Method for synthesizing MOF derivative semiconductor heterojunction material by solvothermal method

A solvothermal method and MOF technology are applied in the preparation of MOF derivative semiconductor heterojunction materials and the preparation of new catalytic materials. Harsh and other problems, to achieve broad scientific research and practical value, suitable for large-scale mass production, the effect of simple instruments

Active Publication Date: 2020-06-09
UNIV OF SCI & TECH BEIJING
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  • Abstract
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Problems solved by technology

[2] At present, there are many reports on the synthesis of semiconductor heterojunction materials, Subha N et al. [3] Using titanium isopropoxide hydrolysis and strontium nitrate as titanium source and strontium source to hydrothermally synthesize SrTiO3 / TiO2 heterojunction materials, this method heats and crystallizes the mixed solution to obtain titanium oxide with rutile crystal form and different morphology Regular and less porous, resulting in limited catalytic performance of the product
Meanwhile, XW Lou et al. [4] During the preparation process, the Ti-Fe-O nanoparticles are converted into a heterostructured Fe2TiO5 / TiO2 by a post-annealing process. The heterogeneous structure obtained in this way cannot ensure the uniform distribution of active sites so as to affect the subsequent photocatalytic reaction.
R Li et al. [5] Using TiO2 nanotubes as templates and reactants, BaTiO3 / TiO2 heterostructure nanotube arrays were prepared by in situ hydrothermal method. accomplish
So far, the preparation of semiconductor heterojunction materials by Ti-MOF by solvothermal method has not been reported

Method used

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  • Method for synthesizing MOF derivative semiconductor heterojunction material by solvothermal method

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Experimental program
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Effect test

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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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/04B01J23/745B01J23/02
CPCB01J23/02B01J23/04B01J23/745B01J35/004
Inventor 于然波何奕磊王祖民张行魏延泽
Owner UNIV OF SCI & TECH BEIJING
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