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A kind of method that catalyzes 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran

A technology of hydroxymethyl furfural and dimethyl furan, applied in the field of organic synthesis, can solve the problems of low selectivity and low activity of non-precious metal catalysts, and achieve the effects of high catalytic activity and selectivity, simple production and convenient operation

Active Publication Date: 2018-08-28
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although non-noble metal catalysts such as copper and nickel have been reported, there are still many problems to be solved, such as the low selectivity of DMF and low activity of non-noble metal catalysts.

Method used

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  • A kind of method that catalyzes 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran

Examples

Experimental program
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Effect test

Embodiment 1

[0039] This embodiment provides a heterogeneous iron-based catalyst, and the raw material components for preparing the heterogeneous iron-based catalyst include ferrous acetate, 1,10-phenanthroline, and activated carbon;

[0040] Wherein, in the above-mentioned heterogeneous iron-based catalyst, the mass percentage content of iron is 3% based on iron element.

[0041] This embodiment also provides a method for preparing the above-mentioned heterogeneous iron-based catalyst, which includes the following steps:

[0042] Mix ferrous acetate and 1,10-phenanthroline with ethanol to dissolve, stir at room temperature for half an hour, then add activated carbon and heat to 60°C for 15 hours, then use a rotary evaporator to spin dry the solvent, and use an oven at 60°C Drying for 8 hours, followed by calcination at 800°C under the protection of an inert gas, to prepare a heterogeneous iron-based catalyst;

[0043] This embodiment also provides a method for preparing 2,5-dimethylfuran...

Embodiment 2

[0047] This embodiment provides a heterogeneous iron-based catalyst, and the raw material components for preparing the heterogeneous iron-based catalyst include hematin and activated carbon;

[0048]Wherein, in the above-mentioned heterogeneous iron-based catalyst, the mass percentage of iron is 3% based on iron element, and the nitrogen-containing compound in this embodiment adopts hematin, which itself contains Fe, so this group of heterogeneous iron is prepared The catalyst does not require the addition of iron compounds.

[0049] This embodiment also provides a method for preparing the above-mentioned heterogeneous iron-based catalyst, which includes the following steps:

[0050] Dissolve hematin with ethanol, stir at room temperature for half an hour, then add activated carbon and heat to 60°C for 15 hours, then use a rotary evaporator to spin dry the solvent, and use an oven to dry at 60°C for 8 hours, then in an inert gas atmosphere Calcining at a temperature of 800°C ...

Embodiment 3

[0055] The preparation of the heterogeneous iron-based catalyst is the same as in Example 1.

[0056] This embodiment also provides a method for preparing 2,5-dimethylfuran from 5-hydroxymethylfurfural catalyzed by the above-mentioned heterogeneous iron-based catalyst, which includes the following steps:

[0057] Step 1, adding 0.5 mmol of 5-hydroxymethylfurfural to 20 mL of n-hexane to prepare a 5-hydroxymethylfurfural solution;

[0058] Step 2, mix the above-mentioned 5-hydroxymethylfurfural solution and 0.1g of the above-mentioned heterogeneous iron-based catalyst in a closed high-pressure reactor, replace the air with hydrogen for 3-4 times, and then fill with hydrogen, and put it under a high pressure of 1MPa The mixture was heated to 240° C. and stirred for 12 hours to carry out hydrodeoxygenation reaction. It was detected by gas chromatography and gas chromatography-mass spectrometry that the conversion rate of HMF was 100%, and the yield of the product DMF was 45.5%. ...

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Abstract

The invention provides a method for preparing 2,5-dimethylfuran by catalyzing 5-hydroxymethylfurfural. The method includes the following steps that firstly, 5-hydroxymethylfurfural is added into organic solvent to prepare a 5-hydroxymethylfurfural solution; secondly, the 5-hydroxymethylfurfural solution is catalyzed by means of a heterogeneous iron-based catalyst for hydrodeoxygenation, and 2,5-dimethylfuran is obtained. According to the method, catalytic active metal of the heterogeneous iron-based catalyst in use is iron, and compared with noble metal ruthenium, palladium, platinum and the like, cost is low; compared with other non-noble metal catalysts, the heterogeneous iron-based catalyst is easy to prepare and convenient to operate, and catalytic activity and selectivity are high; the catalyst is used for catalyzing 5-hydroxymethylfurfural (HMF) to prepare 2,5-dimethylfuran (DMF), an efficient environment-friendly method is provided for preparation of DMF, and the heterogeneous iron-based catalyst recycled after catalytic reaction can be repeatedly used.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and relates to a method for preparing 2,5-dimethylfuran (DMF) from 5-hydroxymethylfurfural (HMF) catalyzed by a heterogeneous iron-based catalyst. Background technique [0002] With the continuous reduction of fossil resources such as petroleum, the continuous increase of greenhouse gas emissions, and the increasingly serious environmental pollution, the use of renewable new energy to replace traditional fossil energy has become an important research direction at present, and biomass energy is the only one containing Renewable energy sources of organic carbon are considered to be the most ideal substitutes for fossil energy sources. [0003] 5-Hydroxymethylfurfural (HMF), which can be prepared by acidic hydrolysis of cellulose, has been considered as one of the most important platform chemicals in biomass conversion processes. The high functionality of HMF allows it to be conv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/36B01J27/24
CPCY02P20/584
Inventor 李江刘俊玲
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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