Method for preparing 2,5-dimethylfuran by catalyzing 5-hydroxymethylfurfural

A technology of hydroxymethylfurfural and dimethylfuran, which is applied in the field of organic synthesis, can solve the problems of low selectivity and low activity of non-precious metal catalysts, and achieve high catalytic activity and selectivity, simple production and convenient operation

Active Publication Date: 2017-01-04
CHINA UNIV OF PETROLEUM (BEIJING)
View PDF4 Cites 11 Cited by
  • 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 ma

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing 2,5-dimethylfuran by catalyzing 5-hydroxymethylfurfural

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0038] Example 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 content of iron is 3% by mass in terms of iron element.

[0041] This embodiment also provides a method for preparing the above 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℃ for 15h, then spin dry the solvent with a rotary evaporator, and use an oven at 60℃ Dry for 8 hours, and then calcine at 800°C under the protection of inert gas to prepare a heterogeneous iron-based catalyst;

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

Example Embodiment

[0046] Example 2

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

[0048] Among them, in the above-mentioned heterogeneous iron-based catalyst, the content of iron is 3% by mass in terms of iron element. The nitrogen-containing compound in this example is blood crystal and contains Fe. Therefore, this group of heterogeneous iron is prepared. The catalyst does not require an additional iron compound.

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

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

Example Embodiment

[0054] Example 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 heterogeneous iron-based catalyst, which includes the following steps:

[0057] Step 1: Add 0.5 mmol of 5-hydroxymethyl furfural to 20 mL of n-hexane to prepare a 5-hydroxymethyl furfural solution;

[0058] Step two, mix the above 5-hydroxymethyl furfural solution and 0.1 g of the above heterogeneous iron-based catalyst in a closed autoclave, replace the air with hydrogen 3-4 times, and then fill it with hydrogen at a high pressure of 1 MPa The hydrodeoxygenation reaction was carried out under heating to 240° C. and stirring for 12 hours. The HMF conversion rate was 100% and the product DMF yield rate was 45.5% by gas chromatography and gas chromatography-mass spectrometry.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D307/36B01J27/24
CPCY02P20/584C07D307/36B01J27/24
Inventor 李江刘俊玲
Owner CHINA UNIV OF PETROLEUM (BEIJING)
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap