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Nickel phosphide catalyst, method for preparing same and application of nickel phosphide catalyst

A catalyst, nickel phosphide technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of complex process, inability to realize catalyst in-situ synthesis-hydrodesulfurization reaction, etc., and achieve the preparation process Simplify the process, solve the effect of high reduction temperature and reduction promotion

Inactive Publication Date: 2017-05-17
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, after the synthesis reaction, it is necessary to remove the non-volatile inorganic salts generated during the reaction process. When using chlorine-containing reagents, it is necessary to remove the residual chlorine on the surface of the solid catalyst. Not only is the process complicated, but also the in-situ synthesis of the catalyst-hydrodesulfurization reaction cannot be realized.

Method used

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  • Nickel phosphide catalyst, method for preparing same and application of nickel phosphide catalyst
  • Nickel phosphide catalyst, method for preparing same and application of nickel phosphide catalyst
  • Nickel phosphide catalyst, method for preparing same and application of nickel phosphide catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1 uses ammonium hypophosphite (NH 4 h 2 PO 2 ) as phosphorus source to prepare Ni 2 P / MCM-41 catalyst, and characterize the prepared catalyst. Specifically include the following steps:

[0027] (1)Ni 2 Preparation of P / MCM-41 catalyst precursor:

[0028] Dissolve nickel acetate (analytical pure, 99%) and ammonium hypophosphite (analytical pure, 99%) in distilled water according to the Ni / P molar ratio of 1:2, stir to obtain a suspension, and then add concentrated nitric acid to it to obtain clarification solution, then add MCM-41 mesoporous molecular sieves, impregnate for 12 hours, dry at 60°C for 30min, and then bake at 480°C for 3 hours to obtain Ni 2 P / MCM-41 catalyst precursor.

[0029] (2)Ni 2 Preparation of P / MCM-41 Catalyst

[0030] Ni prepared by step (1) 2 The P / MCM-41 catalyst precursor is placed in a fixed bed reactor, heated to 350°C in a hydrogen flow of 100mL / min at a rate of 2.5°C / min per minute, kept at this temperature for 2 hours,...

Embodiment 2

[0035] Example 2 provides Ni 2 The preparation method of P / MCM-41 catalyst, and the prepared catalyst is characterized. Specifically include the following steps:

[0036] (1)Ni 2 Preparation of P / MCM-41 Catalyst Precursor

[0037] Dissolve nickel acetate (analytical pure, 99%) and ammonium hypophosphite (analytical pure, 99%) in distilled water according to the Ni / P molar ratio of 1:4, stir to obtain a suspension, and then add concentrated nitric acid to it to obtain clarification solution, then add MCM-41 mesoporous molecular sieves, impregnate for 15 hours, dry at 40°C for 50min, and then bake at 500°C for 2 hours to obtain Ni 2 P / MCM-41 catalyst precursor.

[0038] (2)Ni 2 Preparation of P / MCM-41 Catalyst

[0039] Ni prepared by step (1) 2 The P / MCM-41 catalyst precursor was placed in a fixed bed reactor, heated to 350°C in a hydrogen flow of 120mL / min at a rate of 3°C / min per minute, kept at this temperature for 2.5 hours and then heated to 20°C / min rate to cool d...

Embodiment 3

[0041] The difference between embodiment 3 and embodiment 2 is only in Ni 2 During the preparation of the P / MCM-41 catalyst, the temperature in the fixed-bed reactor was heated to 400°C, and the rest of the steps and parameters were the same.

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PUM

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Abstract

The invention relates to a nickel phosphide catalyst, a method for preparing the same and application of the nickel phosphide catalyst. The method includes steps of dissolving nickel acetate and phosphorus sources in water to obtain suspension, adding concentrated nitric acid into the suspension to obtain clear solution, then adding MCM-41 mesoporous molecular sieves into the clear solution, soaking the MCM-41 mesoporous molecular sieves in the clear solution, drying the MCM-41 mesoporous molecular sieves and then calcining the MCM-41 mesoporous molecular sieves to obtain precursors; placing the precursors in a fixed-bed reactor, heating the fixed-bed reactor in hydrogen flow until the temperature of the fixed-bed reactor reaches 350-600 DEG C, preserving heat for 1.5-2.5 h, then cooling the fixed-bed reactor until the temperature of the fixed-bed reactor reaches the room temperature, and then carrying out passivating treatment to obtain the nickel phosphide catalyst. The nickel phosphide catalyst, the method and the application have the advantages that the nickel acetate is used as a nickel source, accordingly, inorganic salt difficult to volatilize can be prevented in synthetic reaction procedures, and procedures for preparing the nickel phosphide catalyst can be simplified to a great extent; organic nickel acid is used as the nickel source, effects of promoting reduction of nickel phosphide can be realized by organic acid radicals, and accordingly the problem of high reduction temperatures and energy consumption in existing procedures for preparing existing nickel phosphide catalysts can be effectively solved.

Description

technical field [0001] The invention relates to a nickel phosphide catalyst and its preparation method and application. Background technique [0002] In recent years, with the improvement of people's awareness of environmental protection, efficient oil desulfurization technology has attracted much attention. Fuel oil desulfurization technology has gradually shifted to the field of deep desulfurization and ultra-deep desulfurization, and the current commercial hydrodesulfurization (HDS) catalysts have been difficult to meet this requirement. Therefore, improving the original sulfide catalysts and finding new high-efficiency substitutes have become the focus of recent research by researchers. Ni 2 P is a material with high hydrodesulfurization activity discovered in recent years. Under the same test conditions, Ni 2 P / SiO 2 Catalyst activity ratio NiMo / Al 2 o 3 and CoMo / Al 2 o 3 Both are high, and the order of activity of similar phosphides is: Ni 2 P>WP>MoP>...

Claims

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Application Information

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IPC IPC(8): B01J29/76C10G45/12
CPCB01J29/76C10G45/12C10G2300/202C10G2300/70
Inventor 宋华姜楠李锋王雪芹陈彦广张娇静张福勇
Owner NORTHEAST GASOLINEEUM UNIV
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