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Pure alpha-phase molybdenum carbide-loaded noble metal catalyst, and preparation method and application thereof

A noble metal catalyst, molybdenum carbide technology, applied in physical/chemical process catalysts, chemical instruments and methods, catalytic treatment of combustible gases, etc., can solve the problem of reducing the specific surface area of ​​molybdenum carbide and the exposure of surface catalytic active sites, long preparation cycle, The operation process is cumbersome and other problems, and the effect of excellent water vapor shift performance and excellent catalytic performance is achieved.

Active Publication Date: 2015-09-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: ① During the carbonization process, the exchange of lattice nitrogen and carbon atoms of molybdenum nitride needs to be carried out at a relatively high temperature (above 700 ° C), and high temperature will aggravate the polymerization of free carbon on the particle surface and generate carbon deposits. The specific surface area of ​​molybdenum carbide and the exposure of surface catalytic active sites are greatly reduced; ②The operation process is cumbersome and the preparation cycle is long; ③Need to use a strong irritating gas NH 3 , not only corroding equipment but also prone to danger
[0005] So far, the synthesis of pure α-phase molybdenum carbide supported metal catalysts has not been reported by one-step carbonization method (that is, only through carbonization process without first nitriding)

Method used

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  • Pure alpha-phase molybdenum carbide-loaded noble metal catalyst, and preparation method and application thereof
  • Pure alpha-phase molybdenum carbide-loaded noble metal catalyst, and preparation method and application thereof
  • Pure alpha-phase molybdenum carbide-loaded noble metal catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Dissolve 6.92g of ammonium paramolybdate in 40ml of deionized water, stir magnetically at room temperature to dissolve completely; then add 5.93ml of chloroauric acid solution with a concentration of 0.02428mmol / ml into the ammonium paramolybdate solution dropwise , stirred at room temperature in the dark for 4-5 hours, filtered to obtain a white precipitate, washed with water, evaporated to dryness in a water bath at 80°C, and dried overnight at 110°C to obtain a precursor with a loading mass percentage of 0.5% Au;

[0043] (2) Place the precursor with a loading mass percentage of 0.5% Au in a dielectric barrier discharge (DBD) non-equilibrium plasma reactor, use oxygen (100ml / min) as the working gas, and use non-equilibrium plasma for treatment. Two electrodes Apply an AC voltage of 6000v on the top, and the treatment time is 30min to obtain molybdenum oxide with a loading mass percentage of 0.5% Au (recorded as 0.5%Au / MoO 3 -plasma);

[0044] (3) Take 1.2g 0.5% ...

Embodiment 2

[0047] The steps and processing conditions of the present embodiment are all the same as in Example 1, the difference is only in the following two points, 1. take 36.5ml of chloroauric acid solution and prepare the pure α-phase molybdenum carbide catalyst with a loading mass percentage of 3% Au (note 3% Au / α-MoC 1-x ); ②Evaluate its activity, the reaction atmosphere is: by volume fraction, 11%CO / 26%H 2 O / 26%H 2 / 7%CO 2 / 30%N 2 , the gas mass space velocity is 90000ml / g / h, and the reaction temperature is 120-400°C. At 150 °C, the conversion of CO was 82%.

Embodiment 3

[0049] The steps and processing conditions of the present embodiment are all the same as in Example 1, and the difference is only in the following two points. 1. take 62.2ml of chloroauric acid solution to prepare the pure α-phase molybdenum carbide catalyst of loading mass percentage 5% Au (note 5% Au / α-MoC 1-x ); ②Evaluate its activity, the reaction atmosphere is: by volume fraction, 11%CO / 26%H 2 O / 26%H 2 / 7%CO 2 / 30%N 2 , the gas mass space velocity is 90000ml / g / h, and the reaction temperature is 120-400°C. At 150 °C, the conversion of CO was 86%.

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Abstract

The invention discloses a pure alpha-phase molybdenum carbide-loaded noble metal catalyst, and a preparation method thereof. The preparation method comprises the following steps: (1) a noble metal salt solution is mixed with an ammonium paramolybdate water solution, and stirring is carried out; filtering and washing are carried out; and an obtained precipitate is dried, such that a precursor is obtained; (2) the precursor obtained in the step (1) is subjected to a non-equilibrium plasma treatment, such that noble metal-loading molybdenum oxide is obtained; and (3) the noble metal-loading molybdenum oxide obtained in the step (2) is carbonized with a carbon source gas under a temperature of 580-800 DEG C. According to the invention, a traditional roasting process is replaced by the non-equilibrium plasma treatment process. The pure alpha-phase molybdenum carbide-loaded noble metal catalyst can be directly obtained through a one-step carbonization process of the noble metal-loading molybdenum oxide obtained by the treatment process, such that a highly polluting nitridation process is eliminated. The invention also discloses an application of the prepared pure alpha-phase molybdenum carbide-loaded noble metal catalyst in a water gas shift reaction. As a result, the catalyst has excellent water gas shift performance.

Description

technical field [0001] The invention relates to the preparation and application of a molybdenum carbide-supported noble metal catalyst, in particular to a pure α-phase molybdenum carbide-supported noble metal catalyst and its preparation method, as well as its application in water vapor shift reaction. Background technique [0002] The inventor's research group found that in the water vapor shift reaction, pure α-phase molybdenum carbide catalyst (referred to as α-MoC 1-x ) is much more active than pure β-phase molybdenum carbide catalysts (denoted as β-Mo 2 C); pure α-phase gold molybdenum carbide catalyst (recorded as Au / α-MoC 1-x ) has higher catalytic activity than α- and β-phase miscible gold molybdenum carbide catalysts (denoted as Au / MoC x ) catalytic activity, much higher than the pure β-phase gold molybdenum carbide catalyst (recorded as Au / β-Mo 2 C) Catalytic activity. [0003] α-MoC 1-x The synthesis of MoO can only be achieved by a two-step method of nitridi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22C10K3/04
Inventor 石川张晓
Owner DALIAN UNIV OF TECH
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