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Copolyester containing furan ring and its preparation method

A technology of copolyester and furan ring, applied in the field of furan ring-containing copolyester and its preparation, can solve the problems of low tensile strength, deep color in reaction time, low tensile modulus and the like

Active Publication Date: 2021-08-24
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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  • Copolyester containing furan ring and its preparation method
  • Copolyester containing furan ring and its preparation method
  • Copolyester containing furan ring and its preparation method

Examples

Experimental program
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preparation example Construction

[0031] The preparation method of the copolyester containing furan ring provided by the invention comprises the following steps:

[0032] (1) The first component, the second component, the third component and the fourth component are provided, wherein the first component includes at least one of furandicarboxylic acid and furandicarboxylic acid ester, so The second component includes at least one of aromatic diols and aliphatic diols, the third component includes polyhydric alcohols with a hydroxyl number greater than or equal to 3, and the fourth component includes a carbonyl number greater than or equal to 3 anhydrides;

[0033] (2) Mix the first component, the second component, the third component, the fourth component and the esterification catalyst, and react under an inert atmosphere or a nitrogen atmosphere to obtain the first Intermediate product, wherein the molar ratio of the first component, the second component, the third component and the fourth component is 1:(1....

Embodiment 1

[0079] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, pyromellitic anhydride, pentaerythritol and anhydrous zinc acetate into the reaction kettle at a molar ratio of 1:1.6:0.003:0.0005:0.001, and under an inert atmosphere , gradually warming up to 185°C, and reacting for 4.5h. Then add 0.12% antimony trioxide, 0.2% triphenyl phosphate, and 0.1% antioxidant-1010 in the molar weight of dimethyl 2,5-furandicarboxylate, and slowly evacuate 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 a furan ring-containing copolyester.

[0080] from figure 1 It can be seen that the furan ring-containing copolyester obtained in this example is very light yellow.

[0081] figure 2 Among them, 11.31ppm is solvent CF 3 The peak of COOD, 7.17ppm is the peak (2H) of hydrogen on the furan ring, and 4.59ppm is the peak (4H) of hydrogen on the ethylene glycol chain segme...

Embodiment 2

[0086] Add dimethyl 2,5-furandicarboxylate, ethylene glycol, pyromellitic anhydride, pentaerythritol and anhydrous cobalt acetate into the reaction kettle in a molar ratio of 1:1.5:0.003:0.001:0.0012, vacuumize, fill Nitrogen was replaced three times, stirring was started and the temperature was gradually raised to 180°C, and the reaction was carried out for 4.5 hours. Then add 0.15% antimony trioxide, 0.2% diphenyl phosphate, and 0.1% antioxidant-168 in the molar weight of dimethyl 2,5-furandicarboxylate, and slowly vacuum to 300Pa~ 2000Pa, pre-polymerized at 225°C for 0.5h. Then gradually raise the temperature to 240° C., and continue the reaction at a vacuum degree below 200 Pa for 2.5 hours to obtain a copolyester containing a furan ring.

[0087] The furan ring-containing copolyester obtained in this embodiment is very light yellow. After testing, its intrinsic viscosity is 0.98dL / g, the tensile strength is 76.8MPa, the tensile modulus is 2.5GPa, and the carbon dioxide g...

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Abstract

The invention relates to a copolyester of furandicarboxylic acid and a preparation method thereof. The segment structure of the copolyester containing a furan ring is a network structure, and the molar ratio is 1:(1.1~2.0):(0.0001~0.02 ): (0.0001~0.02) of the first component, the second component, the third component and the fourth component are polymerized, wherein the first component includes furandicarboxylic acid, furandicarboxylic acid ester At least one, the second component includes at least one of aromatic diols and aliphatic diols, the third component includes polyols with a hydroxyl number greater than or equal to 3, and the fourth component includes a carbonyl number greater than or equal to 3 of acid anhydride. In the preparation method, the polyhydric alcohol with the number of hydroxyl groups greater than or equal to 3 and the acid anhydride with the number of carbonyl groups greater than or equal to 3 are used as the linking points of the chain segments, so that the chain segment structure of the copolyester containing furan rings is expanded into a network structure, thereby obtaining colorless or light-colored It is a high molecular weight furan ring-containing copolyester with excellent mechanical properties and gas barrier properties.

Description

technical field [0001] The invention relates to the field of material technology, in particular to a furan ring-containing 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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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/668C08G63/78
Inventor 张小琴王静刚刘小青朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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