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Method for producing hydroxymethylfurfural by using two-phase method

A technology of hydroxymethyl furfural and biomass raw materials, applied in the direction of organic chemistry and the like, can solve the problems of high cost, high boiling point, large heat of vaporization, etc., and achieve the effects of fast reaction speed, low temperature, and green process.

Active Publication Date: 2012-11-14
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

(J.AM.CHEM.SOC.2009,131,1979-1985) of Ronald T.Raines of U.S. University of Wisconsin etc. utilize N,N-dimethyl-acetamide / lithium chloride solvent system, under the effect of catalyst, Can increase the yield of cellulose to generate hydroxymethylfurfural to more than 90%, but the solvent N,N-dimethyl-acetamide used has a high boiling point, a large heat of vaporization, and excellent miscibility with most solvents, so it The separation and purification of hydroxymethylfurfural from the generated hydroxymethylfurfural is difficult and costly; since ionic liquids can dissolve a large amount of cellulose, since Haibo Zhao et al. successfully produced hydroxymethylfurfural from glucose in ionic liquids, the use of ionic liquids to produce hydroxymethylfurfural A large number of reports have emerged, however, ionic liquids are expensive, recycling is extremely difficult, and the feasibility of industrial development is extremely small

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) 40g zinc chloride, 5g concentrated hydrochloric acid and 55g water mix evenly, prepare zinc chloride reaction solution 72ml;

[0029] (2) Mix 0.5 g of dried cellulose microcrystals with 100 g of the above-mentioned zinc chloride reaction solution, use 36 ml of 2,5-dimethylpentanone as the extractant, and react at 100° C. for 160 min;

[0030] (3) The 2,5-dimethylpentanone phase obtained after the reaction was concentrated and evaporated to dryness, and crystallized with ethanol to obtain a hydroxymethylfurfural product, and the molar yield of the reaction was 43%.

Embodiment 2

[0032] (1) 45g zinc chloride, 0.1g vitriol oil and 54.9g water are mixed, prepare zinc chloride reaction solution 70ml;

[0033] (2) 10 g of dried wheat straw was mixed with 100 g of zinc chloride reaction solution, and 70 ml of 1-butanol was used as an extractant, and reacted at 110° C. for 15 h;

[0034] (3) The 1-butanol phase obtained after the reaction was concentrated and evaporated to dryness, crystallized with acetone to obtain a hydroxymethylfurfural product, and the molar yield of the reaction was 50%.

Embodiment 3

[0036] (1) 50g zinc chloride, 3g phosphoric acid and 47g water mix evenly, prepare zinc chloride reaction solution 66ml;

[0037] (2) Mix 5 g of dried rice straw with 100 g of zinc chloride reaction solution, use 180 ml of ethyl butyrate as the extractant, and react at 115° C. for 10 h;

[0038] (3) The ethyl butyrate phase obtained after the reaction was concentrated and evaporated to dryness, and the hydroxymethylfurfural product was obtained by crystallization with ethyl acetate, and the molar yield of the reaction was 36%.

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Abstract

The invention discloses a method for producing hydroxymethylfurfural by using a two-phase method. Reaction liquid is prepared by zinc chloride, catalyst and water at the mass ratio of 40-70:0.1-10:20-60; dried cellulose-contained biomass raw material and the reaction liquid are mixed at the mass ratio of 1:5-200; extractant is added to the reaction liquid to form an extractant-water two-phase system; the extractant-water two-phase system reacts for 20min-5h at the temperature of 100-140 DEG C; after the reaction ends, the extractant is condensed and dried to finally prepare the hydroxymethylfurfural product. Because aqueous solution of the zinc chloride can dissolve cellulose, the invention directly utilizes the cellulose to produce the hydroxymethylfurfural, and has high reaction speed and low reaction temperature; the two-phase system has high hydroxymethylfurfural yield; and the adopted zinc chloride solution and catalyst can be reused.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural from cellulose-rich biomass. Background technique [0002] The huge demand for energy around the world, the increasing consumption of petrochemical resources, and global warming have once again stimulated people's interest in renewable energy. Biofuels have become the primary "new force" and have attracted the attention of researchers at home and abroad. The reserves of biological resources are huge. It is estimated that the annual energy stored by plants is about 10 times that of human energy consumption in the world, and the utilization of energy as energy is less than 1% of the total. [0003] A biomass-based liquid fuel - 2,5-dimethylfuran has attracted the attention of many researchers. Many articles have been published in Nature and Science to discuss the preparation process of 2,5-dimethylfuran and the feasibility of replacing ethanol (Nature, 2007, 447, 914-915, 982-985, S...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
Inventor 侯相林邓天昇朱玉雷
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI