Optimization of the controllable crystal size of iron/zeolite nanocomposites using a Box–Behnken design and their catalytic activity

Nurazni Amat Bahari, Wan Isahak Wan Nor Roslam, Mohd Shahbudin Mastar @ Masdar, Muneer M. Ba-Abbad

Research output: Contribution to journalArticle

Abstract

Experimental conditions for the synthesis of an iron nanoparticle (NPs)–zeolite composite (hereinafter denoted as Fe/zeolite NPs) via sol–gel method were optimized using a Box–Behnken design to produce a high formic acid yield. The effects of various parameters, including weight ratio of starting materials (Fe and zeolite), volume of polyethylene glycol (PEG) as a surfactant, and calcination temperature, on controllable crystallite size, and the relationship between crystallite size and formic acid yield were studied. The crystal size, as the main parameter indicating formic acid yield, of Fe NPs was evaluated through polynomial regression. Results revealed that the optimum conditions for producing small Fe NPs based on the model were obtained at a weight ratio of Fe to zeolite of 62.5%, a PEG volume of 2 mL, and a calcination temperature of 500 °C. The experimental results (52.02 nm) versus the predicted results (58.30 nm) of the crystal size of Fe NPs under the optimum synthesis conditions were similar. Furthermore, 62.5% Fe/zeolite NPs with a crystal size of 52.02 nm produced the highest formic acid concentration from CO 2 hydrogenation. Conversely, 100% Fe/zeolite NPs had a smaller crystal size but exhibited a remarkably lower reaction performance. This high ratio of Fe and zeolite contributed to the increased agglomeration of Fe particles. The zeolite surface became fully covered and subsequently reduced the reactant interaction on catalyst surfaces. Highlights: Fe–zeolite nanocomposite was optimized using a Box–Behnken design.The polynomial regression model showed the optimum nanoparticle (NP) crystal size of 52.02 nm.Synthesis parameters significantly affected catalyst morphology and crystal.The effect of calcination plays an important role on crystal and particle size.The influence of NP crystallite size was evaluated in terms of formic acid production.

Original languageEnglish
Pages (from-to)209-224
Number of pages16
JournalApplied Nanoscience (Switzerland)
Volume9
Issue number2
DOIs
Publication statusPublished - 1 Mar 2019

Fingerprint

formic acid
Zeolites
Nanocomposites
catalytic activity
Catalyst activity
nanocomposites
Formic acid
Iron
iron
Crystals
optimization
crystals
Crystallite size
Calcination
Nanoparticles
roasting
Polyethylene glycols
nanoparticles
Polynomials
glycols

Keywords

  • Box–Behnken design
  • Carbon dioxide
  • Fe/zeolite nanoparticles
  • Formic acid
  • Optimization

ASJC Scopus subject areas

  • Biotechnology
  • Materials Science (miscellaneous)
  • Atomic and Molecular Physics, and Optics
  • Electrical and Electronic Engineering
  • Physical and Theoretical Chemistry
  • Cell Biology

Cite this

@article{3e5f5e35647d49e8895208b110c45e0f,
title = "Optimization of the controllable crystal size of iron/zeolite nanocomposites using a Box–Behnken design and their catalytic activity",
abstract = "Experimental conditions for the synthesis of an iron nanoparticle (NPs)–zeolite composite (hereinafter denoted as Fe/zeolite NPs) via sol–gel method were optimized using a Box–Behnken design to produce a high formic acid yield. The effects of various parameters, including weight ratio of starting materials (Fe and zeolite), volume of polyethylene glycol (PEG) as a surfactant, and calcination temperature, on controllable crystallite size, and the relationship between crystallite size and formic acid yield were studied. The crystal size, as the main parameter indicating formic acid yield, of Fe NPs was evaluated through polynomial regression. Results revealed that the optimum conditions for producing small Fe NPs based on the model were obtained at a weight ratio of Fe to zeolite of 62.5{\%}, a PEG volume of 2 mL, and a calcination temperature of 500 °C. The experimental results (52.02 nm) versus the predicted results (58.30 nm) of the crystal size of Fe NPs under the optimum synthesis conditions were similar. Furthermore, 62.5{\%} Fe/zeolite NPs with a crystal size of 52.02 nm produced the highest formic acid concentration from CO 2 hydrogenation. Conversely, 100{\%} Fe/zeolite NPs had a smaller crystal size but exhibited a remarkably lower reaction performance. This high ratio of Fe and zeolite contributed to the increased agglomeration of Fe particles. The zeolite surface became fully covered and subsequently reduced the reactant interaction on catalyst surfaces. Highlights: Fe–zeolite nanocomposite was optimized using a Box–Behnken design.The polynomial regression model showed the optimum nanoparticle (NP) crystal size of 52.02 nm.Synthesis parameters significantly affected catalyst morphology and crystal.The effect of calcination plays an important role on crystal and particle size.The influence of NP crystallite size was evaluated in terms of formic acid production.",
keywords = "Box–Behnken design, Carbon dioxide, Fe/zeolite nanoparticles, Formic acid, Optimization",
author = "Bahari, {Nurazni Amat} and {Wan Nor Roslam}, {Wan Isahak} and {Mastar @ Masdar}, {Mohd Shahbudin} and Ba-Abbad, {Muneer M.}",
year = "2019",
month = "3",
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doi = "10.1007/s13204-018-0920-8",
language = "English",
volume = "9",
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journal = "Applied Nanoscience (Switzerland)",
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TY - JOUR

