Poly(ethylene 2,5-furandicarboxylate) with low diethylene glycol link content and preparation method of poly(ethylene 2,5-furandicarboxylate)

A technology of polyethylene furandicarboxylate and ethylene furandicarboxylate chain links, applied in the field of bio-based polyester-polyethylene furandicarboxylate and its preparation, can solve the problem of slow crystallization of PEF, ether Chemical side reactions, affecting crystallinity and other problems, to achieve the effect of increasing molecular weight, high selectivity, and excellent crystallinity

Inactive Publication Date: 2015-11-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in many research reports, PEF crystallizes slowly or even does not crystallize, which is not conducive to maintaining the above properties
The reason is that we found that PEF is more prone to etherification side reac

Method used

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  • Poly(ethylene 2,5-furandicarboxylate) with low diethylene glycol link content and preparation method of poly(ethylene 2,5-furandicarboxylate)
  • Poly(ethylene 2,5-furandicarboxylate) with low diethylene glycol link content and preparation method of poly(ethylene 2,5-furandicarboxylate)
  • Poly(ethylene 2,5-furandicarboxylate) with low diethylene glycol link content and preparation method of poly(ethylene 2,5-furandicarboxylate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and stannous oxalate (0.1mmol, 20.7mg) into a 250mL three-necked flask, the alkyd molar ratio was 2.5, and reacted at 150-200°C for 2 hours to obtain an esterified product with an esterification rate of 98.7%;

[0052] (2) Add ethylene glycol antimony (0.1mmol, 42.4mg), antioxidant 1010 (90mg), antioxidant 168 (90mg) to the esterification product obtained in step (1), at 200-220°C, 10 5 Under the condition of -2000Pa, the precondensation reaction was carried out for 0.5 hours to remove free ethylene glycol and a small amount of oligomers to obtain a prepolymer;

[0053] (3) The precondensation product obtained in step (2) was subjected to melt polycondensation reaction at 240-250° C. and about 300 Pa for 2 hours to obtain polyethylene furandicarboxylate PEF1.

[0054] The diethylene glycol chain segment content of PEF1 is 1.76mol%, the intrinsic viscosity is 0.62dl / g; the melt crystal...

Embodiment 2

[0056] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and titanium glycolate (0.1mmol, 16.8mg) into a 250mL three-necked flask, The ratio is 2.5, and the esterification product is obtained at 150-200°C for 2 hours, and the esterification rate reaches 98.7%;

[0057] (2) Add ethylene glycol antimony (0.1 mmol, 42.4 mg), triphenyl phosphite (90 mg), and phosphorous acid (50 mg) to the esterification product obtained in step (1), and heat 5 Under the condition of -2000Pa, the precondensation reaction was carried out for 0.5 hours to remove free ethylene glycol and a small amount of oligomers to obtain a prepolymer;

[0058] (3) The precondensation product obtained in step (2) was subjected to melt polycondensation reaction at 240-250° C. and about 300 Pa for 2 hours to obtain polyethylene furandicarboxylate PEF2.

[0059] The diethylene glycol chain segment content of PEF2 is 1.96mol%, and the intrinsic viscosity is 0.63dl / g; the melt cryst...

Embodiment 3

[0061] (1) Add dimethyl furandicarboxylate (0.1mol, 18.4g), ethylene glycol (0.25mol, 15.5g) and n-butyl titanate (0.05mmol, 17mg) into a 250mL three-necked flask, alkyd mole Ratio of 2.5, reacted at 150-200°C for 4 hours to obtain an esterified product with an esterification rate of 98.3%;

[0062] (2) Add 1,8-diazabicycloundec-7-ene (0.1mmol, 15.2mg), antioxidant 1010 (90mg), antioxidant 168 (90mg), at 200-220°C, 10 5 Under the condition of -2500Pa, the precondensation reaction was carried out for 0.5 hours, and the free ethylene glycol and a small amount of oligomers were removed to obtain the prepolymer;

[0063] (3) The precondensation product obtained in step (2) was subjected to melt polycondensation reaction at 240-250° C. and about 200 Pa for 4 hours to obtain polyethylene furandicarboxylate PEF3.

[0064] The diethylene glycol chain segment content of PEF3 is 0.53mol%, the intrinsic viscosity is 0.49dl / g; the melt crystallization peak temperature is 157°C, and the ...

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Abstract

The invention discloses poly(ethylene 2,5-furandicarboxylate) with low diethylene glycol link content and a preparation method of poly(ethylene 2,5-furandicarboxylate). The content of 2,5-furandicarboxylic acid diethylene glycol ester links, short for diethylene glycol links, of poly(ethylene 2,5-furandicarboxylate) is lower than 3 mol%, and poly(ethylene 2,5-furandicarboxylate) is prepared from 2,5-furandicarboxylic acid or ester of 2,5-furandicarboxylic acid and ethylene glycol through an esterification-melt phase polycondensation process or ester exchange-melt phase polycondensation process under the action of a high-efficiency and high-selectivity binary catalyst. According to poly(ethylene 2,5-furandicarboxylate) with the low diethylene glycol link content, poly(ethylene 2,5-furandicarboxylate) has excellent crystallinity due to the low diethylene glycol link content, thereby having better heat resistance and mechanical properties. The preparation method is simple in process, the catalyst has high activity and good selectivity, and poly(ethylene 2,5-furandicarboxylate) with the low diethylene glycol link content can be prepared; an organic solvent is not needed, the process is environment-friendly, and accordingly, realization of industrialization is facilitated.

Description

technical field [0001] The invention relates to bio-based polyester-polyethylene furandicarboxylate and a preparation method thereof, in particular to polyethylene furandicarboxylate with low diethylene glycol chain segment content and a preparation method thereof. Background technique [0002] Furandicarboxylic acid is a dibasic acid in which two hydrogen atoms on the furan ring are replaced by carboxyl groups. According to the different substitution positions of the two carboxyl groups on the furan ring, there are 2,5-furandicarboxylic acid, 2,3-furandicarboxylic acid, 2,4-furandicarboxylic acid or 3,4-furandicarboxylic acid, among which 2,5-furandicarboxylic acid is the most important. 2,5-furandicarboxylic acid (2,5-furandicarboxylic acid, sometimes referred to as furandicarboxylic acid, English abbreviation as FDCA or FA) is a new type of bio-based monomer. It is derived from the most productive biomass resource - cellulose, hemicellulose or starch. Biomass produces h...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/78C08G63/85
Inventor 吴林波吴佳萍徐煜韬
Owner ZHEJIANG UNIV
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