Method for preparing Ni2P catalyst with three-dimensional cascade pore structures at low temperature

A technology of stepped pores and catalysts, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of not having a stepped pore structure, and achieve obvious advantages, mild preparation conditions, and high catalytic activity. Effect

Active Publication Date: 2017-03-08
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses an aqueous solution of hypophosphite, and the prepared Ni 2 P catalysts do not have a stepped pore structure

Method used

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  • Method for preparing Ni2P catalyst with three-dimensional cascade pore structures at low temperature
  • Method for preparing Ni2P catalyst with three-dimensional cascade pore structures at low temperature
  • Method for preparing Ni2P catalyst with three-dimensional cascade pore structures at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of Ni with three-dimensional hierarchical pore structure prepared at low temperature 2 The method of P catalyst, comprises steps as follows:

[0043] 1) Weigh 0.1 g of Ni-MOF-74 precursor and 2.0 g of sodium hypophosphite and place them on both ends of the corundum porcelain boat respectively, put the porcelain boat into a tube furnace, and pass in argon with a flow rate of 100 ml per minute Gas, evacuate the air in the tube furnace;

[0044] 2) Heating to 275 degrees Celsius at a heating rate of 5 degrees Celsius per minute, and holding at this temperature for 180 minutes (continuously using 100 ml per minute of argon purging during the process), you can get a Ni with a three-dimensional hierarchical pore structure. 2 P catalyst.

[0045] figure 1 It is the Ni of the three-dimensional stepped pore structure prepared in this embodiment. 2 X-ray powder diffraction pattern (PXRD) of P catalyst. Depend on figure 1 It can be seen that the prepared Ni 2 P is a ...

Embodiment 2

[0052] A kind of Ni with three-dimensional hierarchical pore structure prepared at low temperature 2 The method of P catalyst, comprises steps as follows:

[0053] 1) Weigh 0.1 g of Ni-MOF-74 precursor and 3.0 g of sodium hypophosphite and place them on both ends of the corundum porcelain boat respectively, put the porcelain boat into a tube furnace, and pass in argon with a flow rate of 100 ml per minute Gas, evacuate the air in the tube furnace;

[0054] 2) Heating to 300 degrees Celsius at a heating rate of 5 degrees Celsius per minute, and holding at this temperature for 200 minutes (continuously using 100 ml per minute of argon purging during the process), you can get a Ni with a three-dimensional hierarchical pore structure. 2 P catalyst.

Embodiment 3

[0056] A kind of Ni with three-dimensional hierarchical pore structure prepared at low temperature 2 The method of P catalyst, comprises steps as follows:

[0057] 1) Weigh 0.1 g of Ni-MOF-74 precursor and 1.0 g of sodium hypophosphite and place them on both ends of the corundum porcelain boat respectively, put the porcelain boat into the tube furnace, and pass in argon with a flow rate of 100 ml per minute Gas, evacuate the air in the tube furnace;

[0058] 2) Heating to 275 degrees Celsius at a heating rate of 5 degrees Celsius per minute, and keeping it at this temperature for 120 minutes (continuously using 100 ml per minute of argon purging during the process), you can get a Ni with a three-dimensional hierarchical pore structure. 2 P catalyst.

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Abstract

The invention relates to a method for preparing a Ni2P catalyst with three-dimensional cascade pore structures at low temperature. Under the protection of inert gas, nickel-based metal organic framework materials and hypophosphite are conducted heat treatment at 200-350DEG C for 1-500 min, obtaining a Ni2P catalyst with a three-dimensional cascade pore structure. The method does not need a catalyst or a solvent, the preparation condition is mild, the craft is simple and the method is suitable for industrial production. The prepared Ni2P catalyst has a higher specific surface area(174 m<2>/g) and a bigger pore volume. The internal pore size distribution is 1-50 nm, which distributes as cascade pores. The internal cascade pores are favorable for electrochemical catalysis, hydrodesulfurization, selective hydrogenation and other hydrogenation reactions, and have broad application prospects.

Description

technical field [0001] The invention relates to a low-temperature preparation of Ni with a three-dimensional hierarchical pore structure 2 A P catalyst method belongs to the technical field of materials and energy. Background technique [0002] Transition metal mineral resources are abundant, cheap and easy to obtain. In recent years, non-noble metal catalysts based on transition metal phosphides have attracted more and more attention from scientists, especially nickel phosphide (Ni 2 The catalyst represented by P) has the best catalytic performance of phosphides and has broad application prospects. Ni 2 P belongs to metal-rich phosphide, which is an interstitial compound with metallic properties formed by phosphorus atoms entering the metal lattice. There are a large number of Ni-Ni metal bonds inside the crystal, so it has better conductivity and stability than phosphorus-rich phosphide , with high hardness, high melting point, corrosion resistance and other properties....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/10C10G45/06
CPCB01J27/1853B01J35/1057B01J35/1061C10G45/06C10G2300/202
Inventor 赵学波闫理停代鹏程李良军顾鑫
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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