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Apparatus and method for preparing metal nitride catalytic material

A technology for catalytic materials and nitrides, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of product purity and quality decline, avoid product quality decline, and eliminate operations. Hazardous and environmental pollution, the effect of eliminating temperature gradient problems

Inactive Publication Date: 2009-02-04
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the above-mentioned problems, the present invention provides a kind of equipment and method for preparing metal nitride catalytic material, adopt temperature-programmed fluidized bed method to prepare metal nitride (γ-Mo 2 N), completely avoiding the problems such as the purity and quality of the product caused by the inherent problems of the packing and the fixed bed itself

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  • Apparatus and method for preparing metal nitride catalytic material
  • Apparatus and method for preparing metal nitride catalytic material

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preparation example Construction

[0022] γ-Mo 2 The preparation technology of N is described in detail. In the present invention, the room temperature generally refers to 16-30°C.

[0023] 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 2Reduction 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.

[0024] The reaction device for preparing molybdenum nitride in a fluidized bed is shown in Figure 1.

[0025] 1. Gas

[0026] 1 nitrogen - high-purity nitrogen (volume concentration of 99.999%), nitriding raw material, from steel cylinders, to the mixer;

[0027] 2 Hydrogen - high-purity hydrogen (volume concentration 99.999%), nitriding raw material, from steel ...

Embodiment 1

[0149] The temperature programming system that the present invention adopts is as figure 2 As shown, the optimal temperature programming regime is:

Embodiment 25

[0150] 1. Rapid heating from room temperature to 673K, the heating rate is 1-50K / min (25K / min in this embodiment);

[0151] 2.673-933K adopts 0.6-1K / min (this embodiment 0.6K / min) speed to heat up;

[0152] 3. 933K constant temperature 0.5-1hr (this embodiment 1hr);

[0153] 4. Cool to room temperature in a fluidized bed reactor;

[0154] 5. React N at room temperature 2 -H 2 The mixed gas is switched to volume ratio 99%Ar-1%O 2 Mixed gas (ie passivation treatment), time 12-24hr, 24hr in this embodiment.

[0155] γ-Mo of the present invention 2 The N-supported catalyst was prepared as follows:

[0156] 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 fluidized bed 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...

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Abstract

The invention relates to a device for preparing metal nitride catalyst, wherein the mixer via tube is connected to the fluidize bend reactor whose outlet via tube is connected to the heat exchanger; the heat exchanger via tube is connected to the mixer, while said tube via six-way valve is connected to the gas spectrum device, and the heat exchanger via tube is connected to the water cooler; the separator via tube and drying part is connected to the compressor whose outlet via tube is connected to the heat exchanger; the cooler is connected to the inlet and outlet tubes of compressor; MoO3 / TiO2, MoO3 / NiO-TiO2, MoO3 / Al2O-TiO2 or MoO3 / Al2O3 is put into fluidize bed reactor, to process N2-H2 reduction to replace MoO3, to prepare the Mo2N / TiO2, Mo2N / NiO-TiO2, Mo2N / Al2O3-TiO2, or Mo2N / Al2O3 carried metal nitride catalyst; the volume ration between N2 and H2 is 3-5:1, and the reaction temperature is 933K+-10K, the temperature kept time is 0.5-1h. The invention can improve the product quality and prepare the gamma-Mo2N with high specific surface area.

Description

technical field [0001] The invention relates to the technical field of catalytic materials, in particular to the preparation of metal nitrides (γ-Mo 2 N) Apparatus and methods for catalytic materials. Background technique [0002] For metal nitrides (γ-Mo 2 The research on N) catalytic materials has a history of many years. Wise and Markel, in summarizing more than 90 years of research on NH 3 Based on the basic principles and kinetics of the synthesis and decomposition of NH 3 with MoO 3 Reaction temperature as a function of reaction product and surface area in a quartz tubular reactor. Polycrystalline MoO when the temperature rises to 473K 3 Fragmentation, slightly increased surface area, unknown phase (804pm) and MoO at 573K 3 , 673K ​​MoO 3 Disappears, MoO appears 2 And another unknown phase (621, 307 and 205pm), above 773K forms Mo 2 N, high content increases with increasing temperature, MoO 2 amount decreased. 980K+2hr constant temperature reaction, the red...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/00B01J8/24B01J21/06
Inventor 熊天英吴杰金花子孔令艳李铁藩曲良龙付玉梅
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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