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Method for preparing photocatalyst with monatomic Pt embedded into covalent organic framework and application of photocatalyst

A covalent organic framework, photocatalyst technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, catalyst activation/preparation, etc. Catalytic water splitting has problems such as low hydrogen production efficiency, low visible light absorption and utilization rate, etc., to achieve the effects of high reusability, short synthesis reaction time, and simple and convenient preparation method.

Pending Publication Date: 2022-05-27
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) At present, photocatalysts have low absorption and utilization efficiency of visible light in sunlight, high recombination rate of photogenerated electron-hole pairs, and few active sites of photocatalytic reaction, resulting in low efficiency of photocatalytic water splitting for hydrogen production;
[0009] (2) The current methods of synthesizing COF-based photocatalysts often require preparation under ultra-high vacuum conditions, harsh reaction conditions, long synthesis time, and high energy consumption, which are not suitable for large-scale actual production of photocatalysts

Method used

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  • Method for preparing photocatalyst with monatomic Pt embedded into covalent organic framework and application of photocatalyst
  • Method for preparing photocatalyst with monatomic Pt embedded into covalent organic framework and application of photocatalyst
  • Method for preparing photocatalyst with monatomic Pt embedded into covalent organic framework and application of photocatalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1 Preparation of TpPa-1-COF Photocatalyst

[0043] Weigh 434.8mg (ie 5mmol) of p-toluenesulfonic acid and 48.6mg (ie 0.9mmol) of p-phenylenediamine, grind for 5min, weigh 64.9mg (ie 0.6mmol) of 1,3,5-trialdehyde-based m-benzene Trisphenol, grind for 10 min, add 100 µL of deionized water dropwise, continue grinding to obtain an orange mud; transfer to a watch glass, react at 170 °C to obtain a dark red product, cool to room temperature, use N,N- Dimethylacetamide, deionized water, and acetone were washed in sequence for 2 each, and the product was dried in a blast drying oven at 60 °C overnight; fully ground for 20-30 min, and then incubated at 125 °C for 1 h under the protection of high-purity Ar. Cool to room temperature with the furnace to obtain a deep red photocatalyst.

Embodiment 2

[0044] Example 2 0.2% Pt 1 Preparation of @TpPa-1-COF Photocatalyst

[0045] Weigh 434.8mg (ie 5mmol) of p-toluenesulfonic acid and 48.6mg (ie 0.9mmol) of p-phenylenediamine, grind for 5min, weigh 64.9mg (ie 0.6mmol) of 1,3,5-trialdehyde-based m-benzene Trisphenol, triturated for 10min, will contain 9.5µL, 100mg•mL -1 H 2 PtCl 6 The solution was diluted to 100µL, added dropwise, and continued to grind to obtain an orange mud; transferred to a watch glass, and reacted at 170 °C for 6 min to obtain a dark red product, which was cooled to room temperature and treated with N,N-dimethylacetamide. , deionized water and acetone were washed twice each in turn, and the product was dried in a blast drying oven at 60°C overnight; fully ground for 20-30min, then kept at 125°C for 1 hour under the protection of high-purity Ar, and cooled to room temperature with the furnace , get dark red Pt 1 The @TpPa-1-COF photocatalyst, in which the loading of single-atom Pt is 0.2 wt%.

Embodiment 3

[0046] Example 3 0.5% Pt 1 Preparation of @TpPa-1-COF Photocatalyst

[0047] Weigh 434.8 mg (i.e. 5 mmol) of p-toluenesulfonic acid and 48.6 mg (i.e. 0.9 mmol) of p-phenylenediamine, grind for 5min, weigh 64.9 mg (i.e. 0.6 mmol) of 1,3,5-trialdehyde m-benzene Trisphenol, triturated for 10 min, will contain 23.9 µL, 100 mg•mL -1 H 2 PtCl 6 The solution was diluted to 100 µL, added dropwise, and continued to grind to obtain an orange slurry; transferred to a watch glass and reacted at 170 °C for 6 min to obtain a dark red product, which was cooled to room temperature and treated with N,N-dimethylethyl acetate. Amide, deionized water, and acetone were washed twice each in turn, and the product was dried in a blast drying oven at 60°C overnight; fully ground for 20-30min, then kept at 125°C for 1 hour under the protection of high-purity Ar, and cooled with the furnace to room temperature to obtain dark red Pt 1 The @TpPa-1-COF photocatalyst with single-atom Pt loading of 0.5...

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Abstract

The invention discloses a method for preparing a photocatalyst with monatomic Pt embedded into a covalent organic framework and application of the photocatalyst. A Pt-containing precursor solution is introduced in the process of preparing TpPa-1-COF, the Pt1 at TpPa-1-COF photocatalyst is obtained through low-temperature calcination and reduction, especially 3% of Pt1 at TpPa-1-COF, and the hydrogen production efficiency reaches 719 molg <-1 > h <-1 > and is 48 times that of water photolysis hydrogen production of a pure TpPa-1-COF catalyst. The preparation process is short in reaction time and mild in reaction condition, characterization tests such as XRD (X-Ray Diffraction) and a spherical aberration corrected high-angle annular dark field scanning transmission electron microscope (AC HAADF-STEM) graph show that the TpPa-1-COF material embedded with the monatomic Pt provides a large number of Pt active sites, favorable conditions are provided for catalyzing water to produce hydrogen, and the application prospect is good.

Description

technical field [0001] The invention relates to the technical field of new material preparation, in particular to a method for preparing a photocatalyst in which single-atom Pt is embedded in a covalent organic framework and its application. Background technique [0002] Solar energy has attracted widespread attention due to its non-polluting and easily accessible advantages. Converting solar energy into chemical energy by simulating photosynthesis in nature is an effective way to develop renewable energy. Facing the increasingly serious energy crisis and environmental problems, photocatalysis, as an ideal technology for clean energy, has achieved environmental purification and energy conversion, and has a good application prospect. [0003] As one of the ways to obtain sustainable new energy, hydrogen energy, photocatalytic water splitting technology has the advantages of green, economical and effective use of solar energy. In the photocatalytic water splitting and hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J23/42B01J37/16C01B3/04
CPCB01J31/06B01J23/42B01J37/16C01B3/042B01J35/39Y02P20/133Y02E60/36
Inventor 奚新国王艳董鹏玉张艾彩珺程婷
Owner YANCHENG INST OF TECH
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