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Method for catalyzing carbohydrate to prepare 5-(hydroxymethyl) furfural (5-HMF) and levulinic acid (LA)

A carbohydrate, hydroxymethyl furfural technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of carboxylate and other directions, can solve the problems of high energy consumption, high cost, difficult catalyst recovery and the like, and achieve high yield , low cost, large-scale industrialization prospects and the effect of strategic significance

Active Publication Date: 2014-12-24
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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  • Method for catalyzing carbohydrate to prepare 5-(hydroxymethyl) furfural (5-HMF) and levulinic acid (LA)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 2.44g of ammonium metatungstate in 20ml of deionized water. After the ammonium metatungstate is completely dissolved, slowly add 5g of tantalum chloride to the ammonium metatungstate solution dropwise, stir at room temperature for 48 hours, and age for 12 hours. ℃ and 110℃ drying, 300℃ activation for 3 hours. The catalyst obtained above was used to catalyze the fructose reaction in a two-phase system composed of water and 2-butanol at 180 ° C, and the reaction liquid after removing the catalyst was detected by high performance liquid chromatography, and the yields of LA and HMF were 86% and 8% respectively .

Embodiment 2

[0026] Take 1.35g of metatungstic acid, dissolve it in water, add 5ml of tantalum ethoxide, stir at room temperature for 52h, let stand for aging for 12h, dry at 65°C, then put it in a vacuum drying oven at 110°C for 2h, then slowly raise the temperature to 300°C in a muffle furnace After activation at ℃ for 3 hours, the desired catalyst can be obtained, which is a tungsten-tantalum catalyst.

[0027] Take 0.01g of the above catalyst (5% tungsten trioxide content), 1.2g of glucose, add 20ml of water and 30ml of methyl isobutyl ketone, seal, react at 160°C for 30min, filter the reaction solution to separate the catalyst, remove the catalyst The reaction solution was detected by high performance liquid chromatography, and the yields of LA and HMF were measured to be 85% and 8%.

Embodiment 3

[0029] Take 1g of tungsten chloride and dissolve it in water. After it dissolves, add 5g of tantalum hydroxide, continue to stir at room temperature for 4h, let it stand for aging for 12h, wash it with water until it does not contain chloride ions, and dry the obtained precipitate at 60°C for 2h. It can be activated and roasted at ℃. The catalysts were characterized and verified by XPS.

[0030] Get this catalyst 0.1g, fructose 2g, add water 20ml, butanol 30ml, 160 ℃ of reaction 60min, reaction solution is filtered to separate catalyst, sample is detected by high performance liquid chromatography, record LA and HMF yield is 69% and 17%. %.

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Abstract

The invention relates to a tungsten and tantalum containing catalyst for efficiently converting a carbohydrate to prepare 5-(hydroxymethyl) furfural (5-HMF) and levulinic acid (LA). The catalyst has high activity of converting the carbohydrate to prepare the HMF and the LA, is environment-friendly, is easy to separate and recover, can be reused, can not corrode equipment, has important industrial application significance and is an ideal solid acid catalyst for converting the carbohydrate.

Description

technical field [0001] The present invention relates to the method for preparing 5-hydroxymethylfurfural (HMF) and levulinic acid (LA) by high-efficiency solid acid catalyst, promptly transforms biomass sugar source (hexose or rich in hexose) with solid acid catalyst Biomass), the catalyst can be recycled and reused, has no corrosion to equipment, is green and environmentally friendly, and has strong industrial application significance. Background technique [0002] 5-Hydroxymethylfurfural (HMF) and levulinic acid (LA) are important bio-based platform compounds, a key intermediate between biomass chemistry and petroleum-based chemistry, using biomass as raw materials Preparation of HMF and LA, and then conversion into liquid fuels or bulk chemicals will be of great help to relieve the increasingly tight oil resources. It is reported that HMF can be converted into 2,5-dimethylfuran. This biofuel has better properties, such as octane number and boiling point, which are higher...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/48C07C59/185C07C51/00
Inventor 杜昱光杨凤丽刘启顺白雪芳赵静玫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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