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High molecular weight aliphatic-aromatic copolyester and its preparation method and application

A high molecular weight, aromatic technology, applied in the field of polymer materials and their preparation, can solve the problems of poor mechanical properties and low molecular weight of polyester, and achieve the effect of controllable structural properties, high molecular weight and good flexibility

Active Publication Date: 2019-04-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the disadvantages of low molecular weight and poor mechanical properties of polyesters based on 1,5-pentanediol in the prior art, the purpose of the present invention is to provide a high molecular weight aliphatic-aromatic copolyester and a preparation method thereof, The obtained aliphatic-aromatic copolyester has high molecular weight, good flexibility, high strength and other excellent mechanical properties, and the structural properties are controllable, which can meet the thermo-mechanical performance requirements of different applications

Method used

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  • High molecular weight aliphatic-aromatic copolyester and its preparation method and application
  • High molecular weight aliphatic-aromatic copolyester and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Add 1,4-butanedioic acid (0.276mol, 32.56g), isophthalic acid (0.226mol, 37.57g), 1,5-pentanediol (0.75mol, 78.11g) into a 250mL four-neck flask ) and n-butyl titanate (0.5mmol, 171mg), with an alcohol-acid ratio of 1.5, reacted at 200°C for 3 hours to obtain an esterified product with an esterification rate of 95.6%;

[0053] (2) Add n-butyl titanate (0.25mmol, 85mg) to the esterification product obtained in step (1), and react at 200°C for 1 hour under the condition of about 130Pa, and react at 240°C for 2.5 hours, and react at 250°C React for 1 hour, remove excess 1,5-pentanediol and a small amount of oligomers, and prepare the high molecular weight aliphatic-aromatic copolyester based on 1,5-pentanediol, its H NMR spectrum Figure such as figure 1 shown.

[0054] After testing, the intrinsic viscosity of the aliphatic-aromatic copolyester prepared in this embodiment is 1.26dL / g, the glass transition temperature is -20.2°C, and the melting point is 40.5°C.

Embodiment 2

[0056] (1) Add 1,4-hexanedioic acid (0.206mol, 30.14g), 2,5-furandicarboxylic acid (0.169mol, 26.34g), 1,5-pentanediol (0.75mol , 78.11g) and titanium dioxide-silicon dioxide-polyvinylpyrrolidone composite catalyst (1mmol, 76mg), the alcohol-acid ratio is 2, reacted at 200 ° C for 3.5 hours to obtain an esterified product, and the esterification rate reached 96.4%;

[0057] (2) In the esterification product obtained in step (1), no further catalyst is added, under the condition of about 160Pa, react at 200°C for 1 hour, react at 240°C for 3 hours, and react at 250°C for 1 hour to remove excess 1,5-pentanediol and a small amount of oligomers to prepare the high molecular weight aliphatic-aromatic copolyester based on 1,5-pentanediol, its H NMR spectrum is as follows figure 2 shown.

[0058] After testing, the intrinsic viscosity of the aliphatic-aromatic copolyester prepared in this embodiment is 0.82dL / g, the glass transition temperature is -24.7°C, and the melting point is ...

Embodiment 3

[0060] (1) 1,9-Azelaic acid (0.125mol, 23.53g), terephthalic acid (0.125mol, 20.77g), 1,5-pentanediol (0.7mol, 72.90g) were added to a 250mL four-neck flask ), 1,4-butanediol (0.05mol, 4.51g) and isopropyl titanate (0.5mmol, 141mg), with an alkyd ratio of 2.5, reacted at 200°C for 3 hours to obtain an esterified product, esterified The rate reached 98.2%;

[0061] (2) Add titanium-phosphorus composite catalyst (306mg, purchased from Nanjing Nengde New Material Technology Co., Ltd., TCAIA10) to the esterification product obtained in step (1), and react at 200°C for 1 hour at about 160Pa, 240 ℃ for 2 hours and 250℃ for 1 hour to remove excess 1,5-pentanediol and a small amount of oligomers to obtain the high molecular weight aliphatic-aromatic based on 1,5-pentanediol Copolyester.

[0062] After testing, the intrinsic viscosity of the aliphatic-aromatic copolyester prepared in this embodiment is 0.98dL / g, the glass transition temperature is -43.7°C, and the melting point is 65...

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Abstract

The invention discloses a high molecular weight aliphatic-aromatic copolyester and a preparation method thereof. The aliphatic-aromatic copolyester is prepared through an esterification-melt polycondensation process of a diol, a diacid and an selectively added polyol. The content of the 1,5-pentanediol in the diol component of the high molecular weight aliphatic-aromatic copolyester is high, and the number of carbon atoms in the 1,5-pentanediol chain segment is odd, so the high molecular weight aliphatic-aromatic copolyester has excellent mechanical properties and has a broad application prospect. The preparation method of the invention has the advantages of simple process, no solvents, friendly environment in the process, high catalyst activity, short reaction time, good product color, and facilitation of industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials and their preparation, and relates to polyesters and their preparation methods, in particular to high molecular weight aliphatic-aromatic copolyesters, their preparation methods and applications. Background technique [0002] Aliphatic-aromatic copolyesters have attracted widespread attention due to their good thermo-mechanical properties and biodegradable properties within a certain composition range, as well as controllable structure-properties, such as polybutylene adipate - Co-butylene terephthalate (PBAT) has been industrialized and used to make agricultural films, disposables, etc. to replace traditional polyolefin materials. While traditional aromatic polyesters are mostly derived from fossil raw materials, bio-based monomers replacing petroleum-based monomers are beneficial to reduce dependence on fossil resources, and new bio-based polyester materials with novel structures and u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/181C08G63/672C08G63/183C08G63/127C08G63/85C08L67/02C08L67/00
CPCC08G63/127C08G63/181C08G63/183C08G63/672C08G63/85C08G2230/00C08L67/00C08L67/02C08L2201/06
Inventor 吴林波陆璟
Owner ZHEJIANG UNIV
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