Preparation method of defect-rich metal oxides and application thereof
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A technology of oxides and metals, applied in the field of preparation of functional catalytic materials, can solve the problems of safety, economy and environmental protection, etc., and achieve the effect of enriching catalytic active sites and large electronic structure
Active Publication Date: 2019-04-09
JIANGSU UNIV
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However, due to the use of hydrogen, metals, reducing agents, and oxidizing agents, the safety, economy, and environmental protection of the preparation process need to be improved.
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Embodiment 1
[0028] (1) Weigh urea and P25 (molar ratio 5:1) and mix them in a stainless steel ball mill tank, add zirconia balls (diameter 3mm, 20g), assemble in a planetary ball mill, set the speed at 450rpm, and the ball mill runs intermittently every 5 minutes , the intermittent time is 2.5 minutes, and the total running time is 4h.
[0029] (2) The ball-milled material is placed in a tubular electric furnace, and under the protection of nitrogen gas with a gas flow rate of 5mL / min, it is raised from room temperature to 900 °C at a rate of 5 °C / min, kept for 60 min, and cooled to room temperature. The gray matter obtained is the defect titanium dioxide material.
Embodiment 2
[0031] (1) Weigh urea and P25 (molar ratio 15:1) and mix them in a stainless steel ball mill tank, add zirconia balls (diameter 3mm, 20g), assemble them in a planetary ball mill, set the speed at 450rpm, and the ball mill runs intermittently every 5 minutes , the intermittent time is 2.5 minutes, and the total running time is 4h.
[0032] (2) The ball-milled material is placed in a tubular electric furnace, and under the protection of nitrogen gas with a gas flow rate of 5mL / min, it is raised from room temperature to 900 °C at a rate of 5 °C / min, kept for 60 min, and cooled to room temperature. The gray matter obtained is the defect titanium dioxide material.
Embodiment 3
[0034] (1) Weigh urea and P25 (molar ratio 30:1) and mix them in a stainless steel ball mill tank, add zirconia balls (diameter 3mm, 20g), assemble in a planetary ball mill, set the speed at 450rpm, and the ball mill runs intermittently every 5 minutes , the intermittent time is 2.5 minutes, and the total running time is 4h.
[0035] (2) The ball-milled material is placed in a tubular electric furnace, and under the protection of nitrogen gas with a gas flow rate of 5mL / min, it is raised from room temperature to 900 °C at a rate of 5 °C / min, kept for 60 min, and cooled to room temperature. The gray matter obtained is the defect titanium dioxide material.
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Abstract
The invention belongs to the field of preparation of catalysis materials and discloses a process for preparing defect-rich metal oxides by using a ball milling pyrolysis method with assistance of micromolecules such as urea and application of the defect-rich metal oxides to a deep oxidation and desulfurization process of diesel. The defect-rich metal oxides are characterized by taking metal oxidesas raw materials and taking urea and melamine as crystal phase transfer assistant agents; through a solid-phase ball milling process, interactions between the metal oxides and the assistant agents are enhanced; through adoption of the characteristics of extremely high possibility of decomposition and gasification of the assistant agents under high temperature and crystal lattice reconstruction ofthe metal oxides, an in-situ etching process of the metal oxides is achieved, so that a large number of crystal lattice defects are constructed on the surfaces of the metal oxides. The prepared defect-rich metal oxides have excellent catalysis effects on activation of air and oxidization and removal of aromatic sulfides in diesel; the method is simple in preparation process, free of strong acid,strong base and hydrogen and free of waste of metal resources, and is used as a green and pollution-free preparation process.
Description
technical field [0001] The invention relates to the field of preparation of functional catalytic materials, in particular to a method for preparing defect-rich metal oxides and its use for activating aromatic sulfides in air catalytic oxidation diesel oil. Background technique [0002] In recent years, transition metal oxides have attracted the attention of many researchers due to the existence of their non-stoichiometric forms. Today, 2014, 225, 2), and supercapacitors (J. Mater. Chem. A, 2014, 2, 229) and other hot research are widely used. In this type of material, the existence of lattice disorder and defects has a certain modulation effect on the electronic structure of metal oxides, which is of great significance for the improvement of its performance. Common methods for producing defect-type oxides include: hydrogen heat treatment, hydrogen plasma treatment, chemical oxidation and chemical reduction. [0003] Among them, the hydrogen heat treatment method and the hy...
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