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Metal organic framework Mn-MOF single-crystal material, nanosheet, preparation and application

A metal-organic framework and single-crystal material technology, which is applied in the field of photocatalytic materials to achieve the effects of simple and easy preparation method, good photocatalytic water splitting hydrogen production performance, and adjustable thickness range

Active Publication Date: 2021-03-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the preparation of two-dimensional MOF nanosheets by ultrasonic exfoliation and their use as photocatalysts in the field of photocatalytic water splitting have not been reported in Chinese patents.

Method used

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  • Metal organic framework Mn-MOF single-crystal material, nanosheet, preparation and application
  • Metal organic framework Mn-MOF single-crystal material, nanosheet, preparation and application
  • Metal organic framework Mn-MOF single-crystal material, nanosheet, preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: Synthesis of metal organic framework Mn-MOF single crystal material

[0048] Weigh manganese chloride tetrahydrate (29.7mg, 0.15mmol), H 4tbapy (66.6mg, 0.1mmol) was added to a 25ml polytetrafluoroethylene-lined hydrothermal reactor, followed by adding 2ml N,N-dimethylformamide, 1ml 1,4-dioxane and 1ml water, Transfer the polytetrafluoroethylene-lined hydrothermal reactor to the oven, and use the programmed temperature control method to raise the temperature from room temperature to 130°C at a heating rate of 40°C / h, then keep it warm for 72h, and the cooling rate is 2°C / h, down to At room temperature, yellow crystals were obtained. After washing with N,N-dimethylformamide, suction filtration, and natural drying at room temperature, the target material Mn-MOF was obtained with a yield of about 85% (based on H 4 calculated by tbapy). The prepared metal-organic framework Mn-MOF single crystal material structure is as follows figure 1 As shown, the Mn-MOF ...

Embodiment 2

[0052] Embodiment 2: Preparation of Mn-MOF nanosheets

[0053] Weigh 50 mg of the Mn-MOF single crystal material prepared in Example 1, and add it to 3 ml of acetonitrile and water in a mixed solvent whose ratios are 1:0, 6:1, 5:1, and 4:1, that is, the ratio of acetonitrile and water The volumes are 3ml and 0ml, 2.57ml and 0.43ml, 2.5ml and 0.5ml, 2.4ml and 0.6ml respectively, and the Mn-MOF nanosheet sample Mn -M-2h, Mn-M-H-6-1-2h, Mn-M-H-5-1-2h, Mn-M-H-4-1-2h.

[0054] This example mainly investigates the effect of the ratio of acetonitrile and water on the morphology of the prepared Mn-MOF nanosheets. The TEM photos of Mn-MOF nanosheets prepared under different solvent ratios are shown in Figure 5 , the figure shows that the addition of water has a significant effect on the morphology of Mn-MOF nanosheets, and the sample Mn-M-H-5-1-2h prepared when the ratio of acetonitrile and water is 5:1 has the most regular rectangular shape. The XRD patterns of Mn-MOF nanosheets p...

Embodiment 3

[0055] Embodiment 3: Preparation of Mn-MOF nanosheets

[0056] Measure 2.5ml of acetonitrile and 0.5ml of water to prepare a total of 3ml of acetonitrile and water mixed solution, weigh 50mg of the Mn-MOF single crystal material prepared in Example 1, and add it to the above mixed solution. When the ultrasonic frequency is 40kHz and the output power is Under the condition of 500W, ultrasonic 2h, 3h, 4h, 5h, respectively, to obtain Mn-MOF nanosheet samples Mn-M-H-5-1-2h, Mn-M-H-5-1-3h, Mn-M-H-5-1- 4h, Mn-M-H-5-1-5h.

[0057] This example mainly investigates the effect of ultrasonic time on the preparation of Mn-MOF nanosheets when the ratio of acetonitrile and water is 5:1. The TEM photos of Mn-MOF nanosheets prepared under different ultrasonic times are shown in Figure 7 , the figure shows that the prepared Mn-MOF nanosheets are all regular rectangular thin flakes, and the ultrasonic time has no significant effect on the shape size of the nanosheets. The thickness of the M...

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Abstract

The invention provides a metal organic framework MnMOF single crystal material, a nanosheet, preparation and application. The preparation method comprises the following steps of: dissolving manganesechloride and / or manganese chloride tetrahydrate and a ligand 1, 3, 6, 8-4-(4-carboxyl benzene) pyrene (H4tbapy) in a mixed solvent of N, N-dimethylformamide, 1, 4-dioxane and water; carrying out solvothermal reaction under program temperature control; slowly cooling to room temperature after the reaction is stopped; carrying out washing, suction filtration and drying on separated crystals to obtain a Mn-MOF single-crystal material; and then adding the obtained Mn-MOF crystal into a mixed solvent of acetonitrile and water or an acetonitrile solvent for ultrasonic treatment to obtain a Mn-MOF nanosheet. The Mn-MOF nanosheet prepared by the method is regular in morphology and adjustable in thickness range, and has higher photocatalytic water splitting hydrogen production performance comparedwith a Mn-MOF single-crystal material of a body. The synthesis method provided by the invention has the advantages of mild conditions, simple operation, high catalytic activity and the like.

Description

technical field [0001] The invention relates to a metal-organic framework Mn-MOF single crystal material and nanosheets as well as their preparation and application, in particular to a MOFs material for photocatalytic water splitting and a preparation method thereof, belonging to the field of photocatalytic materials. Background technique [0002] Hydrogen production from solar photocatalytic water splitting has attracted much attention as a feasible solution to today's energy problems. Two-dimensional materials show unique advantages in the field of photocatalytic water splitting due to their ultra-thin thickness and large specific surface area. The ultra-thin thickness can shorten the migration distance of photogenerated carriers and inhibit the recombination process of carriers, while the larger specific surface area means that more reaction sites are exposed. Therefore, compared with bulk materials, 2D nanosheet materials usually have better photocatalytic performance. ...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/22
CPCB01J31/2239B01J2531/72C08G83/008
Inventor 李灿章福祥肖晔珺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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