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Furan dicarboxylic acid copolyester and preparation method thereof

A technology of furandicarboxylic acid copolyester and dibasic acid, applied in the field of materials, can solve problems such as precocious puberty, infant deformity, slow release of bisphenol A, etc., and achieve the effect of excellent heat resistance

Active Publication Date: 2019-05-07
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, 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
However, PCs currently used in water cups, children's toys, and kitchen appliances will slowly release bisphenol A during use, causing deformities or premature puberty in babies. Countries around the world have banned them from being used in products such as baby bottles

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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) Dibasic acid or its esterified product, dibasic alcohol and esterification reaction catalyst are mixed, carry out esterification reaction under inert atmosphere, obtain the first intermediate product; Wherein, described dibasic acid comprises furandicarboxylic acid, so The dihydric alcohols include ethylene glycol, 1,4-cyclohexanedimethanol and 2,2,4,4-tetramethyl-1,3-cyclobutanedimethanol;

[0033] (2) Under vacuum conditions, subjecting the first intermediate product to a precondensation reaction to obtain a second intermediate product;

[0034] (3) Under vacuum conditions, the second intermediate product is subjected to polycondensation reaction to obtain furandicarboxylic acid copolyester.

[0035] Specifically, the furandicarboxylic acid is 2,5-furandicarboxylic acid, and the 2,5-furandicarboxylate is dimethyl 2,5-furandicarboxylate. ...

Embodiment 1

[0058] Dimethyl 2,5-furandicarboxylate 46g, 1,4-cyclohexanedimethanol 12.6g, 2,2,4,4-tetramethyl-1,3-cyclobutanediol 28.8g and ethyl 7.0 g of diol was added to the polymerization reactor, and then 0.15% of anhydrous zinc acetate based on the molar amount of dimethyl 2,5-furandicarboxylate was added. Under an inert atmosphere, react at 180° C. for 4 hours to obtain the first intermediate product.

[0059] Add 0.2% antimony trioxide, 0.15% triphenyl phosphate and 0.1% antioxidant 1010 based on the molar weight of dimethyl 2,5-furandicarboxylate to the first intermediate product, at a vacuum degree of 500Pa ~3000Pa, 220°C pre-condensation for 0.5h to obtain the second intermediate product.

[0060] Then the second intermediate product was reacted at 240° C. for 3 hours under a vacuum of 200 Pa to obtain furandicarboxylic acid copolyester.

[0061] After testing, the relative number average molecular mass of the furandicarboxylic acid copolyester is 23000g / moL, the relative weig...

Embodiment 2

[0065] Dimethyl 2,5-furandicarboxylate 92.5g, 1,4-cyclohexanedimethanol 54.1g, 2,2,4,4-tetramethyl-1,3-cyclobutanediol 10.0g and 22.0 g of ethylene glycol was added to the polymerization reactor, and then 0.10% of anhydrous zinc acetate based on the molar amount of dimethyl 2,5-furandicarboxylate was added. Under an inert atmosphere, react at 160° C. for 2 h to obtain the first intermediate product.

[0066] Add 0.1% antimony trioxide, 0.25% triphenylphosphine and 0.5% antioxidant 168 based on the molar weight of dimethyl 2,5-furandicarboxylate to the first intermediate product, at a vacuum degree of 500Pa ~3000Pa, 230°C precondensation for 1.0h, to obtain the second intermediate product.

[0067] Then the second intermediate product was reacted at 250° C. for 4 hours under a vacuum of 200 Pa to obtain furandicarboxylic acid copolyester.

[0068] After testing, the relative number average molecular mass of the furandicarboxylic acid copolyester is 36000g / moL, the relative we...

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Abstract

The invention relates to furan dicarboxylic acid copolyester and a preparation method thereof. The furan dicarboxylic acid copolyester has a structural formula as shown in a following formula (1), wherein x, y and z are integers of 10-90. The preparation method comprises the following steps: (1) mixing a dibasic acid or ester of the dibasic acid, dihydric alcohol and an esterification catalyst, and performing an esterification reaction in an inert atmosphere so as to obtain a first intermediate product, wherein the dibasic acid comprises furan dicarboxylic acid, and the dihydric alcohol includes ethylene glycol, 1,4-cyclohexane dimethanol and 2,2,4,4-tetramethyl-1,3-cyclobutane dimethanol; (2) performing a pre-polycondensation reaction on the first intermediate product under vacuum conditions so as to obtain a second intermediate product; and (3) performing a polycondensation reaction on the second intermediate product under vacuum condition so as to obtain the furan dicarboxylic acidcopolyester. The preparation method is simple, and the obtained furan dicarboxylic acid copolyester has excellent heat resistance, transparency and mechanical properties at the same time, and can be used for manufacturing baby nursing bottles, children toys, cups, kitchen utensils, electronic appliances and other products.

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. However, PCs currently used in water cups, children's toys, and kitc...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/86C08K5/134C08K5/523C08K5/526
Inventor 王静刚刘小青张小琴孙藜源代金月朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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