Method of production of gold nanoparticles from raw material containing iron and non-ferrous metals

FIELD: nanotechnology.

SUBSTANCE: invention relates to the technology of production of gold nanoparticles. The method of production of gold nanoparticles from the raw material containing iron and non-ferrous metals comprises preparation of the chlorazotic acid solution of gold using chlorazotic acid. Then floatation extraction of gold precursors is carried out with cationic surfactants from the solution, separation and evaporation of the organic phase to concentrate the gold precursors. Then the concentrate reduction is carried out to obtain dispersion of gold nanoparticles. At that the starting material is first treated with hydrochloric acid to form the insoluble precipitate. Production of chlorazotic acid solution is carried out by dissolving in chlorazotic acid solution of insoluble precipitate. Before floatation extraction of precursors the nitric acid is removed from chlorazotic acid solution with methyl or ethyl alcohol or hydrochloric acid.

EFFECT: improvement of efficiency of the method of production of nanoparticles, namely the increase in the number of gold nanoparticles obtained or its hybrids with noble metals.

3 ex

 

The invention relates to a process for producing nanoparticles of gold or nanohybrids gold with other metals. The gold nanoparticles used in perfumery, cosmetic, chemical, jewelry industry; for the treatment and diagnosis of diseases, for analytical determination of various substances by the method of surface-enhanced Raman spectroscopy.

A method of obtaining gold nanoparticles of iron ore raw materials (patent RF №2424339). He was taken as a prototype. Iron ore platinuum, the concentrate is dissolved in Aqua Regia, the solution is subjected to ion protectable surfactants for concentration of precursors of gold, and then the precursors of gold to restore the extract of the tea leaves. The method has drawbacks. First, iron ore raw materials not processed holistically. Concentrate in addition to the noble metals is possible to obtain nanoparticles of oxides of iron and non-ferrous metals. Secondly, the Imperial vodka gold is extracted from raw materials not fully. Thirdly, the excess of nitric acid that remains after decomposition of the concentrate Imperial vodka, prevents ionic protectable gold, as well flatirons cationic surfactant only chloride complexes of gold.

An object of the invention is to increase the amount of nanoparticles AOR the PTA or its hybrids with noble metals.

The technical result is achieved in that in the method for producing nanoparticles of gold from raw materials containing iron and non-ferrous metals, including obtaining tsarskovodochnom solution of gold using Aqua Regia, protectrail from solution precursors gold cationic surfactant, separation and evaporation of the organic phase to the concentration of precursors and gold recovery concentrate to produce a dispersion of gold nanoparticles, according to the invention, the raw material is first treated with hydrochloric acid with the formation of insoluble sludge, receiving tsarskovodochnom solution is performed by dissolving in Aqua Regia insoluble precipitate and before flomaxtra precursors removed from tsarskovodochnom solution of nitric acid methyl or ethyl alcohol or hydrochloric acid.

If the powder iron ore processing hydrochloric acid, then pass into the solution ions of iron, silicon, Nickel, cobalt, manganese, copper, zinc, silicon. The remaining ore particles become finer and more porous. They are best dissolved in Aqua Regia. After dissolution in Aqua Regia nitric acid prevents the formation of salts chloride complex of gold and cationic surfactants. Nitric acid is removed by the reducing agents of lower alcohols or hydrochloric acid. With this method of processing the raw materials you receive the possibility of the ability of aqueous solutions of hydrochloric acid by known methods to obtain nanoparticles of iron oxide and silicon oxide, nanoparticles of non-ferrous metals. The invention is illustrated by examples.

