The
liquid-assisted grinding cocrystallization of theophylline
with benzamide leading to polymorphic compounds was investigated.
A solvent screening with 17 different solvents was performed. The
dipole moment of the solvent used in the synthesis determines the
structure of the polymorphic product. A detailed investigation leads
to the determination of the kinetically and thermodynamically favored
product. In situ observations of the formation pathway during the
grinding process of both polymorphs show that the thermodynamically
favored cocrystal is formed in a two-step mechanism with the kinetic
cocrystal as an intermediate.
One-part geopolymers were synthesized from two different silica materials (a silica-rich residue from chlorosilane production and a commercial microsilica) and sodium aluminate at three different SiO 2 /Al 2 O 3 ratios and a nominal water/solids ratio of 0.5. The degree of reaction of the silica in the cured geopolymers (i.e. the fraction of silica dissolved to form aluminosilicates and minor products) was determined using two different methods: chemical attack with HCl to dissolve the reaction products and evaluation of peak areas of 29 Si MAS NMR spectra. It was found that the degree of reaction of the silica decreases with increasing the silica content of the starting mix, and that it is almost constant after 1 day of curing and almost independent from the kind of starting silica. From the results of the NMR-based method, the mean SiO 2 /Al 2 O 3 ratio of the reaction products (aluminosilicates and minor products) can be estimated to be ca. 2.0, nearly independent of the starting composition of the geopolymers. The dissolution method is biased, but of sufficient precision to be useful for following changes of the degree of reaction. Major crystalline phases in the cured geopolymers are zeolite A and/or hydrosodalite. Depending on the starting composition, the relative amounts of these zeolites vary; additionally, sodalite (only for the residue from chlorosilane production with [1 wt% Cl -), faujasite, and zeolite EMT can appear in the geopolymers. The 29 Si and 27 Al MAS NMR results indicate mainly Si(4Al) and Al(4Si) sites, in line with the presence of zeolite A, hydrosodalite, sodalite, and geopolymeric gel of comparatively low SiO 2 /Al 2 O 3 ratio.
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