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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 energy consumption and high emission, and achieve the effects of safe and simple preparation process, mild and controllable preparation conditions, and excellent catalytic performance

Active Publication Date: 2013-04-17
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 After O was dried and ground, it was loaded into 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 of 2% was added into the tube furnace 1 at a rate of 0.5 mL / min with a peristaltic pump. After adding the sodium hypophosphite solution, the reactor was closed, and the temperature was lowered to room temperature under the purge of Ar gas, and then the product obtained 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 is the same as that of sample A, except that the added sodium hypophosphite solution is changed to 2.68 g of 20% sodium hypophosphite solution by mass, and other conditions remain unchanged. The resulting sample is named B, and B has attached figure 2 Characteristics.

Embodiment 3

[0020] The preparation process was the same as that of sample A, only the feed rate of the peristaltic pump was changed to 1.4mL / min, and other conditions remained unchanged. The obtained sample was named C, and C has 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 load-type and non-load-type Ni under mild conditions 2 New method of P. The method employs two tube furnace reactors connected in series. The aqueous solution of sodium hypophosphite is thermally decomposed in the first reactor to generate phosphine gas, and then it is dried under the argon gas and then enters the second reactor to react with nickel salt to generate the required Ni 2 p. The present invention is characterized in that the preparation process adopted is safe and simple, 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, the supported and non-supported 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] Hydroge...

Claims

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Application Information

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