A kind of preparation method of 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: 2021-05-18
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 kind of preparation method of polyester composition

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preparation example Construction

[0016]The preparation method of the present invention is prior to the esterification reaction of the aromatic dicarboxylic acid with the aliphatic diol, and then further polymerization, specifically, in the period of time before the esterification reaction begins to the polymerization Add a bismuth compound, a phosphorus-containing mine-containing or phosphorus organic compound, and a phosphate metal salt to the reaction system, and the polymerization is started, and the polymerization reaction has reached 0.5 dl / g to the polymerization reaction before the first time. The manganese compound is added to the reaction system in the polymerization reactant and the polymerization is continuously reacted until it is completed.

[0017]The manganese compound has an inhibiting oxidation, which can capture the oxygen free radicals to cause free radicals, such that hydrogen on the polyester phenyl ring is avoided to a certain extent, inhibiting the occurrence of thermal oxygen degradation. The...

Embodiment 1

[0046]Activated reaction at 250 ° C of 166 parts by weight of terephthalic acid (TPA) and 72 parts by weight of ethylene glycol (Eg) (i.e., EG and TPA of the molar ratio of 1.1%), passed by by-product water Production, the reaction rate to be reacted is more than 97%, and the prepared new p-oligate (BHT) oligomer is transferred to the polymerizer. To the polymerization, a catalyst, a catalyst, a catalyst, a catalyst (AO) having a polyester composition, a polyester composition, and 5 minutes, 5 minutes, 5 minutes, 5 minutes, 5 minutes, 5 minutes, sodium dihydrogen phosphate (NaH)2PO4· 2h2O) and the phosphorus element is equivalent to a mixture of 20 ppm of the polyester composition by the polyester composition. The end of the addition is completed, and the reduced pressure is started, the temperature is warmed, and the reaction time is 3 hours, the inherent viscosity is 0.65 dl / g. The addition of manganese or manganese or manganese acetate is added to a acetate of 50 ppm of the pol...

Embodiment 2

[0048]Activated reaction at 250 ° C of 166 parts by weight of terephthalic acid (TPA) and 72 parts by weight of ethylene glycol (Eg) (i.e., EG and TPA of the molar ratio of 1.1%), passed by by-product water Production, the reaction rate to be reacted is more than 97%, and the prepared new p-oligate (BHT) oligomer is transferred to the polymerizer. The catalysts (AO) of the polyester element were sequentially added to the polyester composition in the polyester composition, and Eg was added to 5 minutes, and 70 ppm was added to 5 minutes. 5 minutes of phosphate sodium dihydrogen (NaH).2PO4· 2h2O) mixed with a phosphoric acid phosphoric acid having a total amount of 20 ppm of the polyester composition by phosphorus element, and 5 minutes at the end of the addition end, the temperature is increased, and the reaction time is 2 hours and 30 minutes, the intrinsic viscosity is 0.55 dl / When G, a manganese acid polyester composition is added to the polyester composition in a manganese elem...

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Abstract

The invention discloses a preparation method of a polyester composition. In the method, an aromatic dicarboxylic acid and an aliphatic dihydric alcohol are subjected to an esterification reaction, and 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; during the period from the time when the intrinsic viscosity of the polymerization reactant reaches 0.5dl / g to the end of the polymerization reaction , add manganese compound to the reaction system, and continue the polymerization reaction until it is completed. The polyester composition prepared by the method has a gel rate of less than 5wt% after heat treatment at 300°C×6hr under a mixed gas of nitrogen / oxygen with an oxygen concentration of 1 vol%, and less foreign matter, and can be used for making films, fibers, etc. .

Description

Technical field[0001]The present invention relates to a preparation method of a polyester composition having a low gel and a small foreign matter.Background technique[0002]Polyester, especially polyethylene terephthalate, polyethylene terephthalate, polyethylene terephthalate, etc., is widely used due to excellent mechanical, physical and chemical properties Production of fibers, films and other molded products. However, most of the polyester will thermal oxygen degradation and thermal decomposition under high temperature conditions, in the thermal oxygen degradation reaction, oxygen free radicals from hydrogen on the polyester phenyl ring, forming a peroxidation functional group, the peroxidation functional group is unstable It also decomposes the generated free radical, the generated free radical as the product generated frame bridge structure after the frame bridge and the polyester thermal decomposition, that is, crosslinking reaction, forming a non-melting rubber, generally ref...

Claims

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Application Information

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Patent Type & Authority Patents(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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