2, 5-furan dicarboxylic polyester/layered silicate nano-composite material, preparation method thereof and application of material

A technology of nano-composite materials and furandicarboxylic acid diester, which is applied in the field of polymer materials, can solve the problems of increasing molecular weight, insufficient effect, low molecular weight, etc., and achieve good tensile strength, simple and feasible method, and uniform dispersion

Active Publication Date: 2018-03-09
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the oxygen atom in the furan ring endows the 2,5-furandicarboxylate with stronger polarity and the asymmetry of the furan ring leads to poor molecular segment mobility, the 2,5-furandicarboxylate The crystallization rate of polyester is slow. For example, in the article "Polymer" (2016, 87:148-158), the synthesized PEF does not have a melt crystallization peak at a cooling rate of 10°C / min.
Although the slow crystallization rate of 2,5-furandicarboxylic acid-based polyester is beneficial to maintain a certain degree of transparency of the sample, it is not conducive to injection molding, and it is also not conducive to increasing its molecular weight through solid-state polycondensation
For 2,5-furandicarboxylic acid-based polyester nanocomposites, there are still some deficiencies, mainly as follows: the synthesized 2,5-furandicarboxylic acid-based polyester nanocomposites have low molecular weight and low intrinsic viscosity. ≦0.5dL / g, the influence of nanoparticles on its mechanical properties has not been reported; the effect of promoting the crystallization of 2,5-furandicarboxylic acid-based polyester is still not good enough, such as PEF nanocomposites, only at a slow cooling rate (≦5℃ / min) melt crystallizes, but the crystallization promotion effect under rapid cooling rate (≥10℃ / min) is not good or has not been reported

Method used

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  • 2, 5-furan dicarboxylic polyester/layered silicate nano-composite material, preparation method thereof and application of material
  • 2, 5-furan dicarboxylic polyester/layered silicate nano-composite material, preparation method thereof and application of material
  • 2, 5-furan dicarboxylic polyester/layered silicate nano-composite material, preparation method thereof and application of material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Mix 0.67g of dried montmorillonite modified with octadecylbishydroxyethylmethylammonium salt with 44.67g of ethylene glycol, stir vigorously for 2 hours, and disperse in an ultrasonic environment for 15 minutes , to obtain an ethylene glycol suspension containing montmorillonite treated with octadecylbishydroxyethylmethylammonium salt;

[0050] (2) Under a nitrogen atmosphere, add the ethylene glycol suspension obtained in step (1), 66.28g dimethyl 2,5-furandicarboxylate and 0.08g stannous oxalate to the reactor, and react at 170°C for 1 hour , react at 180°C for 1 hour, react at 190°C for 1 hour, and react at 200°C for 1 hour to obtain the transesterified product;

[0051] (3) Add 0.1 g of ethylene glycol antimony to the transesterified product obtained in step (2), and conduct polycondensation at 240°C and high vacuum (≦133Pa) for 3 hours to obtain poly-2,5-furandicarboxylic acid Ethylene glycol ester / organic montmorillonite nanocomposite material, the amount of ...

Embodiment 2

[0053] (1) Mix the dried 1.66g of montmorillonite modified with octadecylbishydroxyethylmethyl with 44.67g of ethylene glycol, stir vigorously for 2 hours and then disperse in an ultrasonic environment for 15 minutes to prepare Obtain the ethylene glycol suspension containing the montmorillonite modified by octadecyl bis-hydroxyethyl methyl ammonium salt;

[0054] (2) Under a nitrogen atmosphere, add the ethylene glycol suspension obtained in step (1), 66.28g dimethyl 2,5-furandicarboxylate and 0.08g stannous oxalate to the reactor, and react at 170°C for 1 hour , react at 180°C for 1 hour, react at 190°C for 1 hour, and react at 200°C for 1 hour to obtain the transesterified product;

[0055] (3) Add 0.1 g of ethylene glycol antimony to the transesterified product obtained in step (2), and conduct polycondensation at 240°C and high vacuum (≦133Pa) for 3 hours to obtain poly-2,5-furandicarboxylic acid Ethylene glycol ester / organic montmorillonite nanocomposite material, the a...

Embodiment 3

[0057] (1) 2.32g of dried montmorillonite and 44.67g of ethylene glycol were mixed through 18-bishydroxyethylmethyl ammonium salt modification, stirred vigorously for 2 hours and then dispersed in an ultrasonic environment for 15 minutes to prepare Obtain the ethylene glycol suspension containing the montmorillonite modified by octadecyl bis-hydroxyethyl methyl ammonium salt;

[0058] (2) Under a nitrogen atmosphere, add the ethylene glycol suspension obtained in step (1), 66.28g dimethyl 2,5-furandicarboxylate and 0.08g stannous oxalate to the reactor, and react at 170°C for 1 hour , react at 180°C for 1 hour, react at 190°C for 1 hour, and react at 200°C for 1 hour to obtain the transesterified product;

[0059] (3) Add 0.1 g of ethylene glycol antimony to the transesterification product obtained in step (2), and conduct polycondensation at 240°C and high vacuum (≦133Pa) for 3 hours to obtain poly-2,5-furandicarboxylic acid Ethylene glycol ester / organic montmorillonite nano...

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Abstract

The invention discloses a 2, 5-furan dicarboxylic polyester / layered silicate nano-composite material, a preparation method thereof and an application of the material. The composite material comprises2, 5-furan dicarboxylic polyester and layered silicate and is prepared by an in-situ polymerization method, the stripping degree of the organically-treated layered silicate in an acquired product substrate is high, the molecular weight of the organically-treated layered silicate is high, the tensile strength of the organically-treated layered silicate is high, and the organically-treated layered silicate has a certain crystallization property. The preparation method is simple and feasible and solves the problem of slow crystallization rate of the2, 5-furan dicarboxylic polyester, applicationsof the preparation method can further be widened in the high-resistance air packaging market, and a good foundation is provided for subsequent industrialization.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a high-performance 2,5-furandicarboxylate polyester / layered silicate nanocomposite material and its preparation method and application. Background technique [0002] Polyester based on petroleum-based monomer terephthalic acid or terephthalic diester plays an important role in the polymer industry, such as polyethylene terephthalate (Poly(ethylene terephthalate), abbreviated as PET ) has an annual output of nearly 70 million tons, which are widely used in fiber, film and plastic bottles. However, traditional petrochemical resources are facing the danger of shortage or even depletion due to their non-renewability, so developing a renewable resource to partially replace petrochemical resources is an effective and sustainable development method. At present, 2,5-furandicarboxylic acid and its diesters, which were identified as one of the 12 most competitive bio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/86C08K9/04C08K7/00
CPCC08G63/672C08G63/866C08K7/00C08K9/04C08K2201/011
Inventor 谢鸿洲吴林波
Owner ZHEJIANG UNIV
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