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Preparation method and application of P-type pyrenyl metal organic framework single crystal material and nanobelt

A technology of single crystal materials and organic frameworks, applied in the direction of non-metallic elements, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low efficiency of photolysis of water and reduce the recombination in the body , reduced transfer distance, good chemical stability

Active Publication Date: 2022-03-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0004] Aiming at the problem of low photolysis water efficiency of semiconductor photocatalysts at present, it is committed to solving the charge separation of photolysis water. The present invention provides a P-type pyrene-based metal organic The preparation method of framework single crystal material and nanobelt, the photosensitivity ligand (H4TBAPy) is used as the light-harvesting center and [Ni3O16] Nickel-oxygen clusters as the catalytic center to form a new type of MOFs single crystal (Ni-TBAPy-SC) photocatalyst, the single crystal catalyst formed nanobelts (Ni-TBAPy-NB) after simple ultrasonic exfoliation, the MOFs nano Photo-splitting water reduction reaction can be carried out without supporting co-catalyst

Method used

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  • Preparation method and application of P-type pyrenyl metal organic framework single crystal material and nanobelt
  • Preparation method and application of P-type pyrenyl metal organic framework single crystal material and nanobelt
  • Preparation method and application of P-type pyrenyl metal organic framework single crystal material and nanobelt

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Embodiment 1

[0039] The pyrene-derived ligand 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene H 4 TBAPy (20mg, 0.030mmol) and NiSO 4 ·6H 2 O (5.3mg, 0.02mmol) was placed in a 25mL polytetrafluoroethylene reactor liner, and the mixed solvent deionized water (0.5mL), 1,4-dioxane (0.5mL) and N,N - Dimethylformamide (1mL), put the inner lining in the stainless steel reactor shell and transfer it to a temperature-programmed oven, raise the temperature from room temperature to 120°C at a rate of 30°C / h, keep it warm for 72h, and then heat it at 2°C Cool to room temperature at a rate of 1 / h to generate yellow diamond-shaped crystals, centrifuge, wash, and dry at room temperature to obtain a product named Ni-TBAPy-SC with a yield of 37%.

[0040] Ni-TBAPy-SC single crystal has a layered structure, triclinic crystal system, P-1 space group, and the specific structure of the crystal product is as follows figure 1 shown. Depend on figure 1 a It can be seen that the smallest asymmetric single atom in the...

Embodiment 2

[0043] Place Ni-TBAPy-SC single crystal in a mixed solution of methanol (90mL), water (10mL) and ascorbic acid (264mg) and sonicate for 5min, centrifuge and wash the suspension 3 times, and freeze-dry to obtain Ni-TBAPy- NB nanoribbons.

[0044] The XRD patterns, transmission electron microscopy (TEM) and atomic force microscopy (AFM) patterns of the experimentally synthesized Ni-TBAPy-NB nanobelts are as follows: image 3 with Figure 4 , it can be seen from the TEM and AFM test images that the Ni-TBAPy-NB nanobelt has a regular rectangular shape, the length and width are 2μm and 100nm, and the thickness is 60nm; the specific surface area test results of the Ni-TBAPy-NB nanobelt are as follows Figure 5 , the specific surface area is 548m 2 g -1 .

Embodiment 3

[0046] Ni-TBAPy-NB nanoribbon stability test:

[0047] Weigh 10mg of Ni-TBAPy-NB nanobelts and soak them in 10mL of aqueous solutions with different pHs and in organic solvents such as methanol, ethanol, DMF, acetonitrile, acetone, and dichloromethane for 24 hours, then dry them by centrifugation, and then test the samples after soaking for XRD , compared with the sample before immersion, the results are as follows Image 6 .

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Abstract

The invention discloses a P-type pyrenyl metal organic framework single crystal material and a preparation method and application of a nanobelt. The preparation method comprises the following steps: with H4TBAPy as a bridging ligand and transition metal ions Ni < 2 + > as metal nodes, synthesizing the metal organic framework single crystal material Ni-TBAPy-SC with a [Ni3O16] cluster two-dimensional double-layer structure through a solvothermal method. The Ni-TBAPy-NB nanobelt is successfully prepared through ultrasonic-assisted stripping, the prepared Ni-TBAPy-NB nanobelt has the characteristics that the dimension is low, a p-type semiconductor energy band is bent downwards, output of electrons in the water photolysis process is facilitated, and the electron-hole separation efficiency is improved. The Ni-TBAPy-NB nanobelt shows excellent performance of photocatalytic water decomposition for hydrogen production under the condition of no cocatalyst.

Description

technical field [0001] The invention relates to a preparation method and application of a P-type pyrene-based metal-organic framework single crystal material and a nanobelt, belonging to the technical field of catalytic materials. Background technique [0002] Using solar photocatalytic water splitting to produce green hydrogen is one of the ideal ways to solve the big problem of industrial decarbonization. The efficiency of inorganic semiconductor materials for photocatalytic water splitting to produce hydrogen is far below the goal of industrialization. The main challenge is that the photocatalytic reduction efficiency of most inorganic semiconductors is low, and it is usually necessary to support a cocatalyst as an active center for photocatalytic reaction, which will form an interface between the photocatalyst and the cocatalyst, resulting in energy loss, and the development of new types without cocatalyst The photocatalyst is imperative. [0003] Metal-organic framewo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C01B3/04
CPCB01J31/1691B01J31/223C01B3/042B01J2531/847Y02E60/36
Inventor 章福祥刘利芳郭向阳肖晔珺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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