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Method for preparing poly-1,6-hexanediol 2,5-furandicarboxylate from biomass

A technology for furandicarboxylic acid and hexylene glycol ester is applied in the field of preparing poly-2,5-furandicarboxylic acid-1,6-hexanediol ester by utilizing biomass, which can solve the problems of poor selectivity and low catalytic activity, and achieves the The effect of low cost, improved stability and improved yield

Active Publication Date: 2020-07-14
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Non-precious metal catalysts have problems such as low catalytic activity and poor selectivity.

Method used

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  • Method for preparing poly-1,6-hexanediol 2,5-furandicarboxylate from biomass
  • Method for preparing poly-1,6-hexanediol 2,5-furandicarboxylate from biomass
  • Method for preparing poly-1,6-hexanediol 2,5-furandicarboxylate from biomass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol of HMF and 15mmol of potassium ferrate into the round bottom flask, measure 10mL of deionized water into the beaker, stir evenly, and weigh a certain amount of NaOH , so that the molar concentration in the reaction system is 1.6mol / L, weigh a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.4mol / L. After reacting at 25°C for 15 minutes, the solution is in the form of slurry. The slurry is filtered to obtain the filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until there is a large amount of white Precipitation was formed, the obtained turbid solution was filtered, and the substance was baked in an oven at 50° C. for 24 hours to obtain a dry white product FDCA with a yield of 86.1%.

Embodiment 2

[0056] Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol of HMF and 15mmol of potassium ferrate into the round bottom flask, measure 10mL of deionized water into the beaker, stir evenly, and weigh a certain amount of NaOH , so that the molar concentration in the reaction system is 1.6mol / L, weigh a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.4mol / L, weigh a certain amount of Fe(OH) 3 cocatalyst so that its molar concentration in the reaction system is 0.001mol / L; after reacting at 25°C for 15 minutes, the solution is in the form of a slurry, and the slurry is filtered to obtain a filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until A large amount of white precipitate was formed, and the obtained turbid solution was filtered, and the material was dried in an oven at 50° C. for 24 hours, and the yield of the dry white product FDCA was 91.7%.

Embodiment 3

[0058] Place the round bottom flask in a constant temperature magnetic stirring water bath, weigh 1mmol of HMF and 15mmol of potassium ferrate into the round bottom flask, measure 10mL of deionized water into the beaker, stir evenly, and weigh a certain amount of NaOH , so that the molar concentration in the reaction system is 1.6mol / L, weigh a certain amount of K 2 HPO 4 , so that the molar concentration in the reaction system is 0.4mol / L, weigh a certain amount of MnO 2 Cocatalyst, so that the molar concentration in the reaction system is 0.001mol / L. After reacting at 25°C for 15 minutes, the solution is in the form of slurry. The slurry is filtered to obtain the filtrate, and concentrated hydrochloric acid is added dropwise to the filtrate until there is a large amount of A white precipitate was formed, and the obtained turbid solution was filtered, and the substance was dried in an oven at 50° C. for 24 hours, and the yield of the dry white product FDCA was 88.5%.

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Abstract

The invention relates to technologies of polyester preparation by means of biomass, and provides a method for preparing polyhexylene 2,5-furandicarboxylate (PHF) by means of biomass. The method comprises the steps that 1,6-HDO and FDCA are subjected to esterification reaction to generate oligomer, through condensation polymerization, high polymer is obtained, and through purification, a product PHF is obtained; the FDCA is obtained by using potassium ferrate as a catalyst for catalyzing an oxidized woody biomass based platform chemical compound HMF. According to the method, the FDCA and the 1,6-HDO are used as raw materials, and both the FDCA and the 1,6-HDO are environmentally friendly and come from the biomass, so that green and economic preparation of the PHF is achieved; the method hasthe advantages of being low in catalyst cost, environmentally friendly and pollution-free; the reaction system of a catalyst promoter and the potassium ferrate / sodium hydroxide / dipotassium phosphategenerates a synergistic effect, so that the yield of the FDCA is improved; butyl titanate can not only be used as a catalyst of the esterification reaction, but also be used as a catalyst of condensation polymerization, so that one-time adding in a reaction process is achieved, experimental operation is made simple, convenient and safe, and the synthesis efficiency is high.

Description

technical field [0001] The invention relates to the technology of preparing polyester from biomass, in particular to a method for preparing poly-1,6-hexanediol 2,5-furandicarboxylate by utilizing biomass. Background technique [0002] As an important part of the development of the national economy, the polyester industry's benign development will be of great significance to the sustainable and healthy development of society. Since the industrial revolution, countries around the world have used petroleum resources in large quantities. With the gradual depletion of non-renewable petroleum resources and the increasing price of the world, the traditional petroleum-based polyester industry is facing great challenges. Therefore, it is extremely important to research and develop renewable polyester materials to gradually replace traditional petroleum-based polyesters. [0003] In recent years, the research and industrialization of bio-based polyesters prepared from low-cost biomas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672C08G63/85
CPCC08G63/672C08G63/85
Inventor 张俊华谢文兴梁启迪
Owner ZHEJIANG SCI-TECH UNIV
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