Method using 5-hydroxymethylfurfural to prepare 2,5-furandicarboxylic acid

A technology of hydroxymethyl furfural and furandicarboxylic acid is applied in the field of preparation of 2,5-furandicarboxylic acid and achieves the effects of good stability, high yield and good water resistance

Active Publication Date: 2017-05-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Therefore, the problems faced in the preparation process of 2,5-furandicarboxylic acid in the prior art: a large amount of acid-base solvents are involved in the reaction process, the product exists in the form of salt, and a series of steps are required to obtain 2,5-furandicarboxylic acid. formic acid

Method used

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  • Method using 5-hydroxymethylfurfural to prepare 2,5-furandicarboxylic acid
  • Method using 5-hydroxymethylfurfural to prepare 2,5-furandicarboxylic acid
  • Method using 5-hydroxymethylfurfural to prepare 2,5-furandicarboxylic acid

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Experimental program
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Effect test

Embodiment 1～5

[0027] Take an appropriate amount of zirconia and add it to ethanol for ultrasonic dispersion, evenly spread it on the quartz plate with a dropper, and heat it with an infrared lamp to remove the ethanol. Put the quartz wafer into the deposition chamber, the temperature of the deposition chamber is set at 280 ° C, the platinum source is trimethylcyclopentadiene platinum, the temperature of the platinum source is set at 75 ° C, nitrogen is used as the carrier gas and purification gas, and ozone is the precursor , depositing Pt with different numbers of circles (5, 10, 20, 30 and 50 circles), the Pt content detected by ICP-MS is 0.75-6.10wt%.

[0028] The catalyzed oxidation reaction of 5-hydroxymethylfurfural is carried out in a 5mL stainless steel reactor, heated in an oil bath, and magnetically stirred, and sequentially added to a 5mL stainless steel high-temperature and high-pressure reactor Reaction conditions: catalyst 10mg, raw material 5-hydroxymethylfurfural 15mg , solv...

Embodiment 6～11

[0034] Take an appropriate amount of zirconia and add it to ethanol for ultrasonic dispersion, evenly spread it on the quartz plate with a dropper, and heat it with an infrared lamp to remove the ethanol. Put the quartz wafer into the deposition chamber, the temperature of the deposition chamber is set at 280 ° C, the platinum source is trimethylcyclopentadiene platinum, the temperature of the platinum source is set at 75 ° C, nitrogen is used as the carrier gas and purification gas, and ozone is the precursor , deposited for 30 laps, and the platinum content was determined to be 3.23wt% by ICP-MS.

[0035] Reaction conditions: 10 mg of catalyst, 15 mg of raw material 5-hydroxymethylfurfural, 3 mL of solvent water, different reaction temperatures (20, 40, 60, 80, 100 and 120 °C), oxygen The pressure is 0.4Mpa, the rotation speed is 600r / min, and the reaction time is 2h. The reaction results are shown in Table 2.

[0036] Table 2, the impact of different reaction temperatures ...

Embodiment 12～15

[0041] Take an appropriate amount of zirconia and add it to ethanol for ultrasonic dispersion, evenly spread it on the quartz plate with a dropper, and heat it with an infrared lamp to remove the ethanol. Put the quartz wafer into the deposition chamber, the temperature of the deposition chamber is set at 280 ° C, the platinum source is trimethylcyclopentadiene platinum, the temperature of the platinum source is set at 75 ° C, nitrogen is used as the carrier gas and purification gas, and ozone is the precursor , deposited for 30 laps, and the platinum content was determined to be 3.23wt% by ICP-MS.

[0042] Reaction conditions: 10 mg of catalyst, 15 mg of raw material 5-hydroxymethylfurfural, 3 mL of solvent water, 100 ° C reaction temperature, different oxygen pressures (0, 0.2, 0.4 and 0.6 MPa), The rotating speed is 600r / min, the reaction time is 2h, and the reaction results are shown in Table 3.

[0043] Table 3, the impact of different oxygen pressures on the reaction re...

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Abstract

The invention relates to a method using 5-hydroxymethylfurfural to prepare 2,5-furandicarboxylic acid. The method comprises the following steps of (1) adding a catalyst carrier into an organic solvent to disperse, applying onto a quartz sheet, heating to remove the organic solvent, and using an ALD (atomic layer deposition) method to deposit a platinum source onto the catalyst carrier, so as to obtain a platinum-loaded catalyst; (2) adding the platinum-loaded catalyst obtained in step (1), 5-hydroxymethylfurfural and solvent water into a reactor, and reacting for 2 to 12h at the temperature of 20 to 100 DEG C under the oxygen atmosphere, so as to obtain the 2,5-furandicarboxylic acid. The preparation method has the advantages that the platinum-loaded catalyst is prepared by the ALD method, the good catalyzing property in a water-phase reaction system is realized, and the high-yield 2,5-furandicarboxylic acid is obtained; compared with the catalyst prepared by the traditional method, the stability is better; the water-resistant property is better, and the easiness in deactivation is avoided.

Description

technical field [0001] The invention relates to the field of preparation of 2,5-furandicarboxylic acid, in particular to a method for preparing 2,5-furandicarboxylic acid from 5-hydroxymethylfurfural. Background technique [0002] 5-Hydroxymethylfurfural is an important platform compound in sugar conversion, which can be prepared by acid-catalyzed dehydration of carbohydrates such as fructose, glucose and cellulose. Its derivatives such as 2,5-furandicarboxylic acid, 2,5-diformylfuran and levulinic acid are widely used in medicine, plastics, fuel and other fields. Among them, 2,5-furandicarboxylic acid can be prepared by selective oxidation of 5-hydroxymethylfurfural. It is an important organic compound intermediate and was listed as one of the 12 bio-based platform compounds by the US Department of Energy in 2004. [0003] 2,5-furandicarboxylic acid is considered to be an ideal bio-based substitute for terephthalic acid. Since 2,5-furandicarboxylic acid has a furan ring st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 傅杰沈金山陈皓吕秀阳欧阳平凯
Owner ZHEJIANG UNIV
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