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Preparation method of polyester containing furan ring

A furan ring and polyester technology, applied in the field of polyester preparation, can solve problems such as multiple side reactions, metal residues, complex synthesis, etc., and achieve the effects of accelerating the speed of the prepolymerization reaction, the synthesis method being simple, and making up for the interference of the reverse reaction.

Active Publication Date: 2020-06-05
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention provides pyridine hydrohalide as a catalyst to prepare polyester polymer compounds based on furan ring-containing compounds, so as to solve the problems of cumbersome process, complex synthesis, metal residues and frequent side reactions in the prior art.

Method used

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  • Preparation method of polyester containing furan ring
  • Preparation method of polyester containing furan ring
  • Preparation method of polyester containing furan ring

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060]In the three-necked flask, N2 was pumped three times, the temperature was slowly increased, and the stirring was continued. 90ml of 7 and 88ml of 10 (1:1) were added in a nitrogen-filled state, and 2.5g (1% wt) of 3 was added, and the reaction system was closed. , then heated to 180°C, and after 1.5 hours of reaction, nitrogen was flowed into the reaction system to make the small molecules evaporate with nitrogen. After the small molecules were evaporated, the system was sealed again, and then the temperature was raised to 230°C, and the reaction was continued. 3h, pumped air for 0.5h under 0.5mbar vacuum, stopped heating and stirring, cooled to room temperature with nitrogen, took out the product and washed the surface small molecules and oligomer residues with ethanol, and dried under vacuum to obtain white furan polymer. The ester solid was 216 g, and the yield was 88.0%.

Embodiment 2

[0062] In the three-necked flask, N2 was pumped for three times, the temperature was slowly increased, and the stirring was continued. 100ml of 8 and 166ml of 11 (1:1.2) were added under nitrogen, and 1.4g (0.5% wt) of 5 was added, and the reaction system was closed. , then heated to 170°C, after 1.5h of reaction, nitrogen was flowed into the reaction system to make small molecules evaporate with nitrogen gas, after the small molecules were evaporated, the system was sealed again, and then the temperature was raised to 250°C, and the reaction was continued for 2h , pumped air for 0.5h under 0.5mbar vacuum, stopped heating and stirring, ventilated and cooled to room temperature, took out the product and washed the surface small molecules and oligomer residues with ethanol, and dried under vacuum to obtain light yellow furan polyester solid 235g, 82.1% yield.

Embodiment 3

[0064] In the three-necked flask, N2 was pumped for three times, the temperature was slowly raised, and the reaction system was closed. , then heated to 180°C, after the reaction for 2h, the small molecules were evaporated, the system was sealed again, then the temperature was raised to 240°C, the reaction was continued for 2.5h, and the air was pumped for 0.5h under a vacuum of 0.5mbar, and the heating and stirring were stopped. The mixture was ventilated and cooled to room temperature, and the product was taken out and washed with ethanol to remove surface small molecules and oligomer residues. After drying in vacuum, 357 g of light yellow furan polyester solids were obtained with a yield of 84.3%.

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a preparation method of polyester containing a furan ring. The polyester containing the furan ring is synthesized by polymerizing a single-furan or double-furan compound and an aliphatic chain compound under the catalysis of pyridine halogen salt. The catalyst used in the synthesis method is green and non-toxic, the obtained polymer has no metal residue, and the synthesis method is simple, rapid, economical, wider in applicability and more suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of a furan ring-containing polyester. Background technique [0002] Since the birth of the first polymer in 1970, polymer materials have been widely used in transportation, construction, agriculture, medicine and other fields due to their excellent performance comparable to traditional materials such as metal and wood, as well as high cost performance and easy preparation. application. [0003] With the development of science and technology, polymer materials have spread all over people's daily life. Among them, polyvinyl chloride and polystyrene are difficult to degrade in nature, causing great pollution to the environment. Among them, polylactic acid, polyaliphatic lactone and Polyesters such as polycarbonate are a kind of biodegradable and bioabsorbable polymer materials, which are widely used in the biological and pharmaceutical industries. These synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/87
CPCC08G63/672C08G63/87
Inventor 郭凯李振江刘博陈恺张磊高罗玉张智浩周方园
Owner NANJING UNIV OF TECH
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