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Method to prepare 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural

A technology of hydroxymethyl furfural and dimethyl furan, applied in the field of biomass liquid fuel preparation, can solve problems such as hindering the industrialization process, high price of hydrogen supply agent, etc., and achieve the effects of zero hydrogen consumption and simple preparation process

Inactive Publication Date: 2018-09-28
ZHEJIANG UNIV
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Problems solved by technology

However, the hydrogen donors used in this method to obtain high-yield products are mainly expensive alcohols such as sec-butanol and isopropanol, and the yield of 2,5-dimethylfuran is only 72.9% when ethanol is used as the hydrogen source. %, and the study of cheaper methanol as a hydrogen source has not been reported, so the high price of its hydrogen donor has become the main reason hindering the industrialization of this process
[0006] Secondly, in some studies on the hydrogenation of 5-hydroxymethylfurfural using alcohol as a hydrogen donor to prepare 2,5-dimethylfuran, all the prices used without exception in the case of high yields of the target product More expensive isopropanol, etc. (ChemCatChem, 2014, 6, 848; ChemSusChem, 2014, 7, 268; ACS catal., 2015, 7, 3988; Fuel, 2017, 187, 159)

Method used

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  • Method to prepare 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural
  • Method to prepare 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural
  • Method to prepare 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural

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Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: Preparation of Cu-ZnO-CoO x catalyst

[0037] Preparation of Cu-ZnO-CoO by coprecipitation method x , where the loading of Cu-ZnO is 20wt%, and the molar ratio of Cu to Zn is 2.5:1.

[0038] The specific preparation process is as follows: 1) Preparation of mixed salt solution: according to the component content calculated in the required catalyst, the corresponding Co(NO 3 ) 2 ·6H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Cu(NO 3 ) 2 ·3H 2 O was dissolved in 500mL deionized water, stirred to make it fully dissolved to make a mixed salt solution.

[0039] 2) Preparation of lye: using NaOH and Na 2 CO 3 The mixed solution is used as a precipitant, and the OH is set according to the molar amount of basic anions required for metal ion precipitation. - and CO 3 2- The molar ratio of the substances is 2:1, the calculated NaOH and Na 2 CO 3 Add 500mL deionized water, stir to fully dissolve to obtain the required lye.

[0040] 3) After the preparation is comp...

Embodiment 2

[0042] Embodiment 2: Preparation of 2,5-dimethylfuran

[0043] Add 5g of 5-hydroxymethylfurfural, 50g of ethanol and 0.5g of CuZnCo-2.5 ​​into a 100mL intermittent high-temperature and high-pressure reactor, start stirring, and raise the temperature to 200°C for 0.5h. After quantitative analysis by GC-FID and HPLC, the conversion rate of 5-hydroxymethylfurfural was calculated to be 9.4%, and the molar yield of 2,5-dimethylfuran was 4.2%.

Embodiment 3

[0044] Embodiment 3: Preparation of 2,5-dimethylfuran

[0045] According to the preparation in Example 2, only changing the reaction time to 3 hours, the calculated conversion rate of 5-hydroxymethylfurfural was 60.1%, and the molar yield of 2,5-dimethylfuran was 33.2%.

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Abstract

The invention relates to a method to prepare 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural. The method includes: mixing 5-hydroxymethylfurfural, primary alcohol and a Cu-basedcatalyst, heating to 150-250 DEG C, and enabling reaction to occur for 0.5-7 h to obtain 2,5-dimethylfuran; the Cu-based catalyst is three-way catalyst Cu-ZnO-CoOx. The method gains further increasedconversion rate of 5-hydroxymethylfurfural and further improved selectivity of 2,5-dimethylfuran as preparation conditions are optimized.

Description

technical field [0001] The invention relates to the field of biomass liquid fuel preparation, in particular to a method for preparing 2,5-dimethylfuran by in-situ hydrogenation of 5-hydroxymethylfurfural. Background technique [0002] 2,5-Dimethylfuran is a promising renewable liquid fuel. Compared with traditional biofuel ethanol, it has the following characteristics: 1) high boiling point; 2) energy density close to that of gasoline; 3) octane High alkane number, good explosion-proof performance; 4) easy storage; 5) low energy consumption for separation and purification. Therefore, 2,5-dimethylfuran has broad application value and market prospect. [0003] The current method of producing 2,5-dimethylfuran is mainly obtained by selective hydrogenation-hydrogenolysis of 5-hydroxymethylfurfural under high-pressure hydrogen. This method needs to consume a large amount of hydrogen, and because high-pressure hydrogen is required to be added, Therefore, higher requirements are ...

Claims

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Application Information

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IPC IPC(8): C07D307/36B01J23/80
CPCB01J23/002B01J23/80C07D307/36
Inventor 傅杰张子豪王昌雪吕秀阳欧阳平凯
Owner ZHEJIANG UNIV
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