Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Summary

A protocol for the synthesis of sponge-like and fold-like Ni_1-xNb_xO nanoparticles by chemical precipitation is presented.

Abstract

We demonstrate a method for the synthesis of Ni_xNb_1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of Ni_xNb_1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These Ni_xNb_1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni_0.97Nb_0.03O and Ni_0.92Nb_0.08O on the NiO surface, and the larger surface area of these Ni_xNb_1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m²/g can be obtained for Ni_0.92Nb_0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni_0.92Nb_0.08O catalysts have been investigated.

Introduction

The preparation of nanocomposites has received increasing attention due to their crucial application in various field. To prepare Ni-Nb-O mixed oxide nanoparticles,^1,2,3,4,5,6 different methods have been developed such as dry mixing method,^7,8 evaporation method,^9,10,11,12,

Protocol

Caution: For the proper handling methods, properties and toxicities of the chemicals described in this paper, refer to the relevant material safety data sheets (MSDS). Some of the chemicals used are toxic and carcinogenic and special cares must be taken. Nanomaterials may potentially pose safety hazards and health effects. Inhalation and skin contact should be avoided. Safety precaution must be exercised, such as performing the catalyst synthesis in the fume hood and catalyst performance evaluation with autoclave reactors. Personal protective equipment must be worn.

1. Preparation of Ni_0.97Nb_0.03O Cataly....

Results

X-ray diffraction (XRD) patterns (Figure 1 and Figure 2), BET surface areas, temperature-programmed reduction of hydrogen with hydrogen (H₂-TPR), scanning electron microscopy (SEM) equipped with an energy-dispersive X-ray (EDX) analyzer, X-ray photoelectron spectroscopy (XPS) were collected for the nanoparticles NiO, Ni-Nb-O and Nb₂O₅ oxides¹⁷ (Figure 3.......

Discussion

One of the common methods to prepare the nickel-doped bulk niobium oxide nanoparticles is rotary evaporation method.⁹ By employing various pressure and temperature conditions during the process of rotary evaporation, the precipitation of Ni-Nb-O particles commerce with the slow removal of the solvent. In contrast to the rotary evaporation method, the chemical precipitation method reported in this study has received increasing attention to prepare the nanoparticles as this do not require the remova.......

Materials

List of materials used in this article

Name	Company	Catalog Number	Comments
Niobium(V) oxalate hydrate, 98%	Alfa	L04481902
Nickel nitrate hexahydrate, 99%	Aladdin	N108891
Sodium hydroxide, 98%	Aladdin	S111501
Ammonium hydroxide, 23-25%	Aladdin	A112077
Anisole, 99%	Sinopharm	81001728
Diphenyl ether, 98%	Aladdin	D110644
Phenol, 98%	Sinopharm	100153008
2-Methoxyphenol, 98%	Sinopharm	30114526
Vanillin, 99.5%	Sinopharm	69024316
Potassium hydroxide, AR	Aladdin	P112284
N,N-Dimethylformamide, 99.5%	Sinopharm	40016462
2-Bromoacetophenone,98%	Aladdin	B103328
Diethyl ether,99.5%	Sinopharm	10009318
Decane,98%	Aladdin	D105231
Dodecane,99%	Aladdin	D119697
Niobic acid	CBMM	1313968
Heating and Drying Oven			DHG Series (shanghai jinghong laboratory instrument co. ltd)
Autoclave Reactor			CJF-0.05—0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)
Tube furnace			SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)
Heating magnetic stirrer			DF-101 (Yu Hua Instrument Co. Ltd.)
Rotary evaporator			RE-3000A (Shanghai Yarong Biochemical Instrument Factory)
Synthetic air
Hydrogen gas
Argon gas