A kind of method for preparing 2,5-dimethylfuran by catalytic hydrogenation of 5-hydroxymethylfurfural
A technology of hydroxymethylfurfural and dimethylfuran, which is applied in the field of catalytic hydrogenation of 5-hydroxymethylfurfural to prepare 2,5-dimethylfuran, can solve the problem of high metal loading of tungsten carbide, large amount of catalyst, pressure Large and other problems, to achieve the effect of small amount of catalyst, simple process and high selectivity
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[0040] The preparation method of the supported bifunctional catalyst of the present invention uses 3wt% of Ni-MnO x / C catalyst (the ratio of the amount of Ni and Mn is 3:1) as an example: Ni-MnO prepared by co-impregnation method x / MC (Mesoporous Carbon) catalyst was prepared as follows: 1 g of 200-mesh mesoporous carbon was weighed, placed in a crucible, and calcined at 400° C. for 5 hours. Weigh 0.1115g Ni (NO 3 ) 2 ·6H 2 O placed in another crucible, added 0.7g deionized water, completely dissolved, weighed 0.0335g C 4 H 6 MnO 4 ·4H 2 O was added to the nickel nitrate solution, the nickel nitrate and manganese acetate were fully mixed, the ultrasonic wave was used to make them fully dissolved, the mesoporous carbon was added, and the Reduction in atmosphere for 3 hours to obtain Ni-MnO with a total metal loading of 3 wt% x / MC catalyst;
[0041] Preparation of Ni-MnO by a Step-by-Step Impregnation Method x / AC catalyst was prepared as follows, with 3wt% Ni-MnO ...
Embodiment 1
[0045] Get 0.126g (2mmol) 5-Hydroxymethylfurfural and place it in a beaker, add 6mL of tetrahydrofuran to dissolve, add the solution to a 25mL autoclave, add 0.252g of Ni-MnO with a load of 3wt% x / AC catalyst (the ratio of the amount of Ni and Mn was 3:1, the catalyst was prepared by the co-impregnation method), nitrogen was purged for five times, the reaction temperature was 180 ° C, the hydrogen pressure was 2.0 MPa, and the reaction was carried out for 3 hours. 2,5-dimethylfuran was obtained with a catalytic conversion frequency (TOF) of 50.7h -1 , the yield is 96.7%;
[0046] from figure 1 As can be seen in (a), Ni-MnO x / AC catalyst Ni 2p 3 / 2 It can be divided into two peaks, the corresponding electron binding energies are 853.3eV and 856.9eV, which are respectively attributed to Ni 0 and Ni 2+ . And Ni 2p of Ni / AC catalyst 3 / 2 belong to Ni 0 and Ni 2 + The corresponding electron binding energies of the two peaks are 853.0 eV and 856.6 eV, respectively. Ni 2p ...
Embodiment 2
[0049] Get 0.1260g (1mmol) 5-Hydroxymethylfurfural and place it in a beaker, add 6mL of tetrahydrofuran to dissolve, add the solution to a 25mL autoclave, add 0.025g of Ni-MnO with a load of 3wt% x / AC catalyst (the ratio of the amount of Ni and Mn is 3:1, the catalyst is prepared by the distributed impregnation method and the impregnation sequence is first impregnated with Ni and then impregnated with Mn), purged with nitrogen gas for five times, the reaction temperature is 180 ° C, the hydrogen pressure is 2.0MPa, and the reaction is performed for 3 hours to obtain 2,5-dimethylfuran, and the catalytic conversion frequency (TOF) is 52.9h -1 , the yield is 97.9%.
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