Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides

The synthesis of Mg-Al layered double hydroxide (LDH) was explored, through a one-step wet mechanochemical route, with the use of a NETZSCH LME 1 horizontal bead mill. Raw materials selected comprised of a mixture of metallic oxides/hydroxides promoting green synthesis. The research aims to expand o...

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Main Authors: Brenda Antoinette Barnard, Frederick Johannes Willem Jacobus Labuschagné
Format: Article
Language:English
Published: MDPI AG 2021-03-01
Series:Crystals
Subjects:
Online Access:https://www.mdpi.com/2073-4352/11/3/276
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author Brenda Antoinette Barnard
Frederick Johannes Willem Jacobus Labuschagné
author_facet Brenda Antoinette Barnard
Frederick Johannes Willem Jacobus Labuschagné
author_sort Brenda Antoinette Barnard
collection DOAJ
description The synthesis of Mg-Al layered double hydroxide (LDH) was explored, through a one-step wet mechanochemical route, with the use of a NETZSCH LME 1 horizontal bead mill. Raw materials selected comprised of a mixture of metallic oxides/hydroxides promoting green synthesis. The research aims to expand on the understanding of the wet mechanochemical synthesis of Mg-Al LDH through variation in milling and synthesis parameters. The selected parameters investigated were rotational speed, retention time, solids loading, bead size and jacket water inlet temperature. Samples were collected, filtered and dried at 60 °C for 12 h. Unless stated otherwise, or under investigation, parameters were kept constant at pre-selected conditions adapted from existing literature. LDH synthesis was deemed to occur successfully at elevated jacket water temperatures of 50 °C and longer retention times. It was noted that Al(OH)<sub>3</sub> XRD peak reduction occurred readily for increased rotational speeds and residence times, regardless of system temperature. MgO was deemed to react more readily at elevated temperatures. It was proposed that the amorphitisation and mechanochemical activation of Al(OH)<sub>3</sub> contributed to its dissolution providing the relevant Al<sup>3+</sup> ions necessary for Mg<sup>2+</sup> isomorphic substitution. Increasing the system temperature promoted the hydration of MgO, with the absence of Mg(OH)<sub>2</sub> attributed to its contribution as an intermediate phase prior to LDH formation.
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spelling doaj.art-88388acad06144738fe5685914dd8b942023-11-21T10:02:38ZengMDPI AGCrystals2073-43522021-03-0111327610.3390/cryst11030276Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double HydroxidesBrenda Antoinette Barnard0Frederick Johannes Willem Jacobus Labuschagné1Department of Chemical Engineering, University of Pretoria, Lynnwood Rd, Hatfield, Pretoria 0002, South AfricaDepartment of Chemical Engineering, University of Pretoria, Lynnwood Rd, Hatfield, Pretoria 0002, South AfricaThe synthesis of Mg-Al layered double hydroxide (LDH) was explored, through a one-step wet mechanochemical route, with the use of a NETZSCH LME 1 horizontal bead mill. Raw materials selected comprised of a mixture of metallic oxides/hydroxides promoting green synthesis. The research aims to expand on the understanding of the wet mechanochemical synthesis of Mg-Al LDH through variation in milling and synthesis parameters. The selected parameters investigated were rotational speed, retention time, solids loading, bead size and jacket water inlet temperature. Samples were collected, filtered and dried at 60 °C for 12 h. Unless stated otherwise, or under investigation, parameters were kept constant at pre-selected conditions adapted from existing literature. LDH synthesis was deemed to occur successfully at elevated jacket water temperatures of 50 °C and longer retention times. It was noted that Al(OH)<sub>3</sub> XRD peak reduction occurred readily for increased rotational speeds and residence times, regardless of system temperature. MgO was deemed to react more readily at elevated temperatures. It was proposed that the amorphitisation and mechanochemical activation of Al(OH)<sub>3</sub> contributed to its dissolution providing the relevant Al<sup>3+</sup> ions necessary for Mg<sup>2+</sup> isomorphic substitution. Increasing the system temperature promoted the hydration of MgO, with the absence of Mg(OH)<sub>2</sub> attributed to its contribution as an intermediate phase prior to LDH formation.https://www.mdpi.com/2073-4352/11/3/276layered double hydroxidemechanochemistrysynthesismilling parameterswet grindingbead mill
spellingShingle Brenda Antoinette Barnard
Frederick Johannes Willem Jacobus Labuschagné
Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
Crystals
layered double hydroxide
mechanochemistry
synthesis
milling parameters
wet grinding
bead mill
title Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
title_full Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
title_fullStr Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
title_full_unstemmed Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
title_short Exploring the Influence of Milling Parameters on the Wet Mechanochemical Synthesis of Mg-Al Layered Double Hydroxides
title_sort exploring the influence of milling parameters on the wet mechanochemical synthesis of mg al layered double hydroxides
topic layered double hydroxide
mechanochemistry
synthesis
milling parameters
wet grinding
bead mill
url https://www.mdpi.com/2073-4352/11/3/276
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