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Dye solvent heat-sensitive MOFs photocatalyst, preparation method and application thereof

A photocatalyst and solvothermal technology, which is applied in physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of poor visible light absorption capacity and improve visible light catalysis Effects of hydrogen production activity, improved stability, and easy operation

Active Publication Date: 2020-04-07
XI AN JIAOTONG UNIV
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  • Abstract
  • Description
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Problems solved by technology

[0005] Aiming at the wide band gap of MOFs materials, poor visible light absorption ability, and easy defects, the present invention provides a dye-solvent thermally sensitized MOFs photocatalyst and its preparation method and application. The present invention utilizes the solvent-thermally sensitized dye under high temperature conditions for the first time MOFs, greatly improved the visible light absorption capacity and stability of MOFs, thus greatly improving the visible light catalytic hydrogen production activity of MOFs

Method used

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  • Dye solvent heat-sensitive MOFs photocatalyst, preparation method and application thereof
  • Dye solvent heat-sensitive MOFs photocatalyst, preparation method and application thereof
  • Dye solvent heat-sensitive MOFs photocatalyst, preparation method and application thereof

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preparation example Construction

[0028] A kind of preparation method of dye solvent heat-sensitized MOFs photocatalyst of the present invention, the steps are as follows:

[0029] Step 1: Synthesis of MOFs (UiO-66-NH 2 For example): add 0.2-0.5g zirconium chloride hexahydrate and 10-50mL N,N-dimethylformamide (DMF) polytetrafluoroethylene hydrothermal kettle lining, ultrasonic 20min zirconium chloride completely After dissolving, add 1-8mL concentrated hydrochloric acid dropwise, then add 0.1-0.5g 2-aminoterephthalic acid (H 2 APTA) and 10-30mL DMF, continue to sonicate for 20min. Next, transfer the lining of the hydrothermal kettle to the outer shell of the stainless steel hydrothermal kettle, seal it, and keep it in an oven at 60-120° C. for 12-48 hours. After the reaction was completed, the obtained pale yellow suspension was centrifuged, and the precipitate was washed 3 times with DMF and 3 times with methanol. The yellow sample obtained by centrifugation was dried at 85°C to obtain UiO-66-NH 2 (This ...

Embodiment 1

[0034] Embodiment 1 is the standard preparation method that the present invention uses

[0035] Step 1: Add 0.268g of zirconium chloride hexahydrate to the inner lining of 20mL DMF polytetrafluoroethylene hydrothermal kettle, ultrasonically dissolve the zirconium chloride for 20 minutes, add 2mL of concentrated hydrochloric acid dropwise, and then add 0.250g of 2-amino p- Phthalic acid (H 2 APTA) and 10mL DMF, continue to sonicate for 20min. Next, transfer the inner lining of the hydrothermal kettle to the outer shell of the stainless steel hydrothermal kettle, seal it, and keep it in an oven at 80°C for 24 hours. After the reaction was completed, the obtained pale yellow suspension was centrifuged, and the precipitate was washed 3 times with DMF and 3 times with methanol. The yellow sample obtained by centrifugation was dried at 85°C to obtain UiO-66-NH 2 .

[0036] Step 2: Add EY and MOF to the lining of a hydrothermal kettle containing 20mL of ethanol according to the m...

Embodiment 2

[0038] Embodiment 2 is the preparation method that has changed concentrated hydrochloric acid amount

[0039] Step 1: Add 0.268g of zirconium chloride hexahydrate to the lining of 20mL DMF polytetrafluoroethylene hydrothermal kettle, ultrasonically dissolve the zirconium chloride for 20min, add 1mL of concentrated hydrochloric acid dropwise, and then add 0.250g of 2-amino p- Phthalic acid and 10mL DMF, continue to sonicate for 20min. Next, transfer the inner lining of the hydrothermal kettle to the outer shell of the stainless steel hydrothermal kettle, seal it, and keep it in an oven at 80°C for 24 hours. After the reaction was completed, the obtained pale yellow suspension was centrifuged, and the precipitate was washed 3 times with DMF and 3 times with methanol. The yellow sample obtained by centrifugation was dried at 85°C to obtain UiO-66-NH 2 .

[0040] Step 2: Add EY and MOF to the lining of a hydrothermal kettle containing 20mL of ethanol according to the mass ratio...

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Abstract

The invention provides a dye solvent heat-sensitive MOFs photocatalyst, a preparation method and application thereof. The method includes: adding dye and MOF into a hydrothermal kettle lining containing a solvent for ultrasonic treatment, then loading the hydrothermal kettle lining into a hydrothermal kettle, conducting heat preservation at 80-200DEG C for 6-48h, and then performing natural cooling to the room temperature; at the end of the reaction, washing the precipitate until the washing liquid is colorless and transparent; and drying the washed sample to obtain the dye solvent heat-sensitive MOF photocatalyst. The visible light catalytic activity of the photocatalyst is as high as 2760micromolh<-1>g<-1>, which is 8 times or more that of normal-temperature sensitization. The preparation method effectively improves the visible light catalytic hydrogen production activity of MOF, and at the same time improves the stability of MOF. The method is simple to operate and good in repeatability, and the application of the MOFs in the field of visible light catalytic hydrogen production is expanded.

Description

technical field [0001] The invention belongs to the field of hydrogen energy preparation, and relates to a photocatalytic clean preparation technology of hydrogen energy, that is, a photocatalytic hydrogen production technology using water as a raw material under the condition of simulating sunlight and visible light irradiation, in particular to a dye solvent thermally sensitized MOFs photocatalyst and Its preparation method and application. Background technique [0002] Hydrogen has the advantages of high energy density, easy storage and transportation, non-polluting combustion, clean and renewable, and is known as the most promising new energy in the 21st century. If the widely distributed and difficult-to-storage solar energy can be efficiently converted into clean and renewable hydrogen energy. Possible ways to produce hydrogen on a solar scale include photoelectrochemical water splitting for hydrogen production, solar photocatalytic water splitting for hydrogen produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C09K11/06C01B3/02
CPCB01J31/2208C09K11/06C01B3/042B01J2531/0213B01J2531/48C09K2211/1007C09K2211/1088B01J35/39Y02E60/36
Inventor 师进文李高升候路路陈丰关祥久
Owner XI AN JIAOTONG UNIV
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