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Furan dicarboxylic acid copolyester and preparation method thereof

A technology of furandicarboxylic acid copolyester and furandicarboxylic acid, which is applied in the field of materials and can solve the problems of low tensile modulus, deep color in reaction time, low molecular weight 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

AI Technical Summary

Problems solved by technology

However, the current polyester materials produced by 2,5-furandicarboxylic acid often have some disadvantages, such as darker color due to long reaction time and low tensile modulus due to low molecular weight , low tensile strength, etc.

Method used

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  • Furan dicarboxylic acid copolyester and preparation method thereof
  • Furan dicarboxylic acid copolyester and preparation method thereof
  • Furan dicarboxylic acid copolyester and preparation method thereof

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preparation example Construction

[0031] The preparation method of furandicarboxylic acid copolyester provided by the invention may further comprise the steps:

[0032] (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 polyols with a number of hydroxyl groups greater than or equal to 3;

[0033] (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);

[0034] (3) Under vacuum conditions, the first intermediate product is subjected to a prepolymerization reaction to obtain a second intermediate produ...

Embodiment 1

[0077] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, pentaerythritol and anhydrous zinc acetate into the reaction kettle according to the molar ratio of 1:1.5:0.001:0.0015, vacuumize and replace with nitrogen three times, start stirring and gradually Raise the temperature to 180°C and react for 5h. Then add 0.15% antimony trioxide, 0.1% triphenyl phosphate, and 0.1% antioxidant-1010 in the molar weight of dimethyl 2,5-furandicarboxylate, and slowly vacuum to 600Pa~ 2000Pa, pre-polymerized at 220°C for 0.5h. Then gradually raise the temperature to 240° C., continue vacuuming to below 200 Pa and react for 3 hours to obtain bio-based furandicarboxylic acid copolyester.

[0078] from figure 1 It can be seen that the bio-based furandicarboxylic acid copolyester obtained in this example is very light yellow.

[0079] 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 ...

Embodiment 2

[0084] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, glycerol and anhydrous cobalt acetate into the reaction kettle at a molar ratio of 1:1.6:0.02:0.0005, and gradually raise the temperature to 180°C under an inert atmosphere. Reaction 4h. Then add 0.1% antimony trioxide, 0.1% triphenyl phosphate, and 0.1% antioxidant-1010 of the molar weight of dimethyl 2,5-furandicarboxylate. Pre-polymerization under the condition of ℃ for 0.5h. Then react at a temperature of 240° C. and a vacuum degree below 200 Pa for 4 hours to obtain bio-based furandicarboxylic acid copolyester.

[0085] The bio-based furandicarboxylic acid copolyester obtained in this example is very light yellow, its intrinsic viscosity is 0.80dL / g, the tensile strength is 71.8MPa, the tensile modulus is 2.2GPa, and the carbon dioxide gas barrier performance is 1.1× 10 -12 cm 3 cm / cm 2 ·s·cmHg, oxygen gas barrier performance is 1.2×10 -12 cm 3 cm / cm 2 ·s·cmHg.

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Abstract

The invention relates to furan dicarboxylic acid copolyester and a preparation method thereof. The preparation method comprises the following steps: mixing a first component, a second component and athird 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 oneof 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 polyhydric alcohol with hydroxyl number being greater than or equal to 3; performing prepolymerization reaction and polycondensation on the first intermediate product to obtain the furan dicarboxylic acid copolyester. In the preparation method, the polyhydric alcohol with hydroxyl number being greater than or equal to 3 serves as a connection point of chain segments, so that the chain segment structure of thefuran dicarboxylic acid copolyester is expanded to a network structure, thereby obtaining the colorless or lightcolor furan dicarboxylic acid copolyester with excellent mechanical property and air barrier property and high molecular weight.

Description

technical field [0001] The invention relates to the field of material technology, in particular to furandicarboxylic acid 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-...

Claims

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Application Information

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