Process and apparatus for preparing metal nitride catalyst material

A technology of catalytic materials and special equipment, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of large axial and radial temperature gradients, difficult control of bed temperature, and bed temperature distribution. Uneven problems, to achieve the effect of simplified operation, low cost, and 100% utilization rate

Inactive Publication Date: 2007-01-03
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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Problems solved by technology

For a tube furnace with a diameter of 25 cm, the temperature gradient can reach hundreds of degrees, so it can be concluded that for the large-scale preparation of Mo 2 N, bed temperature control is an extremely difficult problem
in NH 3 When used as a nitriding reagent, there are two key issues affecting product quality: one is to reduce MoO 3 produces water ( ) The presence of water vapor promotes the product Mo 2 N undergoes hydrothermal sintering, and H 2 O and H 2 in MoO 3 competitive adsorption, making Mo 2 The surface area of ​​N decreases; the second is NH 3 The decomposition is an endothermic reaction, which causes the bed temperature distribution in the reactor to be very uneven, and the axial and radial temperature gradients are large

Method used

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  • Process and apparatus for preparing metal nitride catalyst material
  • Process and apparatus for preparing metal nitride catalyst material

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preparation example Construction

[0028] The present invention is based on γ-Mo 2 The preparation technology of N is described in detail.

[0029] In view of the preparation of high specific surface area γ-Mo 2 The research experience of N, the present invention adopts the approach of temperature-programmed gradual reaction, utilizes N 2 Reduction of MoO as a reducing gas 3 . By controlling the heating rate and increasing the gas flow rate, the accumulation of product moisture is prevented; in order to reduce gas consumption, a gas circulation device is designed in the system to reduce production costs.

[0030] Batch molybdenum nitride reaction device such as figure 1 shown.

[0031] 1. Gas

[0032] 1 Nitrogen - high-purity nitrogen (99.999% concentration), nitriding raw material, from steel cylinders, to the mixer;

[0033] 2 Hydrogen - high-purity hydrogen (concentration 99.999%), nitriding raw material, from the cylinder, to the mixer;

[0034] 3 Mixed gas——Mixed by nitrogen, hydrogen, and circulat...

Embodiment 1

[0154] The temperature programming system that the present invention adopts is as figure 2 As shown, the optimal temperature programming regime is:

Embodiment 25

[0155] 1. Rapid heating from room temperature to 673K, the heating rate is 1-50K / min (25K / min in this embodiment);

[0156] 2.673-933K adopts 0.6-1K / min (this embodiment 0.6K / min) speed to heat up;

[0157] 3. 933K constant temperature 0.5-1hr (this embodiment 1hr);

[0158] 4. Cool to room temperature in the reactor;

[0159] 5. Switch N at room temperature 2 -H 2 The mixed gas is 99%Ar-1%O by volume 2 Mixed gas (ie passivation treatment) 12-24hr, 24hr in this embodiment.

[0160] γ-Mo of the present invention 2 The N-supported catalyst was prepared as follows:

[0161] According to the above process, the MoO 3 / TiO 2 、MoO 3 / NiO-TiO 2 、MoO 3 / Al 2 o 3 -TiO 2 or MoO 3 / Al 2 o 3 Put into the reactor of the present invention, carry out N 2 -H 2 Reductive replacement of MoO 3 reaction to produce Mo 2 N / TiO 2 、Mo 2 N / NiO-TiO 2 、Mo 2 N / Al 2 o 3 -TiO 2 or Mo 2 N / Al 2 o 3 Supported metal nitride catalyst. N 2 -H 2 Volume ratio of mixed gas: H 2 / N ...

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Abstract

The present invention relates to catalyst technology, and is especially process and apparatus for preparing metal nitride catalyst material (gamma-Mo2N). MoO3/TiO2, MoO3/NiO-TiO2, MoO3/Al2O3-TiO2 or MoO3/Al2O3 is set in a reactor to replace MoO3 with reducing N2-H2 so as to prepare supported metal nitride catalyst Mo2N/TiO2, Mo2N/NiO-TiO2, Mo2N/Al2O3-TiO2 or Mo2N/Al2O3. The reaction conditions include N2-H2 ratio in the gas mixture of 1/(3-5), reaction temperature of 933K+/-10K and holding time of 0.5-1 hr. The apparatus includes mainly a mixer, a reactor, a heat exchanger, and a gas chromatogaph connected through pipeline. The present invention can prepare gamma-Mo2N with specific surface area as great as 150 sq m/g, and the preparation process has its operation simpler than that with NH3.

Description

technical field [0001] The invention relates to the technical field of catalytic materials, in particular to a metal nitride (γ-Mo 2 N) Preparation method of catalytic material and special equipment thereof. Background technique [0002] It is known that transition metal nitrides and carbides in NH 3 Synthesis and other aspects have the same as traditional noble metal (Pt, Ru, etc.) catalysts, and even have higher catalytic activity. γ-Mo 2 As a heterogeneous catalytic active material, N is more active than the usual industrial transition metal Ni, Co, Mo, W catalysts, etc. in many systems of hydrogenation and hydrofinishing for the cracking of heteroatom (N, S, O) rings. High, but low activity for aromatic ring hydrogenation, such as γ-Mo 2 N-dibenzothiophene hydrodesulfurization (HDS). Activity than industrial Mo 2 S / Al 2 o 3 Catalyst 1.2 times higher, and excellent hydrodenitrogenation (HDN) performance. and found that γ-Mo 2 N and Pd / Al 2 o 3 Catalytic select...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/00
Inventor 吴杰李铁藩熊天英金花子
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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