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Method for high-efficiency hydrogen reduction preparation of transition metal oxide defects

A transition metal and oxide technology, applied in the field of efficient hydrogen reduction to prepare transition metal oxide defects, can solve the problems of uneconomical practicability, high energy consumption and high equipment requirements

Active Publication Date: 2017-06-20
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Now it is common to use high temperature (>400°C) high pressure (20.0bar) high-purity hydrogen conditions to dissociate hydrogen into hydrogen atoms on the surface of transition metal oxides for the preparation of defects in transition metal oxides, which generally have high energy consumption and equipment requirements high, not economical and practical

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  • Method for high-efficiency hydrogen reduction preparation of transition metal oxide defects
  • Method for high-efficiency hydrogen reduction preparation of transition metal oxide defects
  • Method for high-efficiency hydrogen reduction preparation of transition metal oxide defects

Examples

Experimental program
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Effect test

Embodiment 1

[0056] Weigh 0.5g rutile TiO 2 (R), dispersed into 500ml of ethylene glycol solution by ultrasonic or stirring. Then add 25mgNa 2 PdCl 4 , stirred for 6h. 5g of polyvinylpyrrolidone was added to the above mixed solution and stirred for 2h. The above mixed solution was heated to 180°C, stirred and refluxed for 2h. The above solution was centrifuged, the supernatant was poured off to collect the precipitate, and washed with ethanol and deionized water for 3 to 6 times, and after vacuum drying, the powder was calcined at 500° C. for 2 hours. Obtaining rutile TiO loaded with Pd noble metal 2 (R / Pd). Put R / Pd at normal pressure H 2 / Ar(10vol%H 2 ) under the airflow (80cm 3 / min) room temperature treatment for 20min, you can get rutile TiO with a lot of defects 2 (H-R / Pd).

Embodiment 2

[0058] Weigh 0.5g CeO 2 , and dispersed into 500ml of ethylene glycol solution by ultrasonic or stirring. Then add 25mg Na 2 PdCl 4 , stirred for 6h. 5g of polyvinylpyrrolidone was added to the above mixed solution and stirred for 2h. The above mixed solution was heated to 180°C, stirred and refluxed for 2h. The above solution was centrifuged, the supernatant was poured off to collect the precipitate, and washed with ethanol and deionized water for 3 to 6 times, and after vacuum drying, the powder was calcined at 500° C. for 2 hours. Obtaining CeO loaded with Pd noble metal 2 (CeO 2 / Pd). CeO 2 / Pd at atmospheric pressure H 2 / Ar(10vol%H 2 ) under the airflow (80cm 3 / min) at room temperature for 20 minutes, you can get CeO containing a large amount of low-valent reduced state 2 (H-Ce / Pd).

Embodiment 3

[0060] Weigh 0.5g WO 3 , and dispersed into 500ml of ethylene glycol solution by ultrasonic or stirring. Then add 25mg Na 2 PdCl 4 , stirred for 6h. 5g of polyvinylpyrrolidone was added to the above mixed solution and stirred for 2h. The above mixed solution was heated to 180°C, stirred and refluxed for 2h. The above solution was centrifuged, the supernatant was poured off to collect the precipitate, and washed with ethanol and deionized water for 3 to 6 times, and after vacuum drying, the powder was calcined at 500° C. for 2 hours. Obtain WO loaded with Pd noble metal 3 (WO 3 / Pd). WO 3 / Pd at atmospheric pressure H 2 / Ar(10vol%H 2 ) under the airflow (80cm 3 / min) Treated at room temperature for 20 minutes, you can get WO containing a large amount of low-valent reduced state 3 (H-WO 3 / Pd).

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Abstract

The invention relates to a method for high-efficiency hydrogen reduction preparation of transition metal oxide defects, wherein the method includes the steps: loading with a noble metal to obtain a noble metal-loaded transition metal oxide, and carrying out a reduction reaction of the obtained noble metal-loaded transition metal oxide in a reductive atmosphere, to obtain a transition metal oxide containing defects. The noble metal is loaded to the transition metal oxide, so a reaction potential barrier of turning molecular hydrogen into atomic hydrogen can be reduced to a great extent, then the transition metal oxide material having a large number of defects (including the transition metal low valence reduction state and oxygen vacancies) can be prepared by hydrogen reduction with an ordinary hydrogen argon atmosphere under conditions of room temperature and ordinary pressure, and the defects can stably exist for a long term. The method is simple and feasible to implement, ingenious and novel, low in cost and high in efficiency, and the prepared the defect transition metal oxide has a strong catalytic stability.

Description

technical field [0001] The invention provides a method for rapidly preparing a large amount of defective metal oxides in a common reducing atmosphere (such as hydrogen-argon atmosphere) under room temperature or low temperature heating. Metal oxides have strong catalytic stability. The invention belongs to the fields of nanotechnology and environmental energy, and relates to a method for preparing transition metal oxide defects by hydrogen reduction. Background technique [0002] Transition metal oxides play an important role in the field of catalysis. They are widely used as main catalysts, cocatalysts and supports. However, the relationship between the reduced state in the structure and defects such as oxygen vacancies and their catalytic activity has been widely concerned. Taking titanium oxide as an example, the low-valent reduced Ti in its structure 3+ The generation of intermediate energy levels by substances and oxygen vacancies can significantly improve its absorpt...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/63B01J23/652
Inventor 徐颖峰张玲霞施剑林魏晨阳
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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