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Method for preparing 2,5-dimethylfuran through hydrogenation of 5-hydroxymethyl furfural

A technology for hydroxymethylfurfural and dimethylfuran, which is applied in the field of preparation of 2,5-dimethylfuran by catalyzing the hydrogenation of 5-hydroxymethylfurfural to achieve the effects of excellent yield, simple operation and low cost

Active Publication Date: 2019-03-22
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although 2,5-dimethylfuran can be obtained by catalytic hydrogenation reduction of 5-hydroxymethylfurfural, there is no relatively economical, reasonable and efficient method for preparing 2,5-methylfuran by catalytic hydrogenation reduction

Method used

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  • Method for preparing 2,5-dimethylfuran through hydrogenation of 5-hydroxymethyl furfural
  • Method for preparing 2,5-dimethylfuran through hydrogenation of 5-hydroxymethyl furfural
  • Method for preparing 2,5-dimethylfuran through hydrogenation of 5-hydroxymethyl furfural

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preparation example Construction

[0029] Preparation example of HCP-Co nanosheets

[0030] (1) Dissolve cobalt nitrate hexahydrate in deionized water to prepare mixed solution A, then add 2mol / L sodium hydroxide solution dropwise to mixed solution A to obtain suspension B, then carry out suspension B Suction filtration and washing with water for 3 to 5 times to obtain the precipitate, and place the precipitate in a vacuum drying oven at 60°C to dry overnight to obtain the precursor β-Co(OH) 2 ,

[0031] (2) The precursor β-Co(OH) 2 The nanosheets are placed in a quartz tube, and in an atmosphere of argon-hydrogen (9:1) flow rate of 40-80mL / min, the pressure is maintained at 1-1.2bar, and the temperature is raised to 320°C at a heating rate of 9-13°C / min , keep the temperature for 2 ~ 3h, and then naturally cool to room temperature under the atmosphere, then passivate in the nitrogen-oxygen (9:1) atmosphere to obtain HCP-Co mesoporous nanosheets, the obtained HCP-Co mesoporous nanosheets The average size is ...

Embodiment 1

[0037] The hydrogenation of 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran includes the following steps: (1) before the reaction, fill the autoclave with 1.0MPa hydrogen, exhaust the gas 5 times, and then fill it with 1.6MPa hydrogen ;

[0038] (2) Put 0.05g HCP-Co as a catalyst and 12ml tetrahydrofuran solvent into the autoclave, then add 1.0mmol 5-hydroxymethylfurfural, and feed 1.6Mpa of H 2, react at 180°C for 4 hours, and maintain a stirring speed of 500r / min during the reaction to obtain 2,5-dimethylfuran. After the reaction, take down the reactor and cool it down to room temperature naturally. The products were collected and analyzed by Agilent 7890B gas chromatography. The types of products were identified by GC-MS model 7890B-5977B, showing that the conversion rate of HMF was 93.9%, and the yield of DMF reached 38.9%.

[0039] It shows that the hydrogenation reaction of HMF is violent, and HMF reacts with hydrogen. The reason for the reaction is that HCP-Co act...

Embodiment 2

[0041] 5-Hydroxymethylfurfural is hydrogenated to prepare 2,5-dimethylfuran, including the following steps: (1) Before the reaction, fill the autoclave with 1.0MPa hydrogen, exhaust the gas 5 times, and then fill it with 1.8MPa hydrogen ;

[0042] (2) Put 0.05g HCP-Co as a catalyst and 12ml tetrahydrofuran solvent into the autoclave, then add 1.0mmol 5-hydroxymethylfurfural, and feed 1.8Mpa of H 2 , react at 180°C for 4 hours, and maintain a stirring speed of 500r / min during the reaction to obtain 2,5-dimethylfuran. After the reaction, take down the reactor and cool it down to room temperature naturally. The products were collected and analyzed by Agilent 7890B gas chromatography. The types of products were identified by GC-MS model 7890B-5977B, showing that the conversion rate of HMF was 98.7%, and the yield of DMF reached 94.9%.

[0043] It shows that the hydrogenation reaction of HMF is violent, and HMF reacts with hydrogen. The reason for the reaction is that HCP-Co plays...

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Abstract

The invention discloses a method for preparing 2,5-dimethylfuran through hydrogenation of 5-hydroxymethyl furfural. The method comprises the following steps: 1) charging an autoclave with hydrogen gasof 1MPa prior to a reaction, exhausting the gas for 5 times, and then, charging the autoclave with hydrogen gas; 2) putting HCP-Co, which serves as a catalyst, into the autoclave together with a tetrahydrofuran solvent, then, adding the 5-hydroxymethyl furfural, then, introducing hydrogen gas of 1.6MPa to 2.2MPa, and carrying out a reaction at the temperature of 160 DEG C to 200 DEG C for 1.5 to5.0 hours while maintaining the stirring rate of 500r / min, thereby obtaining the 2,5-dimethylfuran, wherein the mole ratio of the HCP-Co to the 5-hydroxymethyl furfural is 1: (1 to 5). According to the method, the process flow is simple in operation, the selectivity is high, and the cost is low; compared with a ruthenium catalyst, the catalyst used in the method is higher in selectivity and higherin DMF yield and is more economical.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a preparation method for catalyzing the hydrogenation of 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran. Background technique [0002] With the progress of the times, the contradiction between the reduction of non-renewable resource petroleum fuels and the increasing demand of human beings for petroleum fuels will become increasingly prominent. Seeking renewable resources to replace petroleum as fuel is of great significance to reduce the dependence of human production and life on petroleum fuels. [0003] 5-Hydroxymethylfurfural is one of the intermediate products of cellulose degradation. Its molecule contains a carbonyl group and a hydroxyl group. It can be derived from chemical reactions such as catalytic hydrogenation, oxidative dehydrogenation, esterification, and halogenation. product. The energy density of 2,5-dimethylfuran (30MJ / L) and the energy density of gas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36B01J23/75B01J35/10
CPCC07D307/36B01J23/75B01J35/23B01J35/647
Inventor 吕宏缨陈乃猛赵玉潮任万忠
Owner YANTAI UNIV
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