Method for preparing metal-modified alpha type molybdenum carbide catalyst and application of metal-modified alpha type molybdenum carbide catalyst in low-temperature water-gas shift reaction

A technology of metal modification and molybdenum carbide, applied in chemical instruments and methods, non-metallic elements, inorganic chemistry, etc., can solve the problems of α-MoC that have not yet been seen, and achieve the effect of simplified preparation process, simple process and good stability

Inactive Publication Date: 2012-10-03
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, no α-MoC 1-x Reports for the water-gas shift reaction

Method used

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  • Method for preparing metal-modified alpha type molybdenum carbide catalyst and application of metal-modified alpha type molybdenum carbide catalyst in low-temperature water-gas shift reaction
  • Method for preparing metal-modified alpha type molybdenum carbide catalyst and application of metal-modified alpha type molybdenum carbide catalyst in low-temperature water-gas shift reaction
  • Method for preparing metal-modified alpha type molybdenum carbide catalyst and application of metal-modified alpha type molybdenum carbide catalyst in low-temperature water-gas shift reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of Au-modified α-molybdenum carbide catalyst samples: (1) 3.531 g (NH 4 ) 6 Mo 7 o 24 4H 2 O was dissolved in 15 ml deionized water to make a solution, and 13.18 ml HAuCl 4 (0.02428 mmol / mL) was added to the ammonium molybdate solution, and the above mixed solution was stirred at room temperature for 4 h, then changed to 80 °C water bath and stirred until the solution evaporated completely to obtain a solid precipitate, which was dried at 110 °C for 12 h, and calcined at 500 °C for 4 h to obtain the oxide precursor. (2) Press the precursor prepared above into 40-60 meshes, weigh the samples required for the reaction and place them in a quartz reactor, in 20% CH 4 / H 2 Carry out temperature-programmed carbonization in a mixed atmosphere, from room temperature to 300 °C, the heating rate is 5 °C / min, and then from 300 °C to the final carbonization temperature of 700 °C, the heating rate is 1 °C / min, at the final carbonization temperature, Constant tempe...

Embodiment 2

[0025] Preparation of Cu-modified α-molybdenum carbide catalyst samples: (1) Weigh 0.2395 g Cu(NO 3 ) 2 ·3H 2 O and 3.531 g (NH 4 ) 6 Mo 7 o 24 4H 2 O was dissolved in 5 ml and 15 ml deionized water respectively to make a solution, and the two solutions were mixed. Stir the above mixed solution at room temperature for 4 h, change to a water bath at 80 °C and stir until the solution evaporates completely to obtain a solid precipitate, which is dried at 110 °C for 12 h and calcined at 500 °C for 4 h to obtain the oxide precursor . (2) The carbonization process is the same as in Example 2, and Cu / α-MoC is finally obtained 1-x catalyst.

Embodiment 3

[0027] The evaluation of the activity of the above two metal-modified α-type molybdenum carbide catalysts was carried out on a self-made miniature fixed-bed catalytic reaction device. A quartz tube with an inner diameter of 6 mm was used as the reactor, and the activity evaluation conditions were: normal pressure, the loading amount of the catalyst composite oxide precursor (40-60 mesh) was 0.4 g, and the original test was carried out as described in step 2 in Example 1. In-situ carbonization, after the carbonization is completed, switch to the reaction gas for in-situ reaction under the protection of argon. The reaction gas composition is: 10.5% CO, 21% H 2 O, the rest is Ar (Ar is the balance gas), the total flow rate is 120 ml / min, and the mass space velocity is 18000 ml g -1 h -1 , The reaction temperature is 150 ℃ ~ 400 ℃. The content of CO in the tail gas was analyzed online by a Timex GC7890Ⅱ gas chromatograph equipped with a thermal conductivity detector.

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Abstract

The invention discloses a method for preparing a metal-modified alpha type molybdenum carbide catalyst. The preparation method comprises the following steps of: continuously raising the temperature of a precursor in the presence of 20 percent of CH4/H2, and carbonizing, wherein a composite oxide of molybdenum and another metal is used as the precursor; and performing an in-situ water-gas shift reaction on the prepared metal-modified alpha type molybdenum carbide catalyst under normal pressure at the operating temperature of 150 to 400 DEG C, wherein feed gas comprises 10.5 percent of CO, 21 percent of H2O and the balance of Ar (serving as balance gas), the total flow is 120ml/min, and the mass space velocity is 18,000ml g<-1> h<-1>. The preparation method has the advantages that the preparation method for the catalyst is simplified, and the production cost is reduced; and simultaneously, the catalyst has the advantages of high low-temperature activity, wide operation temperature range and high stability when used for the water-gas shift reaction.

Description

technical field [0001] The invention belongs to the field of preparation and application of novel catalysts, and relates to a metal-modified α-type molybdenum carbide catalyst for low-temperature water-gas shift reaction. Background technique [0002] The water-gas shift reaction is an important reaction in industry, which can make CO and H in the raw gas of synthetic ammonia. 2 O reacts and converts to CO 2 and H 2 . Therefore, it has a wide range of applications in ammonia synthesis, methanol synthesis, hydrogen production and city gas industry. In recent years, with the development of fuel cell technology, the water-gas shift reaction has a new application background. It can reduce CO in reformed gas while increasing H 2 Therefore, the water-gas shift reaction has become a research hotspot again. [0003] From a thermodynamic point of view, the water gas shift (WGS) reaction is an exothermic reaction, and the equilibrium constant (K p θ ) is significantly affected...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22C01B3/16
CPCY02P20/52
Inventor 石川马宇飞朱爱民李小松
Owner DALIAN UNIV OF TECH
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