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Preparation and application of a supported gold catalyst for the oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid

A technology of hydroxymethyl furfural and furandicarboxylic acid, which is applied in the field of supported gold catalysts, can solve the problems of toxic by-products, low atom utilization rate, large consumption of oxidants, etc., and achieves environmentally friendly, high utilization efficiency and high catalytic activity. Effect

Active Publication Date: 2021-09-24
INNER MONGOLIA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Potassium permanganate, potassium dichromate or high-valent lead compounds are generally used as oxidants in the traditional oxidation process, which is a metered oxidation reaction that requires a large amount of oxidant consumption, low atomic utilization, and produces a large number of toxic by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] (1) Prepare the carrier. Weigh 6.5133g of cerium nitrate hexahydrate (AR) and dissolve it in 50mL of absolute ethanol, slowly add 2.8818g of citric acid complexing agent under stirring, put it in a water bath at 60°C, keep stirring for 3 hours after the temperature stabilizes, and then Let cool for 30 minutes. The mixed solution was rotary evaporated to dryness at 50°C, and then dried at 100°C to obtain a bulky solid. Put the obtained solid into a muffle furnace, heat up to 500°C at a rate of 2°C / min, bake at 500°C for 2 hours, then cool to room temperature naturally, take out the solid and grind it into powder to obtain CeO 2 oxide carrier.

[0013] (2) Preparation of supported gold catalyst. According to the mass fraction of the gold component in the catalyst being 1%, weigh 0.0213g of chloroauric acid and dissolve it in 50mL of secondary water, adjust the pH to 5.92 with NaOH solution, put it in a water bath at 60°C, and slowly add 0.6g of it under stirring Carri...

Embodiment 2

[0015] (1) Prepare the carrier. Weigh 8.0930g of zirconyl nitrate (AR) and dissolve it in 50mL of absolute ethanol, slowly add 6.725g of citric acid complexing agent under stirring, put it in a water bath at 60°C, keep stirring for 3 hours after the temperature stabilizes, and then cool at room temperature 30 minutes. The mixed solution was rotary evaporated to dryness at 50°C, and then dried at 100°C to obtain a bulky solid. Put the obtained solid into a muffle furnace, heat up to 500°C at a rate of 2°C / min, bake at 500°C for 2 hours, then cool naturally to room temperature, take out the solid and grind it into powder to obtain ZrO 2 oxide carrier.

[0016] (2) Preparation of supported gold catalyst. According to the mass fraction of the gold component in the catalyst being 1%, weigh 0.0213g of chloroauric acid and dissolve it in 50mL of secondary water, adjust the pH to 5.92 with NaOH solution, put it in a water bath at 60°C, and slowly add 0.6g of it under stirring Carr...

Embodiment 3

[0018] (1) Prepare the carrier. Weigh 7.8160g of cerium nitrate (AR) hexahydrate and 0.4625g of zirconyl nitrate (AR) and dissolve it in 50mL of absolute ethanol, slowly add 3.8424g of citric acid complexing agent under stirring, put it in a water bath at 60°C, and the temperature is stable Stirring was continued for 3 hours, then cooled at room temperature for 30 minutes. The mixed solution was rotary evaporated to dryness at 50°C, and then dried at 100°C to obtain a bulky solid. Put the obtained solid into a muffle furnace, heat up to 500°C at a rate of 2°C / min, bake at 500°C for 2 hours, then cool naturally to room temperature, take out the solid and grind it into powder to obtain Ce 0.9 Zr 0.1 o 2 Composite oxide carrier.

[0019] (2) Preparation of supported gold catalyst. According to the mass fraction of the gold component in the catalyst being 1%, weigh 0.0213g of chloroauric acid and dissolve it in 50mL of secondary water, adjust the pH to 4.91 with NaOH solution...

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Abstract

The invention relates to the preparation and application of a loaded gold catalyst used for oxidizing 5-hydroxymethylfurfural to synthesize 2,5-furandicarboxylic acid. The support of the supported gold catalyst is CeO 2 Oxide, ZrO 2 Oxide or different ratio of Ce x Zr 1‑x O composite oxide (X value is 0.7-0.9), the mass fraction of the carrier is 97%-99.5%, and the mass fraction of the gold component is 0.5%-3%. The gold content in the supported gold catalyst is low, the utilization efficiency is high, the carrier raw material is cheap and easy to obtain, and the overall preparation process of the catalyst is simple. The supported gold catalyst is used to catalyze the oxidation of 5-hydroxymethylfurfural to synthesize 2,5-furandicarboxylic acid, the reaction conditions are mild, the environment is friendly, the catalytic activity is high, and the ratio of Ce and Zr in the carrier is adjusted And the pH value in the loading process of the active gold component can effectively regulate the selectivity of 2,5-furandicarboxylic acid. When the reaction temperature is 70-100°C, the oxygen pressure is 0.5-1.5MPa, and the reaction time is 2-4 hours, the conversion rate of 5-hydroxymethylfurfural can reach 100%, and the selectivity of 2,5-furandicarboxylic acid can be improved. Reached 97.3%.

Description

technical field [0001] The invention relates to the preparation and application of a loaded gold catalyst used for oxidizing 5-hydroxymethylfurfural to synthesize 2,5-furandicarboxylic acid. Background technique [0002] Biomass resources have the advantages of abundant sources, low price, green environmental protection, and renewability, and are ideal substitutes for fossil resources. 5-Hydroxymethylfurfural is a biomass platform compound obtained by catalytic oxidation conversion of biomass carbohydrates, which can undergo oxidation, reduction, polymerization, hydrolysis and other reactions to generate a series of products. Among them, 2,5-furandicarboxylic acid, the oxidation product of 5-hydroxymethylfurfural, is an important intermediate of biopolymers, fine chemicals and medicines. And 2,5-furandicarboxylic acid has a similar structure to terephthalic acid, so it is considered to be a promising bio-based polyester monomer, which can replace the traditional petroleum-b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/66C07D307/68
CPCB01J23/002B01J23/66C07D307/68
Inventor 郝剑敏闫广飞韩利民王金耀褚福敏
Owner INNER MONGOLIA UNIV OF TECH
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