Method for purifying furandicarboxylic acid

A technology of furandicarboxylic acid and furandicarboxylate, applied in the direction of organic chemistry and the like, can solve the problems of long reaction time, application limitation, cumbersome process, etc., and achieve the effects of reducing yellowing phenomenon, improving molecular weight, and simple process flow

Active Publication Date: 2014-08-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method needs to convert furandicarboxylic acid into acid chloride first, and then use solution polycondensation for polymerization. The process is cu

Method used

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  • Method for purifying furandicarboxylic acid
  • Method for purifying furandicarboxylic acid
  • Method for purifying furandicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Add 12 grams of sodium hydroxide, 20 grams of furandicarboxylic acid to be purified (purity 96.5%, wherein 2-carboxyfurfural content 12000ppm, acetic acid content 8000ppm) and 1 gram of activated carbon into water, fully stir to make the solid matter completely Dissolved to obtain an aqueous solution of furandicarboxylic acid salt.

[0049] (2) After filtering the furandicarboxylic acid salt aqueous solution, add concentrated hydrochloric acid to the filtrate under stirring to make the pH of the solution = 2, and obtain a solid precipitate.

[0050] (3) Filter out the solid precipitate, wash with water, and dry to obtain high-purity furandicarboxylic acid.

[0051] After testing, no impurities remain in the purified high-purity furandicarboxylic acid, and its purity is 100.0%.

Embodiment 2

[0053] The method of Example 1 was repeated. The difference is that the raw material is furandicarboxylic acid to be purified (purity 90.3%, 2-carboxyfurfural content 23000ppm, acetic acid content 9500ppm).

[0054] After testing, the purified high-purity furandicarboxylic acid has a purity of 99.9%, in which the content of 2-carboxyfurfural is 450 ppm and the content of acetic acid is 100 ppm.

Embodiment 3

[0056] (1) 100 grams of furandicarboxylic acid to be purified (purity 90.3%, wherein 2-carboxyfurfural content 23000ppm, acetic acid content 9500ppm) was mixed with 500 grams of acetic acid, and stirred for 240 minutes under heating and reflux;

[0057] (2) Filter out the solid insolubles and wash with water to obtain the purified furandicarboxylic acid.

[0058] After testing, the purified furandicarboxylic acid has a purity of 97.6%, wherein the content of 2-carboxyfurfural is 22000ppm, and the content of acetic acid is 2000ppm.

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Abstract

The invention discloses a method for purifying furandicarboxylic acid. The method comprises the steps as follows: to-be-purified furandicarboxylic acid is dissolved in water through salt forming reaction; a filter liquid is acidized after filtration; and solids obtained through precipitation is filtered out, washed and dried, and the high-purity furandicarboxylic acid is obtained. Meanwhile, in order to solve the problems that the to-be-purified furandicarboxylic acid is low in purity degree and is not suitable for the method, the invention further discloses two pre-purification methods including backflow in acetic acid and recrystallization in water. The method for purifying the furandicarboxylic acid is simple in technological process and mild in reaction condition, and does not adopt an organic agent; and the prepared high-purity furandicarboxylic acid is applied to polymerization, can effectively restrain a polymer from changing color, and simultaneously facilitates acquisition of a polymerization product with a high molecular weight.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for purifying furandicarboxylic acid Background technique [0002] With the gradual depletion of petroleum resources and the intensification of the greenhouse effect, how to strengthen the utilization of renewable biomass resources to replace non-renewable resources such as petroleum has become a hot spot. [0003] As a newly developed bio-based monomer, furandicarboxylic acid can be prepared from cellulose and hemifiber, the most productive biomass resource, and has the potential to become a large variety of bio-based monomer. Listed by the Department of Energy as one of twelve modular compounds from biomass processing. Since the chemical structure of furandicarboxylic acid is similar to that of petroleum-based monomer terephthalic acid, it can replace terephthalic acid to prepare polyester materials, thereby realizing the substitution of biomass resources for petroleu...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 吴林波徐煜韬
Owner ZHEJIANG UNIV
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