Method for synthesizing MOF derivative semiconductor heterojunction material by solvothermal method

Abstract

The invention discloses a method for synthesizing an MOF derivative semiconductor heterojunction material by a solvothermal method, which belongs to the field of catalyst materials. The method specifically comprises the following steps: carrying out hydrothermal crystallization on a mixed reaction system of a soluble ligand organic matter dissolved in an organic solvent and tetra-n-butyl titanate;and washing and drying the obtained product, carrying out continuous two-step calcination in air, dissolving the calcined product and a metal compound in an alkaline solution containing an alcohol solvent, carrying out hydrothermal crystallization for a period of time, washing for multiple times, and finally drying the solid to obtain the target product. The MOF derivative semiconductor heterojunction material product obtained by the method is high in chemical stability and excellent in photocatalytic performance, and the preparation method has the characteristics of simple process flow, lowcost and high product yield.

Description

[0001] Technical field

[0002] The invention belongs to the field of catalyst materials, and relates to a method for preparing a novel catalyst material, in particular to a method for preparing a MOF derivative semiconductor heterojunction material synthesized by a solvothermal method. Background technique

[0003] Metal-organic frameworks (MOFs), also known as porous coordination polymers (PCPs), are synthesized from secondary building blocks (SBUs), metal cation salts or clusters, and multidentate organic ligands with coordination-type linkages. 2D or 3D porous crystalline materials. Due to its metal center, highly ordered porous structure, uniform pore size and environment, extremely high specific surface area and functional organic linking groups, tailorability, and ultra-high specific surface area, MOFs are excellent catalyst templates. . In recent years, MOFs derivatives have shown potential application prospects in many research fields, especially the in-depth resear...

Examples

Embodiment 1

[0034] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, and soak the product (1mmol) in a solution containing Sr(OH) 2 8H2O (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, crystallized After the chemica...

Embodiment 2

[0036] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, soak the product (1mmol) in a solution containing Fe(OH) 2 (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, and the crystallization was completed F...

Embodiment 3

[0038] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, and soak the product (1mmol) in a solution containing Ba(OH) 2 (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, and the crystallization was complete...

[0001] Technical field

[0002] The invention belongs to the field of catalyst materials, and relates to a method for preparing a novel catalyst material, in particular to a method for preparing a MOF derivative semiconductor heterojunction material synthesized by a solvothermal method. Background technique

[0003] Metal-organic frameworks (MOFs), also known as porous coordination polymers (PCPs), are synthesized from secondary building blocks (SBUs), metal cation salts or clusters, and multidentate organic ligands with coordination-type linkages. 2D or 3D porous crystalline materials. Due to its metal center, highly ordered porous structure, uniform pore size and environment, extremely high specific surface area and functional organic linking groups, tailorability, and ultra-high specific surface area, MOFs are excellent catalyst templates. . In recent years, MOFs derivatives have shown potential application prospects in many research fields, especially the in-depth resear...

Examples

Embodiment 1

[0034] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, and soak the product (1mmol) in a solution containing Sr(OH) 2 8H2O (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, crystallized After the chemica...

Embodiment 2

[0036] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, soak the product (1mmol) in a solution containing Fe(OH) 2 (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, and the crystallization was completed F...

Embodiment 3

[0038] At 25°C, weigh 2.49g of terephthalic acid (PTA) (15mmol) and 2.56mL of tetra-n-butyl titanate (7.5mmol) in 45mL of N,N-dimethylformaldehyde containing 0.87mL of acetic acid (15mmol). Amide (DMF) and 5mL of anhydrous methanol, placed in an ultrasonic machine, mixed and stirred until completely dissolved, transferred to a crystallization kettle, crystallized at 180°C for 16h, after the crystallization was completed, centrifuged and dried for 24h to obtain MIL-125 material; then calcined in a muffle furnace: first, the heating rate is 0.5-1°C / min, raised to 250-300°C, and kept for 0.5-1.5h; then, the heating rate is 0.5-2°C / min, raised to 450 -480°C, keep warm for 0.5-1.5h, and soak the product (1mmol) in a solution containing Ba(OH) 2 (1mmol) in 10mL deionized water, 10mL ethylene glycol, 2mL 1,2-propanediol and 2g tetrabutylammonium hydroxide solution (TBAH, 25wt), transferred to a crystallization kettle, crystallized at 160°C for 4h, and the crystallization was complete...

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