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Process for preparing molybdenum nitride and use thereof as hydrogenation and desulfurizing catalyst

A molybdenum nitride and molybdenum trioxide technology, applied in the directions of molybdenum halide, refining to remove heteroatoms, etc., can solve the problems of difficult-to-industrial large-scale preparation, cumbersome preparation process, high cost, easy industrial application, simplified preparation process, The effect of reducing production costs

Inactive Publication Date: 2004-10-27
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the currently prepared molybdenum nitride with desulfurization activity is γ crystal molybdenum nitride, and its XRD crystal phase structure characteristic d values ​​are: 2.404, 2.081, 1.472, 1.255, 1.202, 1.041, and the preparation process is cumbersome and the conditions are harsh. , high cost, difficult to realize industrialized large-scale preparation, which restricts its practical application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Weigh 1 gram of molybdenum trioxide (MoO3) produced by China Shanghai Colloid Chemical Factory, and grind it into a powder smaller than 150 μm.

[0025] (2) With a flow rate of 140ml / min, feed 99.9% nitrogen, and with a flow rate of 260ml / min, feed 99% hydrogen, and make them fully mixed in a mixer.

[0026] (3) Use the following temperature program to react: room temperature-300°C, the heating rate is 10°C / min; 300-500°C, the heating rate is 0.6°C / min; 500-700°C, the heating rate is 2°C / min; 700°C constant temperature for 2 hours.

[0027] (4) After completion of the temperature program reaction, 99.9% nitrogen gas was passed through at a flow rate of 60 ml / min and cooled to room temperature.

[0028] (5) At a flow rate of 100 ml / min, a passivation gas with a volume ratio of oxygen / nitrogen of 1 / 99 is introduced, and passivated for 2 hours. Product A was prepared.

[0029] (6) Carry out catalytic experiments on laboratory microreactors. Fill the reactor with 0....

Embodiment 2

[0031] (1) Take by weighing the same molybdenum trioxide (MoO3) 1 gram among the embodiment 1, grind into powder less than 150 μm.

[0032] (2) At a flow rate of 200ml / min, feed 99.9% nitrogen, and at a flow rate of 200ml / min, feed 99% hydrogen, and mix thoroughly in a mixer.

[0033] (3) Use the following temperature program to react: room temperature-300°C, the heating rate is 10°C / min; 300-500°C, the heating rate is 0.6°C / min; 500-700°C, the heating rate is 2°C / min; 700°C constant temperature for 2 hours.

[0034] (4) After completion of the temperature program reaction, 99.9% nitrogen gas was passed through at a flow rate of 60 ml / min and cooled to room temperature.

[0035] (5) At a flow rate of 100 ml / min, a passivation gas with a volume ratio of oxygen / nitrogen of 1 / 99 is introduced, and passivated for 2 hours. Product B was prepared.

[0036] (6) Carry out catalytic experiments on laboratory microreactors. Fill the reactor with 0.1 gram of product B, the reaction t...

Embodiment 3

[0038] (1) Take by weighing 1 gram of the same molybdenum trioxide (MoO3) as in Example 1, and grind it into 150 μm powder.

[0039] (2) Feed 99.9% nitrogen gas at a flow rate of 80 ml / min, and feed 99% hydrogen gas at a flow rate of 320 ml / min, and mix thoroughly in a mixer.

[0040] (3) Use the following temperature program to react: room temperature-300°C, the heating rate is 10°C / min; 300-500°C, the heating rate is 0.6°C / min; 500-700°C, the heating rate is 2°C / min; 700°C constant temperature for 2 hours.

[0041] (4) After completion of the temperature program reaction, 99.9% nitrogen gas was passed through at a flow rate of 60 ml / min and cooled to room temperature.

[0042] (5) At a flow rate of 100 ml / min, a passivation gas with a volume ratio of oxygen / nitrogen of 1 / 99 is introduced, and passivated for 2 hours. Product C was prepared.

[0043] (6) Carry out catalytic experiments on laboratory microreactors. Fill the reactor with 0.1 gram of product C, the reaction t...

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Abstract

A process for preparing molybdenum nitride from MoO3 includes multi-stage thermal reaction in the mixed atmosphere of N2 and H2, cooling in inert gas and purifying in oxygen. Said product can be used as hydrodesulfurizing catalyst for hdyrodesulfurizing at 250-450 deg.C and 0.2-20 MPa. Its advantages are simple process and low cost.

Description

[0001] Field: [0002] The invention relates to a preparation method of molybdenum nitride and the application of the molybdenum nitride as a hydrodesulfurization catalyst, especially a liquid fuel hydrodesulfurization catalyst. Background technique: [0003] The increasingly stringent environmental regulations require lower and lower sulfur content in liquid fuels, so the research on developing suitable gasoline and diesel deep desulfurization catalysts, as well as heavy petroleum and coal-based liquid fuel hydrorefining and utilization catalysts is increasing. At present, most of the liquid fuel hydrodesulfurization catalysts commonly used in industry are molybdenum sulfide catalysts supported or added with nickel, cobalt and other additives. However, molybdenum sulfide-based catalysts are difficult to remove alkyl-substituted polycyclic aromatic thiophene sulfur-containing compounds in liquid fuels, such as 4,6-dimethyldibenzothiophene. In addition, molybdenum sulfide cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/04C10G45/08
Inventor 陈皓侃龚树文李文李保庆
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI