Preparation method of 2, 5-furandicarboxylic acid-based block copolyester

A technology of furandicarboxylic acid block and furandicarboxylic acid, which is applied in the field of polyester preparation, can solve the problems of the original performance decline of PEF copolyester, and achieve the effect of excellent thermodynamic performance, good hue, and simple and easy preparation method

Inactive Publication Date: 2020-07-28
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the brittleness of PEF obtained by the current synthesis process, and to introduce a dibasic acid or a diol monomer containing a flexible segment or a symmetrical rigid structure for copolymerization and modification to obtain the original properties of the PEF copolyester There will be problems such as decline in different degrees, and a preparation method of 2,5-furandicarboxylic acid-based block copolyester with excellent performance is proposed

Method used

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  • Preparation method of 2, 5-furandicarboxylic acid-based block copolyester

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: a kind of preparation method of 2,5-furandicarboxylate block copolyester, comprises following preparation steps:

[0031] 1) Mix 100g of 2,5-furandicarboxylic acid, 64g of ethylene glycol, 0.1g of catalyst, and 0.1g of stabilizer, and carry out esterification reaction at 195°C to prepare esterified product A;

[0032] 2) Mix 160g of 2,5-furandicarboxylic acid and 146g of thionyl chloride, and react at 60°C for 2 hours to prepare a halogenated furandicarboxylic acid;

[0033]3) Put 195g of furandicarboxylic acid halide, 161g of tetrahydrofuran dimethanol, 0.1g of isopropyl titanate and 0.1g of heat stabilizer 425 in the reaction kettle at room temperature and stir for 1 hour, stir evenly, then raise the temperature to 140°C within 1 hour, and Carry out esterification reaction under protective gas atmosphere to prepare esterified compound B;

[0034] 4) Insulate the esterified product B at 200°C and 1 Pa for 1 hour for precondensation reaction to prepare a ...

Embodiment 2

[0036] Embodiment 2: a kind of preparation method of 2,5-furandicarboxylate block copolyester, comprises following preparation steps:

[0037] 1) Mix 118g dimethyl 2,5-furandicarboxylate, 64g ethylene glycol, 0.1g catalyst, and 0.1g stabilizer, and carry out esterification reaction at 190°C to prepare esterified product A;

[0038] 2) Mix 200g of 2,5-furandicarboxylic acid and 320g of dibromothionyl sulfoxide, and incubate at 80°C for 1 hour to prepare the halogenated furandicarboxylic acid;

[0039] 3) Put 430g of furandicarboxylic acid halides, 275g of tetrahydrofuran dimethanol, 0.1g of stannous octoate and 0.1g of triethyl phosphite in the reaction kettle and stir for 2 hours at room temperature. Stir evenly, and then heat up to 160°C within 1.5 hours. Carry out esterification reaction under protective gas atmosphere to prepare esterified compound B;

[0040] 4) Insulate the esterified product B at 210°C and 200pa for 0.5h for precondensation reaction to prepare a prepoly...

Embodiment 3

[0042] Embodiment 3: a kind of preparation method of 2,5-furandicarboxylate block copolyester, comprises the following preparation steps:

[0043] 1) Mix 100g of 2,5-furandicarboxylic acid, 64g of ethylene glycol, 0.1g of catalyst, and 0.1g of stabilizer, and carry out esterification reaction at 200°C to prepare esterified product A;

[0044] 2) Mix 250g of 2,5-furandicarboxylic acid and 229g of thionyl chloride, and react at 70°C for 1.5h to prepare a halogenated furandicarboxylic acid;

[0045] 3) Put 306g of furandicarboxylic acid halides, 337g of 2,5-furandimethanol, 0.1g of magnesium acetate and 0.1g of diphenyltridecyl phosphite in the reactor at room temperature and stir for 1.5h, stir evenly, and then heat up within 1.3h To 150°C, carry out the esterification reaction under the protective gas atmosphere, and prepare the esterified compound B;

[0046] 4) The esterified product B was incubated at 205°C and 100pa for 0.7h for precondensation reaction to prepare a prepol...

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Abstract

The invention discloses a preparation method of 2, 5-furandicarboxylic acid-based block copolyester, and relates to the technical field of polyester preparation. The preparation method comprises the following preparation steps of: 1) mixing 2, 5-furandicarboxylic acid and/or ester thereof, dihydric alcohol, a catalyst and a heat stabilizer for an esterification reaction to obtain an ester A; 2) mixing 2, 5-furandicarboxylic acid and thionyl dihalide for a reaction to obtain a furandicarboxylic acid halide; 3) performing an esterification reaction among the furandicarboxylic acid halide, bio-based rigid cyclic diol, a catalyst and a heat stabilizer to obtain an ester B; 4) carrying out a pre-polycondensation reaction on the ester B to obtain a prepolymer; and 5) mixing the prepolymer and the ester A prepared in the step 1) to carry out polycondensation to obtain the 2, 5-furandicarboxylic acid-based block copolyester. The method provided by the invention is simple and feasible, is suitable for industrial production, and the product has good toughness, good hue and excellent thermodynamic properties, and can be widely applied to the fields of packaging, fibers and the like.

Description

technical field [0001] The invention relates to the technical field of polyester preparation, in particular to a preparation method of 2,5-furandicarboxylate block copolyester. Background technique [0002] Bio-based polymers refer to polymers converted from bio-based resources as raw materials, as opposed to petroleum-based polymers. As a solution to the shortage of fossil resources, using renewable biomass resources to synthesize various chemicals (including monomers and polymers) and energy is a new direction for the development of the chemical industry (including the polymer industry) and the energy industry. At present, bio-based polymer materials are mainly concentrated in polylactic acid (PLA), polyhydroxy fatty acid (PHA), polyglycolic acid (PGA), butylene adipate and terephthalate (PBAT), poly Butylene succinate (PBS), due to the lack of rigid aromatic ring structure in these bio-based polymer materials, its mechanical properties (such as strength, modulus, etc.) a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/78
CPCC08G63/672C08G63/78
Inventor 胡宇苗徐锦龙王松林董海良
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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