Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides

Amines with two carbon atoms in the organic chain [ethylamine (EA), diethylamine (DEA), triethylamine (TEA)] have been used as precipitant agents to obtain a hydrotalcite-like compound with Zn (II) and Al (III) as layered cations and with nitrate anions in the interlayered region to balance the char...

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Main Authors: Alexander Misol, Alejandro Jiménez, Francisco M. Labajos
Format: Article
Language:English
Published: MDPI AG 2022-07-01
Series:ChemEngineering
Subjects:
Online Access:https://www.mdpi.com/2305-7084/6/4/53
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author Alexander Misol
Alejandro Jiménez
Francisco M. Labajos
author_facet Alexander Misol
Alejandro Jiménez
Francisco M. Labajos
author_sort Alexander Misol
collection DOAJ
description Amines with two carbon atoms in the organic chain [ethylamine (EA), diethylamine (DEA), triethylamine (TEA)] have been used as precipitant agents to obtain a hydrotalcite-like compound with Zn (II) and Al (III) as layered cations and with nitrate anions in the interlayered region to balance the charge. This Layered Double Hydroxide was prepared following the coprecipitation method, and the effect on the crystal and particle sizes was studied. Also, the effect of submitting the obtained solids to hydrothermal post-synthesis treatment by conventional heating and microwave assisted heating were studied. The obtained solids were exhaustively characterized using several instrumental techniques, such as X-ray diffraction, Thermal Analysis (DTA and TG), Chemical Analysis, Infrared Spectroscopy (FT-IR), determination of Particle Size Distribution and BET-Surface area. Well crystallized solids were obtained showing two possible LDH phases, depending on the orientation of the interlayer anion with respect to the brucite-like layers. The results indicated that there is a certain influence of the amine, when used as a precipitating agent, and as a consequence of the degree of substitution, on the crystallinity and particle size of the final solid obtained. The LDHs obtained using TEA exhibited higher crystallinity, which was improved after a long hydrothermal treatment by conventional heating. Regarding the shape of the particles, the formation of aggregates in the former solid was detected, which could be easily disintegrated using ultrasound treatments, producing solid powder with high crystallinity and small particle size, with homogeneous size distribution.
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spelling doaj.art-20d4a58ae54848348667c1a39391b8122023-12-01T23:33:49ZengMDPI AGChemEngineering2305-70842022-07-01645310.3390/chemengineering6040053Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double HydroxidesAlexander Misol0Alejandro Jiménez1Francisco M. Labajos2GIR-QUESCAT, Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, SpainGIR-QUESCAT, Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, SpainGIR-QUESCAT, Departamento de Química Inorgánica, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, SpainAmines with two carbon atoms in the organic chain [ethylamine (EA), diethylamine (DEA), triethylamine (TEA)] have been used as precipitant agents to obtain a hydrotalcite-like compound with Zn (II) and Al (III) as layered cations and with nitrate anions in the interlayered region to balance the charge. This Layered Double Hydroxide was prepared following the coprecipitation method, and the effect on the crystal and particle sizes was studied. Also, the effect of submitting the obtained solids to hydrothermal post-synthesis treatment by conventional heating and microwave assisted heating were studied. The obtained solids were exhaustively characterized using several instrumental techniques, such as X-ray diffraction, Thermal Analysis (DTA and TG), Chemical Analysis, Infrared Spectroscopy (FT-IR), determination of Particle Size Distribution and BET-Surface area. Well crystallized solids were obtained showing two possible LDH phases, depending on the orientation of the interlayer anion with respect to the brucite-like layers. The results indicated that there is a certain influence of the amine, when used as a precipitating agent, and as a consequence of the degree of substitution, on the crystallinity and particle size of the final solid obtained. The LDHs obtained using TEA exhibited higher crystallinity, which was improved after a long hydrothermal treatment by conventional heating. Regarding the shape of the particles, the formation of aggregates in the former solid was detected, which could be easily disintegrated using ultrasound treatments, producing solid powder with high crystallinity and small particle size, with homogeneous size distribution.https://www.mdpi.com/2305-7084/6/4/53LDHshydrotalciteaminescoprecipitation methodhydrothermal treatmentcrystallinity
spellingShingle Alexander Misol
Alejandro Jiménez
Francisco M. Labajos
Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
ChemEngineering
LDHs
hydrotalcite
amines
coprecipitation method
hydrothermal treatment
crystallinity
title Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
title_full Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
title_fullStr Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
title_full_unstemmed Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
title_short Use of Ethylamine, Diethylamine and Triethylamine in the Synthesis of Zn,Al Layered Double Hydroxides
title_sort use of ethylamine diethylamine and triethylamine in the synthesis of zn al layered double hydroxides
topic LDHs
hydrotalcite
amines
coprecipitation method
hydrothermal treatment
crystallinity
url https://www.mdpi.com/2305-7084/6/4/53
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