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Preparation method of 2,5-furandicarboxylic acid

A technology of furandicarboxylic acid and hydroxymethylfurfural, which is applied in the chemical industry, can solve problems such as difficult product separation, complex acidification treatment, and reduced catalyst stability, and achieve the effects of increasing solubility, simple preparation steps, and simplified post-processing steps

Active Publication Date: 2020-04-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to provide a kind of preparation method of 2,5-furandicarboxylic acid, this method utilizes catalyst as the catalyzer of catalytic reaction, the mixed solution of water and organic solvent is used as solvent, does not add alkaline auxiliary agent, to solve the traditional In the synthesis method, an alkaline solution is used as an alkali source, which brings difficulties to product separation, and the subsequent acidification treatment is complicated; or an alkaline compound is used as a carrier, and the loss of alkaline metal ions in the circulation process reduces the stability of the catalyst.

Method used

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Examples

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preparation example Construction

[0032] The invention provides a kind of preparation method of 2,5-furandicarboxylic acid, comprising:

[0033] Under air and / or oxygen conditions, placing 5-hydroxymethylfurfural and a catalyst in a mixed solution of water and an organic solvent, and performing a catalytic oxidation reaction to obtain the 2,5-furandicarboxylic acid;

[0034] Wherein the catalyst comprises a carrier and an active component loaded on the carrier, and the active component is selected from one or more of ruthenium (Ru), palladium (Pd), platinum (Pt) and rhodium (Rh) species; the carrier is selected from activated carbon (AC), graphite (C), fullerene (C 60 ) and graphene oxide (GO) in one or more.

[0035] In some embodiments, the organic solvent is selected from tetrahydrofuran, dioxane, N,N-dimethylformamide, N,N-dimethylacetamide, N,N-dimethylsulfoxide, pyridine and one or more of acetonitrile.

[0036] In some embodiments, the volume ratio of the water and the organic solvent is 1:0.1-8, pre...

preparation example 1

[0054] The preparation of preparation example 1 catalyst Ru / AC

[0055] Mix 2g of carrier activated carbon AC, 8g of melamine with 100g of 25wt% ethanol and 75wt% water, add RuCl 3 , wherein the mass ratio of metal Ru to the carrier activated carbon AC is 0.05:1, reflux and stir treatment in a 60°C water bath for 10h, separate the treated solid, and then dry it in an oven at 120°C for 13h, and then by volume percentage, in 20%H 2 and 80% N 2 The atmosphere was reduced and calcined at 700° C. for 4 hours to obtain a catalyst Ru / AC with an active component content of 4.7 wt%.

preparation example 2

[0056] The preparation of preparation example 2 catalyst Ru / AC

[0057] Mix 2g carrier activated carbon AC, 6g biimidazole with 120g of 20wt% ethanol and 70wt% water, add RuCl 3 , wherein the mass ratio of metal Ru to the carrier activated carbon AC is 0.06:1, reflux and stir treatment in a 70°C water bath for 8h, separate the treated solid, and then dry it in an oven at 110°C for 17h, and then by volume percentage, in 30%H 2 and 70%N 2 The atmosphere was reduced and calcined at 750° C. for 3 hours to obtain a catalyst Ru / AC with an active component content of 5.6 wt%.

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Abstract

The invention provides a preparation method of 2,5-furandicarboxylic acid, which comprises the following steps: under air and / or oxygen conditions, putting 5-hydroxymethylfurfural and a catalyst intoa mixed solution of water and an organic solvent, and carrying out catalytic oxidation reaction to obtain the 2,5-furandicarboxylic acid, wherein the catalyst comprises a carrier and an active component loaded on the carrier; the active component is one or more selected from ruthenium, palladium, platinum and rhodium; the carrier is one or more selected from activated carbon, graphite, fullerene and graphene oxide. The mixed solution of water and the organic solvent is used as the solvent so that solubility of the product 2,5-furandicarboxylic acid is increased, efficient conversion of 5-hydroxymethylfurfural is achieved without adding an alkaline additive to increase the solubility, high-selectivity 2,5-furandicarboxylic acid is obtained, and the method is simple in operation method, mildin reaction condition, environmentally friendly, free of pollution and good in industrial application prospect.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing 2,5-furandicarboxylic acid. Background technique [0002] The fuels and chemicals currently required by society are mainly derived from fossil fuels, and the increase in the cost of fossil fuels, the reduction in supply, and the impact on the environment have created widespread interest in sustainable alternative energy and chemical raw materials, especially Biomass resources, which have a wide range of sources and a large proportion of carbohydrates, can produce liquid fuels and organic chemicals through processes such as selective dehydration or hydrogenation. 5-Hydroxymethylfurfural (HMF) is one of the important biomass-based platform compounds, which can be prepared by acid-catalyzed dehydration of carbohydrates such as fructose, glucose and cellulose, and 2 ,5-furandicarboxylic acid (FDCA). The molecular structure of FDCA contains aromatic rings, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/68B01J23/46B01J23/44B01J23/42
CPCC07D307/68B01J23/462B01J23/464B01J23/44B01J23/42Y02P20/584
Inventor 郑路凡孙乾辉杜泽学宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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