Method for controllably preparing supported and non-supported Ni2P under mild conditions

A supported and non-supported technology, which is applied in the direction of phosphide, can solve the problems of high emission and high energy consumption, and achieve the effects of safe and simple preparation process, mild and controllable preparation conditions, and excellent catalytic performance

Active Publication Date: 2011-04-27
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Loaded Ni 2 P catalyst has excellent catalytic activity in hydrodesulfurization and hydrodenitrogenation reactions of oil products, but its synthesis process brings high energy consumption and high emissions

Method used

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  • Method for controllably preparing supported and non-supported Ni2P under mild conditions
  • Method for controllably preparing supported and non-supported Ni2P under mild conditions
  • Method for controllably preparing supported and non-supported Ni2P under mild conditions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 0.6g of NiCl 2 .6H 2 O was dried and ground into the tube furnace 2, and the flow rate of Ar gas was adjusted to 60 mL / min. Afterwards, both tube furnace 1 and tube furnace 2 were heated to 300° C. and stabilized for 30 min. Then, 20 g of sodium hypophosphite solution with a mass percentage content of 2% was added into the tube furnace 1 by a peristaltic pump at a rate of 0.5 mL / min. After adding the sodium hypophosphite solution, the reactor was closed, the temperature was brought to room temperature under Ar gas purging, and the obtained product was washed with water and then dried. The obtained sample was named A, and A had an attached figure 1 Characteristics.

Embodiment 2

[0018] The preparation process was the same as that of sample A, except that the added sodium hypophosphite solution was changed to 2.68 g sodium hypophosphite solution with a mass percentage of 20%, and other conditions remained unchanged. The resulting sample was named B, B has the attached figure 2 Characteristics.

Embodiment 3

[0020] The preparation process is the same as the preparation process of sample A, only the feeding speed of the peristaltic pump is changed to 1.4 mL / min, and other conditions remain unchanged. The resulting sample was named C, C has the attached image 3 Characteristics.

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Abstract

The invention provides a new method for controllably preparing supported and non-supported Ni2P under mild conditions. In the method, two tube furnace reactors connected in series are adopted; and sodium hypophosphite aqueous solution is subjected to thermal decomposition in the first reactor to generate phosphine gas, and later, carried by argon, the phosphine gas is dried and then enters into the second reactor to react with nickel salt to generate the required Ni2P. The invention is characterized in that the preparation process is safe and concise; the preparation conditions are mild and controllable; simple thermal treatment under normal pressure is only needed in the preparation process; and the supported and non-supported Ni2P can be controllably prepared by controlling the amount of the sodium hypophosphite. With excellent catalytic performances, such type of phosphides can be widely applied to various hydrogenation reactions.

Description

technical field [0001] The present invention proposes a controllable preparation of supported and unsupported Ni under mild conditions 2 A new approach to P. The process employs two tubular furnace reactors in series. The aqueous solution of sodium hypophosphite is thermally decomposed in the first reactor to generate phosphine gas, which is then dried under argon and then enters the second reactor to react with nickel salts to generate the required Ni 2 P. The invention is characterized in that the adopted preparation process is safe and concise, the preparation conditions are mild and controllable, and the preparation process only needs simple heat treatment under normal pressure; by controlling the amount of sodium hypophosphite, supported and unsupported Ni can be controllably prepared 2 P. Such phosphides can be widely used in various hydrogenation reactions due to their excellent catalytic properties. Background technique [0002] Hydrogenation is an important res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08
Inventor 李伟关庆鑫
Owner NANKAI UNIV
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