Ni2P/Al2O3 catalyst and preparation method therefor

A catalyst and carrier technology, applied in the field of supported nickel phosphide solid catalyst and its preparation, can solve the problems of difficult catalyst and high toxicity

Inactive Publication Date: 2015-10-14
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, according to the analysis of da Silva et al. (J.Catal.,2011,279:88-102), these methods have more or less problems, making them difficult to be used in the preparation of industrial heterogeneous Ni 2 P / Al 2 o 3 catalyst
Such as PH 3 It is highly toxic; and when using phosphite as a precursor, the P / Ni molar ratio is still as high as 2. Although the prepared catalyst is highly active, it is deactivated very quickly (J.Phys.Chem.C, 2009, 113: 17032-17044 )

Method used

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  • Ni2P/Al2O3 catalyst and preparation method therefor
  • Ni2P/Al2O3 catalyst and preparation method therefor

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Embodiment 1

[0023] Preparation of Ce Oxide-Modified Pentacoordinate Al-rich Al 2 o 3 .

[0024] Weigh 12 grams of Al(NO 3 ) 3 9H 2 O was dissolved in 15 milliliters of deionized water to make solution A, then weighed 4 grams of glycine (C 2 h 5 NO 2 ) was dissolved in 15 milliliters of deionized water to make solution B, the two were mixed while stirring, then the pH value of the solution was adjusted to 2-3 by adding dilute nitric acid dropwise, and then 0.347 grams of cerium nitrate (Ce(NO 3 ) 3 ·6H 2 O) and 0.2 g of polyethylene glycol. After the solution was fully mixed, it was transferred into a crucible, and left to age at room temperature for 12 hours. Afterwards, the crucible was dried in an oven at 120°C until it was in a colloidal state, and then the crucible was placed in a muffle furnace and heated to 750°C at a rate of 5°C / min, and fired for 4 hours to obtain Ce oxide-modified Al 2 o 3 , denoted as Ce-Al 2 o 3 , where Ce oxides (as CeO 2 The content of mass per...

Embodiment 2

[0026] Al(NO 3 ) 3 Preparation of Al after reaction with citric acid 2 o 3

[0027] Al was prepared according to the method disclosed in the literature 2 o 3 (Colloids and Surfaces A: Physicochem. Eng. Aspects, 2010, 371:126-130). Weigh 3.75 grams of Al(NO 3 ) 3 9H 2 O was dissolved in 20 ml of ethanol to make solution A, and then 0.84 g of citric acid was weighed and dissolved in solution A, then 1 g of P123 was added under vigorous stirring, stirred in a water bath at 60°C for 12 hours, and then placed in an oven at 60 ℃ to dry to a transparent solid state, and then aged at room temperature for 96 hours, transferred to a crucible and heated to 400-800 ℃ for 6 hours in a muffle furnace, recorded as EC-Al 2 o 3 . Combined with references (J.Colloid Interf.Sci.,2003,261:320-324; Acta Catalytica Sinica,2010,31:528-534), by 27 Al MAS NMR spectrum ( figure 1 ), it can be seen that in EC-Al 2 o 3 Among them, the intensity of the five-coordinated aluminum peak is the ...

Embodiment 3

[0029] Starting from nickel phosphate precursor, the supported nickel phosphide catalyst was prepared by hydrogen temperature programmed reduction method.

[0030] Phosphate precursors of supported nickel phosphide catalysts were prepared by a stepwise impregnation method. First weigh 1.12 grams of nickel nitrate hexahydrate (Ni(NO 3 ) 2 ·6H 2 O) be dissolved in 2 milliliters of deionized water and make impregnating liquid, then slowly add dropwise to the gamma-Al of 1.8 grams in above-mentioned impregnating liquid 2 o 3 or Ce-Al 2 o 3 or EC-Al 2 o 3 , aged at room temperature for 8 hours, and then dried in an oven at 120°C to prepare precursor A. Then weigh 0.613 grams of diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was dissolved in 3 ml of deionized water to make an impregnating solution, which was slowly added dropwise to the precursor A, left to age at room temperature for 8 hours, and dried at 120°C to prepare the precursor B. Then the precursor B was calc...

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Abstract

The invention relates to a Ni2P / Al2O3 catalyst and a preparation method therefor. The preparation method comprises the step of performing temperature programmed reduction treatment on a precursor-carrier compound, wherein the precursor is falcial phosphate, and the carrier is an Al2O3 carrier which is rich in 5-coordination aluminum. According to the preparation method disclosed by the invention, the Al2O3 which is rich in the 5-coordination aluminum is used as the carrier, the phosphate with a low P / Ni ratio is used as the precursor, and a temperature programmed reduction method is used for preparing the high-activity Ni2P catalyst. The hydrodesulfurization (HDS) activity of the supported Ni2P / Al2O3 catalyst obtained by the preparation method to dibenzothiophene (DBT) is equivalent to that of the catalyst using SiO2 as the carrier.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and in particular relates to a type of supported nickel phosphide solid catalyst and a preparation method thereof. Background technique [0002] Transition metal phosphides are a general term for covalent compounds formed by phosphorus and transition metals (Co, Ni, Mo, and W, etc.). Transition metal phosphides can be divided into metal-rich phosphides (M / P≥1) and phosphorus-rich phosphides (M / P<1) according to the stoichiometric ratio of phosphorus to metal (M). The latter is unstable, while metal-rich transition metal phosphides are hard and have good thermodynamic and chemical stability, which can be used as catalysts. With Ni 2 P, MoP, WP, Co 2 A series of transition metal phosphides represented by P and CoP have broad application prospects in the fields of hydrofinishing, hydrogenation, dehydrogenation and hydrodeoxygenation due to their high activity and stability. Am...

Claims

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Application Information

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IPC IPC(8): B01J27/185C07C7/163C07C13/50
Inventor 李翔冯建朋王安杰郭靖宇
Owner DALIAN UNIV OF TECH
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