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Method for preparing 2,5-diformyl furan

A technology of diformylfuran and hydroxymethylfurfural, applied in the direction of organic chemistry, can solve the problems of harsh reaction conditions, poor reaction selectivity, and high catalyst cost, and achieve convenient post-processing, high selectivity, and simple and easy-to-operate preparation Effect

Active Publication Date: 2017-07-21
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the existing preparation methods have defects such as harsh reaction conditions, high catalyst cost, poor reaction selectivity, and difficult separation of products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] The preparation method of catalyst in each embodiment:

[0027] The preparation method of the vanadium phosphorus oxide or copper, manganese, bismuth doped vanadium phosphorus oxide refers to the prior art, specifically the following methods can be adopted:

[0028] The vanadium phosphorus oxide can be prepared by the following method: 1.18gV 2 o 5 and 10.46g of H with a mass concentration of 85 %3 PO 4 , was dissolved in 27.5 mL of water, refluxed at 100°C for 16 hours, filtered with suction, dried in vacuum at 30°C for 4 hours, the obtained solid was washed with acetone three times, and dried in static air at room temperature for 2 days to obtain the product. (See prior art, RSC Advances, 2013, 3:9942-9948).

[0029] Bismuth-doped vanadium phosphorus oxide can be prepared as follows:

[0030] Weigh 3.0 g V 2 o 5 and 0.16g Bi(NO 3 ) 3 ·5H 2 O mixed, then added 0.257g dimethyl sulfoxide (DMSO), 24mL isobutanol and 6mL benzyl alcohol in sequence, refluxed at 110...

Embodiment 1

[0032] Example 1: Dissolve 1.30 g of 5-hydroxymethylfurfural (0.0103 mol) in 10 mL of dimethyl sulfoxide, add 1.0 g of vanadium phosphorus oxide and 1.48 g of tert-butyl hydroperoxide with a mass concentration of 65% (0.0107mol), reacted for 3 h at a temperature of 110°C and a stirring speed of 20 rpm to obtain 2,5-diformylfuran.

[0033] The conversion rate of 5-hydroxymethylfurfural was 54.5% and the selectivity of 2,5-diformylfuran was 98.0% according to the reaction results analyzed by high performance liquid chromatography.

[0034] The test conditions of the Agilent 1100 high performance liquid chromatograph are: the chromatographic column is a C18 analytical column (250 × 4.6mm), the UV detector, the detection wavelength is 283 nm, and the mobile phase is acetonitrile and 0.1 wt.% acetic acid (volume ratio is 10 :90), the flow rate was 0.5 mL / min, and the column temperature was 30 ℃. The contents of 5-hydroxymethylfurfural and 2,5-diformylfuran in the sample were calcul...

Embodiment 2

[0035] Example 2: Dissolve 1.42 g of 5-hydroxymethylfurfural (0.0113 mol) in 10 mL of dimethyl sulfoxide, add 0.95 g of vanadium phosphorus oxide and 1.62 g of tert-butyl hydroperoxide with a mass concentration of 65% (0.0117mol), reacted for 11 h at a temperature of 120°C and a stirring speed of 30 rpm to obtain 2,5-diformylfuran. The conversion rate of 5-hydroxymethylfurfural was 96.4%, and the selectivity of 2,5-diformylfuran was 85.2%.

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Abstract

The invention discloses a method for preparing 2,5-diformyl furan. According to the method, in an organic solvent system, with a biomass-based platform compound 5-hydroxymethyl furfural as a raw material, and vanadium phosphorus oxide or copper, manganese and bismuth-doped vanadium phosphorus oxide as a catalyst, highly selective oxidation of 5-hydroxymethyl furfural is catalyzed to obtain the product 2,5-diformyl furan. The method has the advantages as follows: the used catalyst has high activity, is easy to prepare, and has lower cost than other noble metal catalysts; preparation of the 2,5-diformyl furan through oxidation of 5-hydroxymethyl furfural is relatively high in selectivity; the reaction system is carried out under normal pressure, the condition is mild, the catalytic oxidation efficiency is high, few byproducts are produced and the posttreatment is convenient, so that the method is of great guiding significance in achievement of industrial large-scale production of the 2,5-diformyl furan.

Description

technical field [0001] The invention belongs to the field of biomass energy chemical industry and relates to a method for preparing 2,5-diformyl furan by catalyzing 5-hydroxymethylfurfural with vanadium phosphorus oxide. Background technique [0002] Utilizing abundant and renewable biomass resources to produce high-value-added new materials and fine chemical raw materials is one of the important ways to solve human energy and environmental problems in the future, and has very important strategic significance for the replacement of fossil resources. Almost all basic organic chemical raw materials can be produced from biomass, and many products have shown good economics. [0003] 5-Hydroxymethylfurfural is the main product of biomass carbohydrate deoxygenation and an important platform compound for the comprehensive utilization of biomass resources. 5-Hydroxymethylfurfural is also known as 5-Hydroxymethyl-2-furfural or 5-Hydroxymethyl-2-furfuraldehyde, the English abbreviati...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 刘贤响尹笃林刘凯赖金花徐琼
Owner HUNAN NORMAL UNIVERSITY