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Preparation method and application of bottle-grade bio-based 2, 5-furandicarboxylic acid-based copolyester

A technology of furandicarboxylic acid-based copolyester and furandicarboxylate, which is applied in the field of polyester preparation, can solve the problems of long polycondensation time and low intrinsic viscosity of polyester, achieve small steric hindrance effect, increase molecular weight and viscosity, The effect of shortening the final polycondensation time

Active Publication Date: 2020-08-11
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the problems that the intrinsic viscosity of polyester is not high, the polycondensation time is long, and the obtained polyester product needs to undergo solid-phase viscosification to reach the intrinsic viscosity of bottle flakes in the current research process of furyl polyester. , proposed a bottle-grade bio-based 2,5-furandicarboxylic acid-based copolyester preparation method and its application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: A kind of preparation method of bottle grade bio-based 2,5-furandicarboxylate copolyester comprises the following preparation steps:

[0036] (1) Add dimethyl adipate and sorbitol with a molar ratio of 5:1 into the reactor and stir evenly, add 1-butyl-3-methylimidazole lactate ionic liquid (accounting for 20% of sorbitol content) 0.05mol%) as a catalyst, under nitrogen protection atmosphere, carry out transesterification reaction at 98 ° C, the small molecule content to be distilled reaches more than 95% of the theoretical value, the reaction is completed, and the reaction solution is prepared;

[0037] (2) Mix 2,5-furandicarboxylate and ethylene glycol uniformly at a molar ratio of 1:1.8, and then add tetrabutyl titanate with a content of 0.05mol% relative to the molar mass of 2,5-furandicarboxylate The phosphoric acid of ester, 0.003wt% and the antioxidant 1010 of 0.002wt% carry out one-stage transesterification reaction under the condition of 190 ℃ and ...

Embodiment 2

[0040] Embodiment 2: a kind of preparation method of bottle flake grade bio-based 2,5-furandicarboxylate copolyester, comprising the following preparation steps:

[0041] (1) Add dimethyl adipate and sorbitol with a molar ratio of 8:1 into the reactor and stir evenly, add 1-butyl-3-methylimidazole lactate ionic liquid (accounting for 20% of sorbitol content) 0.08mol%) as a catalyst, under nitrogen protection atmosphere, carry out transesterification reaction at 95°C, the small molecule content to be distilled reaches more than 95% of the theoretical value, and the reaction is completed, and the reaction solution is prepared;

[0042] (2) Mix 2,5-furandicarboxylate and ethylene glycol uniformly at a molar ratio of 1:1.8, and then add tetrabutyl titanate with a content of 0.05mol% relative to the molar mass of 2,5-furandicarboxylate The phosphoric acid of ester, 0.003wt% and the antioxidant 1010 of 0.002wt% carry out one-stage transesterification reaction under the condition of ...

Embodiment 3

[0045] Embodiment 3: a kind of preparation method of bottle grade bio-based 2,5-furandicarboxylate copolyester, comprising the following preparation steps:

[0046] (1) Add dimethyl adipate and sorbitol with a molar ratio of 7:1 into the reactor and stir evenly, add 1-butyl-3-methylimidazole lactate ionic liquid (accounting for 20% of sorbitol content) 0.1mol%) as a catalyst, under nitrogen protection atmosphere, carry out transesterification reaction at 102°C, the small molecule content to be distilled reaches more than 95% of the theoretical value, and the reaction is completed, and the reaction solution is prepared;

[0047] (2) Mix 2,5-furandicarboxylate and ethylene glycol uniformly at a molar ratio of 1:1.6, and then add tetraisotitanate with a content of 0.08mol% relative to the molar mass of 2,5-furandicarboxylate Octyl ester, 0.001wt% polyphosphoric acid and 0.005wt% antioxidant 618 were subjected to a primary transesterification reaction at 190°C and 150kPa until the...

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Abstract

The invention discloses a preparation method of bottle-grade bio-based 2, 5-furandicarboxylic acid-based copolyester, and relates to the technical field of polyester preparation. The preparation method comprises the following preparation steps: (1) adding sorbitol, dimethyl adipate and an ionic liquid catalyst into a reactor for transesterification to prepare a reaction solution; (2) adding 2, 5-furandicarboxylate, aliphatic diol, a catalyst, a stabilizer and an antioxidant into a reactor for a primary ester exchange reaction, and then adding the reaction liquid for a secondary ester exchangereaction to prepare an esterification liquid; (3) carrying out a pre-polycondensation reaction on the esterification liquid to obtain a prepolymer; (4) carrying out final polycondensation reaction onthe prepolymer to obtain bottle-grade bio-based 2, 5-furandicarboxylic acid-based copolyester. The dimethyl adipate and sorbitol esterification oligomer is used as a crosslinking center, and a micro-crosslinking structure is constructed in the molecular chain so that the final polycondensation time is greatly shortened, the molecular weight of the copolyester is improved, and the performance of the copolyester is improved.

Description

technical field [0001] The invention relates to the technical field of polyester preparation, in particular to a preparation method and application of bottle flake grade bio-based 2,5-furandicarboxylate copolyester. Background technique [0002] In recent years, with the depletion of petroleum resources, people have paid great attention to renewable biomass resources, especially furan aromatic monomers. 2,5-furandicarboxylic acid is mainly derived from biomass materials such as fructose, cellulose and plant straw, and its molecular structure is similar to that of terephthalic acid. It is known as the most promising biomass monomer to replace terephthalic acid in the future. At the same time, many researchers have studied 2,5-furandicarboxylic acid-based polymers, and successively synthesized polyethylene 2,5-furandicarboxylate (PEF), poly(trimethylene 2,5-furandicarboxylate) ( PPF) and polybutylene 2,5-furandicarboxylate (PBF), etc. Compared with terephthalic acid-based po...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/672C08G63/668
CPCC08G63/78C08G63/672C08G63/668C08G2390/00Y02P20/54
Inventor 张婉迎胡宇苗徐锦龙王松林
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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