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Furyl copolyester and preparation method thereof

A technology of furan-based copolyester and furandicarboxylic acid, applied in the field of furan-based copolyester and its preparation, can solve the problems of low molecular weight, low tensile strength, low tensile modulus and the like

Active Publication Date: 2019-05-28
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current polyester materials produced by 2,5-furandicarboxylic acid often have some disadvantages, such as

Method used

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  • Furyl copolyester and preparation method thereof
  • Furyl copolyester and preparation method thereof
  • Furyl copolyester and preparation method thereof

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[0030] The preparation method of furyl copolyester provided by the invention comprises the following steps:

[0031] (1) A first component, a second component and a third component are provided, wherein the first component includes at least one of furandicarboxylic acid and furandicarboxylate, and the second component Including at least one of aromatic diols and aliphatic diols, the third component includes acid anhydrides with a carbonyl number greater than or equal to 3;

[0032] (2) Mix the first component, the second component, the third component and the esterification catalyst, and react under an inert atmosphere or a nitrogen atmosphere to obtain a first intermediate product, wherein the The molar ratio of the first component, the second component and the third component is 1:(1.1~2.0):(0.0001~0.02);

[0033] (3) Under vacuum conditions, the first intermediate product is subjected to a prepolymerization reaction to obtain a second intermediate product;

[0034] (4) Un...

Embodiment 1

[0076] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, pyromellitic anhydride and anhydrous zinc acetate into the reaction kettle at a molar ratio of 1:1.6:0.003:0.002, vacuumize and replace with inert gas three times , and then gradually increased the temperature to 185°C, and reacted for 4h. Then add 0.12% antimony trioxide, 0.2% triphenyl phosphate, and 0.15% antioxidant-168 in the molar weight of dimethyl 2,5-furandicarboxylate, and slowly vacuum to 200Pa~ 2000Pa, prepolymerized at 220°C for 1h. Then gradually raise the temperature to 250° C., continue vacuuming to below 200 Pa and react for 2.5 hours to obtain furyl copolyester.

[0077] From figure 1 It can be seen that the furyl copolyester obtained in this embodiment is very light yellow.

[0078] figure 2 Among them, 11.31ppm is solvent CF 3 The peak of COOD is the peak of hydrogen on the furan ring at 7.17ppm (2H), and the peak of hydrogen on the ethylene glycol chain segment at 4.59ppm (4H). So, from ...

Embodiment 2

[0083] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, pyromellitic anhydride and anhydrous zinc acetate into the reaction kettle at a molar ratio of 1:1.6:0.0015:0.002, vacuumize and replace with nitrogen three times, Stirring was started and the temperature was gradually raised to 195°C for 2 hours of reaction. Then add 0.3% antimony trioxide, 0.12% trimethyl phosphate, and 0.15% antioxidant-1010 in the molar weight of dimethyl 2,5-furandicarboxylate, and slowly evacuate to 200Pa~ 1500Pa, pre-polymerized at 220°C for 0.5h. Then gradually raise the temperature to 240° C., and continue the reaction at a vacuum degree below 200 Pa for 4 hours to obtain a furyl copolyester.

[0084] The furan-based copolyester obtained in this embodiment is very light yellow. After testing, its intrinsic viscosity is 0.97dL / g, its tensile strength is 76.5MPa, its tensile modulus is 2.4GPa, and its carbon dioxide gas barrier performance is 0.8× 10 -12 cm 3 cm / cm 2 ·s·cmHg, oxygen gas b...

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Abstract

The invention relates to furyl copolyester and a preparation method thereof. The preparation method comprises the following steps: mixing a first component, a second component and a third component with the mole ratio of 1 to (1.1 to 2.0) to (0.0001 to 0.02) with an esterification catalyst to obtain a first intermediate product, wherein the first component comprises at least one of furan dicarboxylic acid and a furan dicarboxylic acid ester compound, the second component comprises at least one of aromatic diol and aliphatic diol, and the third component comprises acid anhydride with carbonyl number being greater than or equal to 3; performing prepolymerization reaction and polycondensation on the first intermediate product to obtain furyl copolyester. In the preparation method, the acid anhydride with carbonyl number being greater than or equal to 3 serves as a connection point of chain segments, so that the chain segment structure of the furyl copolyester is expanded to a network structure, thereby obtaining the colorless or lightcolor furyl copolyester with excellent mechanical property and air barrier property and high molecular weight, and further meeting the application requirement of furyl copolyester in the fields of packing materials, thin films, fibers, engineering plastics and the like.

Description

technical field [0001] The invention relates to the technical field of materials, in particular to a furyl copolyester and a preparation method thereof. Background technique [0002] At present, the widely used bio-based polymer materials mainly include polylactic acid (PLA), polyhydroxy fatty acid (PHA), polyglycolic acid (PGA), polybutylene succinate (PBS) and so on. However, they all belong to aliphatic polymers. Due to the lack of rigid aromatic ring structure in the molecular structure, their mechanical properties (such as strength, modulus, creep resistance, etc.) and heat resistance (such as thermomechanical properties, heat distortion temperature, etc.) They are significantly lower than petroleum-based polymer materials such as polyethylene terephthalate (PET), polycarbonate (PC), aromatic nylon (PA), bisphenol A epoxy resin (Epoxy), which severely limits their scope of application. [0003] The molecular structure of 2,5-furandicarboxylic acid (2,5-FDCA) contains ...

Claims

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Application Information

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IPC IPC(8): C08G63/668C08G63/85C08G63/86C08J5/18D01F6/84C08L67/00
Inventor 张小琴王静刚刘小青孙藜源代金月张传芝朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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