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Pt/TiN@CN catalyst with high oxygen reduction activity and preparation method thereof, and application of Pt/TiN@CN catalyst with high oxygen reduction activity

A catalyst and active technology, applied in the field of Pt/TiN@CN catalyst with high oxygen reduction activity and its preparation, can solve the problems of deactivation, limitation, and cost, and achieve improved stability and durability, increased specific surface area, and improved The effect of mechanical strength

Active Publication Date: 2019-07-12
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, platinum electrocatalysts are time-dependent, easily deactivated by CO poisoning, and Pt catalysts are scarce and expensive, which limit the oxygen reduction reaction.

Method used

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  • Pt/TiN@CN catalyst with high oxygen reduction activity and preparation method thereof, and application of Pt/TiN@CN catalyst with high oxygen reduction activity
  • Pt/TiN@CN catalyst with high oxygen reduction activity and preparation method thereof, and application of Pt/TiN@CN catalyst with high oxygen reduction activity
  • Pt/TiN@CN catalyst with high oxygen reduction activity and preparation method thereof, and application of Pt/TiN@CN catalyst with high oxygen reduction activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of TiN@CN support

[0035] Put the TiN powder into a porcelain boat and place it in a tube furnace, and heat it to 800°C at 5°C / min in an argon atmosphere. Subsequently, will carry saturated CCl 4 A stream of steam argon was introduced into the tube furnace at a flow rate of 50 ml / min. After calcination at 800 °C for 2 h, the furnace was cooled with pure argon to obtain TiN@CN. Such as figure 1 It is a high temperature extraction device designed to control the CCl 4 access. Such as figure 2 As shown, the TiN@CN support is a flaky core-shell structure with a specific surface area of ​​313.5m 2 / g, the total pore volume is 0.49cc / g. image 3 is the isothermal adsorption-desorption curve of TiN@CN catalyst support, from image 3 It can be seen that there are a large number of micropores on the surface of the material, which increases the specific surface area of ​​the material and is conducive to the dispersion of metal Pt, and the material has a flaky...

Embodiment 2

[0039] Put the TiN powder into a porcelain boat and place it in a tube furnace, and heat it to 900°C at 5°C / min in an argon atmosphere. Subsequently, will carry saturated CCl 4 A steamed argon flow was introduced into the furnace at a flow rate of 50 mL / min. After calcination at 900 °C for 1 h, the furnace was cooled with pure argon to obtain TiN@CN.

[0040]Disperse 0.5g of TiN@CN carrier in 65mL of ethylene glycol and ultrasonically disperse it for 20min to make it evenly dispersed; dissolve 0.26g of chloroplatinic acid hexahydrate in 5mL of ethylene glycol and mix it with the above solution; prepare 1M Sodium hydroxide solution, adjust the pH to 11.5; the solution was stirred and reacted for 3 hours at 160° C. under a nitrogen atmosphere, and after the reaction was completed, the pH was adjusted to 0.5 with 10 wt% HCl, stirred for 12 hours, and filtered and washed until the waste liquid was neutral; The washed solid powder was dried at 80°C for 12 hours, and then the abov...

Embodiment 3

[0042] Put the TiN powder into a porcelain boat and place it in a tube furnace, and heat it to 800°C at 5°C / min in an argon atmosphere. Subsequently, a stream of argon carrying saturated CCl4 vapor was introduced into the furnace at a flow rate of 60 mL / min. After calcination at 800 °C for 2 h, the furnace was cooled with pure argon to obtain TiN@CN.

[0043] Disperse 0.5g of TiN@CN carrier in 65mL of ethylene glycol and ultrasonically disperse it for 20min to make it evenly dispersed; dissolve 0.26g of chloroplatinic acid hexahydrate in 5mL of ethylene glycol and mix it with the above solution; prepare 1M Sodium hydroxide solution, adjust the pH to 11.5; the solution was stirred and reacted for 3 hours at 160° C. under a nitrogen atmosphere, and after the reaction was completed, the pH was adjusted to 0.5 with 10 wt% HCl, stirred for 12 hours, and filtered and washed until the waste liquid was neutral; The washed solid powder was dried at 80°C for 12 hours, and then the abov...

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Abstract

The present invention provides a Pt / TiN@CN catalyst with high oxygen reduction activity and a preparation method thereof, and application of a Pt / TiN@CN catalyst with high oxygen reduction activity. The Pt / TiN@CN catalyst comprises an active component Pt and a carrier TiN@CN, wherein the carrier TiN@CN comprises a shell and a core, the shell comprises a CN layer, and the core comprises titanium nitride which is in a nano-sheet shape. The preparation method comprises the following steps of: reacting TiN powder with CCl4 at a high temperature to obtain a carrier TiN@CN; then adding a chloroplatinic acid hexahydrate solution to the carrier TiN@CN, and adjusting the pH value and heating for reaction; and drying the product and reducing the product by hydrogen to obtain the Pt / TiN@CN catalyst.Aiming at the problems that the Pt catalyst used in the existing oxygen reduction reaction is easy to deactivate due to CO poisoning and is high in cost, TiN is used as a carrier to perform C doping on the surface layer TiN, so that the specific surface area of the material is increased, the Pt catalyst is better dispersed, and the catalytic activity is improved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a Pt / TiN@CN catalyst with high oxygen reduction activity and its preparation method and application. Background technique [0002] The oxygen reduction reaction is the most important step reaction in the fuel cell. The catalysts for the oxygen reduction reaction include noble metal catalysts, non-noble metal catalysts (including transition metal doped carbon nitrogen catalysts, transition metal oxides, nitrides, carbides, transition metal sulfide substances, carbon materials with special morphology, etc.), non-metallic catalysts, etc., the best known catalysts are platinum and its alloys. However, platinum electrocatalysts are time-dependent, prone to deactivation due to CO poisoning, and Pt catalysts are scarce and expensive, all of which limit the oxygen reduction reaction. It is necessary to design a new catalyst support that can increase the dispersion of Pt and change the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/86H01M4/92
CPCH01M4/8647H01M4/925H01M4/926Y02E60/50
Inventor 李星运
Owner QINGDAO UNIV