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Method for production of 5-hydroxymethylfurfural or levulinic acid from inulin biomass

A technology of hydroxymethyl furfural and levulinic acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylates, etc., can solve problems such as high energy consumption, difficult control of product 5-HMF or levulinic acid, etc. , to achieve the effect of low reaction temperature, short reaction time and high substrate concentration

Active Publication Date: 2014-11-05
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problems to be solved in the present invention are: in the existing process of preparing platform compounds with biomass as raw material, high boiling point organic solvents need to be used, the energy consumption of the product separation process is high, and the resulting product 5-HMF or levulinic acid is not easy to control, etc. The problem is to provide a catalytic reaction system that can efficiently dissolve inulin-based biomass. In this catalytic reaction system, the product can be precisely controlled to be 5-HMF or levulinic acid.

Method used

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  • Method for production of 5-hydroxymethylfurfural or levulinic acid from inulin biomass
  • Method for production of 5-hydroxymethylfurfural or levulinic acid from inulin biomass

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Prepare 30g of 32% zinc chloride aqueous solution by mass, add 5g of fructose, and react at 120°C for 2 hours.

[0024] (2) After the reaction, 75 mL of butanol was added as an extractant to extract the product 5-HMF.

[0025] (3) Concentrate and evaporate to dryness the obtained butanol phase in which the product 5-HMF is dissolved, and crystallize the obtained solid in petroleum ether-ethyl acetate (1:2 volume ratio) to obtain the 5-HMF product, 5-HMF The molar yield is 35%.

Embodiment 2

[0027] (1) Prepare 50g of zinc chloride aqueous solution with a mass percentage of 67%, add 10g of sucrose with a molecular weight of 342 to form a reaction solution, and react at 100°C for 15 minutes.

[0028] (2) After the reaction, add 120mL methyl isobutyl ketone as an extractant to extract 5-HMF.

[0029] (3) The obtained methyl isobutyl ketone phase containing the product 5-HMF was concentrated and evaporated to dryness, and the obtained solid was crystallized with benzene to obtain the 5-HMF product, and the molar yield of the 5-HMF product was 43%.

Embodiment 3

[0031] (1) Prepare 30g of zinc chloride aqueous solution with a mass percentage of 60%, add 10g of inulin with a molecular weight of 20,000 to mix, add 0.2g of SnCl 4 ·5H 2 O was used as a catalyst, and the reaction was continued at 140 °C for 8 hours.

[0032] (2) After the reaction, add 70mL of 2,5-dimethylpentanone as an extractant to extract the product levulinic acid.

[0033] (3) Concentrate the obtained 2,5-dimethylpentanone by rotary evaporation under reduced pressure, crystallize with a mixed solvent of 1,4-dioxane-ether to obtain the levulinic acid product, and the molar yield of the levulinic acid product is The rate is 55%.

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Abstract

The invention relates to a method for production of 5-hydroxymethylfurfural (5-HMF) or levulinic acid from an inulin biomass. The method includes: mixing a dry inulin biomass raw material, a zinc chloride aqueous solution and a catalyst evenly; or mixing the dry inulin biomass raw material with the zinc chloride aqueous solution uniformly, letting them react for 10min-8h at 60-140DEG C, then performing cooling to room temperature, conducting extraction on the reaction mixture by an organic extraction agent to extract 5-HMF or levulinic acid from the reaction system, then concentrating and drying the extraction agent, and conducting crystallization, thus obtaining the 5-HMF or levulinic acid product. The method provided by the invention has the advantages of accurate control of the product as 5-HMF or levulinic acid.

Description

technical field [0001] The invention belongs to a method for producing 5-hydroxymethylfurfural or levulinic acid by using inulin biomass. technical background [0002] At present, the supply of petrochemical energy in the world is becoming increasingly scarce, and at the same time, environmental pollution is becoming more and more serious, which has led to a significant increase in people's demand for renewable energy and chemicals derived from biomass resources. In the process of preparing energy substances and fine chemicals from biomass resources, 5-hydroxymethylfurfural (5-HMF) and levulinic acid are the two most common platform compound molecules, and these two compounds are recognized as linking biomass resources An important bridge between development and utilization and the fossil industry. Among them, 5-HMF is called "a sleeping giant" by the scientific and technological circles (Supercrit. Fluids, 2005, 36, 118-126.; Supercritical Fluids, 2005, 36, 118-126.). In ...

Claims

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Application Information

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IPC IPC(8): C07D307/46C07C59/185C07C51/00
CPCC07C51/00C07D307/46C07C59/185
Inventor 侯相林王英雄邓天昇贾玲玉乔岩
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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