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Method for preparing furyl glycol from fructosyl biomass

A kind of furanyl diol, biomass technology, applied in the direction of organic chemistry etc.

Active Publication Date: 2014-06-11
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

In summary, the current raw materials for the preparation of DHMF and BHMTF are either expensive HMF or petroleum-based raw materials

Method used

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  • Method for preparing furyl glycol from fructosyl biomass
  • Method for preparing furyl glycol from fructosyl biomass
  • Method for preparing furyl glycol from fructosyl biomass

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Experimental program
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Embodiment 1

[0023] Supported metal catalysts with different loadings can use commercial catalysts or self-made by impregnation (Ji Na, Zhang Tao, Zheng Mingyuan, Wang Aiqin, Wang Hui, Wang Xiaodong, Chen Jingguang, Angew.Chem.Int.Ed.2008,47 ,8510-8513). 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 450°C in a hydrogen atmosphere Reduction for 1 hour, cooling and passivation with 1% O2 / N2 mixed gas for 3 hours to obtain the catalyst.

Embodiment 2

[0025] Weigh 2g 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 regularly sample about 40mg (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.

[0026] Table 1. The reaction results of HMF prepared from fructose dehydration in ionic liquid BmimCl

[0027]

[0028] 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

[0030] 0.5g of HMF, 2g of ionic liquid BmimCl and 70mL of water were added into the autoclave, and 0.15g 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 50°C, stir rapidly (960rpm) for 6 hours, stop heating, and when the temperature of the kettle drops to room temperature, open the vent valve to reduce the pressure in the kettle to normal pressure, and then 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%, the DHMF yield rate was 74.3%, and the BHMTF yield rate was 20.1%. And up to 94.4%.

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Abstract

The invention relates to a method for preparing furyl glycol from fructose and fructosyl biomass, and specifically relates to a method for converting fructose and fructosyl biomass into 2,5-dihydroxy methyl tetrahydrofuran or 2,5- dihydroxy methyl furan through continuous dehydration and hydrogenation reaction in the presence of a catalyst under a proper temperature and pressure based on a mixed solvent ion liquid / water as a reaction medium. The method disclosed by the invention takes the biomass rich in fructose as the material to prepare a target product through a one-pot process, is coupled with multi-step reaction, simple in reaction step, cheap and reproducible in material, convenient to operate, and high in product yield; the invention provides a novel method for directly preparing chemicals from biomass.

Description

technical field [0001] The present invention relates to a method for preparing furanyl diols from fructose and fructose-based biomass. Specifically, using the mixed solvent ionic liquid / water 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-dihydroxy Methyltetrahydrofuran or 2,5-Dihydroxymethylfuran. 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 gradual depletion of fossil energy, the production of chemical products and fuels from biomass has become a hot field...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/42C07D307/12
CPCC07D307/12C07D307/42
Inventor 张涛蔡海乐李昌志王爱琴
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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