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Polymerization catalyst for polyester, polyester produced with the same, and process for producing polyester

A technology of polymerization reaction and catalyst, applied in the field of polymerization reaction catalyst, can solve the problems of high product cost, membrane surface defect, fiber strength decrease and so on

Inactive Publication Date: 2004-01-28
TOYOBO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Antimony trioxide is an inexpensive and highly active catalyst, but if antimony trioxide is used as the main component, that is, when it is used in an amount exhibiting a practical polymerization reaction rate, antimony metal precipitates during polycondensation, causing problems such as Gray discoloration or formation of insoluble particles in polyester
[0006] (1) In the polyester used for the film, the precipitated antimony metal acts as insoluble particles in the polyester, which not only causes pollution of the outlet during the melt extrusion process, but also causes defects on the surface of the film
In addition, if polyester with insoluble particles is used as a starting material for hollow molded articles, it is difficult to obtain hollow molded articles with excellent transparency
[0007] (2) The insoluble particles in the polyester used for the fiber not only cause the fiber strength to decrease, but also deposit around the spinning head during the spinning process
If this known catalyst is used, polyesters with excellent thermal stability can be obtained, but this known catalyst in combination with an alkali metal compound should be added in relatively large amounts to obtain practical catalytic activity, as a result, increased attributable Due to insoluble particles of alkali metal compounds, there arises such a problem that if PET is used for fibers, the spinnability and physical properties of fibers become worse, and if PET is used for films, the physical properties of films become worse, And the resistance to hydrolysis decreases
However, methods using these supercritical fluids are technically difficult and result in higher product costs, and are therefore not preferred

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0222] To a mixture of bis(2-hydroxyethyl) terephthalate and an oligomer made from high-purity terephthalic acid and ethylene glycol in a conventional manner, 0.015 mol- % (in terms of aluminum atoms) of 13 g / l aluminum chloride in ethylene glycol as polycondensation catalyst and relative acid component 0.02 mol-% (in terms of Irganox 1425) of 10 g / l Irganox 1425 in ethylene glycol (Ciba Specialty Chemicals Inc.), the mixture was then stirred at 245° C. for 10 minutes under a nitrogen atmosphere under normal pressure. Then, the temperature was raised to 275°C for 50 minutes while gradually reducing the pressure in the reaction system to 13.3 Pa (0.1 Torr), and then the polycondensation reaction was further carried out at 275°C at 13.3 Pa.

[0223] The polyethylene terephthalate (PET) obtained in the above polycondensation with an IV of 0.65 dl / g was formed into chips in a conventional manner. Table 1 shows the measurement results such as the time required for the polycondensa...

Embodiment 2 and 3

[0227] PET was produced in the same manner as in Example 1 except that the kind of catalyst used was changed. Otherwise, evaluation was performed in the same manner as in Example 1. Table 1 shows the composition and evaluation results of the catalysts used. Catalyst component lithium acetate · 2H 2 O was added as a 50 g / l solution in ethylene glycol in the amounts shown in Table 1 expressed in lithium atoms relative to the acid component in PET. Comparative example 1

Embodiment 4

[0233] A heat transfer medium circulation 2-L stainless steel autoclave equipped with a stirrer was charged with high-purity terephthalic acid and ethylene glycol in a molar ratio of 1:2, and 0.3 mol-% triethyl amine, and the mixture was subjected to an esterification reaction at a pressure of 0.25MPa at 250°C for 110 minutes, while distilling off water from the system, thus obtaining bis(2-hydroxyethyl)terephthalate (BHET) and esters with A mixture of oligomers (hereinafter referred to as BHET mixture) with a degree of conversion of 95% or more. To this BHET mixture was added 2.5 g / l aluminum acetylacetonate in ethylene glycol at 0.014 mol-% (in terms of aluminum atoms) relative to the acid component in the polyester as a polycondensation catalyst and 0.01 mol-% relative to the acid component mol-% (calculated as Irganox 1425) of 100 g / l Irganox 1425 (Ciba Specialty Chemicals Inc.) in ethylene glycol, and the mixture was stirred under normal pressure at 250° C. for 15 minutes...

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Abstract

A polymerization catalyst for polyester production which contains neither a germanium compound nor an antimony compound as a major component. It contains aluminum as the main metallic ingredient, has excellent catalytic activity, and gives a polyester which is effectively inhibited from suffering thermal degradation, during melt molding, without deactivating or removing the catalyst, and is excellent in thermal stability, stability to thermal oxidation, and hydrolytic resistance. The polymerization catalyst contains as a first metallic ingredient at least one member selected among aluminum and compounds thereof and further contains a phosphorus compound represented by a specific chemical formula. The polyester produced with this catalyst is usable as fibers, films, sheets, various moldings including hollow moldings, etc.

Description

technical field [0001] The present invention relates to a polymerization reaction catalyst for polyester, polyester produced by using the same and a method for producing polyester, in particular to a catalyst which does not use germanium or antimony compound as the main catalyst component Novel polyester polymerization catalyst, polyester produced by using the same and a method for producing polyester. The present invention provides fibers, films, sheets and hollow molded articles comprising polyesters produced from such novel polyester polymerization catalysts which do not use germanium or antimony compounds as main catalytic components. Background technique [0002] Polyesters such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), and polyethylene naphthalate (PEN) have excellent mechanical and chemical properties , and used in various fields such as fibers for clothing and industrial materials, films for packaging or for tapes, sheets, bottles such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/82C08G63/83C08G63/84C08G63/87D01F6/62
CPCD01F6/62C08G63/87C08G63/83C08G63/82C08G63/84
Inventor 中塢孝宏塚本健一形舞祥一吉田文和佐藤万纪渡边直树荫山胜彦桑田光启森山畅夫松本治男池畠良知松井义直松田全央奥原宗和福田裕树
Owner TOYOBO CO LTD
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