Preparation method of silica supported nickel phosphide catalyst

A technology of silica and nickel catalysts, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc.

Inactive Publication Date: 2015-07-15
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can prepare monodisperse metal phosphides with different morphologies, but due to the presence of excess phosphorus, it is easy to generate phosphorus-rich phase phosphides (such as Ni 5 P 4 )

Method used

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  • Preparation method of silica supported nickel phosphide catalyst
  • Preparation method of silica supported nickel phosphide catalyst
  • Preparation method of silica supported nickel phosphide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 29.7g Ni(NO 3 ) 2 ·6H 2 O was dissolved in water to make a 100ml solution; another 18.9g NaSiO 3 9H 2 O and 11.7 g Na 2 CO 3 Dissolve in water to make 100ml solution. Add the above two solutions dropwise to 200ml of distilled water at the same time under stirring to form a green precipitate. After washing the precipitate with distilled water, add 200ml of n-butanol, evaporate to dryness in a water bath, and then dry it in a 393K oven to obtain Nickel catalyst supported on silicon.

Embodiment 2

[0018] Weigh 5 g of the silica-supported nickel catalyst of Example 1 and fill it into a reactor, raise the temperature to 673K, feed hydrogen at a flow rate of 100ml / min, reduce the temperature for 2h, then cool down to 543K, and feed 4 wt% triphenyl The n-heptane solution of base phosphine was phosphated for 12h, and the flow rate of n-heptane solution was 15ml / h. 2 Passivate with 1% nitrogen for 12 hours, and the flow rate of nitrogen is 20ml / min, to obtain a passivated silicon dioxide-supported nickel phosphide catalyst. The specific surface area of ​​the prepared catalyst (named NP1) is 123m 2 / g, XRD spectrum is shown in accompanying drawing.

Embodiment 3

[0020] Weigh 5 g of the silica-supported nickel catalyst of Example 1 and fill it into a reactor, raise the temperature to 673K, feed hydrogen at a hydrogen flow rate of 100ml / min, reduce the temperature for 2h, then cool down to 443K, and feed 4wt% triphenyl The n-heptane solution of base phosphine was phosphated for 12h, and the flow rate of n-heptane solution was 15ml / h. 2 Passivate with 1% nitrogen for 12 hours, and the flow rate of nitrogen is 20ml / min, to obtain a passivated silicon dioxide-supported nickel phosphide catalyst. The specific surface area of ​​the prepared catalyst (named NP2) is 197m 2 / g, XRD spectrum is shown in accompanying drawing.

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Abstract

A supported nickel phosphide catalyst has quite high hydrogenation desulfurization activity and relatively good activity stability. A traditional nickel phosphide catalyst is prepared by a way of temperature programming reduction of nickel phosphate, and the dispersion degree of active components is relatively low. Firstly, a silica supported nickel precursor is reduced or roasted under a hydrogen atmosphere, then a phosphating solution is introduced and phosphorization is carried out at lower temperature, and thus the Ni2P / SiO2 catalyst having quite high dispersion degree of the active components and having quite high hydrogenation desulfurization and denitrification activity is obtained. The catalyst can also be used for hydrogenation treatment on diesel oil and for production of clean diesel oil, and also can be used in sulfur-resisting hydrogenation reactions of other occasions.

Description

technical field [0001] The invention relates to a preparation method of a silicon dioxide-loaded nickel phosphide catalyst used for diesel hydrotreating. technical background [0002] As people pay more and more attention to environmental issues, environmental laws and regulations restrict the sulfur content in fuel oil more and more strictly. The current European V fuel standard (EU2009) requires both gasoline and diesel to contain less than 10 ppmw sulfur. Recently, domestic vehicle fuel will implement the National IV quality standard, which stipulates that the sulfur content shall not exceed 50ppmw, which is far from the standards of advanced countries. Therefore, the domestic environmental protection pressure is very high, and it is necessary to accelerate the development of fuel oil hydrogenation refining technology and related processes, and vigorously develop clean fuel oil. However, only improving or optimizing the traditional process can no longer meet the increas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C10G45/06
Inventor 沈俭一王俊恩傅玉川陈慧
Owner NANJING UNIV
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