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Preparation method of palladium modified porous niobium oxide material

A niobium oxide and pore-shaped technology, which is applied in chemical instruments and methods, preparation of imino compounds, catalyst activation/preparation, etc., can solve the problems of long preparation cycle of materials, achieve easy synthesis control, avoid acid-base conditions, and preparation methods simple effect

Pending Publication Date: 2022-03-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the solvent introduced during the introduction of palladium particles needs to be removed after treatment, and the material preparation cycle is relatively long
At present, there are few reports on the preparation of palladium-modified niobium oxide materials by one-step method

Method used

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  • Preparation method of palladium modified porous niobium oxide material
  • Preparation method of palladium modified porous niobium oxide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Disperse 0.6306g of melamine, 0.5380g of niobium oxalate and 0.0230g of palladium nitrate in 30mL of ethanol and stir, transfer the mixture into a round bottom flask, and dry the solvent in an oil bath at 105°C. After drying, cool to room temperature, transfer to a crucible, increase the heating rate of 10 °C / min to 650 °C and bake for 4 hours, and cool to room temperature to obtain a palladium-modified porous niobium oxide material. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the pore volume of the sample. Before the test, the sample was vacuum-processed at 120°C for more than 12h to make the vacuum degree reach 10 -6 about torr, and then tested at the temperature of liquid nitrogen (-196°C). Nitrogen adsorption and desorption experiments show that the material has a pore volume of 0.22 cm 3 / g, the pore size distribution is 1-24nm. The morphology of the samples was observed using a JEM-2100F transmission electron microscope. Before th...

Embodiment 2

[0018] Disperse 1.0090g of melamine, 0.3030g of ammonium niobium oxalate and 0.0225g of palladium acetate in 30mL of ethanol and stir. Transfer the mixture into a round bottom flask and dry the ethanol solvent in an oil bath at 105°C. After the solvent is dried, cool to room temperature, transfer to a crucible, increase the heating rate of 10 °C / min to 650 °C for 4 hours, and cool to room temperature to obtain a palladium-modified porous niobium oxide material. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the pore volume of the sample. Before the test, the sample was vacuum-processed at 120°C for more than 12h to make the vacuum degree reach 10 -6 about torr, and then tested at the temperature of liquid nitrogen (-196°C). Nitrogen adsorption and desorption experiments show that the material has a pore volume of 0.26 cm 3 / g, the pore size distribution is 1-28nm. The morphology of the samples was observed using a JEM-2100F transmission electron m...

Embodiment 3

[0020] Disperse 1.2612g of melamine, 0.3182g of niobium ethoxide and 0.0305g of palladium acetylacetonate in 30mL of ethanol and stir, transfer the mixture into a round bottom flask, and dry the ethanol solvent in an oil bath at 105°C. After the solvent is dried, cool to room temperature, transfer to a crucible, increase the heating rate of 10 °C / min to 650 °C for 4 hours, and cool to room temperature to obtain a palladium-modified porous niobium oxide material. Micromeritics ASAP 2010 physical adsorption instrument was used to measure the pore volume of the sample. Before the test, the sample was vacuum-processed at 120°C for more than 12h to make the vacuum degree reach 10 -6 about torr, and then tested at the temperature of liquid nitrogen (-196°C). Nitrogen adsorption and desorption experiments show that the material has a pore volume of 0.35 cm 3 / g, the pore size distribution is 2-37nm. The morphology of the samples was observed using a JEM-2100F transmission electron ...

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Abstract

The invention relates to a preparation method of a palladium modified porous niobium oxide material. The preparation method of the material utilizes a one-step roasting method and comprises the following steps: dispersing melamine, a compound containing Nb < 5 + > and palladium-containing metal salt in ethanol, evaporating the ethanol, transferring into a crucible, heating from room temperature to 500-700 DEG C, and roasting for 1-10 hours. And cooling to room temperature to obtain the palladium modified porous niobium oxide material. The material is of a porous sheet structure and has potential application in the fields of catalysis, capacitors, sensors and the like.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a preparation method of a palladium-modified porous niobium oxide material. Background technique [0002] Palladium-modified niobium oxide materials have great application prospects in the field of catalysis, sensors and electrode batteries due to their unique acidic and redox properties. Specifically, for the catalytic process, the porous structure on the catalyst is conducive to the exposure of active sites and the adsorption of substrates, thereby increasing the reaction rate. In addition, small-sized palladium particles exhibit unique activity in the reaction (Nat. Commun. 2020, 11, 48.). Therefore, compared with larger palladium-modified niobium oxide materials, in some cases, the preparation of specific small-particle palladium-modified porous niobium oxide materials will show more excellent performance in catalytic reactions. [0003] The preparati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/648B01J35/10B01J37/08C01G33/00B82Y30/00C07C249/02C07C251/24
CPCB01J23/6484B01J37/088B01J37/082C01G33/00B82Y30/00C07C249/02C01P2004/80C01P2006/14C01P2006/17B01J35/40B01J35/60B01J35/633B01J35/643B01J35/647B01J35/67C07C251/24
Inventor 王峰苏凯艺高著衍刘诗阳王雪原
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI