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2,5-dimethylfuran and method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural

A technology of dimethylfuran and hydroxymethylfurfural, applied in directions such as organic chemistry, can solve problems such as increasing operating costs, achieve the effects of saving costs, avoiding the use of precious metal catalysts, and mild reaction conditions

Active Publication Date: 2020-05-08
SHANGHAI OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods require the direct use of gaseous hydrogen to hydrogenate the reactant 5-hydroxymethylfurfural, and the use of noble metal catalysts increases operating costs. Therefore, the development of cheap green liquid hydrogen donors and cheap commercially available metals Catalyst, which is of great significance to the production of 2,5-dimethylfuran

Method used

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  • 2,5-dimethylfuran and method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural
  • 2,5-dimethylfuran and method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural
  • 2,5-dimethylfuran and method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural

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Experimental program
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Effect test

preparation example Construction

[0025] The preparation method of catalyst includes but not limited to following method:

[0026] 21.10g Mg(NO 3 ) 2 ·6H 2 O, 4.71g Zr(NO 3 ) 4 ·5H 2 O and 9.94g Cu(NO 3 ) 2 ·3H 2 O was added to a beaker containing 200 mL of deionized water to make Mg(NO 3 ) 2 ·6H 2 O: Zr(NO 3 ) 4 ·5H 2 O: Cu(NO 3 ) 2 ·3H 2 O=8:1:4 (the ratio of the amount of substances). Seal the mouth of the beaker with a parafilm to avoid liquid splashing, and stir at a speed of 500r / min until all the solids are dissolved, and this operation is carried out at room temperature.

[0027] Configure 1mol / L Na 2 CO 3 Solution 200mL, ready to use.

[0028] Na 2 CO 3 The solution was added dropwise to the prepared Mg(NO 3 ) 2 , Zr(NO 3 ) 4 and Cu(NO 3 ) 2 in the mixed solution, and always control the pH=10 of the solution.

[0029] After the pH was stabilized, the stirring was continued for 2 hours, then the stirring was stopped, and left to age for 24 hours.

[0030] The aged catalyst...

Embodiment 1

[0037] The method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural in this embodiment comprises the following steps:

[0038] 0.2mmol 5-hydroxymethylfurfural, 3mL isopropanol, 20mg CuO / MgO-ZrO 2 Put it into a 10mL stainless steel reactor, and use nitrogen to purge the reactor for 10s, and finally seal the reactor, react at 250°C for 3h, take out the solid-liquid mixture after the reaction and separate to obtain 2,5-dimethylfuran solution.

[0039] The reacted product was analyzed by gas chromatography (see figure 1), the results of gas chromatography showed that the yield of 2,5-dimethylfuran was 54.8%. In industrial applications, a suitable pressure-resistant reactor can be used as required, and the reaction temperature can be controlled at 250°C for 3 hours. Through this reaction, 5-hydroxymethylfurfural can be synthesized into 2,5-dimethylfuran, the operation is simple and the reaction selectivity is good.

Embodiment 2

[0041] The method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural in this embodiment comprises the following steps:

[0042] 0.2mmol 5-hydroxymethylfurfural, 3mL methanol, 20mg CuO / MgO-ZrO 2 Put it into a 10mL stainless steel reactor, and use nitrogen to purge the reactor for 10s, and finally seal the reactor, react at 250°C for 3h, take out the solid-liquid mixture after the reaction and separate to obtain 2,5-dimethylfuran solution.

[0043] The reacted product was analyzed by gas chromatography, and the result of gas chromatography showed that the yield of 2,5-dimethylfuran was 34.8%. In industrial applications, a suitable pressure-resistant reactor can be used as required, and the reaction temperature can be controlled at 250°C for 3 hours. Through this reaction, 5-hydroxymethylfurfural can be synthesized into 2,5-dimethylfuran, the operation is simple and the reaction selectivity is good.

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Abstract

The invention provides a 2,5-dimethylfuran and a method for preparing the 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural. The method comprises the following steps: the 5-hydroxymethylfurfural and a catalyst react in an alcohol solvent in a nitrogen atmosphere at 200-250 DEG C for 1-7 h, solid-liquid separation is performed after the reaction, and the obtained liquid phase product iscollected, and is purified to obtain the 2,5-dimethylfuran, wherein the active component of the supported copper-based catalyst is CuO, the carrier is MgO-ZrO2, and alcohol in the alcohol solvent isselected from than one or more of methanol, isopropanol and 2-butanol. The biomass derivative 5-hydroxymethylfurfural is used as a raw material, the supported copper-based material is used as the catalyst, the alcohol solvent is used as a hydrogen donor, and a noble metal catalyst and high-pressure hydrogen which is difficult to store and transport are not needed, so that the reaction condition ismild, the reaction raw material is a renewable biomass derivative, and a new way is further provided for utilization of renewable biomass energy.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical industry, and specifically relates to 2,5-dimethylfuran and a method for preparing 2,5-dimethylfuran by hydrogenation of 5-hydroxymethylfurfural. Background technique [0002] The excessive dependence and consumption of fossil energy such as coal, oil and natural gas have made human beings face serious energy and environmental crises. The development and utilization of renewable and clean energy such as solar energy, wind energy, tidal energy and biomass energy have attracted much attention. Biomass energy has the advantages of low pollution, wide distribution, abundant sources and large reserves. The effective use of biomass resources can alleviate human demand for fossil energy to a certain extent. 2,5-Dimethylfuran is generally regarded as a promising liquid fuel. Compared with ethanol, 2,5-dimethylfuran has a low boiling point (92°C), is stable in storage, and has a higher volum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36
CPCC07D307/36Y02P20/584
Inventor 霍志保任德章赵学雷姜雪磊张拿慧
Owner SHANGHAI OCEAN UNIV
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