X-ray and laser diffraction methods were used to determine basic physical and chemical properties of conversion calcium carbonate. It was found that for obtaining standard product for use as a filler, it is necessary to regrind it. The results of dispersion changes in conversion chalk (chalk stone) were expressed in terms of median (D50), maximum (D98) and minimum (D10) particle size. It was established that during the grinding process a transition occurs from the initial odiomodal distribution to the bimodal distribution, which is characterized by a sufficiently wide range of the sizes of the particles of the crushed material. The optimum parameters of grinding were determined. With the help of SEM method, used before and after grinding of conversion calcium carbonate, it was established that the particles of primary material are represented by polycrystalline dense aggregates of spherical shape, due to mass crystallization of calcium carbonate at the condition of high supersaturation according to polynuclear growth mechanism. The component composition of water-soluble impurities was quantitatively estimated on the basis of the determination of the content of nitrate N-NO3- and ammonium N-NH4+ forms of nitrogen in various forms of presence-total, bound, water-soluble, and additional determination of the Ca2+ content of calcium ions in aqueous extract. It has been experimentally established that preliminary heat treatment of conversion calcium carbonate allows to significantly reduce the total content of water-soluble substances in the ground product by more than 5 times: at a temperature of 400 ° C, the degree of removal by NH4+ and NO3- ions is ~ 40-50%, and at 500 ° C - ~ 60% for NO3- and ~ 90% for NH4+. The estimation of the possibility of using the obtained product as a filler of polymer composite materials was done comparing the main parameters (CIELab (W and L) color characteristics, bulk density, dispersed composition, specific surface, pH of aqueous extract) with known finely ground natural chalk and microcalcite. Forcitation:Rudakova L.V., Niftaliev S.I., Natarova E.S. Conversion calcium carbonate as filler of thermoplastics. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2017. V. 60. N 4. P. 100-107.
The introduction of fillers into various materials improves its technological, physical and mechanical properties, and leads to a decrease in cost. The main areas of application of natural and synthetic calcium carbonate as highly dispersed fillers are: the construction industry, the production of Portland cement, mineral fertilizers, glass, paper, polymer composite materials, paints and varnishes, and rubbers. A promising direction at present is the use of production by-products as fillers, for example, conversion calcium carbonate - a waste product from the production of a complex mineral fertilizer - nitroammophoska. However, its use in the above areas is limited by the content of water-soluble nitrogen-containing impurities, impurities of heavy metals, strontium carbonate, phosphates, etc. The analysis of scientific, technical and patent literature on methods of purification of conversion calcium carbonate has been carried out. These methods are based on the extraction of impurities from the initial product of calcium carbonate production - a melt of calcium nitrate tetrahydrate by precipitation with various reagents, followed by the isolation of an insoluble precipitate (impurities) and processing of the purified melt into calcium carbonate and nitroammofoska. A method is proposed for the extraction of acid-tonic-soluble iron-containing impurities from the initial calcium nitrate melt in order to obtain a cleaner by-product - conversion calcium carbonate, which will expand the scope of its application. An effective method is to dilute the initial calcium nitrate melt with a 60% solution of ammonium nitrate to a calcium content of 12-13%, followed by the isolation of an acid-insoluble precipitate in a vacuum filter, conversion of the purified calcium nitrate solution with ammonium carbonate and separation of the resulting suspension in a drum filter. The described method can reduce the amount of iron-containing impurities by more than 50%.
Studies have been carried out to improve the quality of conversion calcium carbonate. The process of extraction of insoluble iron-containing impurities at the stage of obtaining calcium carbonate from calcium nitrate melt was studied. It has been determined that the preliminary removal of the acid-insoluble residue from the melt of Ca (NO3)2by filtration or settling allows the Fe2O3content to be reduced by more than 50 % in the form of magnetically susceptible impurities and further increases the whiteness of the final product. The effect of grinding and heat treatment of conversion calcium carbonate on the evolution of nitrogen-containing impurities is studied. It has been established that the amount of water-soluble substances in the sample increases exponentially with increasing shredding time of the material. Heat treatment can significantly reduce (in almost 3 times) the total content of water-soluble substances in the crushed product. Simultaneously with the removal of the "bound" nitrogen, the content of the main component increases by 1.5–2 %. A positive effect of heat treatment is also an increase in the rate of refinement of conversion calcium carbonate, which makes the dispersed composition of the product more homogeneous. A technological scheme for processing conversion calcium carbonate into a disperse filler with specified properties has been developed.
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