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Process for preparing 5-hydroxymethyl-furfural

A single technology of hydroxymethylfurfural, which is applied in the field of sugar synthesis of 5-hydroxymethylfurfural, can solve the problems of equipment corrosion, side reactions, environmental pollution, etc., and achieve the effect of avoiding corrosion and environmental pollution and high yield

Inactive Publication Date: 2008-10-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are a large number of side reactions during the reaction process, resulting in unnecessary by-products, which greatly limit the total amount of HMF finally obtained
At present, the reported preparation of 5-hydroxymethylfurfural mainly uses strong acid as a catalyst. This production process will not only cause equipment corrosion problems, but also cause serious pollution to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Preparation of catalyst phosphotungstic acid cesium salt

[0024] Dissolve 1 g of phosphotungstic acid in 4.1 mL of deionized water, add dropwise 0.027 g of cesium carbonate dissolved in 0.8 mL of water with stirring, and let it stand overnight, then evaporate the water to dryness. The obtained white solid is dried in a vacuum desiccator or muffle. Dry in the furnace at 300℃ for 1h to obtain cesium phosphotungstate Cs 0.5 H 2.5 PW 12 O 40 ·6H 2 O.

[0025] By adjusting the amount of cesium carbonate, other cesium phosphotungstate salts can be obtained according to the above method: CsH 2 PW 12 O 40 ·6H 2 O (0.055g cesium carbonate / 1.7mL water), Cs 1.5 H 1.5 PW 12 O 4 0.6H 2 O (0.082g cesium carbonate / 2.5mL water), Cs 2 HPW 12 O 4 O 6H 2 O (0.109g cesium carbonate / 3.3mL water), Cs 2.5 H 0.5 PW 12 O 40 ·6H 2 O (0.134g cesium carbonate / 4.1mL water), Cs 3 PW 12 O 40 ·6H 2 O (0.164 g cesium carbonate / 5 mL water).

Embodiment 2

[0026] Example 2: Preparation of catalyst phosphotungstic zinc salt

[0027] Dissolve 4.9 g of phosphotungstic acid in 21 mL of deionized water, add 0.212 g of zinc carbonate, stir until the solution is clear, evaporate the water to dryness, and dry the obtained white solid in a vacuum desiccator or in a muffle furnace at 300 °C for 1 h to obtain phosphorus Zinc tungstate salt ZnHPW 12 O 40 ·6H 2 O.

Embodiment 3

[0029] In a three-necked flask equipped with a thermometer and electromagnetic stirring, 18 g of fructose, 1 g of phosphotungstic acid, and 25 mL of dimethyl sulfoxide were added, nitrogen was replaced three times, and the reaction was carried out at 100° C. for 6 h. The reaction solution was poured into water, extracted with ethyl acetate, the organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, concentrated, and separated by column chromatography to obtain 2.5 g of 5-hydroxymethylfurfural with a yield of 20%.

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PUM

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Abstract

The invention relates to a preparation method for 5-hydroxymethyl furfural, which belongs to production technology of chemicals, in particular to a method for synthesizing 5-hydroxymethyl furfural (HMF) from carbohydrates by adopting a catalytic way. The method for preparing the 5-hydroxymethyl furfural uses heteropolyacid or heteropolyacid salt as a catalyst, and the 5-hydroxymethyl furfural with high purity can be obtained at a high yield by modulating the catalyst activity, choosing proper solvents, adding additives, optimizing the reaction temperature and time and improving the post treatment technologies, and the corrosion to devices and the environmental pollution can be avoided when using liquid super acids. In the system of saturated sodium chloride solution-positive butanol, the yield of the HMF can reach 70 percent under the catalysis reaction of phosphotungstic acid for 4 minutes at 175 DEG C.

Description

technical field [0001] The invention relates to a method for preparing 5-Hydroxymethylfurfural, belonging to chemical production technology, in particular to a method for synthesizing 5-Hydroxymethylfurfural (HMF) from saccharides by a catalytic method. Background technique [0002] The rising oil prices and the increasing scarcity of petroleum resources have seriously threatened the entire petroleum-based chemical industry and affected the development of the national economy. Starting from renewable biological resources, through efficient biological and chemical transformation, organic chemical intermediates with important application prospects are obtained, and a reasonable and effective way to seek for the utilization of biomass resources and the replacement of petrochemical products is to solve this problem. effective measures. [0003] 5-Hydroxymethylfurfural is an important organic chemical intermediate, which can be used to further prepare polymer materials, pharmace...

Claims

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Application Information

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IPC IPC(8): C07D307/48
Inventor 曲景平周宇涵刘欣颖邱俊杰曲丽红
Owner DALIAN UNIV OF TECH
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