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Method for preparing 2,5-dimethyl furan through electrocatalytic reduction of 5-hydroxymethyl furfural by ZrO2-doped graphite electrode

A technology of hydroxymethylfurfural and dimethylfuran, applied in the field of biomass energy chemical industry, achieves the effects of mild reaction conditions, good selectivity and good application prospects

Inactive Publication Date: 2014-05-07
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From various literature reports at home and abroad, it has not been found that the method of electrocatalytic reduction of 5-hydroxyfurfural is used to prepare 2,5-dimethylfuran

Method used

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  • Method for preparing 2,5-dimethyl furan through electrocatalytic reduction of 5-hydroxymethyl furfural by ZrO2-doped graphite electrode
  • Method for preparing 2,5-dimethyl furan through electrocatalytic reduction of 5-hydroxymethyl furfural by ZrO2-doped graphite electrode
  • Method for preparing 2,5-dimethyl furan through electrocatalytic reduction of 5-hydroxymethyl furfural by ZrO2-doped graphite electrode

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Experimental program
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Effect test

Embodiment 1

[0037] (1) Accurately weigh 18.80g fructose and 3.43g NH with an electronic balance 4 Br, 0.12g ZnCl 2 Put it into a 250ml round-bottom flask, accurately measure 150.0ml of N,N-dimethylacetamide with a pipette, put it into the round-bottom flask, add magnets, reflux and stir in an oil bath at 120°C for 55min. After the reaction is over, remove the ground glass plug on the round bottom flask cover and cool to room temperature with running water, and the concentration of the prepared 5-hydroxyfurfural stock solution is 100g.L -1 , with a brown bottle for equipment.

[0038] (2) Weigh 4.00g of graphite, 4.00g of polytetrafluoroethylene emulsion with a mass fraction of 60%, 0.12g of ZrO 2 (The relative graphite mass percentage is 3%) into the reactor, add 20mL of absolute ethanol and magnetically stir for 10min; the obtained ZrO 2- Heat the graphite mixture with stirring to evaporate the ethanol, stop heating when the mixture becomes a paste solid, pour the paste solid into a m...

Embodiment 2

[0044] Embodiment 2 Change doping ZrO 2 The relative graphite mass percentage is 8% to prepare ZrO 2 Graphite electrode, other conditions and operation steps are identical with embodiment 1. The calculated concentration of 2,5-dimethylfuran is 6.15g.L -1 , and the yield was 30.75%.

[0045] As can be seen from the foregoing examples, the present invention has investigated ZrO 2 The effect of doping amount on the yield of 2,5-dimethylfuran prepared by catalytic hydrogenation reduction of 5-hydroxyfurfural, the concentration of the obtained 2,5-dimethylfuran is 0.55~6.15g.L -1 . The preparation of 2,5-dimethylfuran by electrochemical catalytic hydrogenation reduction of 5-hydroxyfurfural has mild reaction conditions, simple equipment, low cost and novel method. 5-Hydroxyfurfural in the electrolyte diffuses from the solution and adsorbs to ZrO under the action of the solution potential during electrocatalytic reduction 2 - graphite electrode surface, in ZrO 2 Under the acti...

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Abstract

The invention discloses a method for preparing 2,5-dimethyl furan through electrocatalytic reduction of 5-hydroxymethyl furfural by a ZrO2-doped graphite electrode. The method comprises the steps of preparing a 5-hydroxymethyl furfural / N,N-dimethyl acetamide stock solution through catalyzing dehydration of fructose; and implementing electrocatalytic reduction on the 5-hydroxymethyl furfural in an electrolytic bath by taking a ZrO2-doped graphite electrode as a negative electrode and a platinum electrode as a positive electrode, thus preparing the 2,5-dimethyl furan. The method disclosed by the invention successfully solves a problem of a 2,5-dimethyl furan preparation process through hydrogenation reduction of 5-hydroxymethyl furfural which is relatively high in equipment and catalyst expenses. The method, by taking ZrO2 as a catalyst, avoids use of precious metal (ruthenium, palladium and the like) in a conventional 5-hydroxymethyl furfural hydrogenation process, and simultaneously avoids direct use of H2 so as to effectively reduce cost of producing the 2,5-dimethyl furan; and the method disclosed by the invention is free from environmental pollution, relatively moderate in reaction condition and good in selectivity.

Description

technical field [0001] The present invention relates to a kind of doped ZrO 2 The invention discloses a method for preparing 2,5-dimethylfuran by electrocatalytically reducing 5-hydroxymethylfurfural with a graphite electrode, and belongs to the technical field of biomass energy chemical industry. Background technique [0002] With the continuous reduction of non-renewable fossil fuels and the continuous increase of fuel consumption for people's lives, the problem of energy shortage is becoming more and more prominent. It is imminent to find a method to prepare renewable fuels. Cellulose is a renewable resource that exists widely on the earth, and its main components are hydrocarbons. If it is converted into high-energy biomass fuel, it can solve the shortage of non-renewable petrochemical fuels in the future. [0003] The constituent unit of cellulose is six-carbon sugar, and 5-hydroxymethylfurfural can be prepared by dehydration of six-carbon sugar, and 2,5-dimethylfuran ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/04C25B11/06C25B3/25
Inventor 黎钢袁涛杨芳张松梅
Owner HEBEI UNIV OF TECH
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