Supported metal organic skeleton/graphene oxide hydrogen storage material and preparation method thereof

Abstract

The invention discloses a supported metal organic skeleton / graphene oxide hydrogen storage material and a preparation method thereof. The hydrogen storage material is formed by steeping palladium metal in a metal organic skeleton / graphene oxide carrier, wherein the loading capacity of the palladium metal is 1.0-5.0% of the mass of the carrier; and the metal organic skeleton is ZIF-8. The preparation method comprises the following steps: firstly heating reactants of dissolvable zinc salt, 2-methylimidazole and graphene oxide to prepare a metal organic skeleton / graphene oxide carrier material, and then loading dissolvable palladium salt in the metal organic skeleton / graphene oxide carrier to obtain the supported metal organic skeleton / graphene oxide hydrogen storage material under the condition of existence of a reductant and a dispersant by adopting an excessive steeping method. The supported metal organic skeleton / graphene oxide hydrogen storage material has good hydrogen storage performance at room temperature, and the process is simple.

Description

technical field

[0001] The invention belongs to the technical field of synthesis of hydrogen storage materials, and in particular relates to a loaded metal organic framework / graphene oxide hydrogen storage material and a preparation method thereof. Background technique

[0002] Hydrogen has attracted much attention as a green and renewable energy source. Metal-organic frameworks (MOFs) are considered promising hydrogen storage materials due to their high specific surface area, large porosity, and adjustable structure, such as Suh, M.P.; Park, H.J.; Prasad, T.K.; Lim, D.W. Chem. Rev., 2008, 112, 782. Unfortunately, the physical adsorption mechanism of MOFs can only store a large amount of hydrogen at extremely low temperatures, and its room temperature hydrogen storage capacity is extremely low. Hydrogen overflow technology has become a research hotspot in the field of hydrogen storage because it can significantly increase the hydrogen absorption capacity of MOFs at room tem...

Examples

Embodiment 1

[0023] (1) Dissolve 2.933 g of zinc nitrate and 4.867 g of 2-methylimidazole in 230 mL of methanol, then add 0.390 g of graphene oxide, and stir at 10° C. for 6 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0024] (2) Dissolve 8.38 mg of palladium chloride and 20.6 mg of polyvinyl alcohol in 42 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 15 mg of sodium borohydride, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

Embodiment 2

[0026] (1) Dissolve 2.933 g of zinc sulfate and 6.489 g of 2-methylimidazole in 280 mL of methanol, then add 0.471 g of graphene oxide, and stir at 30° C. for 4 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0027] (2) Dissolve 25.14 mg of tetrachloropalladium acid and 61.80 mg of polyvinyl alcohol in 126 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 45 mg of potassium borohydride, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

Embodiment 3

[0029] (1) Dissolve 2.933g of zinc chloride and 8.111g of 2-methylimidazole in 330mL of methanol, then add 0.552g of graphene oxide, and stir at 50°C for 2 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0030] (2) Dissolve 41.90 mg of palladium acetylacetonate and 103.00 mg of polyvinyl alcohol in 210 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 75 mg of hydrazine hydrate, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

[0031] The room temperature hydrogen storage test of the hydrogen storage materials prepared in Examples 1-3 was completed on the ASAP 2020 device of American Mike Company, and the samples were vacuum degassed at 160° C. for 24 h...

technical field

[0001] The invention belongs to the technical field of synthesis of hydrogen storage materials, and in particular relates to a loaded metal organic framework / graphene oxide hydrogen storage material and a preparation method thereof. Background technique

[0002] Hydrogen has attracted much attention as a green and renewable energy source. Metal-organic frameworks (MOFs) are considered promising hydrogen storage materials due to their high specific surface area, large porosity, and adjustable structure, such as Suh, M.P.; Park, H.J.; Prasad, T.K.; Lim, D.W. Chem. Rev., 2008, 112, 782. Unfortunately, the physical adsorption mechanism of MOFs can only store a large amount of hydrogen at extremely low temperatures, and its room temperature hydrogen storage capacity is extremely low. Hydrogen overflow technology has become a research hotspot in the field of hydrogen storage because it can significantly increase the hydrogen absorption capacity of MOFs at room tem...

Examples

Embodiment 1

[0023] (1) Dissolve 2.933 g of zinc nitrate and 4.867 g of 2-methylimidazole in 230 mL of methanol, then add 0.390 g of graphene oxide, and stir at 10° C. for 6 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0024] (2) Dissolve 8.38 mg of palladium chloride and 20.6 mg of polyvinyl alcohol in 42 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 15 mg of sodium borohydride, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

Embodiment 2

[0026] (1) Dissolve 2.933 g of zinc sulfate and 6.489 g of 2-methylimidazole in 280 mL of methanol, then add 0.471 g of graphene oxide, and stir at 30° C. for 4 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0027] (2) Dissolve 25.14 mg of tetrachloropalladium acid and 61.80 mg of polyvinyl alcohol in 126 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 45 mg of potassium borohydride, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

Embodiment 3

[0029] (1) Dissolve 2.933g of zinc chloride and 8.111g of 2-methylimidazole in 330mL of methanol, then add 0.552g of graphene oxide, and stir at 50°C for 2 hours. The centrifuged product was washed three times with methanol (10 mL each time) to prepare the ZIF-8 / graphene oxide carrier material.

[0030] (2) Dissolve 41.90 mg of palladium acetylacetonate and 103.00 mg of polyvinyl alcohol in 210 mL of deionized water, and stir for 1 hour. Then add 200 mg of ZIF-8 / graphene oxide, stir for 2 hours, then slowly add 75 mg of hydrazine hydrate, and stir for 5 hours. The centrifuged product was washed twice with water (10 mL each time), and dried at 60° C. for 24 hours to obtain a supported metal organic framework / graphene oxide hydrogen storage material.

[0031] The room temperature hydrogen storage test of the hydrogen storage materials prepared in Examples 1-3 was completed on the ASAP 2020 device of American Mike Company, and the samples were vacuum degassed at 160° C. for 24 h...

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