Preparation method of polyester combination, polyester combination and application of polyester combination

A manufacturing method and composition technology, which is applied in the field of polyester composition manufacturing, can solve the problems of reducing the regeneration speed of cyclic trimers, high intrinsic viscosity of polyester compositions, and precipitation of oligomers, etc., and achieve regeneration inhibition effect Good, simple film making process, excellent color tone effect

Active Publication Date: 2017-05-03
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polyester obtained by this method is easy to precipitate chelating agent, boron salt, etc. during the high-temperature processing in the later stage, and the regeneration inhibition effect on the specific oligomer cyclic trimer is not obvious
The second method is to reduce the content of the cyclic trimer in the polyester through solid-state polymerization or heat treatment under an inert gas, but this method can only reduce the content of the initial cyclic trimer in the polyester , cannot solve the problem of its regeneration in the subsequent high-temperature processing environment
There are also methods such as Chinese patent CN102421820A disclosing a kind of polytrimethylene terephthalate pellets with reduced oligomers. The preparation method is to use organic solvents to extract from polyester to remove cyclic trimers. This method Subsequent recovery of a large amount of organic solvents is required, the cost is high, the operation is troublesome, and it is difficult to implement in industry
There is also a method to reduce the regeneration rate of the cyclic trimer by changing the catalyst formulation and increasing the amount of the stabilizer phosphorus compound, but due to the increase in the amount of the phosphorus compound, the low deceleration rate of the cyclic trimer in the solid phase polymerization Reduced, the initial cyclic trimer of the polyester composition after solid-state polymerization is relatively high, even if few cyclic trimers are regenerated during the film-making process, oligomers still precipitate in the film
Although the amount of initial cyclic trimer can be reduced by prolonging the time of solid-phase polymerization, due to the long-term solid-phase polymerization, the intrinsic viscosity of the polyester composition after solid-phase polymerization is too high, and it is not easy to form a film

Method used

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  • Preparation method of polyester combination, polyester combination and application of polyester combination

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] At a temperature of 250°C, 166 parts by weight of PTA and 71.3 parts by weight of EG were added to the esterification reactor, and the esterification reaction was carried out under normal pressure. When the esterification reaction was completed, the temperature in the esterification reactor was 250°C. Fractional distillation of water yields small molecule polymers.

[0052] In the obtained small molecule polymer, add catalyst AO equivalent to 70 ppm of polyester composition weight in terms of antimony element, magnesium acetate equivalent to 10 ppm of polyester composition weight in terms of alkaline earth metal magnesium element, equivalent to polyester composition in terms of phosphorus element The stabilizer PA with a composition weight of 39ppm starts to decompress and heat up after 5 minutes, and the pressure is decompressed to about 300Pa after 1 hour, and the temperature rises to 290°C after 1.5 hours; when the polycondensation reaction ends, the pressure in the r...

Embodiment 2

[0055] At a temperature of 250°C, 166 parts by weight of PTA and 71.3 parts by weight of EG were added to the esterification reactor, and the esterification reaction was carried out under normal pressure. When the esterification reaction was completed, the temperature in the esterification reactor was 250°C. Fractional distillation of water yields small molecule polymers.

[0056] In the obtained small molecular polymer, add the catalyst AO equivalent to 70ppm of the weight of the polyester composition in terms of antimony, magnesium acetate equivalent to 15ppm of the weight of the polyester composition in terms of alkaline earth metal magnesium, and equivalent to polyester in terms of phosphorus. The stabilizer PEP36 with a composition weight of 70ppm, after 5 minutes, start to decompress and heat up, the pressure is decompressed to about 300Pa after 1 hour, and the temperature rises to 290°C after 1.5 hours; when the polycondensation reaction is over, the pressure in the reac...

Embodiment 3

[0059] At a temperature of 250°C, 166 parts by weight of PTA and 71.3 parts by weight of EG were added to the esterification reactor, and the esterification reaction was carried out under normal pressure. When the esterification reaction was completed, the temperature in the esterification reactor was 250°C. Fractional distillation of water yields small molecule polymers.

[0060] In the obtained small molecular polymer, add the catalyst AO equivalent to 100ppm of the weight of the polyester composition in terms of antimony, the magnesium acetate equivalent to 15ppm of the weight of the polyester composition in terms of alkaline earth metal magnesium, and the equivalent of polyester in terms of phosphorus. Composition weight 28ppm stabilizer PA, after 5 minutes, start to decompress and heat up, the pressure is decompressed to about 300Pa after 1 hour, and the temperature rises to 290°C after 1.5 hours; when the polycondensation reaction ends, the pressure in the reactor is abou...

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PUM

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Abstract

The invention discloses a preparation method of a polyester combination with low cyclic trimer content, and the polyester combination prepared through the preparation method. According to the preparation method, aromatic dicarboxylic or esterified derivatives of the aromatic dicarboxylic and aliphatic diol are subjected to a reaction, so that small molecular polymers are obtained, then the small molecular polymers are subjected to the polymerization reaction under the action of a catalyst and stabilizer phosphorus compounds, and finally the polyester combination is obtained through solid phase polymerization, specifically, the temperature of solid phase polymerization is 180-240 DEG C, and the vacuum degree is 200-9000 Pa. As for the obtained polyester combination, the intrinsic viscosity is 0.5-0.8 dl/g, the content of cyclic trimer in the polyester combination is 0.2-0.8 wt%, and the growth speed of cyclic trimer in the polyester combination is below 0.015 wt% at the fusion temperature of 300 DEG C in the nitrogen atmosphere. The polyester combination can be applied to products like films.

Description

technical field [0001] The present invention relates to a method for producing a polyester composition, the polyester composition produced by the method and the use of the polyester composition. Background technique [0002] Polyester, especially polyethylene terephthalate (PET), polytrimethylene terephthalate (PPT), polybutylene terephthalate (PBT), because of its excellent mechanical properties, chemical Characteristic, dimensional stability and transparency, widely used in fiber, film, resin and other fields. [0003] Generally, by-product oligomers are unavoidably produced during the polymerization of polyester, and their amount generally accounts for about 2wt% of the total amount of polyester. Said oligomers mainly refer to polymerized monomers, dimers, cyclic trimers, etc., among which cyclic trimers account for the vast majority, accounting for about 1 wt% of the total polyester. During the process of film making or spinning, oligomers will pollute some components ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/86C08G63/87C08G63/80C08L67/02
Inventor 祁华左文艳旦浩一
Owner TORAY IND INC
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