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A kind of polyester composition and its preparation method and application

A composition and polyester technology, applied in the field of polyester composition and preparation thereof, can solve the problems of insignificant regeneration inhibition effect of oligomer cyclic trimer, troublesome operation, reduction of content and the like, and achieve good regeneration inhibition effect , The effect of low processing cost and industrial simplicity

Active Publication Date: 2019-05-21
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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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

Method used

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  • A kind of polyester composition and its preparation method and application

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preparation example Construction

[0034] The invention also discloses a preparation method of the polyester composition, which includes esterification reaction or transesterification reaction, polymerization reaction, solid phase polymerization reaction and mixing reaction. This preparation method comprises the steps:

[0035] (1) Reaction of aromatic dicarboxylic acid or its esterified derivatives with aliphatic dihydric alcohol to obtain small molecular polymer, and then polycondensation reaction of small molecular polymer to obtain polyester, adding phosphorus element in the polycondensation reaction stage A stabilizer phosphorus compound of 10 to 400 ppm relative to the weight of polyester chips, and an antimony compound of 32 to 420 ppm relative to the weight of polyester chips in terms of antimony elements; and then solid-phase polymerization of the obtained polyester to obtain polyester chips;

[0036] (2) Add the polyester chip and trivalent phosphorus compound in step (1) into a two-shaft mixer to mel...

specific Embodiment approach

[0060] The advantages of the present invention will be described in detail below from the enumerated examples and comparative examples. The present invention is not limited to the following examples.

[0061] Some compounds involved in the examples are as follows:

[0062] (1) Terephthalic acid (PTA): the grade is high purity, Yangzi Petrochemical;

[0063] (2) Ethylene glycol (EG): BASF company;

[0064] (3) Antimony trioxide (AO): Nippon Seiko Co., Ltd.;

[0065] (4) Antimony glycol (AG): Yangzhou Yangtai Chemical Co., Ltd.;

[0066] (5) Phosphoric acid (PA): Shanghai Haohua Chemical Co., Ltd.;

[0067] (6) Bis(2,4-di-tert-butylphenyl) pentaerythritol diphosphite (PEP36): Asahi Denka;

[0068] (7) Bis(2.4-di-tert-butylphenyl) pentaerythritol diphosphite (AT626): Jinhai Yabao;

[0069] (8) Triphenyl phosphate (TPP): Aladdin's reagent

[0070] (9) Phosphite triacetate [P(OEt) 3 ]: Aladdin Reagent

[0071] (10) Phosphite Trilaurate (JP-312L): Chengbei Reagent

Embodiment 1

[0073] Step (1) At a temperature of 250°C, 166 parts by weight of PTA and 71.3 parts by weight of EG are added to the esterification reactor, and the esterification reaction is carried out under normal pressure. When the esterification reaction is completed, the temperature in the esterification reactor At 250°C, water is distilled off to obtain small molecule polymers.

[0074] In the obtained small molecule polymer, add catalyst AO equivalent to 60 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 Composition weight 20ppm stabilizer PA, after 5 minutes, start to depressurize and heat up, the pressure decompresses 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 about 200P...

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Abstract

The invention discloses a polyester composition with relatively low cyclic trimer content, and a preparation method thereof. The polyester composition is obtained by mixing polyester chips and a trivalent phosphorus compound in a kneading machine. The polyester composition comprises 30-400ppm of stibium element and 500-5000ppm of phosphorus element relative to the total amount of the polyester composition. The cyclic trimer content in the polyester composition is 0.2-0.8wt%. When the polyester composition is molten under a temperature of 300 DEG C under nitrogen, a cyclic trimer generation speed is 0.001-0.010wt% / min. The polyester composition can be applied in polyester products such as thin films.

Description

technical field [0001] The invention relates to a polyester composition and its preparation method and application, more specifically, to a polyester composition with low cyclic trimer content and good heat resistance. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L67/02C08K5/526C08K5/524C08G63/183C08G63/86
Inventor 祁华左文艳李旭望月克彦
Owner TORAY FIBER RES INST(CHINA) CO LTD
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