Load type nickel phosphide catalyst and pre-phosphating preparation method thereof

A catalyst, nickel phosphide technology, used in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as poor purity and dispersion, improve purity, avoid oxidative deactivation, and high activity Effect

Inactive Publication Date: 2015-08-19
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] In order to solve the existing Ni 2 The technical problems of poor purity and dispersibility in the P catalyst preparation method, the object of the invention is to provide a kind of supported nickel phosphide catalyst and its pre-phosphating preparation method, the method technology is simple, the prepared Ni 2 The P catalyst has high purity and high dispersion, and the catalyst has higher hydrogenation activity under the same hydrogenation reaction process conditions, and can be applied to deep hydrotreating of inferior middle distillates or heavy distillates

Method used

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  • Load type nickel phosphide catalyst and pre-phosphating preparation method thereof
  • Load type nickel phosphide catalyst and pre-phosphating preparation method thereof
  • Load type nickel phosphide catalyst and pre-phosphating preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Take 42.5g of alumina as a carrier. The water absorption rate of the alumina support was 1.0 ml / g. Weigh 25g of nickel acetate, 10ml of ammonia water, the concentration of ammonia water is 25%~28wt.%, and the density is 0.87g / cm 3 . Dissolve nickel acetate in ammonia water to prepare nickel acetate ammonia solution, that is, impregnation solution. The catalyst was impregnated by equal volume impregnation. Dry at room temperature for 8 hours, and dry at 120°C for 6 hours to prepare a nickel oxide-supported catalyst, sample number S-1.

Embodiment 2

[0061] Take 10ml of catalyst S-1 loaded with nickel oxide and place it in the reactor, and feed H 2 , H 2 The pressure is 2MPa and the space velocity is 2h -1 . 1°C / min to raise the temperature to 120°C, and feed 3wt% triphenylphosphine (PPH 3 ) in cyclohexane solution, the temperature was programmed to 400°C, and pre-phosphating was performed for 12 hours. Obtain supported nickel phosphide catalyst, sample number C-1.

[0062] The Ni prepared in this example 2 P catalyst specific surface area is 253m 2 / g, the average pore diameter is 6.3nm, and the pore volume is 0.53cm 3 / g, the loading of Ni is 15.2%wt, and Ni / P is 1.98 (molar ratio).

Embodiment 3

[0064] Take 10ml of catalyst S-1 loaded with nickel oxide and place it in the reactor, and feed H 2 , H 2 The pressure is 2MPa and the space velocity is 2h -1 , 1°C / min to raise the temperature to 400°C, reduce for 6h, and convert the nickel oxide into the reduced state of nickel. Then the temperature was lowered to 300°C, and 3wt% triphenylphosphine (PPh 3 ) toluene solution, pre-phosphating for 12h. Take out to obtain supported nickel phosphide catalyst, sample number C-2.

[0065] The Ni prepared in this example2 P catalyst specific surface area is 248m 2 / g, the pore diameter is 6.5nm, and the pore volume is 0.52cm 3 / g, the loading of Ni is 15.0%wt, and Ni / P is 2.11 (molar ratio).

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Abstract

The invention discloses a load type nickel phosphide catalyst and a pre-phosphating preparation method thereof, belonging to the technical field of petrochemical engineering. The load type nickel phosphide catalyst is prepared by loading nickel salt on a carrier, then pre-phosphating a nickel oxide-loaded catalyst in a reactor, and enabling nickel oxide to be transformed into nickel phosphide in situ. The prepared catalyst is high in load capacity, better in dispersity, higher in purity and good in hydrogenation performance. Meanwhile, the method remarkably simplifies a preparation method of the nickel phosphide catalyst, simplifies preparation steps, reduces preparation cost and has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of petrochemical industry, in particular to a supported nickel phosphide catalyst and a prephosphating preparation method thereof. The method is simple and safe for preparing nickel phosphide catalyst, and the prepared catalyst has high purity and is used for hydrogenation , hydrodesulfurization and other reaction processes have higher hydrogenation activity. Background technique [0002] 60% of my country's petroleum products are engine fuel oils, such as gasoline, diesel and kerosene. Sulfur and nitrogen in fuel oil will generate NO X and SO X Along with the exhaust gas, it pollutes the air and is also the main cause of acid rain. The presence of sulfur can also cause corrosion to vehicle engines. The world has paid great attention to the sulfur content in fuel oil. Desulfurization technology mainly includes non-hydrodesulfurization and hydrodesulfurization (HDS). Non-hydrogenation desulfurization incl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C10G45/06
Inventor 柴永明刘佳怡刘晨光刘宾李奕川谢坤张迟
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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