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Preparation of high molecular weight polyester

A high-molecular-weight polyester technology, applied in the field of polymer material preparation, can solve the problems of difficult continuous production, easy agglomeration, affecting polymer properties, etc., achieve uniform product properties, prevent agglomeration, and improve heat transfer performance. average effect

Inactive Publication Date: 2009-03-04
TORAY FIBER RES INST(CHINA) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is: (1) there is autoacceleration; (2) dispersant must be used, and after the polymerization is completed, it is difficult to remove from the polymer product, which will affect the performance of the polymer product (such as appearance, aging performance, etc.); ( 3) The particles of the polymerized product will contain a small amount of monomer, which is not easy to be completely clear and affect the performance of the polymer; (4) It is difficult to produce by continuous method.
[0023] The disadvantage of solid phase polymerization is that solid phase particles, especially those with smaller particle sizes, tend to agglomerate during crystallization or polymerization, resulting in difficulty in stirring and flowing

Method used

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  • Preparation of high molecular weight polyester
  • Preparation of high molecular weight polyester
  • Preparation of high molecular weight polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1: N-butylpyridine hexafluorophosphate

[0058] Starting material: lactic acid prepolymer, molecular weight Mw=10k, melting enthalpy ΔHm=60J / g, melting point Tm=158°C, glass transition temperature Tg=45°C

[0059] Ionic liquid: 1-ethyl-3-methylimidazolium tetrafluoroborate

[0060] Inject 250ml of ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate into a 500ml four-neck flask equipped with mechanical stirring (anchor type stirring blade). One port of the four-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the four-necked flask was placed in an oil bath, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, 10 g of lactic acid prepolymer was slowly added into a four-necked flask. After turning on the vacuum and reducing the pressure to 200Pa, raise the temperature to 170°C, and stir at a stirring ...

Embodiment 2

[0062] Starting material: lactic acid prepolymer, molecular weight Mw=10k, melting enthalpy ΔHm=60J / g, melting point Tm=158°C; glass transition temperature Tg=45°C

[0063] Ionic liquid: 1-butyl-3-methylimidazolium tetrafluoroborate

[0064] Inject 250ml of ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate into a 500ml four-neck flask equipped with mechanical stirring (anchor type stirring blade). One port of the four-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the four-necked flask was placed in an oil bath, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, 10 g of lactic acid prepolymer was slowly added into a four-necked flask. After turning on the vacuum and reducing the pressure to 200Pa, raise the temperature to 170°C, and stir at a stirring speed of 1000rpm for 10-30 minutes after the prepolymer is m...

Embodiment 3

[0066] Starting material: lactic acid prepolymer, molecular weight Mw=20k, melting enthalpy ΔHm=58J / g, melting point Tm=160°C; glass transition temperature Tg=47°C

[0067] Ionic liquid: 1-butyl-3-methylimidazolium hexafluorophosphate

[0068] Inject 250ml of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate into a 500ml four-neck flask equipped with mechanical stirring (anchor type stirring blade). One port of the four-neck flask was connected to nitrogen gas, the other port was connected to a vacuum system, and the other port was inserted into a thermocouple thermometer. After the four-necked flask was placed in an oil bath, the vacuum was turned on, and nitrogen was replaced three times. Under a nitrogen atmosphere, 10 g of lactic acid prepolymer was slowly added into a four-necked flask. After turning on the vacuum and reducing the pressure to 200Pa, raise the temperature to 170°C, and stir at a stirring speed of 500rpm for 10-30 minutes after the prepolymer i...

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Abstract

The invention discloses a preparation method for a high molecular weight polyester, the preparation method comprises: a crystalline polyester prepolymer is heated and melted, ionic liquid is added for stirring, the temperature of a system is decreased to the prepolymer crystallization temperature Tc under stirring to crystallize and harden the prepolymer after the polyester prepolymer is dispersed into small droplets by the ionic liquid; the temperature of the system is regulated between the glass transition temperature Tg and the melting point Tm of the prepolymer, and the solid phase polymerization is carried out by stirring. The prepared polyester can effectively reduce the agglomeration phenomena of polyester particles in the solid phase polymerization, the temperature of the system is even, the low molecular weight polyester granulation and the follow-up suspension solid phase polymerization can be continuously carried out, and the ionic liquid used in the system can be recycled for repeated use, thereby being conductive to the environmental protection.

Description

technical field [0001] The invention relates to a preparation method of a polymer material, in particular to a method for preparing a high-molecular-weight polyester by suspending a polyester prepolymer in an inert medium for solid-phase polymerization. Background technique [0002] Polyester: [0003] Polyester refers to the general term for a class of resins that contain —[-O-COR]—links in the main chain of the molecule. According to whether the molecular main chain structure contains aromatic groups, polyesters can be divided into two categories: aromatic polyesters and aliphatic polyesters. Representative of aromatic polyesters are polyethylene terephthalate (PET) and polybutylene terephthalate (PBT). [0004] Polyethylene terephthalate (PET) is polymerized from purified terephthalic acid (PTA) and ethylene glycol (EG). At present, it is mainly used for bottle-grade polyester (widely used in various beverages especially Carbonated beverage packaging), polyester film (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/80C08G63/88
Inventor 樊玲曹晓秀左璞晶于波何勇
Owner TORAY FIBER RES INST(CHINA) CO LTD
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