O. V. Koryakova

Synthesis in a gel and sorption properties of N-2-sulfoethyl chitosan

A new procedure was developed for preparation of chelate amino-containing polymer N-2-sulfoethyl chitosan by synthesis in a gel through the reaction between chitosan and sodium 2-bromoethanesulfonate, yielding a polymer with the degree of substitution of up to 0.5. The structure of the resulting polymers was confirmed by 1H NMR spectroscopy. The sorption characteristics with respect to transition and alkaline-earth metal ions were determined for the cross-linked polymers.

Gel-synthesis, structure, and properties of sulfur-containing chitosan derivatives

The possibility of using the thermochemical approach to thermal decomposition of solids, previously developed by the author, to interpretation of the mechanism and kinetics of reduction of metal oxides with hydrogen was studied. Many properties of NiO reduction with hydrogen, including formation of metal nuclea, the nature of induction period, autocatalysis effect, equimolar and isobaric periods of reduction, the character of the effect of hydrogen pressure on reduction rate, and the nanocrystalline structure of a reduced metal, were explained in terms of the given approach.

Sorbents based on modified polysiloxanes

Organic-inorganic hybrid sorbents based on a polysiloxane modified with amino and thiourea groups have been synthesized for the first time by a sol-gel process. The structure of the sorbents has been determined by X-ray photoelectron spectroscopy and IR spectroscopy. Their thermal stability has been assessed and the mechanism of their degradation has been elucidated. The structural and adsorption parameters of the sorbents have been evaluated. The results demonstrate that the introduction of amino groups into the structure of the polysiloxane yields an effective sorbent for Pb(II) extraction and enables Cu(II) and Zn(II) separation from Co(II) and Ni(II). The thiourea-modified polysiloxane selectively sorbs Bi(III) (0.1–2 M HCl), Pt(IV) (pH 2), and Pb(II) (pH > 3). Divalent Co, Ni, Cu, and Zn can be sorbed from alkaline solutions.

Chemical properties of N-2-Sulfoethylchitosan with a medium degree of substitution

A method was developed for the preparation of N-2-sulfoethylchitosan (SECH) via synthesis in a gel with the use of the reaction of chitosan and sodium 2-bromoethanesulfonate. This method makes it possible to conduct a polymer-like transformation without any acid or base. The structures of the obtained polymers were confirmed via IR and 1H NMR spectroscopy. The study of the sorption of Ag+, Cu2+, Zn2+, Ni2+, Co2+, Cd2+, Pb2+, Mn2+, Mg2+, Ca2+, Sr2+, and Ba2+ ions that were crosslinked by SECH during their joint presence in an ammonia-acetate buffer solution showed high values of selectivity in relation to those of silver(I) and copper(II). The selectivity of the sorption of silver(I) ions with respect to copper(II) ions increased with an increase in the degree of substitution of SECH.

Synthesis of TiO2-SiO2 xerogels via the hydrolysis of a tetrabutoxytitanium-tetraethoxysilane mixture in aqueous ammonia and hydrochloric acid atmospheres

TiO2-SiO2 xerogels have been synthesized by the hydrolysis of tetrabutoxytitanium-tetraethoxysilane mixtures in a 10% aqueous ammonia vapor and concentrated hydrochloric acid vapor atmospheres under static conditions. The dependence of the physical and chemical properties of the xerogels on the synthetic conditions has been investigated.

TiO2-SiO2 binary xerogels: Synthesis and characterization

Silica/titania binary xerogels were prepared by joint hydrolysis of the ingredients. Gels of various compositions were characterized by 1H NMR spectroscopy, IR spectroscopy, and thermogravimetry. The spectral characteristics of binary systems differ considerably from mere superposition of the spectra of the two constituent compounds and the spectrum of a mechanical mixture. A feasibility was demonstrated for controlling the acid properties of binary oxide gels via varying the component mole ratio.

Glycolate Ti1 − xFex(OCH2CH2O)2 − x/2 as a precursor for the preparation of quasi-one-dimensional (1D) solid solutions Ti1 − xFexO2 − 2x/2 (0 ≤ x ≤ 0.1)

Quasi-one-dimensional (1D) solid solutions Ti1 − xFex(OCH2CH2O)2 − x/2 (0 < x ≤ 0.1) with the structure of anatase were prepared by heating the glycolate Ti1 − xFex(OCH2CH2O)2 − x/2 in an atmosphere of air at a temperature of >450°C. The conditions of formation and the properties of the new glycolate Ti3Fe2(OCH2CH2O)9 were described. It was found that the synthesized Ti1 − xFexO2 − 2x/2 solid solutions exhibit photocatalytic activity in the reaction of hydroquinone oxidation in an aqueous solution on irradiation with UV light. A correlation between the rate of oxidation of hydroquinone and the concentration of iron in the catalyst was established. A procedure for the preparation of titanium dioxide with the structure of anatase doped with iron and carbon (Ti1 − xFexO(2 − x/2) − yCy) and also composites on its basis, which contain an excess amount of carbon, was proposed.

Preparation of MnCo2O4 whiskers and spheroids through thermal decomposition of Mn1/3Co2/3C2O4 · 2H2O

The mixed oxalate Mn1/3Co2/3C2O4 · 2H2O has been prepared in the form of whiskers 2–5 μm in diameter and up to 50 μm in length and spheroidal nanofiber arrays 20 μm in diameter using two different coprecipitation procedures. Thermal decomposition of this oxalate in air has led to the formation of MnCo2O4 particles very similar in morphology to their oxalate precursor. The materials have been characterized by chemical analysis, thermogravimetry, x-ray diffraction. IR spectroscopy, and scanning electron microscopy.

Synthesis of poly[N-(2,3-dihydroxypropyl)aminostyrene], a new sorbent for boron(III) ions

A procedure was developed for preparation of poly[N-(2,3-dihydroxypropyl)aminostyrene] via successive stages of nitration, reduction, and glycidol treatment of polystyrene, which gives the polymer with a maximal degree of functionalization. The composition and structure of the intermediates and end products of the polymer-analogous reactions were characterized by elemental analysis, IR spectroscopy, and solid-state 13C NMR spectroscopy. The sorption characteristics of poly[N-(2,3-dihydroxypropyl)aminostyrene] toward boroncontaining ions were assessed.

Synthesis of dispersed silicon, titanium, and zirconium dioxides by pyrolysis of cellulose inorganic composites

The method of the synthesis of dispersed powders of silicon, titanium, and zirconium dioxides was developed, including formation of cellulose inorganic composites by impregnation of pressed granules of powdered cellulose with solutions of tetraethoxysilane and tetrabutoxy zirconium, hydrolysis of the organometallic constituent of the composite, pyrolysis of the cellulose matrix of the composite, and burning of its carbon constituent.