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Method for preparing 2,5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural

A technology of hydroxymethylfurfural and dimethylfuran, which is applied in the field of catalytic hydrogenation of 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran, can solve the problem of high metal loading of tungsten carbide, large amount of catalyst, pressure Large and other problems, to achieve the effect of large active specific surface area, good selectivity, and small dosage

Active Publication Date: 2021-03-19
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the H used 2 The pressure is high, and the loading capacity of tungsten carbide metal is high, tungsten metal is a rare and precious metal, and the amount of catalyst is large, and the cost is high

Method used

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  • Method for preparing 2,5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2,5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2,5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural

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preparation example Construction

[0040] The preparation method of supported bifunctional catalyst of the present invention, with 3wt% Ni-MnO x / C catalyst (the ratio of Ni and Mn is 3:1) as an example: Ni-MnO prepared by co-impregnation method x / MC (mesoporous carbon) catalyst was prepared as follows: weigh 1 g of 200-mesh mesoporous carbon, place it in a crucible, and bake it at 400° C. for 5 hours. Weigh 0.1115g Ni(NO 3 ) 2 ·6H 2 O is placed in another crucible, add 0.7g deionized water, dissolve completely, weigh 0.0335g C 4 h 6 MnO 4 4H 2 O was added to the nickel nitrate solution to fully mix the nickel nitrate and manganese acetate, ultrasonically dissolve it fully, add mesoporous carbon, stir while adding, impregnate at room temperature for 24 hours, dry at 110°C for 12 hours, 500°C in hydrogen Reduction under atmosphere for 3 hours yielded Ni-MnO with a total metal loading of 3 wt%. x / MC catalyst;

[0041] Preparation of Ni-MnO by Step-wise Impregnation Method x The / AC catalyst was prepar...

Embodiment 1

[0045] Take 0.126g (2mmol) 5-hydroxymethylfurfural in a beaker, add 6mL tetrahydrofuran to dissolve, add the solution to a 25mL autoclave, add 0.252g Ni-MnO with a loading capacity of 3wt% x / AC catalyst (the ratio of the amount of Ni and Mn is 3:1, and the catalyst is prepared by the co-impregnation method), and nitrogen is purged five times, the reaction temperature is 180 ° C, the hydrogen pressure is 2.0 MPa, and the reaction is 3 hours. 2,5-Dimethylfuran was obtained, and the catalytic conversion frequency (TOF) was 50.7h -1 , the yield is 96.7%;

[0046] From figure 1 (a), it can be seen that Ni-MnO x / AC Catalyst Ni 2p 3 / 2 It can be divided into two peaks, the corresponding electron binding energy is 853.3eV and 856.9eV, respectively attributed to Ni 0 and Ni 2+ . While the Ni 2p of the Ni / AC catalyst 3 / 2 Belongs to Ni 0 and Ni 2 + The electron binding energies corresponding to the two peaks are 853.0eV and 856.6eV, respectively. Ni 2p on the surface of suppo...

Embodiment 2

[0049] Take 0.1260g (1mmol) of 5-hydroxymethylfurfural in a beaker, add 6mL of tetrahydrofuran to dissolve, add the solution to a 25mL autoclave, and add 0.025g of Ni-MnO with a loading capacity of 3wt%. x / AC catalyst (the ratio of the amount of Ni and Mn is 3:1, the catalyst is prepared by the distribution impregnation method and the impregnation sequence is first impregnated with Ni and then impregnated with Mn), and nitrogen is purged five times, the reaction temperature is 180 °C, and the hydrogen pressure is 2.0MPa, reacted for 3 hours, produced 2,5-dimethylfuran, and the catalytic conversion frequency (TOF) was 52.9h -1 , the yield was 97.9%.

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Abstract

The invention discloses a method for preparing 2,5-dimethylfuran by catalytic hydrogenation of 5-hydroxymethylfurfural, which comprises the following steps: reacting 5-hydroxymethylfurfural used as araw material in a reaction solvent under the action of a supported bifunctional catalyst in a hydrogen atmosphere to obtain the 2,5-dimethylfuran. The supported bifunctional catalyst herein comprisesa carbon carrier and an effective active component supported on the carbon carrier, wherein the carbon carrier is one of activated carbon, mesoporous carbon or nitrogen-doped mesoporous carbon, and the effective active component comprises oxides of nickel and manganese. The yield of the 2,5-dimethylfuran synthesized by the method is more than 90%; wherein the method is simple in process, high in selectivity, clean, environmentally friendly, small in catalyst dosage, capable of reducing cost and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of bioenergy, in particular to a method for preparing 2,5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural. Background technique [0002] With the depletion of non-renewable fossil resources such as coal, oil and natural gas, the research on the production of fuels and chemicals by using typical renewable resource biomass, especially lignocellulosic biomass, as a substitute has attracted more and more attention. Lignocellulose can be converted into bulk platform compounds and biofuels. Among them, biomass-based 2,5-dimethylfuran (2,5-DMF) has an energy density of 30MJ / L, a boiling point of 92-94°C, and an octane number of 119. It is an important platform compound and very Promising renewable liquid biofuels. Especially as a biofuel, it has higher energy density, boiling point and octane number than traditional fuel ethanol, and has better explosion-proof performance. It is a new typ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36B01J23/889B01J37/08B01J37/02B01J37/34B01J37/18
CPCC07D307/36B01J23/8892B01J23/002B01J37/08B01J37/0203B01J37/343B01J37/18B01J37/0201B01J37/024Y02P20/584
Inventor 刘迎新柳凯曾茂叶绿魏作君
Owner ZHEJIANG UNIV OF TECH
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