Method for preparing 2,5-dimethyl furan by use of fructosyl biomass

A dimethyl furan and biomass technology, applied in organic chemistry and other fields, can solve the problems of cumbersome process and strong corrosion, and achieve the effect of simple process operation, mild reaction conditions and renewable raw materials

Inactive Publication Date: 2014-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, the current methods for preparing DMF mostly use strong acid as a catalyst in the fructose dehydration step, which is highly corrosive and prone to waste water; and the generated HMF basically needs to be extracted and separated before the next hydrogenation reaction, and the process is relatively cumbersome.

Method used

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  • Method for preparing 2,5-dimethyl furan by use of fructosyl biomass
  • Method for preparing 2,5-dimethyl furan by use of fructosyl biomass
  • Method for preparing 2,5-dimethyl furan by use of fructosyl biomass

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Embodiment 1

[0025] The supported metal catalysts with different loads can be commercially available or self-made by impregnation. Taking the preparation of Ni / C, Pd / C, Pt / C, Ir / C, Ru / C, Cu / C, Cu-Ru / C as an example: in the corresponding metal precursors nickel nitrate, palladium chloride, platinum chloride Aqueous solution of acid, chloroiridic acid, ruthenium trichloride, copper chloride, etc. impregnated the active carbon carrier with a medium volume, stirred evenly and dried at 60°C, then dried at 120°C for 12 hours, and finally dried at 300°C in a hydrogen atmosphere Reduction for 1 hour, cooling with 1% O 2 / N 2 The catalyst can be obtained by passivating the mixed gas for 4 hours.

Embodiment 2

[0027] Weigh 1g of ionic liquid 1-butyl-3-methylimidazolium chloride (BmimCl) and a certain amount of fructose in a round bottom flask, heat and stir in oil baths at different temperatures, and take samples of about 20mg at regular intervals (accurately weigh the mass and record ) and dilute to 1ml with deionized water, mix well and centrifuge, take the supernatant and analyze it with the external standard method of gas chromatography, the reaction results are shown in Table 1.

[0028] Table 1. The reaction results of HMF prepared from fructose dehydration in ionic liquid BmimCl

[0029]

[0030] The above results show that in the temperature range of 50°C-100°C, in the fructose / ionic liquid solution of 1:10-5:1 (wt / wt), fructose can be converted into HMF with a high yield, and the yield is 35 %-89%.

Embodiment 3

[0032] 0.3g of HMF, 1g of ionic liquid BmimCl and 25mL of THF were added into the autoclave, and 0.1g of 5wt% Ru / C catalyst was added at the same time. Close the reactor, use H 2 Continuously replace the gas in the kettle for 5 times. then H 2Adjust the pressure to 5MPa, heat up to 220°C, stir rapidly (800rpm) for 5 hours, stop heating, and when the temperature of the still is down to room temperature, open the vent valve to reduce the pressure in the still to normal pressure, and discharge. The reaction solution was filtered, and the filtrate was used for analysis. The product was qualitatively analyzed by GC-MS, and quantitatively analyzed by GC external standard method. The HMF conversion rate was 100%, and the DMF yield rate was 50%.

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Abstract

The invention relates to a method for preparing a 2,5-dimethyl furan by use of a fructose and a fructosyl biomass, and specifically relates to a method which comprises the following step: on the basis of adopting a mixed reaction medium of an ionic liquid and an organic solvent, and under the conditions of appropriate temperature and pressure, performing continuous dehydration and hydrogenation reactions on the fructose and the fructosyl biomass in the presence of a catalyst so as to convert the fructose and the fructosyl biomass into the 2,5-dimethyl furan. The method is used for preparing the target product by use of the biomass which is rich in fructose and is taken as the raw material by virtue of a one-pot method; a plurality of steps of reactions are coupled, the reaction steps are simple, the raw materials is cheap and regenerative, the operation is convenient and the product yield is high; a new method for preparing chemicals directly by use of the biomass is provided.

Description

technical field [0001] The invention relates to a method for preparing 2,5-dimethylfuran from fructose and fructose-based biomass. Specifically, using the mixed solvent ionic liquid / organic solvent as the reaction medium, under the appropriate temperature and pressure, fructose and fructose-based biomass undergo continuous hydrolysis, dehydration and hydrogenation reactions under the action of a catalyst to convert 2,5-di methyl furan. The present invention uses fructose-rich biomass as a raw material to prepare the target product in a one-pot method, and has the following advantages: the raw material is cheap and renewable, the reaction steps are simple, the operation is convenient, the multi-step reaction is coupled and completed in a one-pot method, and the product yield is high. Background technique [0002] With the increasingly prominent contradiction between the demand and storage of fossil fuels and the rising global greenhouse gas emissions, the search for a renewa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36
CPCC07D307/36
Inventor 张涛李昌志蔡海乐王爱琴
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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