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Sulfur-containing furandicarboxylic acid polyester and preparation method thereof

A technology of furandicarboxylic acid polyester and furandicarboxylic acid, which is applied in the field of biomass-based polymer materials and can solve the problems of high glass transition temperature and poor low temperature resistance of polyester

Active Publication Date: 2021-07-30
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For example, the patent application with the publication number CN111592642A discloses a method for preparing a high-toughness bio-based polyester, using 2,5-furandicarboxylic acid, diols, polyhydric alcohols, etc. as raw materials to prepare bio-based polyesters, but existing The glass transition temperature of polyester in technology is relatively high, and the low temperature resistance of polyester is poor

Method used

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  • Sulfur-containing furandicarboxylic acid polyester and preparation method thereof
  • Sulfur-containing furandicarboxylic acid polyester and preparation method thereof
  • Sulfur-containing furandicarboxylic acid polyester and preparation method thereof

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Effect test

Embodiment 1

[0054]The preparation method of furandicarboxylic acid polyester monomer comprises the following steps:

[0055] Take 25g of furandicarboxylic acid, 100g of allyl chloride, and 75ml of triethylamine, and add them into a mixed solution of 75ml of acetone and 75ml of dimethylformamide. Place it in an oil bath at 90°C to reflux and stir for 12 hours. The specific reaction equation is as follows:

[0056]

[0057] Finally, dichloromethane and water were added for three extractions, and then the product was recrystallized by adding n-hexane after rotary evaporation to obtain a white powdery solid, which was a polyester monomer.

[0058] The 1H NMR spectrum of the polyester monomer 1 prepared in this embodiment is as follows figure 1 Shown, show the purity of obtained polyester monomer is very high. From figure 1 Peaks a at 5.3ppm and 5.4ppm and peak b at 4.8 show that allyl chloride is successfully incorporated into the monomer, which provides conditions for subsequent reacti...

Embodiment 2

[0060] The preparation method of furandicarboxylic acid polyester specifically comprises the following steps:

[0061] 1000 mg of the polyester monomer in Example 1, 656 mg of hexanedithiol, 27 mg of azobisisobutyronitrile and 10 mL of tetrahydrofuran were added to the reaction vessel. Argon was introduced for 20 minutes, and then the mixture was placed in an oil bath at 65°C for 12 hours. The specific reaction equation is as follows:

[0062]

[0063] The raw material HS-R-SH in the equation (2) is the 1,6-hexanedithiol, and the S-R-S on the main chain of the product in the equation (2) is the disulfide R. Afterwards, a sulfur-containing furandicarboxylic acid polyester was obtained by methanol precipitation, which was named polyester 1.

Embodiment 3

[0065] The difference between this embodiment and embodiment 2 is that: the polyester 1 in embodiment 2 is stretched incrementally by straining the dumbbell-shaped spline of embodiment 2 at a constant stretching speed of 20mm / min, Each increment is 100% of the polymer deformation, recovery is performed after each increment is reached, when the force returns to 0, stretching is followed, and so on.

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Abstract

The invention discloses sulfur-containing furandicarboxylic acid polyester, and relates to the field of biomass-based high polymer materials, and the structural formula of the sulfur-containing furandicarboxylic acid polyester is shown in the specification, n is more than or equal to 5 and less than or equal to 3000, R on the main chain is a disulfide bond, and R is any one of structures shown in the specification. The invention also provides a preparation method of the polyester. The invention has the beneficial effects that the polyester has a unique chemical structure and excellent mechanical properties, and the mechanical property parameters after tabletting and film making are as follows: the breaking strength is 14.7 Mpa, and the elongation at break is 420%.

Description

technical field [0001] The invention relates to the field of biomass-based polymer materials, in particular to a sulfur-containing furandicarboxylic acid polyester and a preparation method thereof. Background technique [0002] With the development of society, the demand for resources is gradually increasing. Non-renewable resources such as fossil fuels will eventually be exhausted one day, so for sustainable development, the development of new materials and new products is crucial. Among them, with the gradual utilization and development of new renewable resources, bio-based polymer resins are found to be very important. Because of their excellent mechanical properties and non-toxic and harmless, they can be used in many aspects of daily life. , so this direction has gradually become an important research direction for the synthesis of new polymer materials. [0003] The main representatives of new bio-based polymers commonly used in production and life have been industri...

Claims

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Application Information

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IPC IPC(8): C08G75/045
CPCC08G75/045Y02E60/10
Inventor 汪钟凯丁永良
Owner ANHUI AGRICULTURAL UNIVERSITY
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