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Method for producing 2,5-dimethyl furan (2,5-DMF) by fructose one-step process

A technology of dimethylfuran and dimethylformamide, which is applied in the field of one-step preparation of 2,5-DMF, can solve the problems of difficulty in separating 5-HMF, poor selectivity, etc., and achieves good reusability and simple and easy experimental operation. The effect of large industrial application value

Active Publication Date: 2015-12-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there is a high yield of 2,5-DMF from 5-HMF, it is very difficult to separate 5-HMF from hydrocarbons
Therefore, the selectivity of producing 2,5-DMF from hydrocarbons is very poor

Method used

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  • Method for producing 2,5-dimethyl furan (2,5-DMF) by fructose one-step process
  • Method for producing 2,5-dimethyl furan (2,5-DMF) by fructose one-step process
  • Method for producing 2,5-dimethyl furan (2,5-DMF) by fructose one-step process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 fructose one-step method produces 2,5-DMF

[0021] The experiment was carried out in a steel autoclave with a volume of 100mL, the amount of raw material fructose was 1.8g (10mmol), and the catalyst Ru / C, AlCl 3 , H 2 SO 4 , H 3 PO 4 The dosage is 0.2g, 0.056g (0.42mmol), 0.098g (1mmol), 0.147g (1.5mmol), the solvent DMF dosage is 60mL, the control speed is 600rpm, the hydrogen pressure is 1.5MPa, the reaction temperature is 200°C, the reaction is 12h, the reaction After the end, take samples directly, use HPLC and gas chromatography to detect, filter the reaction liquid, recover Ru / C from the filter cake, wash Ru / C with DMF, and recycle, add a few grains of zeolite to the filtrate, at 96 ° C, normal pressure conditions The rectification operation was carried out at a lower temperature to obtain a colorless oily liquid. The detection and analysis showed that the yield of 2,5-DMF was 58.5 mol%, and the conversion rate of fructose was >99 mol%.

[0022] ...

Embodiment 2-12

[0025] Referring to the test conditions described in Table 1, the method in Example 1 was used to prepare 2,5-DMF from fructose in one step, and the results are shown in Table 1.

[0026] Table 1 embodiment 2-12 test conditions and results

[0027]

[0028]

Embodiment 13-15

[0030] According to the test conditions described in Table 2, the method described in Example 1 was used to conduct the test with the Ru / C recovered in Example 15. The test conditions and results are shown in Table 2.

[0031] Table 2 Ru / C recycling situation

[0032]

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Abstract

The invention discloses a method for producing 2,5-dimethyl furan (2,5-DMF) by a fructose one-step process. The method comprises the following steps: reacting under the conditions of 140 to 220 DEG C, 400 to1000rpm (revolutions per minute) and 0.5 to 4MPa by taking fructose as a raw materials, Ru / C and mixed liquid of AlCl3 and inorganic acid as catalysts and N,N-dimethylformamide as solvent; after reaction is ended, performing suction filtration on reaction liquid, and recovering Ru / C from a filter cake; performing aftertreatment on filtrate to obtain the product 2,5-dimethyl furan. According to the method disclosed by the invention, 2,5-DMF is produced from the fructose, which is wider in source and lower in price, instead of 5-HMF (5-hydroxymethylfurfural); the method has greater industrial application value; the course of the original two-step process is integrated into one step, therefore the problem that the intermediate product 5-HMF is difficult to separate can be effectively solved; the method has obvious innovation and simple and easy experiment operations; good 2,5-DMF yield can be obtained, and the molar yield reaches 66.3 percent.

Description

(1) Technical field [0001] The invention relates to a method for preparing 2,5-dimethylfuran (2,5-DMF), in particular to a method using fructose as a starting material and using Ru / C and Lewis-Bronster mixed acid as a catalyst, A method for preparing 2,5-DMF in one step. (2) Background technology [0002] 2,5-DMF prepared by hydrogenolysis of the platform compound 5-hydroxymethylfurfural (5-HMF) obtained from the hydrolysis of carbohydrates is considered to be the most promising renewable biomass energy. Compared with traditional biomass energy-ethanol, 2,5-DMF has a higher boiling point (92-94°C vs. 78.4°C), higher octane number (119vs.111), easier to mix with gasoline, and more High energy density (31.5kJ·cm -3 vs. 23kJ·cm -3 ). At the same time, the vapor latent heat of 2,5-DMF is lower (0.30kJ·cm -3 vs. 0.71kJ·cm -3 ), the energy consumed by rectification and purification is lower. [0003] The main method of producing 2,5-DMF is to catalyze the hydrogenolysis of ...

Claims

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Application Information

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IPC IPC(8): C07D307/36
CPCC07D307/36
Inventor 魏作君楼炯涛
Owner ZHEJIANG UNIV
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