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High-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst as well as preparation method and application thereof

A layered titanate and surface modification technology, which is applied in the field of ammonia synthesis, can solve the problems that the nitrogen fixation reaction cannot proceed spontaneously and the kinetics are limited, and achieve mild and not harsh reaction conditions, low equipment requirements, and less time-consuming Effect

Inactive Publication Date: 2021-02-19
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the development of society, the above-mentioned natural nitrogen fixation process can no longer meet the increasing demand of human society for nitrogen-containing compounds, so how to remove N in the air 2 Convert to NH 3 become a research hotspot
N 2 reduced to NH 3 is an exothermic reaction (N 2 +3H 2 =2NH 3 , ΔH 298K =-92.22kJ / mol), from a thermodynamic point of view, hydrogen (H 2 ) participating N 2 The fixation reaction is very feasible, but the nitrogen fixation reaction does not proceed spontaneously at normal temperature and pressure, that is, it is very kinetically limited

Method used

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  • High-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst as well as preparation method and application thereof
  • High-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst as well as preparation method and application thereof
  • High-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of layered titanate nanosheets modified with deficient oxygen: Titanium foil and 50 mL of 5 M NaOH solution were placed in a high-pressure reactor, and then placed in an electric constant temperature blast drying oven at 180° C. for 10 h. After the reaction was completed and cooled to room temperature, the obtained sample was washed several times with ethanol, and the washed sample was calcined at 650° C. for 4 hours in an atmosphere of argon-hydrogen mixture (5% volume hydrogen) to obtain a layered oxygen-deficient modified layer. The transmission electron microscope image of titanate nanosheet HST is shown in Figure (1a). The mass of the prepared catalyst was 2 mg, and the proportion of deficient oxygen in all oxygen elements was 42.9%.

[0028] (2) Preparation of 0% highly dispersed ruthenium-loaded surface-modified layered titanate nanosheets Ru@HST: the HST obtained in step (1) was transferred to the bottom of the quartz reactor, and calcined at 150...

Embodiment 2

[0031] (1) Preparation of layered titanate nanosheets modified by deficient oxygen: same as in Example 1, the ratio of deficient oxygen to all oxygen elements is 42.9%.

[0032] (2) Preparation of 1% highly dispersed ruthenium-loaded surface-modified layered titanate nanosheets Ru@HST: Weigh 0.02 mg of triruthenium dodecacarbonyl and dissolve it in 1.5 mL of anhydrous tetrahydrofuran, and then mix the prepared solution with 2 mg of the catalyst was mixed, the sample was transferred to the bottom of the quartz reactor, the tetrahydrofuran was drained by a diaphragm pump, and the mixture was calcined at 150°C for 1 h under vacuum to obtain a layered titanate nanosheet photocatalyst with a highly dispersed ruthenium-loaded surface modification, the product The mass is 2.00 mg. The mass of metal ruthenium in the photocatalyst accounts for 1% of the mass of the whole catalyst (2 mg).

[0033] (3) The operation of the photocatalytic nitrogen fixation reaction: the quartz reactor eq...

Embodiment 3

[0035] (1) Preparation of layered titanate nanosheets modified by deficient oxygen: same as in Example 1, the ratio of deficient oxygen to all oxygen elements is 42.9%.

[0036] (2) Preparation of 5% highly dispersed ruthenium-loaded surface-modified layered titanate nanosheet Ru@HST: Weigh 0.1 mg triruthenium dodecacarbonyl and dissolve it in 1.5 mL anhydrous tetrahydrofuran, and then mix the prepared solution with 2 mg of the catalyst was mixed, the sample was transferred to the bottom of the quartz reactor, the tetrahydrofuran was drained by a diaphragm pump, and the mixture was calcined at 150°C for 1 h under vacuum to obtain a layered titanate nanosheet photocatalyst with a highly dispersed ruthenium-loaded surface modification, the product The mass is 2.00 mg. The mass of metal ruthenium in the photocatalyst accounts for 5% of the mass of the whole catalyst (2 mg).

[0037] (3) The operation of the photocatalytic nitrogen fixation reaction: the quartz reactor equipped w...

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Abstract

The invention discloses a high-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst, a preparation method and an application of the photocatalyst in a photocatalytic ammonia synthesis reaction, and belongs to the technical field of ammonia synthesis. The preparation method comprises the following steps: firstly, transferring a titanium source and low-concentrationalkali liquor into a polytetrafluoroethylene high-pressure reaction kettle, cooling to room temperature after hydrothermal reaction, washing with a solvent for multiple times, drying and annealing toobtain a layered titanate nanosheet with defect oxygen; and finally, mixing with a precursor solution of metal ruthenium, pumping out the solvent, and calcining to obtain the high-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst Ru-coated HST. The ruthenium nanoparticles are loaded on the surface of a layered titanate heterostructure nanosheet with defect oxygen, and the obtained catalyst is applied to a photocatalytic nitrogen fixation reaction technology. The nitrogen and hydrogen are activated through light driving, the nano-catalyst is designed and constructed, the catalyst is modified, efficient nitrogen fixation under mild conditions can be achieved, meanwhile, energy consumption is reduced, and environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of ammonia synthesis, and in particular relates to a highly dispersed ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst, a preparation method and its application in photocatalytic ammonia synthesis. Background technique [0002] Nitrogen, as an inert gas, is ubiquitous in the atmosphere. Considering that nitrogen accounts for 4 / 5 of the atmosphere, that is, more than 78% of the atmosphere, we can use almost unlimited amounts of nitrogen. Nitrogen is also present in various minerals in the form of nitrates, such as Chilean saltpeter (sodium nitrate), saltpeter (potassium nitrate), and minerals containing ammonium salts. Nitrogen is present in many complex organic molecules, including proteins and amino acids present in all living organisms. It is essential in life and its compounds are used as food or fertilizer. Nitrogen is commonly used to make ammonia and nitric acid. [0003] N...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/58B01J35/00B01J35/02C01C1/02
CPCB01J23/58B01J23/462C01C1/026B01J35/396B01J35/393B01J35/00B01J35/30B01J35/39Y02P20/52
Inventor 李路蔡爽
Owner JILIN UNIV
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