NDLI: Thermal intercalation of layered double hydroxides: capric acid into an Mg

Content Provider	Royal Society of Chemistry (RSC)
Author	Carlino, Simon Hudson, Michael J.
Copyright Year	1995
Abstract	Molten decanoic acid, capric acid, reacted with the layered double hydroxide (LDH) of initial composition Mg6Al3.4(OH)18.82(CO3)1.51(NO3)0.36·4.5 H2O, at a temperature of 150 °C using a heating rate of 1 °C min–1. Powder X-ray diffraction (PXRD) showed that the reaction products were microcrystalline. The polyphasic nature of the reaction products was thought to derive from the presence, in all cases, of some residual unreacted LDH host plus mono- and bi-layers of caprate anion guests in the LDH. Typically, dominant phases were non-intercalated LDH (at initial capric acid:LDH ratios of up to 2:1); stacks of horizontal caprate anions (4:1); full, intercalated monolayers (6:1) and full bilayers (8:1). 27Al Solid-state magic-angle spinning nuclear magnetic resonance (MAS NMR) studies indicated that the exclusively octahedral nature of the aluminium sites of the host LDH were not altered by thermal reaction with capric acid. Two-dimensional (2D)27Al MAS NMR suggested that the thermal reaction products contained two octahedral aluminium environments. 13C MAS NMR confirmed the presence of the monoanion of capric acid, CH3(CH2)8COO–. The suggested mechanism for intercalation involves the removal of the LDH interlayer carbonate in a similar manner to that observed in the corresponding LDH-sebacic acid thermal reactions. The products of the thermal reaction were compared with material prepared via a modified coprecipitation reaction. PXRD suggested that the products of this coprecipitation reaction and the 8:1 thermal reaction product contained bilayers having similar calculated slant angles. 2D 27Al MAS NMR suggested that the coprecipitated reaction differed from the thermal reaction products in that it contained a tetrahedral aluminium site in addition to the two octahedral sites also exhibited by the thermal reactions. There was no direct evidence of kinking of the acid or anion carbon chains in the thermal or coprecipitation reaction products owing to possible interaction with the alcohol during washing of the products.
Starting Page	1433
Ending Page	1442
Page Count	10
File Format	PDF
ISSN	09599428
Volume Number	5
Issue Number	9
Journal	Journal of Materials Chemistry
DOI	10.1039/JM9950501433
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	LDH PXRD Acid Layered double hydroxides Lactate dehydrogenase Properties of water X-ray crystallography Ion Nuclear magnetic resonance Magic angle spinning Aluminium Coprecipitation Carbon
Content Type	Text
Resource Type	Article
Subject	Chemistry Materials Chemistry

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