Preparation method of supported Ni2P catalyst

A catalyst, nickel oxide technology, applied in the field of catalysis, can solve the problems of affecting the performance of the catalyst, prone to agglomeration, weak interaction, etc.

Inactive Publication Date: 2014-06-18
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the process is cumbersome and extremely inconvenient in practical application.
Although the reduction method can be used at a lower temperature (300~550 oC ) to prepare loaded Ni 2 P, but at the same time an impurity phase will be generated and more phosphate remains in the catalyst; when using Al 2 o 3 and silicon-aluminum molecular sieves and other aluminum-containing carriers, hypophosphite and phosphite will react with the carrier to form AlPO 4 , for the preparation of Ni 2 P needs to load more phosphorus species to affect catalyst performance
In addition, with trioctylphosphine or triphenylphosphine as phosphorus source, at 250~370 o C Phosphate metal Ni nanoparticles into monodisperse Ni by liquid phase method 2 P particles, and then loaded onto the carrier by impregnation method; although this method can prepare loaded Ni 2 P, the process is cumbersome, and Ni 2 The interaction between P and the carrier is weak, and it is easy to agglomerate during use

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] 4.36 g Ni(NO 3 ) 2 ?6H 2 O was dissolved in 9.0 ml of deionized water to make a nickel nitrate aqueous solution with a mass concentration of 20.4%, and 5 grams of silica carrier was impregnated in the solution in equal volume, and dried in air at 120°C for 12 hours, 500 ℃ for 4 hours to obtain a silica-supported nickel oxide sample. Get 1 gram of silica-loaded nickel oxide samples and place them in a stainless steel fixed-bed reactor at 450 o C was reduced with hydrogen for 2 h to obtain a Ni precursor supported on silica with a Ni mass content of 15%. Then, lower the temperature to 400 o C, when hydrogen is introduced and the mass space velocity of the solution is 8h -1 And under the condition that the P / Ni molar ratio is controlled to be 0.75, a triphenylphosphine dodecane solution with a mass concentration of 3% is passed into the reactor with a micro-feed pump to carry out phosphating treatment on silica-loaded Ni. After the treatment, the prepared samples wer...

Embodiment 2

[0012] Catalyst preparation process is the same as embodiment 1, and difference is that 0.248 gram of Ni (NO 3 ) 2 ?6H 2 O was dissolved in 10.6 ml of distilled water to form a nickel nitrate aqueous solution with a mass concentration of 1.4%, and an equal volume of 5 grams of silica carrier was impregnated in the solution. The mass content of Ni in the prepared silica-supported Ni sample is 1%, and the sample is prepared after phosphating to obtain silica-supported Ni 2 p.

Embodiment 3

[0014] Catalyst preparation process is the same as embodiment 1, and difference is that 10.59 grams of Ni (NO 3 ) 2 ?6H 2 O was dissolved in 6.8 milliliters of distilled water to form a nickel nitrate aqueous solution with a mass concentration of 38%, and 5 grams of silica carrier was impregnated in the solution in equal volume. The mass content of Ni in the prepared silica-supported Ni sample is 30%, and the sample is prepared after phosphating to obtain silica-supported Ni 2 p.

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Abstract

The invention discloses a preparation method of supported Ni2P catalyst. The preparation method of the supported Ni2P catalyst comprises the following steps: preparing a silicon dioxide, MCM-41, SBA-15, aluminium oxide, titanium oxide, HY molecular sieve or HZSM-5 molecular sieve supported nickel oxide precursor by adopting an impregnation way; reducing the supported nickel oxide precursor into a supported Ni precursor in a fixed bed reactor, then introducing hydrogen, introducing a triphenylphosphine or tri-n-octylphosphine solution into the fixed bed reactor at a certain temperature, and phosphating for a period of time at constant temperature, thus obtaining the supported Ni2P catalyst in situ. Compared with a general method for preparing the supported Ni2P catalyst by adopting a supported nickel phosphate temperature programmed reduction method, the preparation method of the supported Ni2P catalyst is simple and practicable, generation of aluminium phosphate owning to reaction between phosphorus species and aluminium oxide in a carrier can be avoided, and the phosphorus species can be effectively utilized.

Description

technical field [0001] The invention relates to a loaded Ni 2 The invention discloses a method for preparing a P catalyst, belonging to the technical field of catalysis. Background technique [0002] Since the 1990s, many studies have shown that transition metal phosphides exhibit unique catalytic performance in hydrodesulfurization, hydrodenitrogenation, hydrodechlorination, hydrodeoxygenation and some hydrogenation reactions (Journal of Catalysis, 2003, 216: 343; Catalysis Letters, 2012, 142: 1413; Applied Catalysis B: Environmental, 2014, 144: 870), which have attracted more and more attention from scholars and industries at home and abroad in recent years. Among the reported Ni, Co, Fe, Mo and W phosphide catalysts, Ni 2 P catalyst has better catalytic performance. [0003] Ni 2 There are many ways to prepare P catalyst, including phosphate temperature-programmed reduction method, phosphine reduction method, phosphite and hypophosphite reduction method, phosphorus so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J29/76B01J29/14B01J29/46
Inventor 陈吉祥韩蒙蒙
Owner TIANJIN UNIV
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