide-reaction time=73 mins.

[0071] Example 7 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm ammonium oxalate+25 ppm antimony from antimony (III) oxide-reaction time=78 mins.

[0072] Example 8 catalyst-2 ppm titanium from ammonium titanyl oxalate+90 ppm potassium oxalate+25 ppm antimony from antimony (III) oxide-reaction time =79 mins.

[0073] Example 9 catalyst-2 ppm titanium from ammonium titanyl oxalate+90 ppm ammonium oxalate+25 ppm antimony from antimony (III) oxide-reaction time=77 mins.

[0074] Example 10 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm potassium acetate+25 ppm antimony from antimony (III) oxide-reaction time=81 mins.

[0075] Example 11 catalyst-2 ppm titanium from potassium titanyl oxalate+90 ppm potassium benzoate+25 ...

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Abstract

The present invention is based upon the discovery that nontitanyl oxalates can enhance the catalytic functionality of titanyl oxalate catalysts. This invention provides a novel catalytic composition containing a titanyl oxalate catalyst and a metallic oxalate catalyst enhancer and optionally containing a metallic cocatalyst such as an antimony based catalyst. A synergistic relationship has been discovered between titanyl oxalate catalyst and the catalyst enhancer. A synergistic relationship has also been discovered between the titanyl oxalate catalyst, catalyst enhancer and a metallic cocatalyst such as antimony oxide or antimony triacetate. Also provided is an improved process of producing polyester by the polycondensation of polyester forming reactants in the presence of a catalytically effective amount of a polycondensation catalyst, wherein the improvement comprises utilizing, as the polycondensation catalyst, the novel catalyst composition containing a titanyl oxalate such as lithium titanyl oxalate and a catalyst enhancer such as a nontitanyl metallic oxalate like lithium oxalate and optionally containing a metallic catalyst such as antimony oxide or antimony triacetate. The improved process produces an improved polyester having lower acetaldehyde numbers and good color. The titanyl oxalate/catalyst enhancer composition can be used as a polycondensation catalyst in combination with other catalysts to achieve synergistic catalytic activity. Preferred is a combination of lithium or potassium titanyl oxalate, Li2 or K2TiO(C2O4)2, lithium or potassium oxalate, Li2 or K2(C2O4)2 with antimony oxide or antimony triacetate or antimony trisglycoxide.

Description

[0001] REFERENCE TO RELATED APPLICATION[0002] This application is a continuation-in-part of U.S. patent application Ser. No. 09 / 747,115, filed Dec. 22, 2000, which claims priority of U.S. Provisional Application No. 60 / 175,006, filed Jan. 7, 2000, which disclosures are incorporated herein by reference.[0003] This invention relates to synergistic combinations of titanium containing catalysts and catalyst enhancers of carboxylic acid or oxalic acid or their Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba and ammonium salts that are useful for manufacturing polyesters. The synergistic combination of the titanium containing catalysts with a catalyst enhancer such as an oxalic acid, an oxalic acid salt or a carboxylic acid or a carboxylic acid salt provides fast reactions with improved properties such as reduced acetaldehyde content and good color properties for the resulting polyester at substantially reduced catalyst levels.DESCRIPTION OF THE PRIOR ART[0004] Polycondensation reactions that produ...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J31/04C08G63/87B01J31/22B01J31/26C07F7/28C08G63/82C08G63/83C08G63/84C08G63/85
CPCB01J21/063B01J31/04B01J31/2239B01J31/26B01J2531/0205B01J2531/10B01J2531/20B01J2531/46B01J2531/52C08G63/82C08G63/83C08G63/84C08G63/85C08G63/87
Inventor DOWLING, CONOR M.CHEN, BINSESHADRI, SRI R.
Owner ARKEMA INC
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