Characterization of surface NH3+Cl- groups on poly(styrene-co-Boc-aminostyrene) microspheres obtained by controlled acidic treatment.
Different samples of aminated latex of poly(styrene-co-Boc-aminostyrene) microspheres with mean diameters varying from 0.7 to 1.0 microm were prepared by dispersion copolymerization of styrene (ST) and Boc-aminostyrene (Boc-AMST). The copolymer compositions determined by nuclear magnetic resonance (1H NMR) were Boc-AMST/ST 6.9/93.1 mol/mol % (BOC7 sample) and Boc-AMST/ST 31.3/68.7 mol/mol % (BOC30 sample). The average molecular weights determined by gel permeation chromatography were 126 kDa (BOC7 sample) and 51 kDa (BOC30 sample). The latex containing NH-carbo-tert-butoxy groups (NH-Boc) were treated with 2 M HCl in isopropyl alcohol/water (1:1 vol/vol), at 50 degrees C for 3, 6, 9, 24, and 30 h, in order to control the extent of deprotection reaction of the NH-Boc. The deprotection reaction resulted in the formation of NH3+Cl- groups on the particle surfaces. The kinetic of the deprotection reaction was investigated by 1H NMR analyses and the yield varied from 20 to 40%. The resulting -NH3+Cl- groups on the microsphere surfaces were examined, in particular, by electron spectroscopy imaging (ESI) using an energy-filtered transmission electron microscope (EFTEM) that clearly demonstrated the presence of Cl on the particle surfaces. Scanning electron photomicrographs recorded for the above samples showed that the particle morphology was maintained after the acidic treatment.
Polystyrene particles with surface amino groups
ABSTRACT Poly[(vinyl alcohol)-co-(vinyl amine)] was prepared by copolymerization of vinyl acetate and N-vinyl forma-mide, followed by a two-step alkaline hydrolysis in which the vinyl acetate groups were hydrolyzed to vinyl alcohol groups, and the N-vinyl formamide groups, to amino groups. This copolymer was used as the stabilizer for the emulsion polymerization of styrene using persul-fate-ion initiator. The latexes were cationic; the particles were relatively uniform and of 100–500 nm diameter. The presence of amino groups was shown by electro-phoresis and Kjeldahl analysis. Comparison with sodium lauryl sulfate showed that the mechanism of particle nucleation was apparently entry of radicals into fine emulsion droplets rather than the conventional entry of radicals into emulsifier micelles.
Effects of the mineral phase and valence of vanadium on vanadium extraction from stone coal
The influence of roasting on the leaching rate and valence of vanadium was evaluated during vanadium extraction from stone coal. Vanadium in stone coal is hard to be leached and the leaching rate is less than 10% when the raw ore is leached by 4 mol/L H2SO4 at 90°C for 2 h. After the sample is roasted at 900°C for 2 h, the leaching rate of vanadium reaches the maximum, and more than 70% of vanadium can be leached. The crystal of vanadium-bearing mica minerals decomposes and the content of V(V) increases with the rise of roasting temperature from 600 to 900°C, therefore the leaching rate of vanadium increases significantly with the decomposition of the mica minerals. Some new phases, anorthite for example, form when the roasting temperature reaches 1000°C. A part of vanadium may be enwrapped in the sintered materials and newly formed phases, which may impede the oxidation of low valent vanadium and make the leaching rate of vanadium drop dramatically. The leaching rate of vanadium is not only determined by the valence state of vanadium but also controlled by the decomposition of vanadium-bearing minerals and the existence state of vanadium to a large extent.