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Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS

Dissertation (MSc)--University of Pretoria, 2014.

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Other Authors: Labuschagne, F.J.W.J. (Frederick Johannes Willem Jacobus)
Format: Thesis
Language:English
Published: University of Pretoria 2022
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author2 Labuschagne, F.J.W.J. (Frederick Johannes Willem Jacobus)
author_browse Labuschagne, F.J.W.J. (Frederick Johannes Willem Jacobus)
author_facet Labuschagne, F.J.W.J. (Frederick Johannes Willem Jacobus)
collection Thesis
dc_rights_str_mv © 2021 University of Pretoria. All rights reserved. The copyright in this work vests in the University of Pretoria. No part of this work may be reproduced or transmitted in any form or by any means, without the prior written permission of the University of Pretoria.
description Dissertation (MSc)--University of Pretoria, 2014.
format Thesis
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institution University of Pretoria (South Africa)
language English
last_indexed 2026-06-10T12:38:39.945Z
license_str Other — see source repository
provenance_str_mv Harvested via OAI-PMH from UPSpace — University of Pretoria Institutional Repository
publishDate 2022
publishDateRange 2022
publishDateSort 2022
publisher University of Pretoria
publisherStr University of Pretoria
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source_str UPSpace — University of Pretoria Institutional Repository
spelling oai:repository.up.ac.za:2263/84055 Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS Labuschagne, F.J.W.J. (Frederick Johannes Willem Jacobus) johan.labuschagne@up.ac.za Venter, H.P. UCTD Layered double hydroxides Co-precipitation Dissolution-precipitation Crystal phase Solubility Dissertation (MSc)--University of Pretoria, 2014. A green synthesis method for the synthesis of hydrotalcite has been previously developed but this process has not yet been optimised. The main focus of this dissertation was on aluminium-based LDHs. The purpose of this investigation were; to determine optimum synthesis conditions for the formation of hydrotalcite using the dissolution-precipitation method and to determine the possibility of partial substituting the divalent metal species in hydrotalcite and hydrocalumite with other metal species. During the optimisation process for the formation of hydrotalcite using the dissolution precipitation method, the formation of hydromagnesite was proved to be dominant reaction at lower reaction temperatures. With the increase in reaction time and temperature the decomposition of hydromagnesite occurred to form magnesite. At low temperatures the formation of Mg-Al-CO3 LDH is limited due to the low solubility of gibbsite. Mg-Al-CO3 LDH formation of 80 % was achieved at 140 oC after 2 hours reaction time, but crystallinity was low. To achieve an Mg-Al-CO3 LDH conversion higher than 96 % a reaction temperature of 160 oC for a minimum of 4 hours is required, but is achieved within 1 hour at 180 oC. A 99.37 % conversion was achieved at 180 oC for 5 hours with a high crystallinity and homogeneity. The surface area for Mg-Al-CO3 LDH at 180 oC after 5 hours reaction time proved to be 9.19 m2/g. The average particle size obtained for a high crystalline LDH was in the range of approx. 3 μm and 6.8 μm at temperatures of 160 oC and above for a minimum of 3 hours reaction time. The following are recommended for future work:  Determine the effect of mixing speed on the shape of the platelets.  Determine the difference between freshly precipitated metal oxides/hydroxides as reagents compared to aged metal oxides/hydroxides. The presence of Mg(OH)2 and Ca(OH)2 in solution (respectively) did increase the pH enough for the dissolution of gibbsite and most of the Mx+ metal species. A reaction time and temperature of 5 hours at 180 oC in a carbonate environment proved to be close to the ideal conditions for the formation of Mg/Mo-Al-CO3 LDH and Mg/Zn-Al-CO3 LDH. The results for the formation of Mg/Ti-Al-CO3 LDH were inconclusive. Isolation of the possible Mg/Ti-Al-CO3 LDH is recommended to determine the degree of substitution. The conditions for the dissolution of the metal species for the following experiments were proven to be successful:  Ca/Mn(lV)-Al  Ca/Mo-Al  Ca/Ni-Al  Ca/Ti-Al The following recommendations are made for the improvement on the formation of an Mx+-impregnated LDH/precursor:  Determine the effect of different reaction time and temperature.  Determine the effect of adding the carbonate source at temperatures above 100 oC under pressure.  Determine the effect of synthesising at different pH conditions. Cobalt and tin showed no/negligible amount of possible solubility. Chemical Engineering MSc Unrestricted 2022-02-18T07:52:55Z 2022-02-18T07:52:55Z 2014 2014 Dissertation * A2015 http://hdl.handle.net/2263/84055 en © 2021 University of Pretoria. All rights reserved. The copyright in this work vests in the University of Pretoria. No part of this work may be reproduced or transmitted in any form or by any means, without the prior written permission of the University of Pretoria. application/pdf University of Pretoria
spellingShingle UCTD
Layered double hydroxides
Co-precipitation
Dissolution-precipitation
Crystal phase
Solubility
Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title_full Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title_fullStr Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title_full_unstemmed Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title_short Optimisation of the synthesis of Mg-AI-CO3 LDH and the partial substitution of Mg/Ca-based LDHS
title_sort optimisation of the synthesis of mg ai co3 ldh and the partial substitution of mg ca based ldhs
topic UCTD
Layered double hydroxides
Co-precipitation
Dissolution-precipitation
Crystal phase
Solubility
url http://hdl.handle.net/2263/84055