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A preparing method for polyester composition

A composition and polyester technology, applied in the field of polyester composition preparation, can solve the problems of limited use, decreased film quality, increased filter pressure, etc., and achieves simple preparation process, low gel rate, and easy operation. Effect

Active Publication Date: 2018-07-31
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Japanese Patent Laid-Open 2005-314643 and Japanese Patent Laid-Open 2006-225621 describe that gelation can be suppressed to some extent by adding titanium compounds in processes such as transesterification, but the heat resistance of polyester itself is reduced. Thermal cracking will occur during long-term film production, so gel formation cannot be sufficiently suppressed
At the same time, a stabilizer phosphorus compound is generally added during the polymerization process, and after the added phosphorus compound reacts with the metal co-catalyst, it is easy to form insoluble matter in the polyester and form particles, which will cause the filter pressure of the filter to rise during the molding process. It is easy to break during spinning, which will affect the spinning performance, or cause the filter pressure of the filter to increase during the membrane production process, and the filter will be replaced frequently, resulting in waste of raw materials and an increase in cost
In addition, the occurrence of gel defects on the film leads to a decrease in the quality of the film and limits its use

Method used

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  • A preparing method for polyester composition

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preparation example Construction

[0016] In the preparation method of the present invention, the aromatic dicarboxylic acid and the aliphatic dihydric alcohol are first subjected to an esterification reaction, and then the polymerization reaction is further carried out, specifically, during the period from the end of the esterification reaction to the start of the polymerization reaction Add antimony compound, phosphorus-containing inorganic acid or phosphorus-containing organic compound, and alkali metal phosphate to the reaction system to start the polymerization reaction. After the intrinsic viscosity of the polymerization reactant reaches 0.5dl / g and before the end of the polymerization reaction, Add manganese compound to the reaction system in the polymerization reactant, and continue the polymerization reaction until completion.

[0017] The manganese compound has the effect of inhibiting oxidation, can capture oxygen free radicals, and promote the inactivation of free radicals, which to a certain extent ...

Embodiment 1

[0046] At 250°C, 166 parts by weight of terephthalic acid (TPA) and 72 parts by weight of ethylene glycol (EG) (that is, the molar ratio of EG to TPA is 1.15:1) were subjected to esterification reaction, through the by-product water Production capacity, when the esterification reaction rate reaches over 97%, transfer the obtained new diethylene terephthalate (BHT) oligomers to the polymerization tank. Add antimony trioxide (AO) catalyst which is equivalent to 80ppm of the total amount of the polyester composition in terms of antimony to the polymerization kettle in sequence, add EG solution after 5 minutes, add 70ppm sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O) and the mixed solution of stabilizer phosphoric acid equivalent to 20ppm of the total amount of the polyester composition in terms of phosphorus element, the pressure is reduced and the temperature is raised 5 minutes after the addition is completed. When the reaction time is 3 hours and the intrinsic viscosity is 0...

Embodiment 2

[0048] At 250°C, 166 parts by weight of terephthalic acid (TPA) and 72 parts by weight of ethylene glycol (EG) (that is, the molar ratio of EG to TPA is 1.15:1) were subjected to esterification reaction, through the by-product water Production capacity, when the esterification reaction rate reaches over 97%, transfer the obtained new diethylene terephthalate (BHT) oligomers to the polymerization tank. Add antimony trioxide (AO) catalyst which is equivalent to 80ppm of the total amount of the polyester composition in terms of antimony to the polymerization kettle in sequence, add EG after 5 minutes, and add 70ppm of sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O) and the mixed solution of stabilizer phosphoric acid equivalent to 20ppm of the total amount of the polyester composition in terms of phosphorus element, start to reduce pressure and heat up 5 minutes after the addition, when the reaction time is 2 hours and 30 minutes, the intrinsic viscosity is 0.55dl / At the time ...

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Abstract

The invention discloses a preparing method for a polyester composition. An esterification reaction between aromatic dicarboxylic acid and aliphatic dihydric alcohol is firstly performed in the method;an antimony compound, an inorganic acid containing phosphorus, or an organic compound containing phosphorus and phosphoric acid alkali metal salt are added to the reaction system from the end of esterification reaction to the beginning of a polymerization reaction to begin the polymerization reaction; in the time period from the inherent viscosity of the polymerized reactant reaching 0.5dl / g to the end of the polymerization reaction, a manganese compound is added to the reaction system to the continue the polymerization reaction until the end of the polymerization reaction. The gel fraction of the polyester composition prepared through the method is under 5wt% in a N2 / O2 gas mixture (oxygen concentration is 1 vol%) after thermal treatment of 300DEG C * 6hr and the polyester composition can be used for preparing thin films and fibers with little foreign material.

Description

technical field [0001] The invention relates to a preparation method of a polyester composition with low gel rate and few foreign substances. Background technique [0002] Polyesters, especially polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, etc., are widely used due to their excellent mechanical, physical and chemical properties Production of fibers, films and other molded products. However, most polyesters will undergo thermal oxygen degradation and thermal decomposition under high temperature conditions. In the thermal oxygen degradation reaction, oxygen radicals attack the hydrogen on the benzene ring of polyester to generate peroxide functional groups, which are unstable. It will also decompose to generate free radicals, and the generated free radicals serve as bridging points and the products of polyester thermal decomposition to form bridging structures, that is, cross-linking reactions occur to form infusible gels, which are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/86C08K3/32C08K5/098C08K3/30C08K3/16
CPCC08G63/183C08G63/866C08K3/16C08K3/30C08K3/32C08K5/098C08K2003/3045C08K2003/329
Inventor 祁华梅涛锋旦浩一
Owner TORAY FIBER RES INST(CHINA) CO LTD
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