T1 - Optimization of the controllable crystal size of iron/zeolite nanocomposites using a Box–Behnken design and their catalytic activity

AU - Bahari, Nurazni Amat

AU - Wan Nor Roslam, Wan Isahak

AU - Mastar @ Masdar, Mohd Shahbudin

AU - Ba-Abbad, Muneer M.

PY - 2019/3/1

Y1 - 2019/3/1

N2 - Experimental conditions for the synthesis of an iron nanoparticle (NPs)–zeolite composite (hereinafter denoted as Fe/zeolite NPs) via sol–gel method were optimized using a Box–Behnken design to produce a high formic acid yield. The effects of various parameters, including weight ratio of starting materials (Fe and zeolite), volume of polyethylene glycol (PEG) as a surfactant, and calcination temperature, on controllable crystallite size, and the relationship between crystallite size and formic acid yield were studied. The crystal size, as the main parameter indicating formic acid yield, of Fe NPs was evaluated through polynomial regression. Results revealed that the optimum conditions for producing small Fe NPs based on the model were obtained at a weight ratio of Fe to zeolite of 62.5%, a PEG volume of 2 mL, and a calcination temperature of 500 °C. The experimental results (52.02 nm) versus the predicted results (58.30 nm) of the crystal size of Fe NPs under the optimum synthesis conditions were similar. Furthermore, 62.5% Fe/zeolite NPs with a crystal size of 52.02 nm produced the highest formic acid concentration from CO 2 hydrogenation. Conversely, 100% Fe/zeolite NPs had a smaller crystal size but exhibited a remarkably lower reaction performance. This high ratio of Fe and zeolite contributed to the increased agglomeration of Fe particles. The zeolite surface became fully covered and subsequently reduced the reactant interaction on catalyst surfaces. Highlights: Fe–zeolite nanocomposite was optimized using a Box–Behnken design.The polynomial regression model showed the optimum nanoparticle (NP) crystal size of 52.02 nm.Synthesis parameters significantly affected catalyst morphology and crystal.The effect of calcination plays an important role on crystal and particle size.The influence of NP crystallite size was evaluated in terms of formic acid production.

AB - Experimental conditions for the synthesis of an iron nanoparticle (NPs)–zeolite composite (hereinafter denoted as Fe/zeolite NPs) via sol–gel method were optimized using a Box–Behnken design to produce a high formic acid yield. The effects of various parameters, including weight ratio of starting materials (Fe and zeolite), volume of polyethylene glycol (PEG) as a surfactant, and calcination temperature, on controllable crystallite size, and the relationship between crystallite size and formic acid yield were studied. The crystal size, as the main parameter indicating formic acid yield, of Fe NPs was evaluated through polynomial regression. Results revealed that the optimum conditions for producing small Fe NPs based on the model were obtained at a weight ratio of Fe to zeolite of 62.5%, a PEG volume of 2 mL, and a calcination temperature of 500 °C. The experimental results (52.02 nm) versus the predicted results (58.30 nm) of the crystal size of Fe NPs under the optimum synthesis conditions were similar. Furthermore, 62.5% Fe/zeolite NPs with a crystal size of 52.02 nm produced the highest formic acid concentration from CO 2 hydrogenation. Conversely, 100% Fe/zeolite NPs had a smaller crystal size but exhibited a remarkably lower reaction performance. This high ratio of Fe and zeolite contributed to the increased agglomeration of Fe particles. The zeolite surface became fully covered and subsequently reduced the reactant interaction on catalyst surfaces. Highlights: Fe–zeolite nanocomposite was optimized using a Box–Behnken design.The polynomial regression model showed the optimum nanoparticle (NP) crystal size of 52.02 nm.Synthesis parameters significantly affected catalyst morphology and crystal.The effect of calcination plays an important role on crystal and particle size.The influence of NP crystallite size was evaluated in terms of formic acid production.

KW - Box–Behnken design

KW - Carbon dioxide

KW - Fe/zeolite nanoparticles

KW - Formic acid

KW - Optimization

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