Method for preparing 2, 5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural

A technology for hydroxymethylfurfural and dimethylfuran, which is applied in the field of preparation of 2,5-dimethylfuran, can solve the problems of complicated catalyst preparation and maintenance process, catalyst deactivation, catalyst deactivation and other problems, and achieves obvious advantages and industrial application value, simple preparation method and high reactivity

Active Publication Date: 2021-05-11
DALIAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions are relatively mild, but Ni will be gradually oxidized and aggregated during repeated use, resulting in a sudden drop in catalyst activity
Li D, Liu Q, Zhu C, et al. Selective hydrogenolysis of 5-hydroxymethylfurfural to 2,5-dimethylfuran over Co 3 o 4 ,catalyst by controlled reduction[J].Journal of Energy Chemistry,2019,30,34-41. Co 3 o 4 , the partially reduced Co / CoO x Catalyst, at 170°C, 12h and 1MPa of H 2 Under pressure, the yield of DMF is 83.3%, but in the process of recycling, metals accumulate, and the catalyst loses its original structure, resulting in catalyst deactivation
In addition, the non-precious metal catalysts reported in the literature usually require reduction pretreatment before being put into the reaction system. The pre-reduction treatment not only complicates the catalyst preparation and maintenance process, but also increases energy consumption, and some reduced catalysts may lose their activity due to oxidation.

Method used

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  • Method for preparing 2, 5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2, 5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural
  • Method for preparing 2, 5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural

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Experimental program
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preparation example Construction

[0025] (1) Preparation of graphene carrier: take 230mL concentrated sulfuric acid and 5.0gNaNO 3 , stir and add 10g of natural flake graphite powder, stir for 2.5h and add 30g of KMnO 4 , transferred to a constant temperature water bath at 35°C for 2 hours, added 460 mL of deionized water, stirred in an oil bath at 98°C for 15 minutes, and finally added 1.4L of deionized water to terminate the reaction, and at the same time added 25 mL of 30% H 2 o 2 , down to room temperature, deionized water centrifugal washing to neutrality, to obtain paste graphene oxide (GO), record its dry basis content as 1wt%; get the GO paste prepared by the above-mentioned method of 100g, disperse in 1000mL deionized water, Ultrasonic treatment for 30 minutes, static aging, adding 25mL of 30% ammonia water and 6mL of 80% hydrazine hydrate, refluxed in an oil bath at 95°C for 3 hours, adding 4mL of 80% hydrazine hydrate for 30 minutes, adding 4% hydrochloric acid solution, suction filtration while ho...

Embodiment 2

[0041] The intermittent reaction of embodiment 2,4-6 different reaction pressures

[0042] 1. Catalyst preparation: the same as the catalyst preparation process in Examples 1-3.

[0043] 2. Reaction test: the operation process is the same as the reaction test process in the embodiment 1-3, and the specific reaction conditions: after ensuring that the device does not leak, pass into the specified pressure H 2 , a stirring rate of 500 rpm, and a set temperature of 200° C. for 3 h.

[0044] 3. The reaction results are shown in Table 2.

[0045] Table 2 Results of different reaction pressures

[0046]

[0047] From Examples 2, 4-6, it can be seen that the conversion rate of HMF can reach 100% under the conditions of 1 MPa-4 MPa and 200° C. for 3 hours. When H 2 When the pressure is 1.0MPa, it also has good catalytic activity, and the DMF yield can reach 78%; when H 2 When the pressure increased to 2.0MPa, the yield of DMF reached 97%. Explain that 2.0MPa H in the reaction...

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Abstract

The invention relates to a method for preparing 2, 5-dimethylfuran through catalytic hydrogenation of 5-hydroxymethylfurfural, i.e., 5-hydroxymethylfurfural is subjected to selective hydrogenation reaction under the action of a NiFe and reduced graphene oxide composite material catalyst to generate 2, 5-dimethylfuran. The NiFe/rGO catalyst does not need to be subjected to high-temperature pre-reduction treatment before being used, reaction is carried out for 3 h under the conditions of 200 DEG C and the hydrogen pressure of 2 MPa, the conversion rate of 5-hydroxymethylfurfural can reach 100%, and the yield and selectivity of 2, 5-dimethylfuran can reach 97%. The NiFe/rGO catalyst needing no reduction pretreatment has higher catalytic activity and selectivity than Ni/rGO, Fe/rGO, NiFe/Al2O3, NiFe/HY and NiFe/SiO2 catalysts, is cheaper than noble metal catalysts such as Pt and Pd, and has industrial application value.

Description

technical field [0001] The invention relates to the field of 2,5-dimethylfuran preparation, in particular to a method for preparing 2,5-dimethylfuran by catalytically hydrogenating 5-hydroxymethylfurfural. Background technique [0002] At present, the increasing depletion of fossil resources and the greenhouse effect and air pollution caused by large-scale use have become the focus of world attention. Therefore, the development of green and efficient renewable energy has become a hot spot in future scientific research. Biomass energy is different from wind energy, water energy, tidal energy, nuclear energy and other new energy sources. It is the only renewable energy that can replace petroleum and continuously supply human hydrocarbons. It has a wide range of sources and is in line with the concept of green chemical development in the process of use. Effective integration and utilization of biomass resources can meet the energy needs of the future society and is an importan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/36B01J23/755B01J37/12B01J37/16B01J37/02B01J37/00B01J37/08
CPCC07D307/36B01J23/755B01J37/12B01J37/16B01J37/0213B01J37/0036B01J37/088Y02P20/584
Inventor 周锦霞吕洋毛璟博李慎敏尹静梅
Owner DALIAN UNIV
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