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Bio-based polyester elastomer and preparation method thereof

A polyester elastomer, bio-based technology, applied in the field of preparation of polyester elastomers, can solve the problems of insufficient performance of elastomers, difficulty in recycling, etc., and achieve the effects of excellent elasticity, easy recycling, good elasticity and strength

Inactive Publication Date: 2018-09-28
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of insufficient performance and difficult recycling of existing elastomers, the present invention provides a bio-based polyester elastomer and a preparation method thereof. The obtained bio-based polyester elastomer has excellent elasticity and maintains excellent mechanical strength, easy to recycle

Method used

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  • Bio-based polyester elastomer and preparation method thereof
  • Bio-based polyester elastomer and preparation method thereof
  • Bio-based polyester elastomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] (1) Add 2,5-furandicarboxylic acid (0.375mol, 58.53g), 1,5-pentanediol (0.75mol, 78.11g) and n-butyl titanate (0.375mmol, 128mg) into a 250mL four-necked flask ), with an alkyd ratio of 2, reacted at 200°C for 1 hour, at 220°C for 1 hour, and at 230°C for 1.5 hours to obtain an esterified product with an esterification rate of 98.9%;

[0093] (2) Add isopropyl titanate (0.375mmol, 106mg) to the esterification product obtained in step (1), and react at 230°C for 2 hours at about 140Pa, 2 hours at 240°C, and react at 250°C After 1 hour, excess 1,5-pentanediol and a small amount of oligomers were removed to obtain polypentylene-2,5-furandicarboxylate, abbreviated as PPeF.

[0094] The proton nuclear magnetic resonance spectrum figure of the PPeF prepared in this embodiment is as follows figure 2 Shown; Intrinsic viscosity is 0.84dL / g; Shows typical elastic body tensile behavior in tensile test, tensile modulus is 9.5MPa, tensile strength is 11.2MPa, elongation at break i...

Embodiment 2

[0096] (1) Add isophthalic acid (0.375mol, 58.53g), 1,5-pentanediol (0.675mol, 70.30g) and n-butyl titanate (0.125mmol, 42.7mg) into a 250mL four-neck flask, The alkyd-acid ratio is 1.8, and the esterification product is obtained after reacting at 230°C for 3 hours, and the esterification rate reaches 98.9%;

[0097](2) The catalyst n-butyl titanate (0.125mmol, 42.7mg) was added to the esterification product obtained in step (1), and reacted at 230°C for 1 hour and 250°C for 4 hours under the condition of about 120Pa, to remove Excess 1,5-pentanediol and a small amount of oligomers can produce polypentylene isophthalate, abbreviated as PPeI.

[0098] After testing, the intrinsic viscosity of the PPeI prepared in this example is 0.81dL / g; in the tensile test, it exhibits a typical tensile behavior of an elastomer, with a tensile modulus of 4.2MPa and a tensile strength of 4.2MPa. Elongation > 1000%, the tensile curve see image 3 .

Embodiment 3

[0100] (1) Add 0.275 mol of adipic acid, 0.225 mol of furandicarboxylic acid and 1.0 mol of 1,4-butanediol (alcohol-acid ratio is 2) into a 250 mL four-necked flask. Stir and heat to 200°C under nitrogen atmosphere, then add the catalyst n-butyl titanate (0.1mol% of the total amount of dibasic acid), react for 1h, then raise the temperature to 210°C and continue the reaction for 2h, and finally raise the temperature to 220°C for 1-2h End the esterification reaction until the esterification rate reaches more than 98%.

[0101] (2) After the esterification reaction, the temperature is gradually raised to 230°C, and the vacuum is gradually evacuated to below 240Pa, and the reaction is performed for 1 hour, and then the temperature is raised to 240°C for 4 hours to complete the reaction and obtain PBA. 55 f 45 Copolyester samples.

[0102] After testing, the PBA prepared in this embodiment 55 f 45 The H NMR spectrum of Figure 5 ; Intrinsic viscosity is 0.81dL / g; In the tensi...

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Abstract

The present invention provides a bio-based polyester elastomer containing a diacid component, a diol component and a branched monomer residue. The diacid component comprises the following materials: (i) 40-100 mol% of an asymmetric-structure aromatic diacid residue, and (ii) 0-60 mol% of a terephthalic acid residue and / or a C4 to C12 aliphatic saturated diacid residue; the diol component comprisesthe following materials: (i) 50-100 mol% of a C4 to C12 aliphatic saturated diol residue, and (ii) 0-50 mol% of a C2 to C3 aliphatic saturated diol residue; and a molar ratio of the diacid componentto the diol component to the branched monomer residue is 1:(1.05-2):(0-0.05). The bio-based polyester elastomer provided by the present invention is prepared by melt polycondensation, a plurality of raw materials of the bio-based elastomer are from biomass resources, the bio-based polyester elastomer has excellent elasticity and other mechanical properties, and industrialization of a preparation method is easy to realize.

Description

technical field [0001] The invention relates to the field of preparation of polyester elastomers, in particular to a bio-based polyester elastomer and a preparation method thereof. Background technique [0002] Rubber, including chemically cross-linked (thermosetting) vulcanized rubber and thermoplastic elastomer, is one of the three major synthetic materials and is widely used in tires, seals, shock absorbers, hoses, tapes, rubber rollers, cables due to its excellent elasticity and other fields. [0003] At present, all commercialized rubber and elastomers are derived from natural latex or synthesized from fossil resources as starting materials. Their huge production and application have caused a series of resource and environmental problems. Therefore, it is beneficial to develop renewable resources to partially replace fossil resources. Sustainability in the rubber industry. In recent years, with the in-depth research on biomass conversion and utilization and the vigoro...

Claims

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Application Information

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IPC IPC(8): C08G63/42C08G63/181C08G63/672C08G63/91
CPCC08G63/42C08G63/181C08G63/672C08G63/916
Inventor 吴林波彭双宝陆璟谢鸿洲
Owner ZHEJIANG UNIV
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