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Preparation method of furfuran bio-based polyether ester copolymer and novel furfuran bio-based polyether ester copolymer

A technology of copolymer and polyether ester, which is applied in the field of furyl polyether ester synthesis, can solve the problems of high cost, reduced environmental significance, and loss, and achieve the effects of easy control, mild conditions, and good thermodynamic properties

Active Publication Date: 2018-10-09
芜湖万隆新材料有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] However, these newly introduced comonomers often have high cost, or non-bio-based monomers, such as terephthalic acid, which makes all-bio-based polyester products lose the attributes of 100% bio-based materials, and the significance of environmental protection is greatly reduced

Method used

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  • Preparation method of furfuran bio-based polyether ester copolymer and novel furfuran bio-based polyether ester copolymer
  • Preparation method of furfuran bio-based polyether ester copolymer and novel furfuran bio-based polyether ester copolymer
  • Preparation method of furfuran bio-based polyether ester copolymer and novel furfuran bio-based polyether ester copolymer

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preparation example Construction

[0048] The invention provides a kind of preparation method of polyether ester copolymer, comprises the following steps:

[0049] 1) Under the conditions of a protective atmosphere and a metal complex catalyst, 2,5-furandicarboxylic acid and ethylene glycol undergo an esterification reaction, and then undergo a precondensation reaction and a polycondensation reaction to obtain a polyetherester copolymer.

[0050] The present invention has no special restrictions on the structure of the polyether ester copolymer, the structure of the polyether ester copolymer well known to those skilled in the art can be used, and those skilled in the art can select according to actual production conditions, quality control and product requirements And adjustment, in the polyether ester copolymer of the present invention, the percentage content of the molar number of ethylene glycol segment accounts for the molar number of described polyether ester copolymer is preferably 30%~70%, that is more pr...

Embodiment 1

[0125] In the reactor, add 15.6 grams (0.1mol) of 2,5-furandicarboxylic acid, 18.0 grams (0.3mol) of ethylene glycol, and add 87 mg of samarium trifluoromethanesulfonate (accounting for the total amount of dicarboxylic acid monomers) 0.15% of 0.15%), under a nitrogen atmosphere, esterify at 180°C for 105 minutes to obtain an esterified product; Hours, yellow poly(ethylene glycol 2,5-furandicarboxylate-co-2,5-diethylene glycol furandicarboxylate-co-2,5-triethylene glycol furandicarboxylate) was obtained. for PPEGF.

[0126] The furyl polyether ester copolymer prepared in Example 1 of the present invention was characterized, and the PPEGF copolyester was subjected to nuclear magnetic resonance analysis using deuterated trifluoroacetic acid as a solvent.

[0127] see figure 1 , figure 1 The proton nuclear magnetic resonance spectrum of the furanyl polyether ester copolyester prepared for Example 1 of the present invention. Depend on figure 1 It can be seen that the PPEGF cop...

Embodiment 2

[0135] In the reactor, add 15.6 grams (0.1mol) of 2,5-furandicarboxylic acid, 18.0 grams (0.3mol) of ethylene glycol, and add 72 milligrams of scandium trifluoromethanesulfonate (accounting for the total amount of dicarboxylic acid monomers) 0.15% of 0.15%), under a nitrogen atmosphere, esterify at 180°C for 105 minutes to obtain an esterified product; Hours, a yellow PPEGF copolymer was obtained.

[0136] Using deuterated trifluoroacetic acid as a solvent, the PPEGF copolyester is subjected to nuclear magnetic resonance analysis, the ratio of the ethylene glycol segment in the PPEGF copolyester structure to the glycol segment is 1:1, and the glycerol segment in the structure is Alcohol segments include diethylene glycol and triethylene glycol.

[0137] The PPEGF copolyester was dissolved in a mixed solvent of phenol and tetrachloroethane with a mass ratio of 1:1 at 25° C. to measure its intrinsic viscosity, and its intrinsic viscosity was 1.01 dL / g.

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Abstract

The invention provides a preparation method of a polyether ester copolymer. The preparation method comprises the following steps: carrying out an esterification reaction on 2,5-furandicarboxylic acidand ethylene glycol under the conditions of a protective atmosphere and a metal complex catalyst, and then, carrying out a pre-polycondensation reaction and a polycondensation reaction to obtain the polyether ester copolymer. A high-viscosity furfuran full-bio-based polyether ester copolymer with a novel structure can be efficiently prepared at relatively low temperature and within relatively short time by directly carrying out the polycondensation reaction on FDCA and bio-based ethylene glycol under the catalysis of the metal complex catalyst by using a simple synthesis means, a molecule of the furfuran bio-based polyether ester copolymer contains oligomeric glycol chain segments with controllable content, and the preparation method is stable in reaction process, easy to control, mild inconditions, economic, environment-friendly and suitable for large-scale industrial production. The furfuran bio-based polyether ester copolymer provided by the invention contains high-content glycol chain segments in a product structure so as to have relatively good thermodynamic properties and product colors and luster.

Description

technical field [0001] The invention belongs to the technical field of furan-based polyether ester synthesis, and relates to a preparation method of a polyether-ester copolymer and a polyether-ester copolymer, in particular to a preparation method of a furan-based polyether-ester copolymer and a novel furan-based polyether-ester copolymer. Polyetherester copolymer. Background technique [0002] 2,5-furandicarboxylic acid (FDCA), the chemical formula is C 6 h 4 o 5 , the structural formula is As an important derivative of furan, its bio-based polymer aromatic ring monomer with a "rigid" planar structure can be polymerized with monomers such as diols and diamines to prepare new bio-based polymer synthetic materials with excellent performance. It is an important chemical raw material and organic chemical intermediate. [0003] At present, with the wide application of polyester products, the rapid development of the polyester raw material industry has been driven. Among t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/84C08G63/85
CPCC08G63/672C08G63/84C08G63/85
Inventor 周光远王瑞姜敏王国强张强
Owner 芜湖万隆新材料有限公司
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