Method for preparing Ni2P catalyst

A technology of catalyst and inert gas, which is applied in the field of preparation of nickel phosphide catalyst and can solve problems such as limiting practical application

Inactive Publication Date: 2013-08-28
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Metal nickel precursor and pH 3 Mixed hydrogen reaction can produce Ni under very mild conditions 2 P catalyst and no impurities are introduced (Chem.Commun.,2005,4

Method used

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  • Method for preparing Ni2P catalyst
  • Method for preparing Ni2P catalyst
  • Method for preparing Ni2P catalyst

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0026] Example 1

[0027] Take 2g NaH 2 PO 2 .H 2 O is placed in a closed reactor (such as figure 1 (Shown) outside the reaction bed, weigh the metal nickel powder with a P / Ni molar ratio of 3 and place it on the inner reaction bed of the reactor. Reactor access N 2 After venting, vacuumize again, and after repeated air changes for 3 times, the reactor is vented into normal pressure N 2 Under airtight conditions, heat up to 250°C at a rate of 5°C / min, react at a constant temperature for 1h, cool to room temperature, vacuum and pass N 2 After replacing the reaction gas with gas, the sample located in the reaction bed inside the reactor is the prepared unloaded Ni 2 P catalyst, represented by Sample1, the XRD spectrum of Sample1 is shown in figure 2 .

Example Embodiment

[0028] Example 2

[0029] Take 2g NaH 2 PO 2 .H 2 O is placed on the outer reaction bed of a closed reactor, and metal nickel powder with a P / Ni molar ratio of 2 is weighed and placed on the inner reaction bed of the reactor. The reactor was ventilated with Ar gas, and then evacuated. After repeated air changes for 3 times, the reactor was ventilated with Ar gas at normal pressure. Under airtight conditions, the reactor was heated to 300℃ at a rate of 15℃ / min, reacted at a constant temperature for 2h, and cooled to At room temperature, after evacuating and ventilating Ar gas to replace the reaction gas, the sample located in the reaction bed inside the reactor is made of unloaded Ni 2 P catalyst, represented by Sample2, the XRD spectrum of Sample2 is shown in image 3 .

Example Embodiment

[0030] Example 3

[0031] Take 2g KH 2 PO 2 .H 2 O is placed on the outer reaction bed of a closed reactor, and metal nickel powder with a P / Ni molar ratio of 4 is weighed and placed on the inner reaction bed of the reactor. The reactor was vented with He gas, and then evacuated. After repeated air changes for 3 times, the reactor was evacuated. Under airtight conditions, the reactor was heated to 150°C at a rate of 30°C / min, reacted at a constant temperature for 3 hours, cooled to room temperature, and evacuated After replacing the reaction gas with He gas, the sample located in the reaction bed inside the reactor is made of unloaded Ni 2 P catalyst, represented by Sample3, see the XRD spectrum of Sample3 Figure 4 .

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Abstract

The invention provides a method for preparing a Ni2P catalyst, which belongs to the field of the petrochemical industry. The method comprises the following steps of: using metallic nickel as a precursor; separately placing a catalyst precursor (non-loading or loading nickel) and hypophosphite by the P/Ni mole ratio of 2 to 4 on two reaction beds in a closed reactor in which gas can flow; and heating to 150 to 300 DEG C to react for 1 to 3 hours at the speed of 5 to 30 DEG C/min in an inert gas atmosphere and under a closed condition, so as to prepare various non-loading or loading Ni2P catalysts. By using the preparation method provided by the invention, the catalyst can be prevented from introducing impurities, high-temperature and high-pressure treatment is not needed in the preparation process, PH3 poisonous gas is not used, the preparation methods and the advantages of the preparation methods of various efficient nickel catalysts can be transplanted to be used for preparing the Ni2P catalyst, and the preparation method is suitable for the industrial production.

Description

technical field [0001] The invention belongs to the field of petrochemical technology, in particular to a nickel phosphide (Ni 2 P) Preparation method of the catalyst. Background technique [0002] With the increasing demand for oil, the supply structure of oil resources has undergone major changes, and conventional oil resources have shown an obvious trend of heavy and inferior quality. In view of the increasingly stringent environmental regulations, hydrogenation for clean fuel production The performance of desulfurization (HDS) and hydrodenitrogenation (HDN) catalysts puts forward higher requirements. In addition to improving the performance of existing catalysts, the development of new high-efficiency catalysts is another powerful means to meet the requirements. Transition metal phosphides have similar physical properties to transition metal nitrides and carbides and excellent HDS, HDN activity and catalytic selectivity, and have attracted widespread attention. Among th...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J29/76C01B25/08
Inventor 任世彪文宏志水恒福王知彩雷智平
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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