Kasim Mohammed Hello

The immobilization of 3-(chloropropyl)triethoxysilane onto silica by a simple one-pot synthesis

Sodium silicate from rice husk ash (RHA) was transformed to functionalized silica with 3-(chloropropyl)triethoxysilane (CPTES) via a simple sol-gel technique in a one-pot synthesis. The (29)Si MAS NMR of the organo-silica complex (RHACCl) showed the presence of T(2), T(3), Q(3) and Q(4) silicon centers. The (13)C MAS NMR showed that RHACCl had three chemical shifts at 10.37, 26.70 and 47.69 ppm consistent with the three carbon atoms of the CPTES moiety. The presence of carbon, silicon and chlorine was determined by a combination of elemental analysis and EDX study.

One-step synthesis of solid sulfonic acid catalyst and its application in the acetalization of glycerol: crystal structure of cis-5-hydroxy-2-phenyl-1,3-dioxane trimer

A one-pot method was employed to immobilize sulfonic acid onto silica obtained from rice husk ash using 3-(mercaptopropyl)trimethoxysilane to form a solid catalyst denoted as RHASO3H. BET measurements of the catalyst showed the surface area to be 340 m2 g−1 with the average pore volume of 0.24 mL g−1 and the pore diameter of 2.9 nm. Acidity test of cation exchange capacity and pyridine adsorption studies revealed the presence of Brønsted acid sites on the catalyst surface. The catalyst was used in the acetalization reaction of glycerol with benzaldehyde. Under optimized conditions, the reaction showed the maximum conversion of 78 % after 8 h with 67 % selectivity towards the five membered ring isomer. Variation in the glycerol concentration had a significant effect on the reactants conversion. A single crystal X-ray study of one of the products proved the existence of a unique trimer formed by hydrogen bonding by the six-membered cis-isomer. The catalyst was several times recycled without any loss of its catalytic activity.

Melaminium nitrate–melamine–water (1/1/1)

In the crystal structure of the title salt, C3H7N6 +·NO3 −·C3H6N6·H2O, the asymmetric unit consists of two neutral melamine (1,3,5-triazine-2,4,6-triamine) molecules, two melaminium cations, two nitrate anions and two solvent water molecules. One of the nitrate anions is disordered over two sets of positions, with a refined occupancy ratio of 0.909 (3):0.091 (3). The cations and neutral molecules are approximately planar, with maximum deviations of 0.018 (2), 0.024 (2), 0.019 (2) and 0.007 (2) Å for each, respectively. In the crystal structure, melaminium cations and netural melamine molecules self-assemble via N—H⋯N hydrogen bonds to form a supramolecular hexagonal-shaped motif. In addition, the nitrate anions and water molecules are connected by N—H⋯O hydrogen bonds to form a three-dimensional network.

Modification of Silica Rice Husk Ash to Solid Ammonium Sulphate for Second Generation Biofuels Productions

A new approach has been demonstrated for the synthesis of solid ammonium sulphate attached to silica rice husk ash. The 3-(aminopropyl)triethoxysilane was immobilized onto silica at room temperature to functionalize the silica with ammine end groups (–NH2). The amine group was sulphated with sulphuric acid to produce a novel micro-rod-like shaped acidic catalyst (as seen with TEM) designated RHNH3SO4H (RH = rice husk). The TGA analysis shows that the catalyst is stable at temperatures below 200°C. The acidity measurement of the catalyst indicates that it has Bronsted acid sites. Cellulose extracted from waste of rice husk and cellulose extracted from office paper were hydrolysed to glucose in 6 h, and the glucose was hydrolysed afterwards to other products within 13 h. The catalyst is reusable many times without a significant loss of catalytic activity.

Melaminium nitrate–melamine–water (1/1/1). Corrigendum

Corrigendum to Acta Cryst. (2010), E66, o3033–o3034.