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<p>Synthesis and characterization of some binuclear alkylene dithiophosphate complexes of bis(acetylacetonato)aluminium(III)-di-(μ-isopropoxo)di-isopropoxoaluminium(III) and sol-gel synthesis of nanosized θ-alumina</p>

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Title Statement <p>Synthesis and characterization of some binuclear alkylene dithiophosphate complexes of bis(acetylacetonato)aluminium(III)-di-(μ-isopropoxo)di-isopropoxoaluminium(III) and sol-gel synthesis of nanosized θ-alumina</p>
 
Added Entry - Uncontrolled Name Sharma, Vinita ; BBD Govt. College, Chimanpur, Jaipur.
Sanwaria, Anita Raj; University of Rajasthan, Jaipur
Sharma, Nikita ; Directorate of college education
 
Uncontrolled Index Term Synthetic and structural inorganic chemistry; spectroscopy
Bis(acetylacetonato)aluminum(III))-di-(μ–isopropoxo)-di-isopropoxoaluminum(III), alkylenedithiophosphoric acid, sol-gel transformation, nano-sized θ -Al2O3 .  
 
Summary, etc. <p>Reactions of bis(acetylacetonato)aluminum(III)-di-(μ–isopropoxo)-di-isopropoxoaluminum(III)<strong> (A) </strong> with a variety of alkylenedithiophosphoric acids in different molar ratio yield products of the type  [(CH<sub>3</sub>COCHCOCH<sub>3</sub>)<sub>2</sub>Al(μ-OPr<sup>i</sup>)<sub>2</sub>Al{S(S)P(O-G-O)<sub>n</sub>(OPr<sup>i</sup>)<sub>2-n</sub>] (<strong>1-9</strong>) {where G = C(CH<sub>3</sub>)<sub>2</sub>C(CH<sub>3</sub>)<sub>2</sub>, n=1[<strong>1</strong>], n=2[<strong>2</strong>]; -CH<sub>2</sub>CH(C<sub>2</sub>H<sub>5</sub>), n=1[<strong>3</strong>], n=2[<strong>4</strong>]; CH<sub>2</sub>CH(CH<sub>3</sub>), n=1[<strong>5</strong>], n=2[<strong>6</strong>];C(CH<sub>3</sub>)<sub>2</sub>CH<sub>2</sub>CH(CH<sub>3</sub>), n=1[<strong>7</strong>]; CH(CH<sub>3</sub>)CH(CH<sub>3</sub>) n=1[<strong>8</strong>], n=2[<strong>9</strong>]}. Progress of the reactions was monitored by estimating liberated 2-propanol in benzene-2-propanol azeotrope by oxidimetric method. All pale coloured viscous products were soluble in common organic solvents and were characterized by elemental analyses, FT-IR and NMR (<sup>1</sup>H and <sup>13</sup>C{<sup>1</sup>H} NMR) spectral studies. Molecular weight measurements in refluxing anhydrous benzene indicated binuclear nature of the complexes. <sup>27</sup>Al NMR spectra of two of the derivatives, (<strong>1</strong>) and (<strong>2</strong>), suggested the presence of aluminium(III) atoms in different coordination states. <sup>31</sup>P NMR spectra of the representative derivatives (<strong>1</strong>) and (<strong>2</strong>) exhibited only a single peak at 95.71 and 90.59 ppm, respectively suggesting tetra-coordination around phosphorus atom and a bidentate mode of chelation of the dithio ligand. Sol-gel transformation of  Al(OPr<sup>i</sup>)<sub>3 </sub>and  [(CH<sub>3</sub>COCHCOCH<sub>3</sub>)<sub>2</sub>Al(μ-OPr<sup>i</sup>)<sub>2</sub>Al(OPr<sup>i</sup>)<sub>2</sub>] <strong>(A) </strong>followed by sintering at ~850<strong>°</strong>C yield alumina <strong>(a) </strong>and<strong> (b)</strong>, respectively. The powder X-ray diffraction patterns, SEM images and FT-IR spectral studies of <strong>(a) </strong>and<strong> (b)</strong> indicated formation of nano-crystallites of <em>θ</em> -Al<sub>2</sub>O<sub>3 </sub>[PDF # 110517] in both the cases. The energy band gaps of 4.78 eV and 5.01 eV for (a) and (b), respectively were obtained from the absorption spectra.</p> <p> </p>
 
Publication, Distribution, Etc. Indian Journal of Chemistry -Section A (IJCA)
2021-11-11 16:14:19
 
Electronic Location and Access application/pdf
http://op.niscair.res.in/index.php/IJCA/article/view/49384
 
Data Source Entry Indian Journal of Chemistry -Section A (IJCA); ##issue.vol## 60, ##issue.no## 10 (2021): INDIAN JOURNAL OF CHEMISTRY- SECTION A
 
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