Example 1

Powder iron ore, containing according to x-ray diffractometry Fe2O3+Fe3O413,5%, SiO286,5%, a weight of 300 g was treated with 580 ml of 6 M HCl. Boiled for 5 hours under stirring. The top brown layer of liquid hydrochloric acid salts of iron and other elements were merged. They gave magnetite particles and silicon oxide by known methods. Insoluble blue precipitate was treated by boiling in Aqua Regia for 5 hours. The resulting solution was treated twice by boiling with 6 M HCl for the decomposition of nitric acid. The remainder of the wet salt was dissolved in 1 M HCl with 10 ml of solution. In the flotation machine with 1000 ml of 0.5 M HCl was added to 10 ml of the resulting solution and 0,03345 g of pyridinium chloride (CPH), dissolved in 5 ml of ethanol, to 0.0001 M in the flotation cell. Added in the flotation machine 50 ml of an organic solvent and fluoroware 1 hour. After separation and evaporation of the organic phase has received a small amount of white powder, which was dissolved in 10 ml of water. The solution in the test tube was purged with nitrogen and was stirred by ultrasound. Received the solution pink color, to which was added 1.5 ml of 0.6 M solution of the reducing agent hydrazine hydrate is added and stirred for another 10 minutes. To the mixture was added 1 ml of 2 M KOH, peremeci the Ali 10 minutes. Got a hazy solution, which one day became brown. Brown color dispersion indicates that the size of gold nanoparticles is equal to about 20 nm. UV-visible spectrum of this dispersion had a streak of plasma absorption with a maximum at 530 nm.

After settling solution appeared brown precipitate resulting from the aggregation of the nanoparticles. The precipitate was separated by centrifugation, washed with ethyl alcohol and dried. Obtained 0.45 g of powder. The gold nanopowder used to remove photos on transmission electron microscope. The size of the nanoparticles according to the TEM data was 15±6 nm.

Example 2

Scrap gold plated legs of the transistors was dissolved in Aqua Regia. For removal of oxides of nitrogen, the resulting solution was treated with methyl alcohol and evaporated to moist salts, which then was dissolved in 1 M HCl. The resulting solution was 50 ml was combined with 1000 ml of 0.5 M HCl and loaded into the flotation cell. There was added to 1.34 g CP dissolved in 10 ml of ethanol. The solution immediately became turbid. Top in the flotation cell was added 50 ml of a mixture of chloroform, toluene and amyl alcohol in a ratio of 1:3:6 (by volume) and was fluoroware for 1 hour. The top layer of the gold precursor with a solvent separated. The solvents were evaporated. Received the remains of the precursor paste is dark brown. Pasta in the amount of 0.26 g was dissolved in 20 ml of dist is therouanne water under stirring with ultrasound for 10 minutes. Received a clear solution, which was dark after addition of 3 ml of 0.6 M solution of hydrazine hydrate is added. In a test tube was added 2 ml of 2 M KOH solution and stirred for another 10 minutes. Got dark brown dispersion of gold nanoparticles. Thus obtained several times the dispersion was diluted with ethyl alcohol 2 times and centrifuged. Precipitates were washed with ethanol and centrifuged. After evaporation of the alcohol the nanopowder gold investigated by TEM. The gold nanoparticles have a size of 5±3 nm.

Example 3

Powder iron ore weighing 300 g of composition, as in example 1, was dissolved Imperial vodka in a known manner. Received 0,23 g nanopowder with gold instead of 0.45 g according to the new method.

Thus, removing the pre-iron and silica from the ore and nitric acid Aqua Regia, get more gold nanoparticles.

Method for producing nanoparticles of gold from raw materials containing iron and non-ferrous metals, including obtaining tsarskovodochnom solution of gold using Aqua Regia, protectrail from a solution of precursors of gold cationic surfactant, separation and evaporation of the organic phase to the concentration of recursion gold and the recovery of the concentrate to produce a dispersion of gold nanoparticles, characterized in that the raw material is first treated with hydrochloric acid with the formation of insoluble sludge, the floor is giving tsarskovodochnom solution is performed by dissolving in Aqua Regia insoluble precipitate and before flomaxtra precursors removed from tsarskovodochnom solution of nitric acid methyl or ethyl alcohol or hydrochloric acid.



 

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