Method for catalytic preparation of 5-hydroxymethyl furfural from carbohydrates

A technology of carbohydrates and hydroxymethylfurfural, applied in the direction of organic chemistry, can solve the problems of high cost, difficult recovery of catalysts, high energy consumption, etc., and achieve the effects of low cost, reduced reuse, and high yield

Inactive Publication Date: 2011-06-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of simple and convenient method for preparing HMF by six-carbon sugar or sugar-based carbohydrate, this process environment is friendly, condition is gentle, catalyst can be used repeatedly, to overcome the high cost in the prior art, high energy consumption, Disadvantages such as catalysts are not easy to recycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 1.5g of niobium hydroxide, add 20ml of prepared 1M phosphoric acid, stir at room temperature for 52h, let stand for aging for 12h, centrifuge to separate the white precipitate, then wash with water until the pH becomes neutral, dry at 60°C, grind, and then dry in vacuum In the oven at 110°C for 2h, and then in a muffle furnace, slowly raise the temperature to 300°C for 3h activation, to obtain the desired catalyst, which is a phosphoric acid-treated niobium oxide catalyst.

[0024] Take the niobium oxide catalyst 0.01g obtained after phosphoric acid treatment, glucose 1.2g, add 20ml water and 30ml methyl isobutyl ketone, seal, react at 160°C for 30min, filter the reaction solution to separate the catalyst, and remove the catalyst. The liquid was detected by high performance liquid chromatography, and the yield of HMF was measured to be 78%.

Embodiment 2

[0026] Take 1g of niobium pentachloride and dissolve it in 10ml of anhydrous methanol. After it dissolves, add 0.2g of zirconium oxychloride, add ammonia water dropwise under stirring to adjust the pH to neutral, continue stirring for 4h, and let it stand for aging for 12h. Wash with water until there is no chloride ion, dry the obtained precipitate at 60°C for 2 hours, activate and roast at 500°C to obtain ZrO / Nb with a loading capacity of 20%. 2 o 5 . It was characterized and verified by XPS.

[0027] Take 0.1 g of the catalyst, 2 g of fructose, add 20 ml of water, 30 ml of butanol, and react at 160° C. for 60 min. The reaction solution is filtered to separate the catalyst. The sample is detected by high performance liquid chromatography, and the yield of HMF is 69%.

Embodiment 3

[0029] Take 0.2g of niobium chloride, add 20ml of absolute ethanol, after it dissolves, add 2g of silicon dioxide, stir for 3 hours, let it stand for 5 hours, filter to obtain the precipitate, wash with water until it does not contain chloride ions, then dry, and roast at 450°C to obtain 10% Nb loading 2 o 5 / SiO 2 .

[0030] Take 0.1 g of the above catalyst, 1.4 g of fructose, 10 ml of water, and 40 ml of methyl isobutyl ketone, put them in an autoclave, stop the reaction at 160° C. for 45 minutes, take out a sample, and detect that the yield of HMF is 82%.

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PUM

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Abstract

The invention relates to a niobium-containing compound catalyst for efficiently converting carbohydrates into 5-hydroxymethyl furfural, which has high activity and selectivity for preparing hydroxymethyl furfural (HMF) by dehydrolyzing saccharides and is an ideal catalyst for preparing HMF. When the reaction is performed under moderate conditions, the target product HMF can have a high yield. The catalyst is environment-friendly, is easy to separate and recycle, can be reused, is convenient and practical to operate, and can not corrode the equipment, thereby being an ideal solid acid catalyst for preparing HMF, and having significant industrial application meanings.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural (HMF) by a high-efficiency solid acid catalyst, that is, a solid acid catalyst is used to efficiently convert biomass sugar sources (six-carbon sugar or biomass rich in six-carbon sugar), and the catalyst can be recycled Repeated use, no corrosion to equipment, green and environmental protection, has strong industrial application significance. Background technique [0002] 5-Hydroxymethylfurfural (HMF) is an important furyl compound. Because its molecule contains active groups aldehyde and hydroxymethyl, its properties are relatively active, and it can be used as an intermediate for the preparation of many materials and chemicals. It is expected to become a new platform compound. Moreover, HMF is a key intermediate between biomass chemistry and petroleum-based chemistry, and HMF is prepared from biomass as a raw material and then converted into liquid fuel 2,5-dimethylfuran or alk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46B01J23/20
Inventor 杜昱光杨凤丽刘启顺程受衔白雪芳赵静玫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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