Method for purifying crude 2,5-furandicarboxylic acid by crystallization

A technology of furandicarboxylic acid and furanic acid, applied in directions such as organic chemistry, can solve problems such as environmental burden, and achieve the effect of improving purity

Pending Publication Date: 2019-05-07
IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Other FDCA purification methods such as salt formation will generate a lot of waste water, causing environmental burdens

Method used

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  • Method for purifying crude 2,5-furandicarboxylic acid by crystallization
  • Method for purifying crude 2,5-furandicarboxylic acid by crystallization
  • Method for purifying crude 2,5-furandicarboxylic acid by crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11

[0024] 75g of DMSO was mixed with 50g of FDCA crude product (FDCA purity 96.2wt%, FFCA content 2.12wt%) to form a mixture, and the mixture was heated to 100°C. After stirring the mixture at 100°C for 30 minutes, the mixture was cooled to room temperature at a rate of 1°C / min, and the mixture was filtered to obtain a filter cake. After washing the filter cake with DMSO, the filter cake was collected, and the filter cake was sent to an oven for drying to obtain a solid product. The purity of the product was analyzed by high performance liquid chromatography (HPLC), as shown in Table 1.

Embodiment 12

[0026]100 g of DMAC was mixed with 20 g of FDCA crude product (FDCA purity 96.2 wt%, FFCA content 2.12 wt%) to form a mixture, and the mixture was heated to 60°C. After stirring the mixture at 60°C for 30 minutes, the mixture was cooled to room temperature at a rate of 1°C / min, and the mixture was filtered to obtain a filter cake. After washing the filter cake with DMAC, the filter cake was collected, and the filter cake was sent to an oven for drying to obtain a solid product. The product purity was analyzed by HPLC, as shown in Table 1.

Embodiment 21

[0035] 100 g of DMAC was mixed with 20 g of FDCA crude product (FDCA purity 98.01 wt%, FFCA content 0.88 wt%) to form a mixture, and the mixture was heated to 60°C. After stirring the mixture at 60°C for 30 minutes, the mixture was cooled to room temperature at a rate of 1°C / min, and the mixture was filtered to obtain a filter cake. After washing the filter cake with DMAC, the filter cake was collected, and the filter cake was sent to an oven for drying to obtain a solid product. The product purity was analyzed by HPLC, as shown in Table 2.

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Abstract

Method for purifying a crude of 2,5-furandicarboxylic acid (cFDCA) by crystallization is provided. The method includes (a) mixing the cFDCA and a solvent to form a mixture, wherein the solvent includes dimethyl acetamide, acetonitrile, dimethylformamide, 2-nitropropane, N-methyl-2-pyrrolidone, or a combination thereof; (b) heating the mixture; (c) after step (b), cooling the mixture to precipitatea solid; and (dl) after step (c), filtering the mixture to collect a wet filter cake of the solid, and drying the wet filter cake to obtain purified FDCA. The purified FDCA has a higher FDCA purity than that of the cFDCA. The method for purifying a crude of 2,5-furandicarboxylic acid (cFDCA) by crystallization is simple and mild.

Description

technical field [0001] The present disclosure relates to the method of purifying the crude product of FDCA by crystallization, and more particularly to the solvent employed therefor. Background technique [0002] Biomaterials have attracted a lot of attention in recent years, among which 2,5-furandicarboxylic acid (FDCA) has the potential to replace terephthalic acid (TPA). FDCA can be polymerized with ethylene glycol (EG) to form polyester (polyethylene furanoate, PEF), but the impurity in FDCA 2-formyl-5-furancarboxylic acid (2-formyl-5-furancarboxylic acid, FFCA ) content will affect the molecular weight and color of polyester. The structure of the above FDCA is And the structure of FFCA is [0003] The existing FDCA purification methods mostly use hydrogenation or oxidation, and these methods usually require high temperature and high pressure processes. Other FDCA purification methods such as salt formation will generate a lot of waste water and cause environmenta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68
CPCC07D307/68C08G63/672
Inventor 黄英婷汪进忠陈招宏
Owner IND TECH RES INST
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