Preparation method of transition metal phosphide MoP

A technology of transition metals and phosphides, which is applied in the direction of phosphides, can solve the problems of difficult control of product crystal phase, poor catalytic activity of products, and inability to prepare phosphides, etc., and achieves the effect of low price, low cost and novel synthesis method

Inactive Publication Date: 2012-06-20
天津天环光伏太阳能有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 1. Using organophosphorus or phosphine as a phosphorus source is highly toxic;
[0004] 2. Hydrothermal synthesis cannot prepare supported phosphides, and the obtained products have poor catalytic acti...

Method used

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  • Preparation method of transition metal phosphide MoP
  • Preparation method of transition metal phosphide MoP
  • Preparation method of transition metal phosphide MoP

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] Precursor preparation

[0021] Weigh at a molar ratio of 1:14 (NH 4 ) 6 Mo 7 o 24 4H 2 O and NH 4 h 2 PO 4 , solid-phase reaction occurs by grinding in a mortar; continue to grind until dry, and sinter the resulting powder at 500 °C for 5 h to obtain a precursor.

Embodiment 1

[0023] 1. Weigh the above precursor and KBH with a molar ratio of 1:1.5 4 , mix well in a mortar;

[0024] 2. The mixture was reacted under the protection of argon at 600°C for 30 minutes; the obtained product was finely ground, washed three times with distilled water and absolute ethanol, and then vacuum-dried at 60°C for 12 hours to obtain the product.

[0025] figure 1 is the XRD pattern of the obtained material. It can be seen from the standard card that the synthesized material is MoP.

Embodiment 2

[0027] 1. Weigh the above precursor and KBH with a molar ratio of 1:2 4 , mix well in a mortar;

[0028] 2. The mixture was reacted at 500°C under the protection of argon for 60 minutes; the obtained product was finely ground, washed three times with distilled water and absolute ethanol, and then vacuum-dried at 60°C for 12 hours to obtain the product.

[0029] figure 2 is the XRD pattern of the obtained material. It can be seen from the standard card that the synthesized material is MoP.

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Abstract

The invention discloses a preparation method of transition metal phosphide MoP. The preparation method includes 1), weighing (NH4)6Mo7024 4H2O and NH4H2PO5 to be ground in a mortar to realize solid phase reaction according to a molar ratio of 1:14, continuing grinding until mixture is dry, sintering obtained powder at the temperature of 500 DEG C for 5 hours and obtaining a precursor; and 2), grinding the precursor and reducing agent in the mortar according to a certain molar ratio, mixing the precursor with the reducing agent uniformly, performing reaction under argon shield at the temperature ranging from 500 DEG C to 600 DEG C for 30 minutes to 60 minutes, finely grinding an obtained product, washing the finely ground product by the aid of distilled water and anhydrous ethanol for three times, drying the washed product in a vacuum condition at the temperature of 60 DEG C for 12 hours, and obtaining a product MoP. The preparation method has the advantages that main raw materials are rich in source, prices are cheap, cost is low, the synthesis method is novel, process is simple, complicated steps with conditions of high temperature and high pressure are omitted, a preparation flow is simplified, energy consumption is lowered, simultaneously, environmental pollution is prevented in a preparation procedure, and the preparation method is applicable to large-scale production.

Description

technical field [0001] The invention relates to a method for preparing transition metal phosphide, more specifically, relates to a method for preparing transition metal phosphide MoP. Background technique [0002] Transition metal phosphides are an important class of multifunctional materials, and their applications in catalysis and magnetism have attracted wide attention. Among them, MoP has been widely studied and applied as a low-cost and high-performance phosphide. However, the existing methods for synthesizing MoP have the following disadvantages: [0003] 1. Using organophosphorus or phosphine as a phosphorus source is highly toxic; [0004] 2. Hydrothermal synthesis cannot prepare supported phosphides, and the obtained products have poor catalytic activity; [0005] 3. The direct smelting method requires high temperature and a large amount of excess elemental phosphorus (due to volatilization), and the crystal phase of the obtained product is not easy to control; ...

Claims

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Application Information

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IPC IPC(8): C01B25/08
Inventor 宋大卫苏振馨郞平苏金风
Owner 天津天环光伏太阳能有限公司
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